Water Quality Sampling Procedures BY Carol Sweetnam
Water Quality Sampling Procedures BY Carol Sweetnam
Water Quality Sampling Procedures BY Carol Sweetnam
BY
CAROL SWEETNAM
This project is subm itted in part fulfilm ent o f the N C E A requirem ents for
June, 2004
Sampling is the first operational stage in any water quality monitoring programme. No matter
how good the analytical method is or how carefully the analysis is performed if the sampling is
not carried out correctly then subsequent analytical results will not be representative of the water
body sampled.
Detailed water sampling requirements are specified in ISO 5667. A questionnaire found that no
laboratory, which responded, is currently accredited or in the process of attaining accreditation to
this standard. In general, the procedures and practices in environmental laboratories questioned
fall significantly short of the requirements of ISO 5667, particularly in relation to the
preservation of samples, the documentation of sampling training procedures and the maintenance
of training records.
Information received from the questionnaire indicated similar trends between Limerick County
Council and other Local Authority (LA) laboratories. For example, LA laboratories generally do
not preserve samples, very few analyse quality control field blanks or have considered obtaining
accreditation specifically to ISO 5667. The trends in EPA laboratories are somewhat different
from those in LA laboratories in that all of the laboratories use chain-of custody forms and most
analyse quality control field blanks and preserve samples. The majority of EPA laboratories have
considered obtaining accreditation specifically to ISO 5667, although none are in the process of
doing so.
Current water sampling procedures and practices employed at the environmental laboratory of
Limerick County Council were used, as a case study, to determine the level of work required to
achieve ISO 5667 accreditation. This study revealed that approximately 80% of the
requirements of ISO 5667 could be implemented using existing facilities provided adequate
resources are allocated e.g. the documentation and implementation of comprehensive sampling
programmes and sampling procedures and the maintenance of detailed records. The
implementation of the remainder of the requirements would however, require specific expertise,
unlikely to be available within most laboratories For example, ISO requires that sampling
locations should be assessed for stratification and degree of turbulence. This information could
not be readily obtained using existing resources and therefore external consultants would have to
be employed requiring a significant financial backing.
AC KN O W LED G EM EN TS
I wish to express my gratitude to the many people who helped me in the completion of this
thesis.
I would like to express my sincere gratitude to my project supervisor, Dr. Ann-Marie Duddy
whose suggestions and ideas in relation to the content of this thesis were invaluable.
Thanks also to all those people who took time to complete the questionnaire and to my work
colleagues who gave me guidance along the way.
A special thanks to my best friend and fiancé Aidan who gave me great support and
encouragement throughout the project. Thanks also to my family and friends for their
encouragement and support.
C O N TEN TS
Page No.
A BSTR A C T i
A C K N O W LE D G E M EN TS ii
C O N TENTS iii
INTR O D U CTIO N 1
iii
M ATERIALS AND METHODS 23
Questionnaire 23
2.1.1 Introduction 23
2.1.2 Questionnaire circulation 23
Gap Analysis 27
2.2.1 Introduction 27
2.2.2 Gap analysis 27
SECTION 4. DISCUSSION 90
4.1 Results Obtained from the Q uestionnaire 90
4.1.1 Laboratories involvement in water sampling 90
4.1.2 Sampling procedures 91
4.1.3 Guides used in preparing sampling programmes 92
and procedures
4.1.4 Training of sampling personnel 93
4.1.5 On-site analysis of water pollutants 93
4.1.6 Calibration and checking of in-si tu monitoring equipment 94
4.1.7 Sampling containers used for sampling 94
4.1.8 Sample preservation 95
4.1.9 Quality control 96
4.1.10 Labelling of sampling containers 96
4.1.11 Transportation of samples 96
4.1.12 Use of chain of custody forms 97
4.1.13 Samples used as evidence in court cases 97
4.1.14 Accreditation of laboratories 98
4.1.15 LCC v’s other Environmental Laboratories 98
4.2 Results Obtained from the G ap Analysis 99
4.2.1 Sampling programme 100
4.2.2 Quality control 102
4.2.3 Preservation 103
4.2.4 Sampling procedures 105
REFERENCES 119
v
P age N o.
A PPEN D IX A:
The court report by Mr. Michael Finbarr Collins, barrister-at-law; County Council
of the County of Limerick (Complainant) v’s A .IB P (Accused) Rathkeale District
Court - 14thJuly 1997
A PPEN D IX B
Limerick Co. Co. SOP No. 6 - Routine drinking water sampling. B -l
Limerick Co. Co. SOP No. 8 - Routine river sampling B-2
Limerick Co. Co. SOP No. 10 -Sewage treatment plant sampling B-3
Limerick Co. Co. SOP No. 11 - Industrial effluent sampling B-5
Limerick Co. Co. SOP No. 43 - Procedure for handling of test samples B-6
Limerick Co. Co. SOP No. 47 -Sampling of Surface Waters B-7
A PPEN D IX C:
Table C -l: Summary of the Local Authority Laboratories replies to the questionnaire C -l
Table C-2: Summary of the EPA Laboratories replies to the questionnaire C-5
Table C-3: Summary of the Independent Laboratories replies to the questionnaire C-8
A PPEN D IX D
Document 1: Gap analysis results for I.S. EN 25667-1:1994 Water Quality Sampling D -l
Part 1: Guidance on the design o f sampling programmes
Document 2: Summary of the corrective actions required in order to comply with D-22
1.5. E N 25667-1:1994
Document 3: Gap analysis results for l.S. EN 25667-2:1994 Water quality - Sampling D-25
Part 2: Guidance on sampling techniques.
Document 4: Summary of the corrective actions required in order to comply with D-35
1.5. E N 25667-2:1994
Document 5: Gap analysis results for ISO 5667-3:1994 Water quality Sampling D-37
Part3 : Guidance on the preservation and handling o f samples.
Document 6: Summary of the corrective actions required in order to comply with D-50
ISO 5667-3:1994
Document 7: Gap analysis results for ISO 5667-5:1991 Water quality Sampling D-52
Part 5: Guidance on sampling o f drinking water and water used fo r
fo o d and beverage processing.
vi
Page No.
Document 8: Summary of the corrective actions required in order to comply with D-66
ISO 5667-5:1991
Document 9: Gap analysis results for ISO 5667-6:1990 Water- Sampling-Part 6: D-69
Guidance on sampling o f rivers and streams
Document 10: Summary of the corrective actions required in order to comply with D-83
ISO 5667-6:1990
Document 11 : Gap analysis results for ISO 5667-10:1992 Water - Sampling- Part 10: D-85
Guidance on sampling o f waste waters.
Document 12: Summary of the corrective actions required in order to comply with D-101
ISO 5667-10:1992
Document 13: Gap analysis results for ISO 5667-14:1998 Water- Sampling-Part 14: D-104
Guidance on quality assurance o f environmental water sampling and
handling.
Document 14: Summary of the corrective actions required in order to comply with D-109
ISO 5667-14:1998
Document 15: Sampling programme corrective actions D-110
Document 16: Quality control corrective actions D -112
Document 17: Preservation corrective actions D-113
Document 18: Drinking water corrective actions D-114
Document 19: River water corrective actions D-116
Document 20: Wastewater corrective actions D-118
LIST OF FIGURES
Figure 2.1 Questionnaire forwarded to the laboratories 24
Figure 3.1 Percentage of LA and EPA laboratories which (a) carry out their own 32
water sampling and (b) have personnel designated solely for sampling.
Figure 3.2 Percentage of LA and EPA laboratories which routinely sample rivers, 32
industrial effluents, sewage treatment plants and drinking waters.
vii
Page No.
Figure 3.3 Percentage of LA and EPA laboratories that document (a) sampling 33
procedures (b) the type of sampling container to be used (c) the sample
types that are to be preserved and (d) procedures for labelling samples
Figure 3.4 Percentage of LA and EPA laboratories, which use (a) ISO 5667 34
(b) Local Authority Implementation Handbooks and (c) A.P H. A
‘Standard Methods’ when preparing sampling programmes and procedures.
Figure 3.5 Percentage of LA and EPA laboratories which (a) have documented 35
procedures with regard to training sampling personnel and (b) maintain
sampling training records
Figure 3.6 Percentage of LA and EPA laboratories that (a) check or calibrate field 36
meters prior to sampling and (b) record this calibration/check
Figure 3.7 Percentage of LA and EPA laboratories that use the correct sampling 36
containers for fluoride (glass), FOGs (glass), phosphates (glass),
metals (glass/plastic) and microbiological samples (sterile glass/plastic).
Figure 3.9 Percentage of LA and EPA laboratories which (a) analyse field blanks 38
with each sample run and (b) carry out quality control tests on preservative
used.
Figure 3.10 Percentage of LA and EPA laboratories that use chain-of-custody forms 40
for samples taken (a) by laboratory personnel (b) by non-laboratory
personnel and (c) for prosecution cases.
viii
P a g e N o.
Figure 3.11 Percentage of LA and EPA laboratories that (a) use samples taken 41
as evidence in court, as required and (b) have had their sampling
procedures questioned in court.
LIST OF TABLES
Table 3.1 Comparison of the percentage ‘yes’ responses received from LA 30
and EPA laboratories when questioned in relation to various aspects
of sampling and sampling procedures. The Table also shows the
responses from Limerick County Council (LCC) Laboratory.
ix
Page No.
T a b le 3 .6 : An assessment of the ability of Limerick County Council’s 67
Environmental Laboratory to implement the proposed corrective actions
in relation to river water sampling.
X
IN T R O D U C T IO N
Local Authorities and the Environmental Protection Agency (EPA) are primarily responsible for
monitoring and assessing water quality in Ireland. This is primarily done to assess compliance
with specific regulatory requirements.
The importance of the sampling stage cannot be over emphasised. If the sample taken is not
representative, it will not be possible to relate the analytical result obtained to that in the original
water body, no matter how good the analytical method is or how carefully the analysis is
performed.
This study concentrates specifically on the sampling stage of a water quality monitoring
programme and aims to:
I
1.0 L IT E R A T U R E R E V IE W
Local Authorities are required to monitor the quality of surface water under a number of pieces
of legislation including the Local Government (Water Pollution) Act, 1977, Local Government
(Water Pollution) Act 1977 (Water Quality Standards for Phosphorus) Regulations 1998,
European Communities (Quality of Salmonid Waters) Regulations 1988, European
Communities (Quality of Surface Water Intended for the Abstraction of Drinking Water)
Regulations 1989, European Communities (Drinking Water) Regulations 2000,
The EPA are responsible for monitoring surface water quality under the EPA Act 1992 and
Protection of the Environment Act 2003. This legislation also obliges them to publish reports
on the quality of Irish waterways. A number of these reports have been published to date (EPA,
2004; McGarrigle, Bowman, Clabby, Lucey, Cunningham, MacCarthaigh, Keegan, Cantrell,
Lehane, Clenaghan, and Toner, 2002; Stapleton, Lehane and Toner, 2000; Lehane, Le Bolloch,
and Crawley, 2002).
Wastewaters discharged from various sources, for example sewage treatment plants or industrial
facilities, may impair water quality. Local Authorities and the EPA are responsible for
monitoring, assessing and controlling these discharges and their subsequent impact on the
receiving water. This is required under the Local Government (Water Pollution) Act, 1977, EPA
Act, 1992 and EPA Act, 1992 Urban Waste Water (Treatment) Regulations, 1994.
Yet another responsibility of the local authorities is the provision of a safe and wholesome
supply of drinking water. The European Communities (Drinking Water) Regulations, 2000
requires that water ‘be free from any micro-organisms and parasites and from any substances
which, in numbers or concentrations constitute a potential danger to public health.’
2
In order for water quality to be determined, a monitoring programme must be implemented.
The main elements of a monitoring programme include:
a) Identification of specific objectives of the programme.
b) Sampling.
c) Sample analysis and interpretation.
This study concentrates specifically on parts a and b above. The other elements are discussed in
detail by other workers (Crosby et al., 1999; Anon., 1998 and Butler, Carty, Kelly and
Lehane,1995).
The specific objectives of a monitoring programme will be determined by the nature of work
being carried out e.g. these objectives may be the establishment of baseline monitoring results or
assessing compliance with specific legislative requirements or specific licence conditions.
Sampling is the first operational stage in any water monitoring programme. Sampling is defined
as “the process of selecting a portion of material, in some manner, to represent or provide
information about a larger body of material.” (Crosby et al., 1999). The importance of the
sampling stage in a water quality monitoring programme cannot be over emphasised. If the
sample taken is not representative, it will not be possible to relate the analytical result obtained to
that in the original water body, no matter how good the analytical method is or how carefully the
analysis is performed.
In order for sampling to be carried out correctly, sampling procedures are necessary. A sampling
procedure is a set of instructions that must be followed when sampling. They are designed to
give credibility to data by ensuring that the same procedures are followed each time sampling is
performed. Procedures for sampling are generally less well documented than for analytical
procedures. This is due to the difficultly in specifying universal sampling procedures which are
applicable to each set of conditions at each sampling location The use of various sampling
procedures has been investigated by many workers (Anon., 1998; ISO, 1998; ISO, 1992; ISO,
1991; ISO, 1990; ISO, 1987; NSAI, 1994; NSAI, 1996) and a number of sampling guidelines do
exist. These include ISO 5667, Standard Methods for the Examination of Water and Wastewater
(Anon, 1998) and ISO 17025. In addition, sampling guidelines are provided in various pieces of
environmental legislation and associated implementation handbooks.
3
This Section attempts to review the various sampling guidelines in relation to sampling
procedures. Before doing so, an overview of these guidelines is provided.
ISO 5667 is comprised of a number of parts under the general title - Water quality - Sampling.
These parts are;
Part I : Guidance on the design of sampling programmes
Part 2: Guidance on sampling techniques.
Part 3: Guidance on the preservation and handling of samples.
Part 4: Guidance on sampling from lakes, natural and man-made.
Part 5: Guidance on sampling of drinking water and water used from food and beverage
processing.
Part 6: Guidance on sampling of rivers and streams.
Part 7: Guidance on sampling of water and steam in boiler plants.
Part 8: Guidance on sampling of wet deposition.
Part 9: Guidance on sampling from marine waters.
Part 10: Guidance on sampling of wastewaters.
Part 11: Guidance on sampling of groundwaters.
Part 12: Guidance on sampling of industrial cooling water.
Part 13: Guidance on sampling of sludges and sediments.
Parts 1, 2 and 3 of this standard have been adopted as Irish standards, I.S. EN 25667-1: 1994;
I.S. EN 25667-2: 1994; I.S. EN ISO 5667-3:1994, respectively
4
1.2.2 Standard M ethods for the Exam ination o f W aters and W astew aters
Standard Methods specifies methods and techniques for the sampling and examination of many
types of samples encountered in the assessment and control of water quality and water pollution.
A Joint Task Group is established for the approval of each method. The twentieth edition is the
most recent edition in which significant revision occurred, from the previous, in the section on
sampling.
5
1.3 SAM PLING PROCEDURES
The principle objective of water sampling is to collect a volume of water that adequately
represents the relative concentrations of all components present in the water or wastewater being
sampled (NSAI, 19946). In order that this objective be met, the development of a sampling
procedure is crucial. Sampling procedures are task specific since they depend on the type of
medium being sampled, the proposed method of sampling, the equipment used, the intended use
of the sample and data recording procedures (Anon., 1998; NSAI, 1994b). Each laboratory
should produce a sampling manual that includes the procedures and precautions to be adopted
for each parameter or group of parameters of interest (Flanagan et al, 2003; ISO, 1998; NSAI,
1994a). This procedure should include information on sampling location, sample type, sampling
method, sample collection and sample storage and preservation. It is important when
documenting a sampling procedure to ensure that all of the terms used are clearly defined so that
the procedure will be clear to other users (Working Group CITAC & EURACHEM, 2002).
Anon., 1998 state that sampling points should be fixed by detailed description in the sampling
plan, by maps, or with the aid of stakes, buoys or landmarks in a manner that will permit their
identification by other persons without reliance on memory or personal guidance. This will
make it easier to repeat the sampling at a later date and also may assist in drawing conclusions
from the test results. Global positioning systems (GPS) can also be used to supply accurate
sampling position data. (Working Group CITAC & EURACHEM, 2002)
Sampling location is dealt with in a very general sense in environmental legislation. For
example;
Article 6 (1) of the European Communities (Quality of Surface Water Intended for the
Abstraction of Drinking Water) Regulations, 1989 states: “that a sanitary authority shall
regularly monitor the quality of surface water, and for this purpose samples shall be taken for
analysis at the point or points at which the water is abstracted prior to treatment”.
6
- Article 10(1) of the Environmental Protection Agency Act, 1992 (Urban Waste Water
Treatment) Regulations, 1994 states that; “A sanitary authority shall carry out, cause to
be carried out, or arrange for, the monitoring of:
(a) discharges from urban wastewater treatment plants in accordance with the procedures
set out in the Fifth Schedule to the Regulations.
(b) waters subject to a discharge from an urban waste water treatment plant where it can
be expected that the receiving waters will be significantly affected.”
The difficulty in selecting a sampling location has been recognised by the Department of
Environment in the implementation handbook published with respect to the European
Communities (Quality of Surface Water Intended for the Abstraction of Drinking Water)
Regulations 1989. In this document it was stated that “As actual conditions e.g. accessibility of
site, immersion depth of sample intake pipe, distance from lake shore/bank of actual inlet, and so
on, will vary from case to case, it is not possible to specify a definitive sampling procedure”.
The draft implementation handbook published, by the EPA, with respect to the European
Communities (Drinking Water) Regulations, 2000 requires that a monitoring programme set out
each point at which drinking water samples are to be taken for particular parameters and that
these points should be selected at random.
ISO 5667 provides more detailed guidelines in relation to sampling locations for rivers, lakes,
drinking waters and wastewaters. For example, when sampling from rivers the following
guidelines should be adhered to;
Samples should preferably be taken where marked quality changes are likely to occur or
where there are important river uses.
Sample should be taken where flow data is available.
7
Sampling of weirs or small discharges that are only very local in effect should be
avoided.
If only one sample can be collected, take it in the middle of the main channel of the stream
and at mid-depth.
If monitoring the effects of a discharge at least two sites are necessary, one just upstream of
the confluence and the other sufficiently downstream to ensure mixing is complete.
(NSAI, 1994a), (ISO, 1990)
With regard to lake monitoring, the exact sampling locations can only be properly decided after
detailed preliminary investigations using a large number of sampling locations. This will
provide the information to which statistical analysis may be applied (ISO, 1987). In the case of
drinking water, sampling points should be at different locations and in particular from the end of
the distribution system (ISO, 1991). Wastewaters samples should be taken where the wastewater
is well mixed and representative of the entire flow (ISO, 1992).
Grab samples should always be used for parameters whose concentrations are susceptible to
being changed relatively rapidly in the interval between sampling and analyses because of
physical, chemical or biological reactions e.g. parameters such as pH, temperature, cyanides,
total phenols, residual chlorine, oils, fat, grease and faecal coliforms (Carty, O’Leary, Donlon
and Henry, 1998 and Anon., 1998). In the case of river and lake sampling, grab samples are
acceptable for quality characterization over a long period of time. Grab samples are the only
relevant types of sample for monitoring drinking water quality (NSAI, 1994)
Automatic composite samplers may be either time dependant or volume dependent. Time
dependent samplers collect a predetermined sample volume at a number of pre-determined time
intervals. Volume dependant samplers also collect samples at pre-determined time intervals
however, the volume collected is proportional to the flow at the time of sampling.
Composite samples are best suited to situations where information is required on the average
composition of a water/wastewater over a given period of time. They should not be used where
information is required on transient peak conditions as information on the time and duration of
occurrence will not be apparent. If pollutants peak for only short periods at a time, taking
composite samples will result in the potential dilution of the parameters of interest, perhaps
below limits of detection.
Where composite samples are used, it should be verified that the parameters of interest do not
vary significantly during the sampling period due to, for example, increased interactions between
analytes or an increase in potential analytical interference (Anon., 1998 and NSAI, 1994).
Composite sampling is unsuitable for certain unstable parameters such as oil and grease, acidity,
alkalinity, carbon dioxide, chlorine residual, iodine, nitrate, volatile organic compounds,
dissolved oxygen, temperature and pH, particularly where quantitative values are required.
Changes in these components may produce secondary changes in certain inorganic constituents
such as iron, manganese, alkalinity or hardness (Anon., 1998).
9
Composite sampling is required under certain legislation. For example, the EPA Act, 1992
(Urban Waste Water Treatment) Regulations, 1994 require that ‘Flow-proportional or time-based
24-hour samples shall be collected at the same well-defined point in the outlet and if necessary in
the inlet of the treatment plant, in order to monitor compliance with the requirements for
discharged waste water specified in these Regulations’ Composite sampling of wastewaters is
also required under ISO 5667-10 (ISO, 1992). Composite sampling is generally not
recommended for drinking water (ISO, 1991)
10
which critical appraisal of field conditions and complex sample collection techniques are
essential (Department of Environment, 1981).
Automatic sampling has a number of advantages over manual sampling. For example, human
errors associated with manually compositing samples are often reduced, labour costs are lower
and more frequent sampling is possible.
Sorbent sampling is useful when the parameter of interest is present only in trace amounts.
Sorbent sampling offers advantages of rapid, inexpensive sampling when the analyte of interest
is readily adsorbed and desorbed from the sorbent. The water sampled must be free of
particulate matter since these tend to plug the sorbent. ISO 5667 recommends the use of sorbent
sampling for virological sampling.
11
1.3.4 Sam pling equipm ent.
A variety of equipment is used for sampling waters and wastewaters including samplers and
sample containers. Samplers may be a bucket or long-armed sampler with liquid holding device
or an automatic sampling device. Sample containers are discussed in Section 2.3.5 below.
Portable field meters such as pH, conductivity and D.O. meters are also used when monitoring
water quality in situ.
The sampling equipment used must be suitable to site location and the sample to be taken (NSAI,
1994). It must be such that it will not contaminate the sample from its constituents or through
lack of cleanliness. Sampling equipment must be constructed from a suitable material and be of
adequate strength suitable for the purpose. It is also important to ensure that the sampling
equipment and containers are mutually compatible. Sampling equipment should be cleaned,
prior to use, with detergent and water (ISO, 1992; Crosby and Patel, 1995; Anon., 1998).
Prior to sampling, the sampler should ensure that the sample container is clean, free of
contaminants and pre-prepared as per the required analytical method. (Flanagan et al., 2003;
Anon., 1998; NSAI, 1996; ISO, 1987 and Department of Environment, 1981). Sample
containers should be tested to ensure that they are free of analytes of interest, especially when
sampling and analysing for very low analyte levels (Anon., 1998).
12
T here are tw o m ain types o f sam ple containers used. T hese are glass and plastic.
Although glass is generally thought of as an inert material, it may not be suitable for some
samples. For example, sodium, potassium and boron are major constituents of glass. The use of
glass bottles for the storage of samples, intended for analysis of these parameters, is not
recommended as they may be leached from the bottle to the sample in the interval prior to
analysis. Soda-glass bottles are unsuitable for the storage of poorly buffered waters (i.e. those of
low conductivity or alkalinity).
A number of workers specify that glass containers should be used for phosphates, oil and grease,
hydrocarbons, detergents and pesticides. (Anon., 1998 and Crosby and Patel 1995).
Bacteriological sampling also requires the use of glass bottles, with a minimum capacity of
250ml. These bottles should be capable of withstanding temperatures used in sterilisation
procedures. (Flanagan, 1990a and Flanagan et al., 2003).
13
of one litre is usually sufficient for most physical and chemical analyses (Anon., 1998).
Reference should be made to the relevant International Standards for the volumes required for
each analytical method. (NSAI, 1994b)
In contrast to the above NSAI, 1994 specifics that samples, ideally, should be taken from
turbulent, well-mixed liquids and whenever possible turbulence should be induced in flows that
are streamlined. NSAI 1994 does state however that sampling in turbulent areas does not apply
to the collection of sample whose concentration may be altered by induced turbulence e.g.
dissolved gases and volatile materials. NSAI, 1994 also specifies that when sampling physical
and chemical parameters, it is often sufficient to immerse an open-mouthed vessel (e.g. a bucket
or can) just below the surface in order to collect the sample. In situations where it is necessary to
sample at specified depths other sampling devices (e.g. a weighted bottle with removable stopper
or plunger device) may be used.
14
Opinions differ among workers in relation to the rinsing of sampling containers. The
Department of Environment Implementation handbook (1981) states that sampling bottles should
be rinsed out two to three times prior to sampling. Flanagan (1990) states that the sampling
container should be rinsed out with the liquid to be sampled before the actual sample is taken
except in the case of microbiological sampling. Anon., (1998) specify that containers should not
be pre-rinsed with sample as pre-rinsing results in loss of any pre-added preservative and
sometimes can bias results yielding artificially high concentrations when certain components
adhere to the sides of the container. ISO 5667 does not specify any requirement with regard to
the pre-rinsing of containers.
Sampling containers should be filled to the brim for most organic compound determinations e.g.
BOD, ammonia, iron, and manganese. (Flanagan et al., 2003; Flanagan et al., 2002; Anon.,
1998; NSAI, 1996 and Crosby and Patel, 1995). In the case of microbiological sampling,
samples should not be filled to the brim but allowed a space for aeration purposes (Flanagan et
al., 2003; Flanagan et al., 2002; Anon., 1998; Crosby and Patel, 1995; ISO, 1994/?).
The collection of samples for microbiological analysis requires extreme care in order to prevent
contamination by micro-organisms other than those of interest. (Flanagan et al., 2002; ISO,
1991; Flanagan, 1990a; Hammer, 1986 and Galal-Gorchev and Lewis, 1984).
There are many reasons why a water sample may undergo physical, chemical and/or biological
reactions. These include;
Bacteria, algae and other organisms can consume certain constituents present in the samples
and/or modify the nature of the constituents to produce new constituents. This biological
activity may affect dissolved oxygen and carbon dioxide levels. It may also affect, nitrogen,
phosphorus and sometimes silicon concentrations (Anon., 1998 and NSAI, 1996).
15
Certain compounds can be oxidized by the dissolved oxygen contained in samples or by
atmospheric oxygen e.g. organic compounds and iron(II), sulphides (Flanagan et al., 2003
and NSAI, 1996).
Certain substances can precipitate out of solution or be lost to the vapour phase e.g. oxygen,
cyanides, and mercury (NSAI, 1996).
pH, conductivity and carbon dioxide levels can be modified by the absorption of carbon
dioxide from the air (NSAI, 1996 and Galal-Gorchev and Lewis, 1984).
Dissolved metals, metals in the colloidal state and certain organic compounds can be
adsorbed or absorbed irreversibly onto or into the sampling containers or solid materials
contained in the samples (Anon., 1998 and NSAI, 1996)
- An increase in temperature (even if slightly elevated above ambient temperatures) can favour
microbiological activity. This may cause changes in sample composition (Flanagan et al.,
2003 and NSAI, 1996).
Prompt analysis is undoubtedly the most positive assurance against error due to sample
deterioration. When the interval between sample collection and analysis is long enough to
produce changes in either the concentration or the physical state of the constituent to be
measured, water samples should be preserved. A preservative is an additive, which will retard
biological, chemical or physical changes in the target analyte. A suitable preservative should not
interfere with the subsequent analytical determination or have its effects countered by the
chemistry of the test method (Crosby and Patel 1995 and Flanagan, 1990b). The most common
methods of preservation are acidification, filtration or cooling/freezing.
Acidification is normally used for the preservation of metals, ammonia, total phosphorus, oil and
grease. The sample is normally acidified to pH <2 using a suitable concentrated acid (such as
sulphuric acid or nitric acid) which is added to the sampling container either prior to leaving the
laboratory or at the sampling location. The amount of acid to be added should be determined
beforehand on a separate sample and then the same relative amount of acid added to all samples.
Ultra-pure acid preservative should be used to prevent contamination. The dilution caused by
acidification should be negligible or sufficiently reproducible to apply an appropriate correction
factor (Flanagan et al., 2002; Anon., 1998; NSAI, 1996; ISO, 1987 and Department of
Environment, 1981).
16
Sample filtration is necessary if the analyte of interest is dissolved in solution e.g. heavy metals.
Filtration should take place in the field, if possible. If carried out in conjunction with
acidification then filtration should be performed first (Anon., 1998 and Crosby and Patel 1995).
Care must be taken to ensure that the filter used is not a cause of contamination and is carefully
washed before use (Anon., 1998)
Cooling is used for the preservation of samples for BOD, conductivity, suspended solids,
sulphates and microbiological analysis. Cooling or freezing of samples is only truly effective if
it is applied immediately after sampling. This necessitates the use of cool-boxes or refrigerators
in vehicles at the sampling site. In most cases, cooling to temperatures of less than 4°C is
sufficient to preserve samples during transport to the laboratory and for a relatively short period
of time afterwards. Cooling is not considered as a means of long-term storage.
Freezing to temperatures of less than 20°C allows an increase in the period of storage however, it
is necessary to control the freezing and thawing technique fully in order to return the sample to
its initial equilibrium after thawing. (Crosby and Patel 1995 and NSAI, 1996).
There is no “catch-all” preservative that is suitable for a wide range of parameters. In some
instances the use of a particular preservation technique for one analyte may prove determinantal
to the analysis of another analyte. For example, samples preserved with nitric acid cannot be
analysed for pH, acidity, alkalinity or nitrate. The use of preservatives for a range of analytes
and sample types are discussed in a number of publications including Flanagan et al., 2003;
Flanagan et aL, 2002; Anon., 1998; NSAI, 1996 and Flanagan, 1990.
Quality control tests must be performed on the chosen method of preservation to ensure that
there is no significant difference between the result of an analytical determination carried out
immediately and the result obtained after preservation. The time elapsed between sampling and
analysis should be recorded together with the name of the preservative added (Anon., 1998;
Carty et al., 1998; NSAI, 1996 and ISO, 1990).
17
Paragraph 2). The associated implementation handbook (EPA, 1996) states that each hourly
sample portion taken (whether of influent or effluent) should be stored immediately under
refrigeration, until the 24-hour composite sampling period is completed. It is recognised in the
handbook, however, that it would be unreasonable to expect sanitary authorities to
retrospectively equip all their treatment plants with two refrigerated flow-proportional samplers,
especially in the case of smaller works where less frequent sampling is required.
European Communities (Quality of Surface Water Intended for the Abstraction Drinking Water)
Regulations, 1989 states that sample preservation should not significantly affect the values of the
results obtained from samples.
Every bottle should be identified with a unique sample number, preferably by attaching an
appropriately inscribed tag or label using a waterproof ink. Sufficient information should be
documented to provide positive sample identification at a latter date. If there is insufficient
space for all pertinent information on the label, the information should be recorded in a bound
field logbook at the sampling site at the time of sample collection (Anon., 1998; ISO, 1992; ISO,
1991; ISO, 1990; ISO, 1987; NSAI, 1994 and NSAI, 1996). Some workers require that a
detailed field log sheet be filled in (in duplicate) at the time of sampling (Flanagan et al., 2002
and Flanagan et al., 1990).
The amount of detail required in the sampling records will depend on the objectives of the
sampling programme. If the same sampling location is used permanently, it is not necessary to
repeat all details every time. Many workers have cited that at a minimum, the following details
be recorded- unique sample identification number, purpose of sampling, sampling date and time,
name of sampler, sampling location point, weather conditions, name and address of field contact
(if applicable), type of sample, preservation carried out and data generated in the field (Anon.,
1998; Bartram et al., 1996; Crosby and Patel,1995; ISO, 1992; ISO, 1991; ISO, 1990; Flanagan
et al, 2003a, 2003b and 1990 and Department of Environment, 1981). In some instances,
18
additional information must be recorded. For example, in Local Authority pollution
investigations, information relating to the name and address of the discharger and the name of
the receiving watercourse or sewer must also be recorded (Department of Environment, 1981).
It is essential that all field records and chain-of-custody forms are legible and maintained in a
secure location for a predetermined length of time. Accurate sample records are essential in
order to allow correlation between the laboratory analytical result and the field situation, thereby
allowing conclusions to be drawn and subsequent action taken if required.
Each laboratory must devise their own sampling record requirements since guidelines are not
provided in ISO 5667, Standard Methods, relevant environmental legislation or associated
implementation handbooks. The records maintained will normally be dependent on individual
laboratory requirements.
The conditions under which a sample is stored during transport depends on the analyte of
interest. For example, samples undergoing bacteriological assays must be stored in an icebox and
maintained at temperatures not greater than 10°C during transport. These samples should not be
19
stored for more than 30 hours, particularly if analysing for coliform bacteria (Flanagan et al,
2003 and Flanagan et al, 2002). In the case of volatile components (e.g. ammonia) the sample
must be stored in a gas-tight bottle to prevent evaporative loss of the component (Flanagan et al,
2003; Flanagan et al, 2002 and Anon., 1998). Easily oxidised components, e.g. nitrite, sulphite
and hydrogen sulphide, must be stored in air-tight-bottles to prevent the oxidation process
(Flanagan et al, 2003 and Flanagan et al, 2002).
ISO 5667 states that samples should be kept as cool as practicable and protected from light
during transportation. European Communities (Quality of Surface Water Intended for the
Abstraction Drinking Water) Regulations, 1989 states that sample transport should not
significantly affect the values of the results obtained from samples. There is no reference made
to sample transport in EPA (1996).
ISO 5667 (ISO, 1998) describes a number of quality control techniques and these include:
the collection of replicate samples as a check on the precision of sampling
the use of field blank samples. This is done by dividing a sample of deionized water into two
parts, one of which is processed as a real sample (i.e. by filling into a sample container and
adding preservative etc.) while the other is unused. The comparison of results from both
samples identifies errors due to contamination of sampling containers or sampling process,
the use of spiked samples. This is done by either spiking deionized water samples or
environmental samples with a known concentration of the analyte of interest. The spiked
sample used is divided into two parts, one of which is processed as a real sample using the
sampling container while the other is unused. The comparison of results from both samples
identifies errors due to contamination of sampling containers or sampling processes.
Standard Methods (Anon 1998) recommends that field blanks are used in order to assess whether
the sampling container used is affecting the analyte result obtained.
20
Legislation implementation handbooks e.g. Flanagan et al 2003; EPA, 1996 and Flanagan P.J.,
1990a) do not specify specific requirements with regard to sampling quality control techniques.
More recent implementation handbooks e.g. Flanagan et al 2003 deal in detail with analytical
quality control but do not refer to sampling quality control.
Limerick County Council (LCC) carries out its own water sampling using trained scientific staff
and is currently in the process of attaining accreditation to ISO 17025 (General requirements for
the competence of testing and calibration laboratories). In order to comply with Condition 5.7 of
this standard the laboratory has produced a sampling programme and sampling procedures.
The laboratory's current sampling programme contains maps and lists of all sampling locations
in the county. These sampling locations include rivers, surface waters used for the abstraction of
drinking waters, licensed industrial plants and urban wastewater treatment plants. The sampling
programme also contains a map and list of all drinking water supplies in the county and details
the number of samples required per year for each supply.
The laboratory’s sampling procedures are documented in SOPs (Standard Operating Procedures).
These have been prepared by senior members of staff who carry out the sampling procedure on a
regular basis, using guidelines given in Standard Methods (A.P.HA. 1998), legislation and
associated handbooks. The sampling SOPs describe the sampling equipment, sampling location,
sampling method, field analyses required, the sample storage conditions and safety precautions
necessary when sampling various water bodies. They therefore describe the sampling tasks in
sufficient detail in order that a competent sampler unfamiliar with the method can conduct the
21
procedure and provide a solid training tool in assuring uniform procedures are adhered to at all
times.
LCC SOP’s are identified with a unique number together with the date of issue, revision number
and page numbers and are only issued by authorised personnel. A master list identifying current
revision status of SOP’s and their distribution status established. This ensures that only valid
copies are available and that obsolete SOP’s are properly removed. The control over SOP’s, in
such a manner, is required under Condition 4.3 of ISO 17025. A copy of the current sampling
SOPs, documented by Limerick County Council, are given in Appendix C.
Samples taken correctly may have serious implications if legal action is initiated on foot of the
subsequent results. For example a prosecution taken by LCC against A.I.B.P Ltd. under Section
3 of the Local Government (Water Pollution) Act, 1977, in July 1997, was dismissed from the
district court case for the following reasons:
1. The samples were not taken properly
2. The samples were not taken from the proper location
3. The chain of evidence with regard to handling of the samples was not established.
4. The improper handling and storage of the samples bythesampler, the courierand the sub
contracting laboratory raised question of possible contamination.
A copy of the court report filed by Mr. Michael Finbarr Collins, Barrister-at-law is given in
Appendix A.
22
2.0 M A T E R IA L S A N D M E T H O D S
2.1 Q U ESTIO N N A IR E
2.1.1 Introduction
In order to investigate how laboratories in Ireland are currently taking water samples (physical,
chemical and microbiological) a questionnaire was forwarded to a number of Local Authority
(LA), EPA and independent laboratories. This questionnaire was of the format shown in Figure
2.1. The questionnaire was accompanied by a cover letter which gave details on the purpose of
the questionnaire, guaranteed confidentiality on all information obtained and offered a copy of
the findings to interested laboratories.
In order to obtain an overview of common water sampling practice and procedures in various
environmental laboratories, recipients of the questionnaire were asked to answer a total of 32
questions. The questions were based on requirements of the ISO 5667 standard, Standard
Methods (Anon, 1998), specified requirements in relevant legislation and associated handbooks
(Refer to Section 1.2 of the Literature Review). In order to reduce the length of time that the
survey would take to complete several of the questions asked required yes/no answers. This was
hoped to encourage a high response rate.
Once the laboratories had responded to the questionnaire the results from the various laboratory
sectors were collated and summarised. This allowed statistical analysis to be carried out, the
results to be presented in graphical format and comparisons to be made between the various
sectors.
23
F ig u r e 2.1 T h e Q u e stio n n a ir e fo r w a rd ed to la b o r a to r ie s
L ab oratory:__________
C ontact Nam e:________
C ontact Telephone No.:
Q. Answer
No.
1. Does the laboratory carry out its own sampling9
2. Does the laboratory have personnel designated solely for sampling?
3. Are sampling procedures documented?
4. Are there documented procedures for the training of personnel involved
in sampling?
5. Is the above training carried out in-house or by an independent outside
body?
6. Are sampling training records maintained?
7. Has the laboratory ever considered obtaining accreditation specifically
for sampling work carried out by the laboratory?
8. If YES to Q7please give brief details:
9. Does the laboratory use any of the following as a guide when preparing
sampling programmes and procedures? (Please tick)
IS05667 □
LA Implementation handbooks □
Standard Methods (Anon) □
10. Are samples taken/analysed by the laboratory used as evidence in court?
11. Have laboratory sampling procedures used by your laboratory ever been
questioned in court?
12. Which of the following samples are routinely sampled by your
laboratory: (Please tick)
River water: □
Wastewater - Industrial effluent: □
Wastewater - Sewage treatment plants: □
Drinking water: □
24
F ig u r e 2.1 (c td .)
Q. A nsw er
No.
13. Please list the parameters which are routinely monitored at the following
samcling
sampling locations:
locations;
17. What type of sampling containers does the laboratory use to sample the
following:
a Microbiological :
b Fluoride :
c. Oil and grease :
d Phosphate:
e. Metals :
18. Do the laboratory procedures document what type of sampling container
is to be used?
19. Are field blanks analysed for each sample run?
20 . Are any of the following samples chemically preserved prior to analysis:
a) Ammonia: □
b) Phosphate: □
c) Total Phosphorus: □
d) Metals: □
e) Oil and grease: □
21 . If YE Sto Q20 - How soc
a) Ammonia:
b) Phosphate:
c) Total Phosphorus:
d) Metals:
e) Oil and grease:
25
F ig u r e 2.1 (ctd .)
Q* Answer
No.
22. Do the laboratory procedures document which samples are to be
preserved?
24. Are quality control tests carried out in order to ensure that the
preservatives used does not interfere with subsequent determinations?
If YES please give brief details:
26. Are samples transported from the sampling site to the laboratory in a
refrigerated van or cooler box?
29. Are there standard field log-sheets for the various water bodies being
sampled?
31. If YES to Q30 how many tests is the laboratory accredited for?
26
2 .2 G A P A N A L Y S IS
2.2.1 Introduction
There is currently no laboratory in Ireland accredited specifically to ISO 5667, nor is there any
published information available with regard to attaining accreditation to the standard. In order
to ascertain the level of work required attaining accreditation to ISO 5667 a gap analysis was
carried out.
2.2.2 G ap A nalysis
Current water sampling procedures and practices at Limerick County Council’s (LCC)
Environmental Laboratory were used as a case study in order to determine the level of work
required to attain accreditation to ISO 5667. This was done by carrying out a gap analysis. The
gap analysis looked in detail at the requirements of the standard versus current practice and
procedures in the laboratory.
The following parts of IS05667 are relevant to the work carried out by the laboratory and were
therefore used for the gap analysis:
Part 1: Guidance on the design of sampling programmes
Part 2: Guidance on sampling techniques.
Part 3: Guidance on the preservation and handling of samples.
Part 5: Guidance on sampling of drinking water and water used from food and beverage
processing.
Part 6: Guidance on sampling of rivers and streams.
Part 10: Guidance on sampling of wastewaters.
Part 14: Guidance on quality assurance of environmental water sampling and handling.
The following laboratory documented standard operating procedures (SOP’s) are relevant to the
gap analysis:
SOP No. 6 - Routine Drinking Water Supply Schemes
SOP No. 8 - Routine River Sampling
SOP No. 10 - Sewage Treatment Plant Sampling
SOP No. 1 1 - Industrial Effluent Sampling
SOP No. 43 - Procedure for Handling Test Samples/Items
27
SOP No. 47- Surface Waters for Abstraction of Waters Intended for Human Consumption -
Sampling Procedure.
(Refer to Appendix B for copies of the above SOP’s)
The gap analysis was performed by comparing each relevant section of each part of the ISO
5667 standard with current procedures and practices in LCC’s environmental laboratory. This
allowed non conformances between the requirements of ISO 5667 and current practices and
procedures in the LCC’s environmental laboratory to be quickly identified. A non
conformance was raised where there was evidence of a failure to comply with a requirement of
ISO 5667. When there was evidence of a non-conformance, appropriate corrective actions were
identified.
For ease of assessment, the corrective actions were categorised into a number of areas, namely.
> Sampling programme
> Quality control
> Preservation
> Drinking water sampling
> River water sampling
> Wastewater sampling
Each proposed corrective action was then assessed in order to determine the following:
> Whether the facilities/resources are currently available within the laboratory to implement
the corrective action.
> A proposed time scale for implementation i.e.
Short term: less than 6 months
Medium term: 6 months - year
Long term: greater than 1 year
The time scale was based on one member of the laboratory personnel having 30-40% (1.5-2
days) of their working week dedicated solely to the implementation of this standard.
> An estimated cost for implementation of the corrective standard
Low: Cost is minimal.
- Medium: Cost can probably be met using the laboratory’s annual allocated budget.
High: Cost cannot be met using the laboratory’s annual allocated budget.
> Whether staff can be trained on-site or if off-site training is required.
28
3.0 R ESU LTS A N D D E S C R IP T IO N O F R ESU LTS
There are currently 6 EPA laboratories in Ireland. Since each of these laboratories responded to
the questionnaire, the information obtained from these can be considered to be truly
representative of water sampling practices in the EPA laboratory sector.
There are approximately 17 independent laboratories, involved in water analysis, in Ireland. The
questionnaire was forwarded to 11 of these laboratories. Although 4 independent laboratories
replied to the questionnaire, one of these laboratories does not carry out routine water quality
sampling. Drawing conclusions from the results obtained from 3 independent laboratories
cannot be considered to be truly representative of water sampling practices in this sector. These
results, therefore, are not discussed as part of this dissertation, but summarised in Appendix C
(Table C3).
29
Table 3.1 Comparison of the percentage ‘yes’ responses received from LA and EPA
laboratories when questioned in relation to various aspects of sampling and
sampling procedures. The Table also shows the responses from Limerick County
Council Laboratory.
30
T a b le 3 .1 (c td .)
Of the 6 EPA laboratories in Ireland, just 5 carry out water sampling i.e. 83%. Of the
laboratories which carry out water sampling, 80% have personnel designated solely to sampling.
31
Figure 3.1 P e r c e n ta g e o f L A and E P A la b o ra to ries w h ic h (a ) carry ou t their o w n w a ter
EDLocal Authority
0 EPA
Figure 3.2 details the type of water samples collected by the LA, EPA and private laboratories,
which replied to the questionnaire.
Figure 3.2 Percentage of LA and EPA laboratories, which routinely sample rivers, industrial
effluents, sewage treatment plants and drinking waters.
110
100
90
80
70
xo 60
^ 50
40
30
20
10
0
Rivers Industrial STP Drinking
effluent Water
32
The routine sampling carried out by LA laboratories varies. Of the LA laboratories that replied
to the questionnaire, 72% routinely sample rivers, 67% routinely sample industrial wastewaters,
72% routinely sample sewage treatment plants and just 61% routinely sample drinking waters.
All EPA laboratories routinely sample industrial wastewaters and rivers. 60% of EPA
laboratories routinely monitoring sewage treatment plants while 40% routinely monitor drinking
waters.
A number of questions were asked regarding the existence and documentation of sampling
procedures in the laboratory. Tables 3.1 and Figure 3.3 summarise the replies obtained.
Figure 3.3 Percentage of LA and EPA laboratories that document (a) sampling procedures
(b) the type of sampling container to be used (c) the sample types that are to be
preserved and (d) procedures for labelling samples
Of the laboratories which responded to the questionnaire, 74% of LA laboratories and 60% of
EPA laboratories have documented sampling procedures in place The level of detail in these
sampling procedures varies. For example, 100% of EPA and 56% of LA laboratories document
the type of sampling container to be used. 80% of EPA and 64% of LA laboratories document,
which samples are to be preserved. 60% of EPA and 53% of LA document procedures regarding
the labelling of samples.
33
3.1.3 Guides used in Preparing Sampling Program m es and Procedures
Figure 3.4 shows the guides used by the laboratories in preparing sampling programmes and
procedures.
Figure 3.4 Percentage of LA and EPA laboratories, which use (a) ISO 5667 (b) Local
Authority Implementation Handbooks and (c) American Public Health
Association ‘Standard Methods’ when preparing sampling programmes and
procedures.
90 T -
Among the laboratories questioned, Standard Methods (Anon., 1998) is the most commonly used
guide for preparing sampling procedures i.e. 83% of LA laboratories and 60% of EPA
laboratories use this guide. A significantly lower number of the laboratory respondents use ISO
5667 as a guide namely 1 1 % of LA laboratories and 20% of EPA laboratories. 56% of LA
laboratories, which responded, use these LA implementation handbooks when preparing
sampling programmes and procedures however only 20% of EPA laboratories use these
handbooks
34
laboratories (40%) maintain sampling training records (Figure 3.5). All laboratories questioned
carry out in-house training of sampling personnel.
Figure 3.5 Percentage of LA and EPA which (a) have documented procedures with regard to
training sampling personnel and (b) maintain sampling training records
100
90
80
70
60 ILocal Authority
50
40 IEPA
30
20
10
0
Documented training Maintain training records
procedures
In total five laboratories interpreted the question correctly. Temperature, chlorine and dissolved
oxygen are measured in the field by all these laboratories. However pH and conductivity are
only measured in the field by two of these laboratories.
35
Figure 3.6 P e r c e n ta g e o f L A and E P A la b o ra to ries that (a ) c h e c k or ca lib ra te fie ld m eters
□ Local Authority
□ HPA
Figure 3.7 Percentage of LA and EPA laboratories that use the correct sampling containers
for fluoride (glass), FOGs (glass), phosphates (glass), metals (glass/plastic) and microbiological
samples (sterile glass/plastic).
□ Local Authority
H EPA
36
All laboratories use the correct type of sampling containers when sampling for fluoride, metals
and microbiological samples. In relation to oil and grease, all EPA laboratories use the correct
container i.e glass, when sampling for this parameter however only 63% of LA laboratories use
the correct container. All laboratories who replied to the questionnaire use the incorrect type of
sampling container i.e. plastic containers, when sampling for phosphate. Nevertheless, one LA
laboratory did state that it used plastic or glass for very low levels.
Figure 3.8 Percentage of LA and EPA laboratories, which chemically preserve samples taken
for ammonia, oil and grease, metal, phosphate and total phosphorus analyses.
110
67% of EPA laboratories chemically preserve samples for ammonia analysis, however, only 5 %
of LA laboratories that responded preserve for this parameter. All EPA laboratories chemically
preserve samples taken for oil and grease analysis. None of the LA laboratories, which
responded, preserve for oil and grease. All EPA laboratories chemically preserve samples taken
for metal analysis. 60% of the LA laboratories also preserve samples taken for metal analyses.
Of the laboratories that responded, only one LA and one EPA laboratory chemically preserve for
phosphate.
37
With regard to the preservation of drinking water samples, all LA laboratories, which responded
use sodium thiosulphate to counteract the effects of chlorine during sample transport. Only 75%
of EPA laboratories however use sodium thiosulphate.
Q21 of the questionnaire, asked, “how soon after sampling are samples preserved?”the most
common answer given was ‘when samples are returned to the lab”
Although 80% of EPA laboratories and 64% of LA laboratories document, as part of their
methods, the samples which are to be preserved, a much lower percentage maintain records of
the preservation carried out i.e. 40% of EPA and 45% of LA laboratories.
Figure 3.9 Percentage of LA and EPA laboratories which (a) analyse field blankswith each
each sample run (b) carry out quality control tests on preservative used.
38
LA laboratories generally do not use the above quality control procedures with only 27% of LA
respondents analysing field blanks and 18% carrying out quality control tests with regard to the
preservatives used. Most EPA laboratories use the quality control procedures outlined above
with 60% analysing field blanks and 80% carrying out quality control tests on preservatives
used.
60% of the EPA respondents answered “yes” to the above question. The remaining 40% of EPA
laboratories use field sheets to record sampling information. 37% of LA respondents replied
“yes” to the above question. Of the remaining laboratories, 50% record the information on the
sampling bottle, 25% use field sheets and 25% use both sampling bottles and field sheets.
Of the laboratories which use a log-sheet 100% of EPA laboratories and 33% of LA laboratories
have standard field log-sheets for the various water bodies being sampled.
39
Figure 3.10 Percentage of LA and EPA laboratories that use chain-of-custody forms for
samples taken (a) by laboratory personnel (b) by non-laboratory personnel and
(c) for prosecution cases.
110 !
All EPA laboratories use chain-of-custody forms for samples taken by laboratory personnel, by
non-laboratory personnel and for prosecution cases. In contrast, LA laboratories do not
frequently use chain-of-custody forms. Figure 3.10 shows that only 25% of LA respondents use
chain-of-custody forms for samples taken by the laboratory personnel, 36% use the forms for
samples taken for prosecution cases and 47% of LA laboratories use the forms for samples taken
by non-laboratory personnel.
40
Figure 3 .1 1 Percentage of LA and EPA laboratories that (a) use samples taken as evidence in
court, as required and (b) have had their sampling procedures questioned in
court.
From Figure 3.11 it is evident that all EPA laboratories use the results from samples analysed as
evidence in court, when necessary. In contrast, only 47% of LA laboratories use the results from
samples analysed as evidence in court. 25% of EPA laboratories indicated that they have had
their sampling procedures questioned in a court of law. A lower percentage (16%) of LA
laboratory respondents indicated that they have had their sampling procedures questioned in a
court of law. Details regarding the areas cross-examined in court were not requested in the
questionnaire
There are currently 66 laboratories in Ireland accredited by the National Accreditation Board
(NAB) to ISO 17025. Several of these laboratories are based in private industrial plants and were
not considered as part of the survey.
41
Figure 3 .12 shows the accreditation status of the LA and EPA laboratories which replied to the
questionnaire.
Figure 3.12 Percentage of LA and EPA laboratories which are (a) accredited to ISO 17025
(b) considering accreditation to ISO 17025 and (c) considering accreditation to
ISO 5667.
100
90
80
70
Although none of the LA laboratory respondents are presently accredited to ISO 17025, 48% are
currently considering attaining accreditation to this standard. Subsequent investigations revealed
that two LA laboratories were accredited to ISO 17025 when the questionnaire was sent out
however, these did not reply to the questionnaire. 60% of EPA laboratories are accredited to
ISO 17025 while 50% of those not currently accredited are considering accreditation to this
standard.
There are currently no laboratories in Ireland accredited to the ISO 5667 water quality sampling
standard. However, 16% of the LA laboratories, which responded, have considered obtaining
accreditation specifically for sampling. One LA laboratory stated that it would be more cost
effective to contract out the sampling work than apply for accreditation.
60% of EPA respondents have considered obtaining accreditation to ISO 5667. Two EPA
laboratories have it as part of their long-term plan, while another EPA laboratory found it too
complex to implement and decided after some preliminary investigations not to apply.
42
3.2 RESULTS OBTAINED FROM THE GAP ANALYSIS
C.A.’s No. 2 and 3 require that the objectives of sampling and the degree of detail and precision
adequate for analytical field results be documented in the sampling programme. These measures
can be dealt with in the short term at a low cost because most of the sampling currently
undertaken is specifically done in order to assess compliance with particular pieces of
legislation. The manner in which results are to be presented is often stated in legislation. The
relevant legislation would have to be identified for each sampling programme.
C.A. No. 4 requires that sampling locations be reviewed in order to ensure samples are taken
from turbulent, well-mixed liquids. This would involve the assessment of each sampling
location to ensure there is adequate mixing throughout the body of the water, thereby ensuring
that representative samples are taken. To assess this would require external expertise thereby
incurring a high cost and hence long term implementation.
43
Table 3.2: An assessment of the ability of Limerick County Council's Environmental Laboratory to implement the proposed corrective actions
to their sampling programme.
Note: More detailed information with regard to these corrective actions are contained in Appendix D
Corrective Action Are the Proposed time Cost of Staff Comments
facilities/ scale for implementation: training: on
resources implementation: High/Medium/ site /off-site
available Short/Medium/ Low
Long term
L
Amend sampling programme to include Yes Short Low N/A - The frequency of most
details of: sampling programmes is
a) how sampling sites (location and point) dictated by the relevant
were selected, ensuring that safety and legislation.
health aspects are considered.(ISO 5667-
1:1980 Section 1 (3))
b) how the frequency of analysis is
calculated, ensuring it is done in a
systematic manner. (ISO 5667-1:1980
Section 3 (16.1), ISO 5667-6:1990 (1),
(5-2))
c) when spot and composite samples are to
be taken. (ISO 5667-2:1991 (4.2), (5))
2.
State the objectives for the various sampling Yes Short Low N/A
programmes.
(ISO 5667-1:1980 Section 1 (3), IS05667-
5:1999 (1), ISO 5667-10:1992 (1), (5.1.3),
(5.3.1.1))
3.
a) Identify and document the degree of detail Yes Short Low N/A
and precision that will be adequate for
analytical field results. Outline the manner
Table 3.2(ctd..):
Corrective Action Are the Proposed time Cost of Staff Comments
facilities/ scale for implementation: training: on
resources implementation: High/Medium/ site /ofTf-site
available Short/Medium/ Low
Long term
3. tctd.)
a) in which the results are to be expressed and Yes Short Low N/A
presented, as part of the sampling
programme. (ISO 5667-1:1980 Section 1
(3))
b) Amend sampling programme to include
definition of the magnitude of the tolerable
error in analytical field results. (ISO 5667-
6:1990 (1), (5.2))
4.
Review the sampling locations ensuring No Long High Off-site Would require external
samples are taken from turbulent, well-mixed expertise to determine
liquids. (ISO 5667-1:1980 Section 2 (8.3)) whether there is sufficient
turbulence at the various
sampling locations
L
Amend sampling programme to give details on No Long High Off-site - Would require external
the introduction of turbulent flow conditions, expertise to determine
where necessary. (ISO 5667-10:1992 (5.1.2)) whether there are turbulent
flow conditions at the
sampling site and how the
turbulent flow conditions
should be introduced, if
required.
6.
Ascertain the need to statistically determine Yes Medium Low N/A
the number of samples required for a given
Table 3.2(ctd.)
Corrective Action Are the Proposed time Cost of Staff Comments
facilities/ scale for implementation: training: on
resources implementation: High/Medium/ site /off-site
available Short/Medium/ Low
Long term
6. (ctd.I
confidence interval. If required, carry out Yes Medium Low N/A
statistical analysis, document results and
amend sampling programme as required.
(ISO 5667-1:1980 Section 3 (16.4))
7.
Identify and document the wastewater Yes Short Low N/A
sampling times required. These can be
ascertained using the formulae given in ISO
5667 - 10:1992 (5 . 2 . 3), which calculates the
sampling times over a specified control period
e.g. one year, a number of months or weeks.
8.
a) Identify whether the water bodies sampled No Long High Off-site Would require outside
have random or systematic variations in expertise to determine:
quality. a) whether the water
b) Determine statistically the number of bodies sampled have
samples required to determine whether random or systematic
random or systematic variation occurs. variations in quality
c) If systematic variations in quality exist, b) statistically the
determine the times of sampling (these number of samples
should be spaced approximately equally required to determine
over trend periods) whether random or
d) Document results and amend sampling systematic variation
programme as required. occurs
(ISO 5667-1:1980 Section 3 (16.5)) c) the times of sampling,
if systematic variation
4-
Os
Table 3.2(ctd.)
Corrective Action Are the Proposed time Cost of Staff Comments
facilities/ scale for implementation: training: on
resources implementation: High/Medium/ site /off-site
available Short/Medium/ Low
Long term.
9,
As part of the sampling programme compile a Yes Short Low N/A
list of the parameters of interest for each
sample body e g wastewater, river, etc. with
reference to the relevant analytical procedure
used in the laboratory. (ISO 5667-1:1980
Section 1 (3))
10.
Amend ‘sampling programme’ to include map Yes Short Low N/A
of surface waters used for the abstraction of
drinking water. Outline the various sampling
points in these water bodies (ISO 5667-6:1990
(5.1.1))
C.A. No. 5 follows from the above and requires details to be given on how turbulent flow
conditions would be introduced, where necessary. This again would require external expertise
and its implementation would occur only after C.A. No. 4 is implemented.
C.A. No. 6 deals with identifying the need to statistically determine the number of samples
required for establishing a given confidence interval. This would firstly involve identifying the
confidence interval necessary, from either legislation or other appropriate documentation. The
sampling programme would then have to be amended if the current sample numbers were not
sufficient. This corrective may not be necessary for all sampling programmes as the number of
samples required is often specifically stated as part of the legislative requirements. Where
required, the number of samples can be determined for a given confidence interval using the
formulae provided in ISO 5667-1:1994 (16.4).
C.A No. 7 requires that the sampling programme document wastewater sampling times and
details on how these were selected. The EPA Act, 1992 (Urban Wastewater Treatment)
Regulations, 1994 and associated implementation handbooks state the number of samples
required per calender year. This is based on the size of the wastewater treatment plant.
Currently, LCC environmental laboratory takes the required number of samples but the exact
sampling dates are not documented, therefore the sampling may not be spread evenly over the
calender year. In order to comply with ISO 5667-10:1992 the sampling times should be spread
evenly throughout the year. This can easily be calculated using the formulae given in ISO 5667-
10:1992 (5.2.3) and the sampling programme amended accordingly. This measure could
therefore be dealt with in the short time at a low cost.
C.A. No 8 action deals with identifying whether the water bodies sampled have random or
systematic variations in quality and based on these results determining statistically the number of
samples required to be taken The sampling programme may have to be amended based on these
findings. In-house expertise is not available to determine this and therefore a high cost would be
incurred in obtaining external expertise as each of the water bodies being sampled would have to
be assessed.
C.A. No. 9 requires that as part of the sampling programme a list of the parameters of interest for
each sample body e.g wastewater, river etc be complied together with reference to the relevant
48
analytical procedure. This could be carried out within a short period as it simply involves
collating the methods used within the laboratory.
C.A. No. 10 requires that a map of the sampling points in surface waters, used for the abstraction
of drinking water, be included in the sampling programme. This could be collated in the short
term using current mapping facilities within the Local Authority.
C.A. No. 2 requires that a procedure be developed, documented and implemented to deal with
situations where the time-of -travel exceeds the maximum recommended preservation time. This
cannot be accurately documented until a comprehensive preservation programme is firstly
implemented as per ISO 5667- 1, 3 and 14.
C.A. No. 3 requires that a procedure be developed, documented and implemented in order to
verify that the number of samples received at the laboratory coincides with the number recorded
on the field sheet. On arrival at the laboratory, samples are currently logged and marked by the
sampler with a unique laboratory identification (ID) code. As it is simply a matter of
documenting current procedure, the above could be dealt with in the short term at a low cost.
C.A. No. 4 requires that a method be developed, documented and implemented to ensure
samples are preserved and stored in the correct containers as soon as possible after sampling.
This may require using different storage containers and preservation techniques for each analyte
of interest, which would significantly increase the sampling time.
49
Table 3.3: An assessment of the ability of Limerick County Council’s Environmental Laboratory’s to implement the proposed corrective actions
to their quality control programme.
Note: More detailed information with regard to these corrective actions are contained in Appendix D
Corrective Action Are the Proposed time Cost of Staff Comments
facilities/ scale for implementation: training: on-
resources implementation: High/Medium/ site/off-site?
available Short/Medium/ Low
Long term.
L
Implement a procedure for assessing whether At present, samples are not
the filter type used to filter samples is a cause filtered on-site. The need
of contamination. (ISO 5667-3:1994 (3.2.5)) for this will have to be
assessed as per ISO 5667-
3:1994 (3.2.5)
2.
Develop, document and implement a Yes Medium Low On-site Correct preservation
procedure for situations where the time-of - techniques are currently
travel exceeds the maximum recommend not in place. This will have
preservation time. (ISO 5667-3:1994 (5)). to be addressed first, as per
ISO 5667- 1, 3 and 14.
3.
Develop, document and implement procedure Yes Short Low On-site Samples are currently
for verifying that the number of samples logged and marked by the
received at the laboratory coincides with the sampler, on arrival at the
number recorded on the field sheet. (ISO laboratory, with the
5667-3:1994 (6)). appropriate laboratory
identification code.
4. Document the container
Develop, document and implement method to Yes Medium Low On-site type to be used for various
ensure samples are preserved and stored in the parameters.
correct containers as soon as possible after Document which samples
sampling. (IS05667-5:1999 (7.2)) are to be preserved and
Table 3.3(ctd.)
Corrective Action Are the Proposed time Cost of Staff Comments
facilities/ scale for implementation: training: on-
resources implementation: High/Medium/ site/ofT-site?
available Short/Medium/ Low
Long term.
4. (ctd.)
how this preservation is to
be carried out.
Implement system of
recording the type of
container used together
with preservation
technique.
L
Develop, document and implement analytical Yes Long term High On-site ( may A lot of time is required to
quality control (QC) programme for need some implement and carry out
periodically testing the sampling methods outside the QC programme fully
used. This should include the use of field training) - Document the various QC
blanks, samples with added determinands techniques and implement
and/or duplicate samples. (ISO 5667-6:1990 procedure for recording
(5.5)), (ISO 5667-14:1998(E)) and interpreting the results
obtained from the QC
programme.
Determine when to
accept/reject the results, by
the application of statistical
methods i.e. Shewart charts
(Standard Methods Anon
1998)
Identify measures
necessary when QC result
has to be rejected based on
Table 3.3 (ctd.)
Corrective Action Are the Proposed time Cost of Staff Comments
facilities/ scale for implementation: training: on-
resources implementation: High/Medium/ site/off-site?
available Short/Medium/ Low
Long term.
5. fctd.)
the above statistical
method.
6.
a) Develop, document and implement Yes Short Low On-site Identify the training
procedure for training sampling personnel required
with regard to correct sampling and on-site Review the training process
measurement techniques. (IS05667-5:1999 on a regular basis.
(9).
b) Document the sampling training procedure
and develop detailed training records. (/SO
5667-14:1998 (5.1)), (ISO 5667-3:1994
(3.2.1))
7.
Identify, document and implement a procedure Yes Short Low On-site
to assess the suitability of polyethylene
containers for the collection of samples for
trace metal analyses. (ISO 5667-6:1990 (4.1))
C.A. No. 5 requires that an analytical quality control (QC) programme be developed,
documented and implemented for periodically testing the sampling methods used. This should
include the use of field blanks, samples with added determinands and/or duplicate samples. The
QC programme must document how the results of the above are to be recorded and subsequently
interpreted i.e. accepted/rejected. The method use to determine when to accept/reject results
must be clearly stated. This is normally done by statistical methods e.g. Shewart charts (Anon
1998). Shewart charts set control and warning limits. If the result obtained is outside the control
limit the result is rejected. If the result is outside the warning limit the result is rejected if the
previous two results are also outside the warning limit but accepted if the previous two results
are within the warning limit. The measures necessary when a QC result must be rejected should
be clearly documented. The complete implementation of this measure could take a long time
and incur a high cost owing to the increased workload on both the sampler and the analyst.
C.A. No. 6 requires that a procedure is developed, documented and implemented for training
sampling personnel with regard to correct sampling and on-site measurement techniques.
Detailed training records would also have to be maintained. As the laboratory currently has a
non-documented training procedure it is simply a matter of collating and documenting what is
currently being carried out. This can achieved in the short term at a low cost.
C.A. No. 7 requires that a procedure is identified, documented and implemented to assess the
suitability of polyethylene containers for the collection of samples for trace metal analyses. ISO
5667 (Part 6) states that polyethylene containers may not be suitable for collecting samples
undergoing some trace metal analyses since they may be a source of contamination of some trace
metals e.g. mercury. An assessment of the suitability of polyethylene containers for trace metal
analysis would involve carrying out a series of metal analyses on known samples stored in
polyethylene containers. This could be carried out in the short term using existing resources.
3.2.3 Preservation.
Table 3 .4 outlines four corrective actions which are required in order to bring Limerick County
Council’s sample preservation procedures in line with the requirements of ISO 5667.
53
Table 3.4 An assessment of the ability of Limerick County Council’s Environmental Laboratory’s to implement the proposed corrective actions
to their preservation programme.
Note: More detailed information with regard to hese corrective actions are contained in Appendix D
Corrective Action Are the Proposed time Cost of Staff Comments
(Standard Ref.) facilities/ scale for implementation: training: on-
resources implementation: High/ Medium/ site/off-site?
available Short/Medium/ Low
Long term.
L
a) Identify and document the preservation Yes Medium Low On-site The implementation of
method(s) required for various sample comprehensive
types preservation techniques
b) Implement preservation methods, where will increase the sampler’s
required. workload.
c) Develop method of recording when Refer to ISO 5667 and
samples are preserved. Standard Methods (Anon.,
(ISO 5667-1:1980 Section I (3), (5.3)), (ISO 1998) for reference to the
5667-3:1994 (3.1)), (ISO 5667-14:1998 (6)) correct preservation
techniques for the various
parameters.
2.
Ascertain the need to preserve samples during No Long Medium On-site The laboratory is presently
the collection of composite samples. If operating at maximum
necessary, implement system of sample capacity therefore the
preservation. (ISO 5667-2:1991 (4.6)), (ISO resources e.g. staff/ time
5667-10:1992 (5.4)) are not currently available
Develop method to
determine whether the
parameters of interest vary
significantly during the
composite sampling
Table 3.4 (ctd.)
Corrective Action Are the Proposed time Cost of Staff Comments
(Standard Ref.) facilities/ scale for implementation: training: on-
resources implementation: High/ Medium/ site/off-site?
available Short/Medium/ Low
Long term.
2. (ctd.)
period, when preservation
is not used.
Determine if there is a
statistical difference
between the samples with
and without preservation.
Implement appropriate
preservation method(s).
3.
Document and implement method for ensuring Yes Medium Medium On-site
that the preservative used does not result in
dilution of the analyte or interfere with the
subsequent analysis thereby influencing the
final result. (ISO 5667-3:1994 (3.2.6)), (ISO
5667-14:1998 (6)).
4.
The efficiency of the preservation process Yes Long Medium On-site The laboratory is presently
depends on the constituents which have to be operating at maximum
analysed, their levels and on the nature of the capacity therefore the
sample. Therefore develop, document and resources e.g. staff/ time
implement a procedure to verify whether or are not currently available
not the preservation suggestions in ISO 5667-
3:1994 (Table 1-5) are suitable for the sample
with which it is concerned. (ISO 5667-3:1994
(3.3))
LLf»
/»
C.A. No. 1 requires that the preservation method(s) for the various sample types be identified,
documented and implemented. The preservation method required shall be identified from either
Standard Methods (Anon, 1998) and/or ISO 5667 Part 3 All preservation carried out should be
accurately recorded in order that the analyst is aware of the preservative used. This could take
time to implement fully as the sampler’s workload is increased, particularly in relation to the
increased number of samples to be taken and associated preparatory work.
C.A. No. 2 relates to ascertaining the need to preserve samples during the collection of
composite samples and if required implementing an appropriate preservation system. To
determine whether the above is required would involve taking a number of samples with and
without preservatives and determining statistically if there is a difference. The laboratory
currently does not have the resources in terms of staff/ time to carry this out and hence the time
scale for implementation would be long term.
C.A. No. 3 requires that a method be documented and implemented for ensuring that the
preservative used does not result in dilution of the analyte or interfere with the subsequent
analysis, thereby influencing the final result. This would have to be considered in conjunction
with C.A. No. 1 as the preservation methods are not yet documented or implemented. This C.A.
could be implemented in the medium term.
C.A. No. 4 requires that a procedure be developed, documented and implemented to verify
whether or not the preservation suggestions in ISO 5667 are suitable for the sample for which it
is to be used. As the efficiency of the preservation process depends on the constituents to be
analysed, their levels and on the nature of the sample, it shall be necessary to examine the
preservation suggestions in Table 1 to 5 of ISO 5667-3:1994 for each type of sample. This
would involve a significant amount of work and could only be implemented in the long term,
provided there are adequate resources.
56
Table 3.5: An assessment of the ability of Limerick County Council’s Environmental Laboratory to implement the proposed corrective actions
in relation to drinking water sampling.
Note: More detailed information with regard to :hese corrective actions are contained in Appendix D
Corrective Action Are the Proposed time Cost of Staff Comments
(Standard Ref.) facilities/ scale for implementation: training:
resources implementation: High/ Medium/ on-site/
available Short/Medium/ Low off-site?
Long term
L
(a) Map drinking water locations and Yes Short Low N/A - Currently done as part of EC
predetermined sampling points for the (Drinking Water)
various water supplies. (ISO 5667-1:1980 Regulations, 2000
Section 1 (3), Section 2 (8.2)),(IS05667- - Slow process as there are
5:1999 (4.1.4)). currently 42 Public Water
(b) Amend sampling programme to include Supplies and 84 Group
details on how the various drinking water Water Supplies in Co.
sampling points are selected. (ISO 5667- Limerick.
1:1980 Section 2 (9.8.1))
2.
Amend SOP 6 to include details regarding; Short Low On-site
a) selection of drinking water sampling taps,
stating that “anti-splash or similar devices
should be removed before sampling and
that mixer taps are not recommended for
sampling”. (ISO 5667-1:1980 Section 2
(9.8.1), (9.8.3)), (ISOS667-5:1999 (4.1.5).
b) sampling in areas of low flow and
avoiding disturbance of sedimentary
material. (IS05667-5:1999 (4.1.4))
Table 3.5 (ctd.)
Corrective Action Are the Proposed time Cost of Staff Comments
(Standard Ref.) facilities/ scale for implementation: training:
resources implementation: High/ Medium/ on-site/
available Short/Medium/ Low off-site?
Long term.
2 ictd.)
c) flushing for extended periods prior to Yes Short Low On-site
sampling from stagnant systems.
(ISO5667-5:1999 (5.3)). '
d) the exact type of sampling container that is
to be used for each parameter. (ISO 5667-
2:1991 (6.1.1)), (ISO 5667-3:1994 (3.2.2),
(3.2.3.2), (3.2.3.3))
e) cleaning and preparation of the sampling
containers used for each parameter. (ISO
5667-3:1994 (3.2.3.1) (3.2.3.2) (3.2.3.3))
f) calibration/checking of field meters prior
to sampling. (ISO 5667-14:1998 (5.1))
g) volume of sample that is to be collected for
the various parameters. (ISO 5667-2:1991
(6.3.1)) (ISO5667-5:1999 (7.1)).
h) sampling large volumes e.g. for
Cryptosporidium analysis. (ISO 5667-
2:1991(4.7))
i) minimum sample bottle capacity of 300ml
(IS05667-5:1999 (5.3))
j) filling and sealing of sample container
(ISO 5667-3:1994 (3.2.1), (3.2.2)),
(ISO5667-5:1999 (5.1), (5.3), (7.2))
'V i
00
Table 3.5 (ctd.)
Corrective Action Are the Proposed time Cost of Staff Comments
(Standard Réf.) facilities/ scale for implementation: training:
resources implementation: High/ Medium/ on-site/
available Short/Medium/ Low off-site?
Long term.
2 (ctd.)
k) parameters, which are measured on site.
(ISO 5667-2:1991 (4.1)), (ISO 5667-
3:1994 (3.1)), (ISO 5667-14:1998 (6))
(ISO5667-5:1999 (4.1)).
1) the taking, preservation and analyses of
blank samples. (ISO 5667-3:1994 (3.2.2)),
(ISO5667-5.1999 (9)).
m) the requirement to complete the field sheet
(ISO 5667-2:1991 (7.1)), (ISO
5667-3:1994 (4),(IS05667-5:199 (8))
n) sealing samples and transportation of
samples to laboratory (ISO 5667-2:1991
(6.2.4)), (ISO 5667-3:1994 (3.1), (3.2.4),
(5)), (ISO 5667-14:1998 (5.1),(6)),
(ISO5667-5.1999 (7.2))
o) prompt storage of samples in refrigerator in
cases where immediate analyses is not
being carried out (ISO 5667-3:1994 (6)).
p) safety precautions required with reference
to the Safety Statement for the
Environment Section (ISO 5667-1:1980
Section 2 (7.1)), (IS 0 5 6 6 7 -5 :1999 ( 6 ))
3.
Assess the need to use a flexible inert tube, to Yes Medium Low On-site - An accurate assessment
deliver liquid to the bottom of the sampling would have to be based on
bottle, when sampling from a tap or pump a large number of samples.
Table 3.5 (ctd.)
Corrective Action Are the Proposed time Cost of Staff Comments
(Standard Ref.) facilities/ scale for implementation: training:
resources implementation: High/ Medium/ on-site/
available Short/Medium/ Low off-site?
Long term.
3. (ctd.)
outlet. (ISO 5667-2:1991 (6.7)) Must address the
possibility of cross
contamination by repeat
use of the tube.
4.
Asses need to disinfect using a chlorine Yes Medium Low On-site Refer to Standard Methods
solution versus alcohol (which is currently and other relevant
being used). Amend SOP if necessary. published documentation.
(IS05667-5:1999 (4.1.5))
L
Develop, document and implement method of Yes Short Low On-site May be a safety risk in
on-site analysis of odour and taste. tasting samples on-site, as
(1S05667-5:1999 (4.1)) the quality of water is
unknown.
6.
Develop, document and implement procedure Yes Short Low On-site - Necessary for compliance
for: with EC (Drinking Water)
a) sampling from water treatment plants. Regulations 2000.
(ISO5667-5.1999 (4.1.2)); reservoirs (ISO
5667-1:1980 Section 2 (9.5), (9.8.2)),
(IS05667-5:1999 (4.1.1)) and hydrants.
(IS05667-5:1999 (4.1.4))
b) assessing efficiency of disinfection plant.
(IS05667-5:1999 (4.1.3))
c) investigating dissolution of materials from
ON
o
Table 3.5 (ctd.)
Corrective Action Are the Proposed time Cost of Staff Comments
(Standard Ref.) facilities/ scale for implementation: training:
resources implementation: High/ Medium/ on-site/
available Short/Medium/ Low off-site?
Long term
6 . (ctd.)
from pipework or growth of
microorganisms within pipework.
(IS05667-5:1999 (4.1.4), (4.1.5))
d) sampling during abnormal conditions i.e.
drinking water contamination, and the
subsequent reporting of these results. (ISO
5667-1:1980 Section 3 (17)), (ISO 5667-
14:1998 (8)).
e) selection and purchase of sampling
containers (for microbiolgical, physical
and chemical analysis). Include details on
cap types to be used for the various
parameters. (ISO 5667-2:1991 (6.1.1),
(6.2.1), (6.2.3), (6.2.4), (6.5))
7.
Develop, document and implement SOP Yes Short Low On-site - Blank /known samples are
detailing how bottles are to be sterilized and a run with each batch of
method to assess if the sampling container microbiological samples in
materials used produce or release chemicals. the same type of sampling
(ISO5667-5:1999 (5.3)) container. If the sample
container were releasing
chemicals this would affect
microbiological count.
8 ,
Identify and document samples (a) with which Yes Short Low On-site
contact with the air must be avoided and
Table 3.5 (ctd.)
Corrective Action Are the Proposed time Cost of Staff Comments
(Standard Réf.) facilities/ scale for implementation: training:
resources implementation: High/ Medium/ on-site/
available Short/Medium/ Low off-site?
Long term
8 . (ctd.)
(b) that require vigorous mixing before taking
portions for analyses. Document procedure for
dealing with both types of samples. (IS05667-
5:1999 (7.2))
9.
Identify samples that require to be filtered/ Yes Medium Medium On-site - Document samples to be
centrifuged at the time of taking the sample or filtered/ centrifuged and
immediately afterwards. Implement procedure method for same
for filtration/ centrifuging of samples. (ISO - Document which samples are
5667-3:1994 (3.2.5)), (IS05667-5:1999 (7.2)) filtered/centrifuged and how
it was carried out
1 0 .
Amend SOP No. 43 to include details on the Yes Short Low On-site
max. length of sample storage for the various
analyses, making reference to guidelines in
Standard Methods (Anon. 20thEd.).
(ISO 5667-3:1994 (3.1))
IL
Amend field sheet to include details on Yes Short Low On-site
weather conditions, unusual observations and
information on samples taken for a specific
reason. (ISO 5667-1:1980 Section 2 (8.13)),
(ISO 5667-2:1991 (7.2), ISO 5667-3:1994 (4)),
(ISO566 7-5:1999 (8))
ON
K>
C.A. No. 1 requires the mapping of drinking water sampling locations for the various water
supplies within the county. Details should be included in the sampling programme as to how the
various drinking water sampling points were selected. Mapping of the various water sampling
locations is currently being undertaken at LCC in order to comply with the EPA implementation
handbook on the EC (Drinking Water) Regulations, 2000. This is a slow process as there are
currently 42 Public Water Supplies and 84 Group Water Supplies in Co. Limerick.
At present, LCC’s drinking water sampling SOP (SOP 6) does not contain sufficient detail to
meet the requirements of ISO 5667. C.A. No. 2 requires the inclusion, in SOP 6, of specific
details on correct sampling equipment, sampling procedures, in-situ monitoring, sample
preservation, completion of field report forms and sample storage and transportation.
In relation to sampling equipment, details must be included on the type of container to be used
for various samples and the type of treatment required of these containers prior to sampling.
This information is available in both ISO 5667 Part 3 and Standard Methods (Anon., 1998) and
therefore can be readily collated. Detailed instructions must also be included in SOP 6 in
relation to correct procedures to be followed prior to taking a drinking water sample e.g.
adequate flushing of stagnant systems, avoidance of mixer taps, removal of anti-splash devices.
These procedures are currently being used by LCC environmental samplers and therefore merely
require the incorporation of relevant details into the SOP. Details on the actual sampling process
itself (e.g. sample volume to be taken for various parameters), preservation of samples (if
required) and sealing of sample container must also be included in SOP 6 in order to fulfil ISO
5667 requirements.
Current practice at LCC is to take a 250ml sample for microbiological analyses and a 500ml
sample for all other analyses. Sodium thiosulphate is added to microbiological sample
containers prior to sterilisation in order to neutralise any effect of chlorine during transit, other
samples are not preserved. The samples requiring preservation need to be identified and an
appropriate method(s) implemented. As information with regard to the above is readily
available, the above can be documented in the short term. The implementation of a
comprehensive preservation programme may take somewhat longer due to the increased
workload on the sampler.
63
Certain unstable parameters must be measured in-situ when monitoring drinking water quality
otherwise the result obtained will not be representative. Currently, LCC samplers monitor pH,
temperature, conductivity and total and free chlorine at the sampling site. Some of these
parameters are omitted in the current SOP and therefore this must be amended. This can easily
be done in the short term. Details must also be included in SOP No. 6 on the way in which field
meters are checked/calibrated prior to use. LCC environmental samplers transport all drinking
water samples from the sampling location to the laboratory in a cooler box. On arrival to the
laboratory, samples not undergoing immediate analysis are stored in a refrigerator. SOP No. 6
needs to be amended to incorporate these details.
C.A. No. 3 deals with assessing the need to use a flexible inert tube, to deliver liquid to the
bottom of the sampling bottle, when sampling from a tap or pump outlet. ISO 5667 Part 2
recommends this is done to ensure that liquid is displaced from the bottom of the bottle thereby
minimising aeration. In order to assess if the above is required a large number of samples would
have to be analysed from samples taken with and without the use of tubing. The possibility of
cross contamination by repeat use of the tube would also have to be addressed. If flexible inert
tubes were to be used the cost incurred would be minimal however, the sampling rate would be
decreased.
ISO 5667 Part 5 states that plastic taps should be disinfected using an available chlorine solution.
LCC sampling staff currently use 90% isopropanol alcohol to sterilise taps. C.A. No. 4 deals
with the need to assess the current practice of disinfection using alcohol versus the requirement
of ISO 5667 to disinfect using a chlorine solution. Standard methods and other relevant
published documentation would have to be consulted in order to determine the above.
C.A. No. 5 requires that a method be documented and implemented for the on-site analysis of
odour and taste. A safety risk may be posed in tasting samples on-site, as the quality is unknown
at this stage. This would have to be taken into account prior to documenting or implementing a
procedure.
C.A. No. 6 requires that procedures be documented and implemented for a number of different
situations. These include sampling from water treatment plants, reservoirs, hydrants and also
sampling during abnormal conditions. Procedures must also be developed , documented and
implemented to investigate the dissolution of materials from pipework and also the growth of
64
materials within the pipework. These requirements are also necessary for compliance with the
EC (Drinking Water) Regulations 2000 and therefore will most likely be implemented in the
short term.
C.A. No. 7 requires that a SOP be documented and implemented to include details on how
bottles are to be sterilized. The SOP should include details on how the sampling container
material used is assessed in order to determine whether it produces or releases chemicals.
Current practice at LCC is to run blank and known samples with each batch of microbiological
samples in the same type of sampling container as the sample in order to determine whether
materials are released from the container. As this procedure is currently in place within the
laboratory, the SOP can be documented in the short term and at no additional cost to the
laboratory.
C.A. No. 8 requires the identification and documentation of samples types for which contact with
air must be avoided and those that require vigorous mixing before taking portions for analyses.
If contact of the sample with air has to be avoided the sample container should be filled
completely and then immediately stoppered. If samples require vigorous mixing before taking
portions for analyses, the sample container should not be filled completely. If air has to be
excluded a few pieces of clean, sterile, inert solids should be placed in the sampling container.
The above types of samples should be identified and an appropriate procedure documented and
implemented. This corrective action can be implemented in the short term at a relatively low
cost as these types of samples can be readily identified and an appropriate procedure
implemented
C.A. No. 9 requires the identification of drinking water samples that need to be
filtered/centrifuged at the time of taking the sample or immediately afterwards. A procedure for
the filtration/ centrifuging of these samples will then have to be implemented and details on how
the specific samples are filtered/centrifuged recorded. Drinking water samples are not currently
filtered/centrifuged at the time of sampling by LCC staff. This corrective action could take some
time to implement and incur a medium cost in purchasing the required consumables.
SOP No. 43 deals with the handling of test samples on arrival to the laboratory and states that
samples are to be stored in the appropriate fridge until analysis is complete. C.A. No. 10 requires
that SOP No. 43 is amended to include details on the maximum time allowable for sample
65
storage for each of the parameters of interest. Details regarding maximum sample storage can be
obtained from Standard Methods (Anon. 1998).
C.A. No. 11 requires that the existing field report sheet be amended to include details on the
weather conditions and any unusual observations noted at the time of sampling. In addition the
field report sheet should be amended to provide information on samples taken for a specific
reason (e.g. determination of compliance of drinking water with specific Regulations or
contamination investigation). This corrective action can be implemented in the short term at a
relatively low cost.
C.A. No. 2 requires that an appropriate method be identified to assess stratification at each river
sampling location. As in-house expertise is not available to assess stratification, a high cost
would be incurred in engaging the services of external consultant, particularly as there are a large
number of sampling sites to be assessed. This assessment could only be carried out in the long
term when adequate funding is secured.
66
Table 3.6: An assessm ent o f the ability o f Lim erick County C ouncil’s Environm ental Laboratory to im plem ent the proposed corrective
actions in relation to river w ater sampling.
Note: More detailed information with regard to these corrective actions are contained in Appendix D
Corrective Action Are the Proposed time Cost of Staff Comments
(Standard Ref.) facilities/ scale for implementation training:
resources implementation High/ Medium/ on-site/off-
available Short/Medium/ Low site?
Long term
L
Reassess river sampling locations to: Yes Long. Low N/A Time scale is ‘Long’
a) take flow stations into account. because the river sampling
(ISO 5667-1:1980 Section 2 (8.1)) programme for this year
b) ensure they provide representative samples has already been initiated
by taking into account locations where Sampling points must be
marked quality changes are likely to occur accessible all year round.
or locations where there are important river Ensure sampling personnel
uses. (ISO 5667-1:1980 Section 2 (9.3.2)) can carry out sampling
using existing resources.
- Amend sampling
programmes accordingly.
2 .
Identify appropriate method to assess each No Long High Off-site In-house expertise not
river sampling location for stratification and available to assess
take appropriate measures following the results stratification
of this assessment. (ISO 5667-1:1980 Section May be considered under
2 (9.3.1)) the Water Framework
Directive (WFD)
3.
Identify and document an appropriate method No Long High Off-site Identify and document how
to assess the effects of a discharge on a river the relevant points will be
by selecting representative upstream and selected.
downstream locations. (Note: the discharge
O
-4
'
Table 3.6 (ctd.)
Corrective Action Are the Proposed time Cost of Staff Comments
(Standard Ref.) facilities/ scale for implementation training:
resources implementation: High/ Medium/ on-site/off-
available Short/Medium/ Low site?
Long term
3. (ctd.)
may be a wastewater discharge or an adjoining No Long High Off-site - May be considered under
tributary). (ISO 5667-1:1980 Section 2 the WFD
(9.3.2)), (ISO 5667-6:1990 (5.1.1.1)).
4.
Amend SOPs No. 8 and 47 to include details Yes Short Low On-site
of the:
a) safety precautions necessary when
sampling from rivers, with reference to
‘Safety Statement for the Environment
Section’. (ISO 5667-1:1980 Section 2
(7.1)), (ISO 5667-6:1990 (6)).
b) measures required to ensure the sampling
location is safe prior to commencing
sampling. (ISO 5667-1:1980 Section 2
(7.4))
c) calibration/ checking of field meters prior
to sampling. (ISO 5667-14:1998 (5.1))
d) sampling equipment to be used (ISO 5667-
6:1990 (4.2)).
e) type of sampling container that is to be
used for each parameter. (ISO 5667-2:1991
(6.1.1)), (ISO 5667-3:1994 (3.2.2),
(3.2.3.2), (3.2.3.3), (ISO 5667-6:1990
(4.1)).
f) cleaning and preparation of the sampling
containers used for each parameter.
SC
ON
Table 3.6 (ctd.)
Corrective Action Are the Proposed time Cost of Staff Comments
(Standard Réf.) facilities/ scale for implementation training:
resources implementation: High/ Medium/ on-site/off-
available Short/Medium/ Low site?
Long term
4. (ctd.)
(ISO 5667-3:1994 (3.2.3.1) (3.2.3.2)
(3.2.3.3))
g) when the sampling of surface films is
required and when it should be avoided.
(ISO 5667-6:1990 (5.3.1)).
h) when sample containers can/cannot be pre
rinsed. (ISO 5667-6:1990 (5.4)).
i) volume of sample to be collected for
various parameters (ISO 5667-2:1991
(6.3.1))
j) filling and sealing of sample container(s)
(ISO 5667-3:1994 (3.2.1), (3.2.2)),
k) parameters which are to be measured and
recorded on site. (ISO 5667-2:1991 (4.1),
ISO 5667-3:1994 (3.1), ISO 5667-6:1990
(5.4), ISO 5667-14:1998 (6)).
1) taking, preservation and analyses of blank
samples.(ZSO 5667-3:1994 (3.2.2).
m) labelling of sampling bottles and
completion of the field sheet. (ISO 5667-
2:1991 (7.1)), (ISO 5667-3:1994 (4)), (ISO
5667-6:1990 (7)).
n) sample transportation and the sealing of
sampling containers. (ISO 5667-2:1991
(6.2.4)), (ISO 5667-3:1994 (3.1), (3.2.4),
(5)), (ISO 5667-6:1990 (5.4)),
Os
SC
Table 3.6 (ctd.)
Corrective Action Are the Proposed time Cost of Staff Comments
(Standard Ref.) facilities/ scale for implementation training:
resources implementation: High/ Medium/ on-site/off-
available Short/Medium/ Low site?
Long term
4. (ctd.)
(ISO 5667-14:1998 (5.1), (6))
o) storage of samples in a refrigerator on
arrival to the laboratory, where immediate
analyses is not being carried out (ISO
5667-3:1994 (6)).
5.
Amend SOP No. 47 to include details on: Yes Short Low On-site
a) the type of sampling containers to be used
for microbiological samples and
preparation of same
b) how microbiological samples are to be
taken. (ISO 5667-6:1990 (4.2), (5.3.2))
6.
Develop appropriate field report sheet for Yes Short Low On-site
sampling rivers and surface water used for
abstraction. ISO 5667-1:1980 Section 2
(8.13)), (ISO 5667-2:1991 (7.2)), (ISO 5667-
3:1994 (4)), (ISO 5667-6:1990 (7)).
7.
Identify the samples which require to be Yes Medium Medium On-site - Document the samples which
filtered/centrifuged at the time of taking the require to be filtered/
sample or immediately afterwards. Implement centrifuged and the
a procedure for the filtration/ centrifuging of appropriate method to be
these samples. (ISO 5667-3:1994 (3.2.5)), used.
(IS05667-6:1990 (5.4)) - Purchase required
consumables.
Table 3.6 (ctd.)
Corrective Action Are the Proposed time Cost of Staff Comments
(Standard Réf.) facilities/ scale for implementation: training:
resources implementation: High/ Medium/ on-site/off-
available Short/Medium/ Low site?
Long term.
7. (ctd.) Document, which samples
are filtered/centrifuged and
how it was carried out
8 .
Document and implement procedures for Yes Short Low N/A - Ensure personnel responsible
the selection of effective samplers (ISO 5667- for purchasing laboratory
2:1991 (6.3.1)) and containers. Include details goods are aware of the
on the cap types to be used for the various sampling container and
parameters. (ISO 5667-2:1991 (6.1.1), (6.2.1), sampler types to be
(6.2.3), (6.2.4), (6.5)). purchased.
9.
Identify abnormal sampling situations (e.g. Yes Short Medium On-site - Identify and document
flood conditions in a river or times of an algal possible abnormal
bloom). Prepare SOP detailing the procedure conditions and the sampling
for sampling during these conditions and the requirements for each.
subsequent reporting of these results. (ISO - Purchase appropriate
5667-1:1980 Section 3 (17), ISO 5667- sampling containers and
14:1998 (8)). preservatives.
1 0 .
Assess whether an accurate determination of Yes Short Unknown On-site If D O readings must be
dissolved oxygen (D O.) is required i.e. a taken in the waterbody then
measurement of D O. taken directly in the new DO probes will have
water-body as opposed to the current practice to be purchased, which
of measuring D O. in the sampling bucket. shall incur a high cost.
(ISO 5667-2:1991 (6.7)) Sampling time will be
increased as probes have to
be extended from bridge.
Table 3.6 (ctd.)
Corrective Action Are the Proposed time Cost of Staff Comments
(Standard Ref.) facilities/ scale for implementation: training:
resources implementation: High/ Medium/ on-site/off-
available Short/Medium/ Low site?
Long term
IL
Assess the need to ascertain the time-of-travel No Long High Off-site - External resources required,
of pollutants in rivers. If required identify, as in-house expertise not
document and implement method for assessing available.
the time-of-travel of pollutants in rivers. (ISO - May be considered under the
5667-6:1990 (5.1.1.2)) WFD
IL
Determine the possibility of a non- No. Long High Off-site - External resources required,
homogeneous distribution of determinands of as in-house expertise not
interest at the various sampling sites. Identify, available.
document and implement method for assessing - May be considered under the
same ISO 5667-6:1990 (5.1.2) WFD
13.
Amend SOP No. 43 to include details on the Yes Short Low On-site
max. length of sample storage for the various
analyses (ISO 5667-3:1994 (3.1))
C.A. No. 3 requires that an appropriate method be identified and documented to assess the
effects of a discharge (wastewater discharge or an adjoining tributary) on a river by selecting
representative upstream and downstream locations. The distance over which the discharges
mixes in the vertical, lateral and longitudinal dimensions need to be considered in the selection
of sampling sites. Therefore the physical characteristics, water velocity and physico-chemical
parameters of the water body need to be taken into account. In-house expertise is not available
to assess all of the above accurately thus a high cost would be incurred in employing external
consultants. This could only be carried out in the long-term when adequate funding is secured.
C.A. No. 4 deals with the amendments which are required to the current laboratory river
sampling SOPs (SOP No. 8 and 47) to meet the requirements of ISO 5667. A significant
number of these amendments involve the documentation of procedures which are currently being
carried out. For example, the calibration and checking of field meters prior to sampling, the
monitoring of parameters in-situ, the recording of monitoring results and sample details on a
field sheet and the transportation of samples to the laboratory in cooler boxes. Other
amendments involve the documentation and implementation of measures which are not currently
being carried out correctly. For example, documenting the correct type of sampling container(s)
to be used, the preparation and cleaning of sampling containers, the volume of sample that is to
be collected for the various parameters, the filling and sealing of sample containers, details on
when the sampling of surface films is required and when it should be avoided and the safety
precautions required when sampling. As this information is readily available, both in ISO 5667
and Standard Methods (Anon., 1998) this corrective action can be implemented in the short term
at a low cost to the laboratory.
C.A. No. 5 deals with the amendments that are required to SOP No.47 (sampling of surface
water for abstraction of waters intended for human consumption) with regard to microbiological
sampling. The amendments required include documentation of the type of sample container to
be used and preparation of same and also details on how microbiological samples are to be taken.
As this corrective action involves the amendment of an existing SOP to include procedures
which are currently being carried out it can be implemented in the short term at a low cost to the
laboratory.
C.A. No. 6 requires that an appropriate field report sheet be developed as per ISO 5667 for
sampling rivers and also for sampling surface waters used for the abstraction of drinking water.
73
This involves the amendment of the current river sampling field report sheet and the
development of an appropriate field report sheet for sampling of surface water used for
abstraction of drinking water. This corrective action can be implemented in the short term at a
low cost to the laboratory.
C.A. No. 7 deals with the requirement to filter/centrifuge samples at the time of taking the
sample or immediately afterwards. This C.A. has been dealt with previously in Section 3.2.4.
C.A. No. 8 requires that procedures be documented and implemented with regard to the selection
of effective samplers and sampling containers. Laboratory personnel responsible for purchasing
laboratory goods should be aware of the sampler and container types to be purchased. Firstly,
this involves identifying the correct type of samplers and sampling containers that have to be
purchased and then documenting the findings. As this information is readily available, this
corrective action can be implemented in the short term at a low cost to the laboratory.
C.A. No. 9 requires that abnormal sampling situations are identified e.g. flood conditions in a
river or times of an algal bloom. Once identified, an SOP detailing the procedure for sampling
during these conditions shall have to be documented. This would be best documented in a
separate SOP with a reference made to it in SOP No. 8 and 47. The SOP must include details
regarding the reporting of results obtained during abnormal sampling conditions. Abnormal
sampling situations can be identified and an appropriate SOP documented in the short term
however, the implementation time of this C.A will be dependant on the sampling equipment and
the analysis required. If the facilities are available in-house the procedures can be documented
in the short term.
74
high cost on the laboratory. The rate of sampling would also be slowed down as it would take
longer to measure the D O. directly in the water-body as the D O. probe particularly when
extending the D O. probe from large bridges
The time-of-travel of pollutants will primarily depend on the type of pollutant, the characteristics
of the water body and the mixing conditions. Determining the time-of-travel of pollutants
involves the use of tracers or measurement of flow with knowledge of cross-sectional areas. C. A.
No. 11 deals with the need to assess whether the time-of-travel of pollutants in rivers needs to be
ascertained. This may be necessary where certain constituents or pollutants are being traced
through a system or where the rate of change of unstable constituents is being investigated (e.g.
in the self-purification of a water body the time-of-travel can provide information on kinetic rate
co-efficients). As in-house expertise is not available to determine the above, external consultants
would be required thereby incurring a high cost.
C.A. No. 12 deals with the need to determine the possibility of a non-homogeneous distribution
of the determinands of interest at the various sampling sites. As in-house expertise are not
available to determine this, external consultants would be required thereby incurring a high cost
particularly as each sampling site shall have to be assessed. If a non-homogeneous distribution
of the determinands of interest is identified a method shall have to be developed and documented
to take this into account. Again, external consultants would be required to develop the most
appropriate method. Bearing these factors in mind, this corrective action could only be
implemented in the long term.
C.A. No. 13 requires that SOP No. 43 is amended to include details on the maximum time
allowable for sample storage for each of the parameters of interest. Details regarding maximum
sample storage can be obtained from Standard Methods (Anon. 1998).
75
Table 3.7: An assessm ent o f the ability o f Lim erick C ounty C ouncil’s Environm ental Laboratory to im plem ent the proposed corrective actions
in relation to w astewater sampling.
Corrective Action Are the Proposed time Cost of Staff training Com ments
(Standard Ref.) facilities/ scale for im plem entation: on-site/
resources im plem entation: H igh/M edium / off-site?
available Short/M edium / Low
Long term.
L
a) Review wastewater sampling locations to No Long High N/A The implementation of this
ensure sufficient turbulence is present at all Corrective Action would
sites. (ISO 5667-1:1980 Section 2 (8.9)), require external expertise
(ISO 5667-10:1992 (5.1.2)) to determine whether there
b) Identify sampling points where incomplete is sufficient turbulence at
mixing of wastewaters exists due to low the various sampling
flow rates or mixing of wastewaters from locations.
different sources. (ISO 5667-1:1980
Section 2 (12.1.1))
2 .
Identify, document and implement measures to No Long High N/A The implementation of this
overcome or minimize heterogeneity caused CA would require external
by suspended solids and/or thermal expertise to identify,
stratification in wastewater streams. document and implement
(ISO 5667-10:1992 (5.1.3)) the appropriate measures.
3.
Identify and document when and how Yes Short Low On-site - Purchase the required
emulsified and floating material are to be sampling equipment and
sampled. (ISO 5667-10:1992 (5.1.4), ISO containers, if required.
5667-1:1980 Section 2 (12.1.1))
4.
Identify and document exact sampling points
used;
Table 3.7 (ctd.)
Corrective Action Are the Proposed time Cost of Staff training Com ments
(Standard Ref.) facilities/ scale for im plem entation: on-site/
resources im plem entation: H igh/M edium / off-site?
available Short/M edium / Low
Long term.
4. (ctd.t
a) for influent and effluent at all wastewater Yes Short Low On-site Train sampling personnel
plants routinely sampled. (ISO 5667- to ensure samples are
10:1992 (5.1.3)), (ISO 5667-1:1980 always taken at the exact
Section 2 (12.1.1)) same location.
b) to extract samples from aeration tanks in a
wastewater treatment plant. (ISO 5667-
1:1980 Section 3 (19.2))
5.
Develop, document and implement system for Yes Short Low On-site Document the reviews
frequently reviewing the plant’s sampling carried out on the plant’s
locations. (ISO 5667-10:1992 (5.1.3)) sampling locations
6 .
Prepare SOP for sampling of storm sewage Yes Short Low On-site
and surface run-off taking into account the
guidelines provided in ISO 5667-1:1980
Section 2 (13).
7.
Amend SOPs 10 & 11 to include details on.
a) Calibration/checking of field meters prior
to sampling. (ISO 5667-14:1998 (5.1))
b) Cleaning/preparation of the sampling
containers and equipment. (ISO 5667-
3:1994 (3.2.3.1) (3.2.3.2) (3.2.3.3), ISO
5667-10:1992 (4.2.1))
c) sample container type to be used for
various analyses. (ISO 5667-2:1991
Table 3.7 (ctd.)
Corrective Action Are the Proposed time Cost of Staff training Com ments
(Standard Réf.) facilities/ scale for im plem entation: on-site/
resources im plem entation: H igh/M edium / off-site?
available Short/M edium / Low
Long term
7. (ctd.)
(6.1.1)), (ISO 5667-3:1994 (3.2.2), Yes Short Low On-site
(3.2.3.2), (3.2.3.3)), (ISO 5667-10:1992
(4.1))
d) taking of samples and filling of sampling
containers (ISO 5667-3:1994 (3.2.1),
(3.2.2), (ISO 5667-10:1992 (4.2.1))
e) sample volume required for the various
analyses. (ISO 5667-2:1991 (6.3.1)) (ISO
5667-10:1992 (4.2.1))
f) the depth at which the samples should be
taken e.g. one-third of the effluent water
depth below the surface of the water.
(ISO 5667-10:1992 (5.1.2))
g) handling corrosive or abrasive liquids.
(ISO 5667-1:1980 Section 2 (8.7))
h) parameters measured on site.
(ISO 5667-2:1991 (4.1)), (ISO 5667-3; 1994
(3.1)), (ISO 5667-14:1998 (6))
i) preservation and storage of samples.
(ISO 5667-10:1992 (5.4))
j) taking, preservation and analyses of blank
samples. (ISO 5667-3:1994 (3.2.2)
k) the requirement to complete field sheet
(ISO 5667-2:1991 (7.1)), (ISO 5667-
3:1994 (4).
Table 3.7 (ctd.)
C orrective Action Are the Proposed time Cost of Staff training Com m ents
(Standard Réf.) facilities/ scale for im plem entation: on-site/
resources im plem entation: H igh/M edium / off-site?
available Short/M edium / Low
Long term.
7. tctd.i
1) the sealing and transportation of samples to
the laboratory (ISO 5667-2:1991 (6.2.4),
ISO 5667-3:1994 (3.1), (3.2.4), (5), ISO
5667-14:1998 (5.1),(6),
m) storage of samples in a refrigerator, on
arrival to the laboratory, where immediate
analyses is not being carried out (ISO
5667-3:1994 (6)).
n) safety precautions necessary (include
details from Laboratory Safety Statement
CISO 5667-1:1980 Section 2(7.1))
8.
Develop, document and implement sampling Yes Short Low On-site
report form for STP and industrial wastewater
sampling as per ISO 5667. (ISO 5667-1:1980
Section 2 (8.13), ISO 5667-2:1991 (7.2), ISO
5667-3:1994 (4)), (ISO 5667-10:1992 (7))
9.
Identify and document whether sampling No Medium Low On-site The implementation of this
locations require to be cleaned (to remove corrective action would
scale, sludge, bacterial film etc. from the require;
walls) prior to sampling and detail how Reassessment of each
cleaning is to be carried out. sampling location to be
(ISO 5667-10:1992 (5.1.2)) reassessed
Identification of an
effective method of
Table 3.7 (ctd.)
C orrective Action Are the Proposed time Cost of Staff training Com ments
(Standard Ref.) facilities/ scale for im plem entation: on-site/
resources im plem entation: H igh/M edium / off-site?
available Short/M edium / Low
Long term
9. ictd.)
cleaning be identified
Access to a water supply
- Documentation of cleaning
procedure
1 0 ,
Assess the need to use a flexible inert tube, to Yes Medium Low On-site Assessment would have to
deliver liquid to the bottom of the sampling be based on a large number
bottle, when sampling from a tap or pump of samples.
outlet. (ISO 5667-2:1991 (6.7)) The possibility of cross
contamination by repeat
use of the tube would have
to be addressed.
J_L
Identify the samples which require to be Yes Medium Medium On-site Document the samples
filtered/centrifuged at the time of taking the which require to be
sample or immediately afterwards. Implement filtered/ centrifuged.
a procedure for the filtration/ centrifuging of - Document method for
these samples. (ISO 5667-3:1994 (3.2.5). filtering and centrifuging.
- Purchase the required
consumables.
Document, which samples
are filtered/centrifuged and
how it was carried out ie
type of filter and filter pore
size.
T a b le 3 .7 (c td .)
Corrective Action Are the Proposed time Cost o f Staff training Com ments
(Standard Ref.) facilities/ scale for im plem entation: on-site/
resources implementation: H igh/M edium / off-site?
available Short/M edium / Low
Long term.
1 2 1
to
00
Table 3.7 (ctd.)
Corrective Action Are the Proposed time Cost of Staff training Com m ents
(Standard Ref.) facilities/ scale for im plem entation: on-site/
resources im plem entation: H igh/M edium / off-site?
available Short/M edium / Low
Long term.
Develop and document procedure for the Yes Long Low On-site Shall depend on outcome
taking of composite samples, including the of Points 16-18 above.
type of composite sample and details on the
volumes to be taken. (ISO 5667-10:1992
(5.3.1.2))
2 0 .
Implement a procedure for: Yes Medium High - Need to identify what
dealing with samples of anomalous anomalous material may
material arise and document
identifying hazardous materials procedure for dealing with
(ISO 5667-3:1994 (4)) same.
Identify protocol for
dealing with hazardous
material, if need arises.
2 L
a) Identify areas where a site inspection may No Long High Off-site Applicable for licensed
be necessary in order to ensure the discharges to sewers
locations of the sewers and path of the Would have to form part of
waste stream correspond to the site map licence review process
drawings and the selected location is
representative for sampling purpose.
b) Develop a system of carrying out site
inspections using chemical tracer studies or
other approved method. Develop an
appropriate method to document results of
same. (ISO 5667-10:1992 (5.1.1))
00
T a b le 3 .7 (c td .)
C orrective Action Are the Proposed time Cost of Staff training Com m ents
(Standard Réf.) facilities/ scale for im plem entation: on-site/
resources im plem entation: H igh/M edium / off-site?
available Short/M edium / Low
Long term.
22.
Develop, document and implement procedure Yes Short Low On-site The implementation of this
for noting and recording conditions inside a corrective action would
licensed industrial plant prior to sampling (ISO require communication
5667-10:1992 (5.1.2)) with relevant industrial
personnel at the time of
sampling.
C.A. No. 1 requires that current wastewater sampling locations be reviewed in order to ensure
sufficient turbulence is present at all sites. Incomplete mixing of wastewaters may occur due to
low flow rates or mixing of wastewaters from different sources. This could be a particular
problem in the case of influent where wastewater may be contained in large cross-sectional
channels that slow down the rate of flow. Locations where incomplete mixing of wastewater
occurs should be identified. As in-house expertise is not available to determine whether
sufficient turbulence exists at the sampling locations, external consultants would be required.
This would incur a high cost especially as there are a large number of sites to be assessed.
Additional cost would also be incurred if any of the assessed sites had to be altered to ensure
sufficient turbulence is present.
C.A. No. 2 requires that measures be identified, documented and implemented to overcome or
minimize the heterogeneity caused by suspended solids and/or thermal stratification in
wastewater streams. Sampling sites, where heterogeneity is likely to occur, must first be
identified before appropriate measures could be identified to promote the mixing of such streams
before sampling. As in-house expertise is not available to determine the above, external
consultants would be required. This would incur a high cost especially if measures to overcome
heterogeneity had to be implemented. Therefore, the full implementation of this would be very
long-term.
C.A. No. 3 requires the identification of situations where emulsified and floating material is to be
sampled. Sampling for emulsified and floating material, such as oil and grease, is a qualitative
sampling procedure as it involves skimming the sample surface. An appropriate method must be
documented for same. Additional sampling equipment and containers may need to be purchased
e.g wide mouth jars. The cost incurred here would be low and so this corrective action could be
implemented in the short term.
C.A. No. 4 requires the identification and documentation of exact sampling points at the influent,
effluent and aeration tanks of all wastewater plants routinely sampled within the County. It is
important that the wastewater samples are always taken at the exact same sampling location in
order to allow comparisons to be made between the various results over time. C.A. No. 5
requires that a system be developed, documented and implemented for frequently reviewing the
plant’s sampling locations (as stated in C.A. No. 4). Both C.A’s No. 4 and 5 can be
implemented in the short term at a low cost.
85
C A. No. 6 requires that an SOP be prepared with regard to the sampling of storm sewage and
surface water run-off. LCC does not currently sample storm sewage or surface run-off on a
regular basis, therefore this procedure would be best documented as a separate SOP with a
reference made to it in both SOP No’s. 10 and 11. This procedure should take into account the
guidelines provided in ISO 5667-1:1980 Section 2 (13). This can be implemented in the short
term at a low cost.
C.A. No. 7 deals with the amendments which are required to the current laboratory wastewater
sampling SOPs (SOP No. 10 and 11) in order to meet the requirements of ISO 5667. A
significant number of these amendments involve the documentation of procedures, which are
currently being carried out. For example, the calibration and checking of field meters prior to
sampling, the monitoring of parameters in-situ, the recording of monitoring results and sample
details on a field sheet and the transportation of samples to the laboratory in cooler boxes. Other
amendments involve the documentation and implementation of procedures that are already in
place but do not comply fully with ISO 5667 requirements e.g. procedures relating to the use of
correct sampling equipment and containers, the preparation and cleaning of sample containers,
the filling and sealing of sampling containers (including detail on the correct sample volume to
be collected for each parameter), the handling of corrosive or abrasive liquids and the use of
safety precautions. An extensive body of information exists regarding these details, therefore
these procedures could be easily incorporated into SOP No. 10 in the short term. Some of the
amendments required shall involve the documentation and implementation of new procedures,
e.g. the preservation of samples at the time of sampling and the taking, preservation and analyses
of blank samples. The above amendments can be documented and implemented in the short
term at a low cost to the laboratory.
C.A. No. 8 requires that an appropriate field report sheet be developed for sampling wastewaters
as per ISO 5667. LCC laboratory does not currently have an appropriate field report sheet
however this can be rectified in the short term at a low cost to the laboratory.
C.A. No. 9 deals with identifying whether the walls of the various wastewater sampling locations
need to be cleaned prior to sampling in order to remove scale, sludge, bacterial film, etc. If this
is necessary then a procedure should be documented detailing how cleaning is to be carried out.
This C.A. could take a considerable period of time to implement since each sampling location
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would have to be assessed and an effective method of cleaning identified and documented
Cleaning procedures undertaken at the sampling location would slow down the rate of sampling,
particularly if the location is difficult to clean or if a readily available source of water cannot be
identified.
C.A. No. 10 deals with assessing the need to use a flexible inert tube to deliver liquid to the
bottom of the sampling bottle when sampling from a tap or pump outlet. This C.A. has been
dealt with previously in Section 3.2.4.
C.A. No. 11 deals with the requirement to filter/centrifuge samples at the time of taking the
sample or immediately afterwards. This C.A. has been dealt with previously in Section 3.2.4.
C.A. No. 12 requires that a procedure be developed, documented and implemented with regard
to the freezing and thawing of samples. This can be carried out in the short term at no additional
cost to the laboratory.
C.A. No. 13 requires that SOP No. 43 is amended to include details on the maximum time
allowable for sample storage for each of the parameters of interest. These details, which can
readily be obtained from Standard Methods (Anon. 1998), can be incorporated into the
appropriate SOP in the short term at a low cost to the laboratory.
C.A. No. 14 requires that procedures be documented and implemented with regard to the
selection of effective samplers and sampling containers for wastewater sampling. As this
involves the documentation of existing procedures, the C.A. can be implemented in the short
term at no additional cost to the laboratory.
C.A. No. 15 requires that the criteria for the selection of automatic sampling equipment be
documented. The criteria stated must take into account the relevant features and attributes stated
in ISO 5667-10:1992 (4.2.2). The criteria selected shall depend on the intended use(s) of the
automatic sampler. Current automatic samplers can then be assessed for their suitability. If the
current samplers do not meet the necessary requirements, the cost of implementing this C.A. may
be high.
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C A No. 16 requires that a method be documented and implemented for selecting the period
over which a composite sample is to be taken. The period selected should take into account the
objective of the sampling programme and the stability of the sample. This will result in a long
time-scale for implementation.
C.A. No. 17 deals with statistically determining the number of samples to be taken during each
composite sampling period. In order to do this correctly, off-site statistical training may be
required thereby increasing the cost of implementation and the length of time to achieve full
implementation.
Certain parameters can only be measured on spot samples because of the instability of the
parameter e.g. temperature and pH. C.A. No. 18 requires that parameters to be determined on
spot samples only be identified and documented. This can easily be implemented at no
additional cost to the laboratory.
C.A. No. 19 requires that a method be documented and implemented with regard to the taking of
composite samples. This should include details on the type of composite sample (i.e. time-
weighted or flow-weighted samples) and the volumes to be taken. As this procedure is
dependent on C.A. No.’s 16-18 being fully implemented, the time-scale for implementation
would be long-term.
C.A. No. 20 deals with the requirement to implement a procedure for identifying hazardous
materials and dealing with samples of anomalous material. This would involve a considerable
amount of work and time to document accurately as firstly the various types of anomalous and
hazardous material would have to be identified and only then could an appropriate procedure be
documented
C.A. No. 21 requires identification of those areas where a site inspection may be necessary in
order to ensure that (a) the locations of the sewers and path of the waste stream correspond to the
site map drawings and (b) the selected location is representative for sampling purpose. A system
for carrying out these site inspections must be developed and may consist of chemical tracer
studies or other approved methods. The results of all such inspections should be documented.
This requirement is particularly applicable to licensed discharges to sewers and would have to
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form part o f licence review process. The tim e-scale for im plem entation w ould therefore be long
term and a high cost may be incurred, particularly for larger and older premises.
C.A. No. 22 requires that a procedure be developed and im plem ented for noting and recording
conditions inside a licensed industrial plant prior to sampling the effluent discharge. This w ould
require com m unication w ith the relevant industrial personnel at the tim e o f sampling. This could
be im plem ented in the short term by amending the relevant sam pling SOP (SOP No. 11) and
associated field report sheet.
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4.0 DISCUSSION
o f the entire private laboratory sector. They are therefore not discussed as part o f this
dissertation but included for the readers inform ation in A ppendix C (Table C3). A reason for the
low response rate received from private laboratories could not be ascertained as each o f the
laboratories w ere contacted by telephone and most agreed to com plete and return the
questionnaire. The low response rate may indicate a reluctance by private laboratories to
disclose this inform ation to a potential custom er(s) for fear o f negative publicity.
M ost E PA laboratories (80% ) have personnel designated solely for sam pling (Table 3.1, Figure
3.1). LA laboratories seem to operate differently in that only 11% o f those w hich responded
have personnel designated solely for sampling. This trend is probably due to LA laboratories
covering sm aller geographical areas than E PA laboratories and subsequently having low er
laboratory staffing rates w here it would be im practical to have dedicated samplers.
72% o f L A laboratory respondents routinely sam ple rivers (Figure 3.2). A higher percentage
was expected since all LAs are required to regularly m onitor rivers in their catchm ent area in
order to assess com pliance w ith the Local G overnm ent (W ater Pollution) Act, 1977 (W ater
Q uality Standards for Phosphorus) Regulations, 1998. The low er percentage o f LA s actually
involved in river sam pling may be due to the fact that some rivers are m onitored as part o f
specific projects e.g. the Three Rivers project and the L ough R ee/ Lough D erg project. This
m onitoring is carried out by designated laboratories set up by the LA responsible for the project.
The num ber o f LA laboratories involved in river sam pling is likely to decrease further in the near
future because o f the im plem entation o f the W ater Fram ew ork Directive. U nder this D irective
river basin districts are being designated and associated laboratories are likely to be set up.
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72% o f the LA laboratories, which responded, routinely sample STPs (Figure 3.2). Again a
higher percentage would have been expected as L A ’s are required to regularly m onitor STPs in
order to assess their com pliance with the Environm ental Protection Agency Act, 1992 (Urban
W aste W ater Treatm ent) Regulations, 1994. This lower than expected percentage may be due to
the fact that in a num ber o f STPs, dedicated LA staff are responsible for the required m onitoring
at the plant These staff are assigned solely to the STP and do not form part o f the main
laboratories m onitoring programme, which were the focus o f the questionnaire.
67% o f L A ’s routinely sample industrial w astew aters (Figure 3.2). This figure w ould be
expected to vary betw een L A ’s depending on the num ber o f licensed industries under the Local
G overnm ent (W ater Pollution) Acts 1977 and 1990. M onitoring is carried out to assess if the
effluent being discharged com plies with the specified licence limits.
Just 61% o f LA laboratories, w hich responded, routinely sample drinking w aters (Figure 3.2).
Again a higher percentage would have been expected as LA s are required to regularly m onitor
drinking w aters w ithin their catchment area in order to assess com pliance w ith the European
Com m unities (Q uality o f W ater Intended for Human Consum ption) Regulations, 2000. The
low er percentage revealed in the questionnaire may be due to fact that the local H ealth Board
carry out the required monitoring in some counties.
The results obtained from the questionnaire indicate that all E PA laboratories routinely sample
industrial w astew aters and rivers (Table 3.1 and Figure 3.2) therefore indicating that the E PA is
fulfilling its regulatory roles and its role in m onitoring the quality o f the environm ent. 60% o f
EPA laboratories m onitor sewage treatment plants and drinking w ater (Figure 3.2). The
percentage o f E P A laboratories sampling STPs and drinking w aters is quite high as this
m onitoring is generally carried out by LA s and H ealth B oards w ho subsequently submit results
to the EPA.
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sam pling procedures in the laboratory. O f the laboratories, w hich replied to the questionnaire,
only 74% o f LA and 60% o fE P A laboratories have docum ented sampling procedures (Table 3.1
and Figure 3.3). Documented sampling procedures in EPA laboratories seem to be more detailed
than those in LA laboratories, particularly with regard to the type o f sampling container used and
the types o f sam ples which are to be preserved. The fact that not all laboratories have
docum ented sampling procedures in place is o f concern and raises questions with regard to how
sam pling is carried out and whether there is continuity in procedures between sam pling staff.
11% o f LA and 20% o f the EPA laboratory respondents, use ISO 5667 as a guide w hen
preparing sam pling program m es and procedures. A lthough 16% o f LA and 40% o f the EPA
respondents have considered accreditation specifically to ISO 5667 (Figure 3.12) a much low er
percentage, o f these laboratories use the standard w hen preparing sam pling procedures. This
may indicate that the standard is too com prehensive or onerous to use or it may also indicate that
these laboratories are at the initial stages o f considering accreditation to the standard and have
not begun to use the standard to prepare sampling program m es and procedures.
LA im plem entation handbooks are published by either the EPA or the D epartm ent o f the
Environm ent to give guidance to LAs with regard to the im plem entation o f specific legislation.
Details w ith regard to sampling procedures are often stated. 56% o f the LA laboratory
respondents, use these guides when preparing sam pling program m es and procedures. This low
percentage is o f concern as these publications often state specific requirem ents w ith regard to
type o f sample, sam pling location, etc. For exam ple, the 1996 E PA Im plem entation H andbook,
published to accom pany the Environmental Protection A gency Act, 1992 (Urban W aste W ater
Treatm ent) Regulations, 1994, strongly recom m ends the use o f flow -proportional sam plers for
w astew ater samples. This direction is more specific than the R egulations them selves w hich state
that either flow -proportional or time-based 24-hour sam ples can be taken. Sim ilarly the
im plem entation handbook for the European C om m unities (D rinking W ater) Regulations, 2000,
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Flanagan et al. 2003 state that drinking w ater samples taken in order to assess com pliance with
the R egulations should not be taken from outside taps. The R egulations do not state this.
Only 20% o f EPA laboratories use im plem entation handbooks w hen preparing sampling
program m es and procedures (Figure 3.3). As these handbooks are very specific to the
im plem entation o f specific legislation by LAs they w ould not, in most cases, be applicable to
EPA sam pling program m es.
3.5). These low percentages are o f concern because assurance is not dem onstrated to external
parties, that the sam pling procedure is carried out correctly or that there is continuity w ithin a
laboratory w ith regard to how samples are taken or that sam pling staff have obtained proper
training.
On-site analysis is recom m ended for pH, chlorine, dissolved oxygen, conductivity and
tem perature (A non., 1998 and ISO 5667. O f the five laboratories, w hich interpreted the question
correctly, all m easure D O, chlorine and tem perature on-site, however, only tw o m easure pH and
conductivity on-site. The failure to m onitor pH on site is o f particular concern especially in the
case o f sam ples w ith a low pH. These samples continually absorb carbon dioxide from the
atm osphere thereby resulting in a continual increase in pH during storage and/or transit (Anon.,
1998).
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4.1.6 C alibration and checking o f in-situ m onitoring equipm ent
In order to ensure accurate readings are taken in field the field m eters used should be
calibrated/checked prior to sampling (NSAI, 1994). All laboratories, which responded to the
questionnaire, check/calibrate their field meters prior to use in the field. However, just 63% o f
LA and 50% o f EPA laboratories maintain a record o f this check/calibration (Table 3.1 and
Figure 3.6). Failure to record the above inform ation reduces the traceability o f the results
obtained as it could not be subsequently proved that the particular param eter measured was done
so using a properly calibrated/checked instrument.
In the questionnaire, the laboratories were asked about the type o f sampling container used to
sample for m icrobiological, fluoride, oil/grease, phosphate and metals. All laboratories, w hich
replied to the questionnaire, use the correct type o f sam pling containers when sam pling for
fluoride, m etals and m icrobiological samples (Figure 3.7). All E P A laboratories use the correct
container i.e glass, w hen sampling for oil and grease, how ever, only 63% o f LA laboratories use
the correct type o f sam pling containers. The rem ainder o f L A laboratories incorrectly use plastic
sampling containers. The sample result(s) obtained from these laboratories may not be accurate
as oil and grease is absorbed into the walls o f plastic containers (A non., 1998). This w ould be o f
particular concern w hen measuring low levels o f oil and grease.
All laboratories, w hich replied to the questionnaire, use the incorrect type o f sam pling container
i.e. plastic containers, w hen sampling for phosphate (Table 3.1 and Figure 3.7). Phosphate is
absorbed into the w alls o f plastic containers thereby resulting in false low readings, particularly
w here low levels are being detected (Anon., 1998). The Local G overnm ent (W ater Pollution)
Act, 1977 (W ater Quality Standards for Phosphorus) R egulations, 1998 cite a concentration o f
0.07m g/l P O 4-P as being indicative o f seriously polluted. This is a very low level in analytical
term s and hence the absorption o f phosphate into the sam pling container may have significant
consequences. B earing this in mind, questions may be posed regarding the accuracy o f
phosphate m onitoring in Irish rivers by LA and EPA laboratories.
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4.1.8 Sam ple Preservation
Sample preservation is required to ensure the integrity o f a sample for a number o f determinands.
W hen the interval between sample collection and analysis is long enough to produce changes in
either the concentration or the physical state o f the constituent to be measured, the samples
should be preserved (Crosby and Patel 1995 and Flanagan, 19906). Samples undergoing analysis
for am m onia or trace metals should be analysed as soon as possible or acidified to pFI <2.
Samples undergoing phosphate analysis should be refrigerated and analysed w ithin 48 hours
(Crosby and Patel 1995; Flanagan, 1990 and Anon., 1998).
67% o f EPA laboratories chem ically preserve sam ples for am m onia analysis, in contrast only 5%
o f the LA laboratory respondents preserve for am m onia (Table 3.1 and Figure 3 .8). This is o f
concern as am m onia once in contact with air is im m ediately oxidised to nitrite and nitrate. I f the
sample is not preserved or analysed im m ediately the am m onia level m easured may not be
representative o f the sample taken.
All EPA laboratories chem ically preserve sam ples taken for oil and grease analysis, however,
none o f the L A laboratory respondents, preserve fo r oil and grease. This may have a significant
effect on sam ple results particularly where low levels o f oil and grease are being m easured as the
oil and grease may be broken down by bacteria present in the sample.
All EPA laboratories chem ically preserve sam ples taken for metal analysis. A high percentage
o f the LA laboratories (60% ) also preserve these sam ples (Figure 3.8).
O f the laboratories that responded to the questionnaire, one LA and one EPA laboratory
chem ically preserves for phosphate. This is not required in Standard M ethods.
64% o f LA and 80% o f EPA laboratories docum ent w hich sam ples are to be preserved (Figure
3.3), how ever, a lot fewer (45% and 40% respectively) m aintain records o f the type o f
preservation w hich is carried out or record details o f the preservative used. This is o f particular
concern if the sam pler does not carry out the laboratory analyses as the type o f preservative used
w ould be unknow n to the analyst.
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4.1.9 Q uality Control
It is recom m ended that a quality control (Q C) program m e be im plem ented with regard to
sam pling (IS 0 5 6 6 7 -5 :1999 (9), ISO 5667-6:1990 (5.5) and ISO 5667-14:1998(E)). Among the
QC procedures recom m ended in ISO 5667 are the use o f field blanks and also the use o f QC
tests on the preservatives used. Field blanks are used to establish w hether the sample container
or the sampling process is a source o f contamination. A QC test on the preservative procedure
will establish if the preservative used is a source o f contam ination (i.e. if it contains the analyte
M ost o f the EPA laboratories carry out these quality control procedures, i.e. 60% analyse field
blanks and 80% carry out a quality control test on the preservatives used (Table 3.1 and Figure
3.9). A significantly low er percentage o f the L A laboratory respondents use these procedures i.e.
27% analyse field blanks and 18% carry out a QC test on the preservatives used. These results
indicate a lack o f quality control over sampling procedures in LA laboratories. This could be
significant if, on the im plem entation o f these procedures, it was found that the sample container
or the preservative used were having a significant effect on the result obtained.
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o f EPA laboratory respondents do not transport samples in a cooled environm ent (Table 3.1).
This is o f concern particularly during w armer w eather since specific param eters o f interest e.g.
m icrobiological, BO D and ammonia, may be significantly altered during sample transit due to
the increase in tem perature.
Anyone taking possession o f samples during transport is technically part o f the chain-of-custody
and may need to account for the samples whilst they are under their im m ediate control (Treble
and N icholson, 2000 and Anon., 1998). This process is essential w hen the data is to be used for
litigation purposes.
All EPA laboratories use chain-of-custody forms fo r various types o f sam ples i.e. those taken by
laboratory personnel, by non-laboratory personnel and for prosecution cases (Table 3.1 and
Figure 3.10). In contrast, LA laboratory respondents rarely use chain-of-custody forms. O nly
25% use the form for samples taken by the laboratory personnel, 36% use the form s for sam ples
taken for prosecution cases and 47% use the form s for samples taken by non-laboratory
personnel. This may becom e a significant issue, particularly for legal cases, if the sam pler does
not subsequently analyse the sample or if the sample is sub-contracted to an external laboratory
for specific analyses.
Results from the questionnaire indicate that all E P A laboratories use the results from sam ples
analysed, as evidence in court (Table 3.1 and Figure 3.11). In contrast, only 47% o f LA
laboratory respondents use the results from sam ples analysed as evidence in court. This
indicates that the EPA is more likely to be involved in prosecution cases than L A ’s. In a court-
of-law it w ould be extrem ely difficult to prove the im pact o f a pollution incident on a
w atercourse w ithout presenting analytical analysis. The results o f the questionnaire therefore
97
indicates that LAs are not using their enforcement pow ers fully under the Local Government
(W ater Pollution) Acts, 1977 and 1990.
Just 16% o f LA and 25% o f EPA laboratories, which responded, have had their sampling
procedures questioned in a court-of-law. D etails regarding the areas cross-exam ined in court
w ere not requested in the questionnaire. This low percentage indicates that defending solicitors
are currently not questioning the manner in w hich w ater/w astew ater samples are taken. This
may be linked to the reason why no laboratory is currently accredited or in the process o f
accreditation to ISO 5667. It may also account for the low percentage o f laboratories
docum enting sam pling training procedures and m aintaining sam pling training records.
There are currently no laboratories in Ireland accredited to the ISO 5667 standard 60% o f EPA
laboratory respondents and 16% o f LA laboratory respondents have considered accreditation to
this standard. The high percentage o f EPA laboratories having considered accreditation to
IS 0 5 6 6 7 may be linked to the regulatory and leadership role w ith w hich this organisation has
over LAs and private industry.
98
fluoride and metals. Similarly, LCC have docum ented sam pling procedures in place, transport
samples in a cooled environm ent and use chain-of-custody forms w hen samples are taken by
non-laboratory personnel. This is also the situation in most other laboratories questioned. LCC
do not, however, use the correct type o f sampling container w hen sam pling for phosphate nor do
they docum ent sampling training procedures or maintain records o f staff training. This
m alpractice was also reflected in most other environm ental laboratories questioned.
In general, LCC shares m ore practices and procedures in com m on w ith other L A laboratories
than w ith EPA laboratories. For example, LCC do not preserve samples for oil and grease or
am m onia nor do they analyse quality control blanks. This is the situation in m ost other LA
laboratories but not in most EPA laboratories.
LCC do, however, share some practices in com m on with EPA laboratories that are not com m on
in LA laboratories. F or example, LCC maintain sampling training records, have standard field
log-sheets for the sam pling o f various w ater bodies and has been questioned in court regarding
sampling procedures. In addition, LCC has considered obtaining accreditation specifically to the
ISO 5667 standard.
The gap analysis revealed links between the various parts o f the ISO 5667 standard. These w ere
subdivided into a num ber o f key areas and included general requirem ents w ith regard to the:
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The discussion, w hich follows, gives details o f the required corrective actions under the above
sub-headings.
The gap analysis undertaken between the various sam pling program m es o f LCC and ISO 5667
revealed that the sam pling program m es o f the environm ental laboratory o f LCC are, in general,
lacking in specific detail, particularly, in relation to the objectives o f the sampling program m e,
sam pling locations, sam pling times, frequency o f sampling, num bers o f samples required and the
precision adequate for analytical field results (Table 3.2- C .A 1-10; Table 3.5- C.A 1 and Table
3.7-C.A 4). Inform ation on the above can be incorporated into L C C ’s existing sam pling
program m es in a relatively short period o f time, at a low cost using existing resources. The
reason for this being that the bulk o f w ater sam pling carried out by the laboratory is done in
accordance w ith relevant legislation which specifies the above inform ation. In relation to the
precision o f analytical field results, the relevant specifications m ust be extracted from the
appropriate legislation and compared to the precision o f current analytical field results. The
precision o f a current analytical field method is determ ined by m easuring the param eter o f
interest a num ber o f tim es on a particular sample. The standard deviation o f these results is then
used to calculate precision. If the required precision is not being obtained this indicates that the
current m eter is not capable o f meeting the required specification. The m eter and/or the probe
may then need to be re-calibrated, serviced by the m anufacturer or replaced by a m ore precise
meter.
The gap analysis undertaken between the current sam pling program m es at LCC and ISO 5667
revealed that records do not exist in LC C ’s drinking w ater, river w ater or urban/industrial
w astew aters sam pling program m es as to how sam pling locations are selected. This is required
under ISO 5667 in order to ensure that the samples taken at these locations are representative.
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L C C ’s drinking w ater sampling programme lists all o f the drinking w ater supplies (public and
group w ater schemes) m onitored within the county and states the frequency o f monitoring
required for these under the European Com m unities (D rinking W ater) Regulations, 2000. The
selection and m apping o f sampling locations is currently underw ay follow ing w hich an annual
sampling program m e will be documented. The sampling locations are selected random ly
throughout the distribution system, however, this is not stated in the sam pling program m e as is
required in ISO 5667 (Table 3.5- C.A. 1). This can easily be rectified in the short term.
L C C ’s river w ater sam pling program m e identifies and m aps river sam pling locations and also
sampling locations for surface w aters used for the abstraction o f drinking water. There are no
records, however, w ith regard to how these locations w ere selected. Surface w ater sampling
locations m ust be representative o f the whole aquatic system (C lesceri et a/, 1998; Crosby and
Patel, 1995; N SA I, 1994 and Galal-Gorchev and Lewis, 1984) and therefore the surface w ater
sampling locations used by LCC staff must be reassessed to ensure that they are indeed
providing representative samples. This reassessm ent must take into account inter a lia , locations
w here m arked quality changes are likely to occur, locations w here there are im portant river uses
and also the presence o f EPA flow stations (Table 3.6- C.A 1). This can only be done in the long
term as the river sam pling programm e for the current year has already been initiated. Any
additional points selected must be assessed to ensure they are accessible all year round. The cost
o f im plem entation o f this m easure would be low provided any additional sam pling required
could be carried out using existing resources.
L C C ’s w astew ater sam pling program m e identifies and maps all LA urban w astew ater treatm ent
plants (W W TPs) in the county and details the frequency o f m onitoring for each plant. The
sampling program m e also lists the industries licensed under the Local G overnm ent (W ater
Pollution) Act, 1977-1990. Sampling times for both urban and industrial W W TPs are spread
evenly throughout the year based on the requirem ents o f the above legislation. This is
docum ented on a wall planner prepared at the beginning o f each calendar year. The location o f
sampling points at LA W W TPs and industrial discharge points is not stated in the sampling
program m e (Table 3.2- C.A. 1)
ISO 5667 requires the identification and docum entation o f an exact sam pling point at the
influent, effluent and aeration tank(s) o f all W W TPs routinely sam pled (Table 3.7- C.A. 4). The
reason for this being to ensure that variations detected in pollutant concentration are due to
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w astew ater quality changes rather than the use o f different sam pling points e.g. samples taken
from an influent stream before screening will yield different values to those taken o f the same
influent stream after screening. The sampling locations at each o f the urban and industrial
W W TPs could be identified and included in the sam pling program m e in the short term at a low
cost to the laboratory.
ISO 5667-10 requires that a system be im plem ented in the sam pling program m e for frequently
review ing the sam pling locations chosen. This w ould involve assessing each sampling site to
ensure there is sufficient turbulence and mixing o f the w astew aters. Insufficient mixing may
result in unrepresentative samples being obtained. As the expertise necessary to carry out such a
study is not available in LCC, implementation w ould be expensive and tim e consum ing (Table
3.7-C.A. 1).
W ith regard to licensed discharges to sewers, ISO 5667-10 requires identification o f those areas
where a site inspection may be necessary in order to ensure that the locations o f the sewers and
path o f the w aste stream correspond to the site map draw ings and that the selected location is
representative for sam pling purpose (Table 3.7-C .A 21). A system for carrying out these site
inspections m ust be developed and may consist o f chem ical tracer studies or other approved
methods. The results o f all such inspections should be docum ented. This requirem ent would
have to form part o f licence review process. T he tim e-scale for im plem entation w ould therefore
be long-term and a high cost may be incurred, particularly for larger and older premises.
In order to com ply fully w ith the requirements o f ISO 5667 a num ber o f additional QC m easures
must be introduced (Table 3.3). These corrective actions can be im plem ented using existing
resources, however, the tim e scale and cost o f im plem entation o f the proposed corrective actions
vary. F or exam ple, the docum entation o f sam pling training procedures, training o f sam pling
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personnel and developm ent o f detailed training records can be readily im plem ented within a
short period o f tim e and at a relatively low cost. On the other hand, the developm ent,
docum entation and im plem entation o f a complete analytical QC program m e for periodically
testing sam pling m ethods used would take considerable tim e and expense to im plem ent fully.
The reason for this being that such a programm e would require the use o f field blanks, sam ples
w ith added determ inands and/or duplicate samples in order to identify possible sources o f error
in the sam pling method. The im plem entation o f these techniques w ould also result in an
increased w orkload for both the sampler and the analyst. The introduction o f an adequate
preservation program m e, to ensure that the concentration or physical state o f the determ inand o f
interest is not altered during storage, would also be tim e consum ing and expensive to im plem ent
fully (see Section 4.2.3)
4.2.3 Preservation
Samples should be preserved w hen the interval betw een sample collection and analysis is long
enough to produce changes in either the concentration or the physical state o f the constituent to
be m easured (Crosby and Patel 1995 and Flanagan, 1990Z>). A side from the preservation o f
m icrobiological sam ples (by the addition o f sodium thiosulphate prior to sterilisation), staff o f
the environm ental laboratory at LCC do not carry out preservation o f any physical/chem ical
sam ples at the sam pling site. Laboratory staff do, however, m onitor a num ber o f unstable
param eters at the sam pling site. The param eters m easured in situ are tem perature, pH, dissolved
oxygen and chlorine.
From the results obtained from the questionnaire, it is apparent that, similar to LCC laboratory,
m ost LA s do not preserve samples. Figure 3.8 (page 38) shows that no LA laboratory preserves
for oil and grease w hile a mere 5% preserve for ammonia. EPA laboratories do, however,
generally preserve samples. All EPA laboratories preserve samples taken for oil and grease and
metals, w hile 67% preserve samples for ammonia.
The requirem ent to preserve samples, during sam pling or im m ediately afterwards, is stated in
each part o f ISO 5667 audited. Other w orkers have also stressed the im portance o f preservation.
(Flanagan el a l , 2003; Clesceri el a!., 1998 and Bartram el a/., 1996) This highlights the
im portance o f sam ple preservation in m aintaining the integrity o f a sample during transport and
storage.
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A num ber o f corrective actions in relation to sample preservation em erged from the gap analysis
undertaken betw een ISO 5667 and current LCC sam ple preservation practices (Table 3 .4). Some
o f these corrective actions can be implemented in the medium term at a low/m edium cost using
existing laboratory facilities and resources e.g. the preservation m ethod(s) required for the
various sam ples could be readily identified and docum ented. The im plem entation o f these
sam pling procedures in the field, however, will require extra resources. These resources are
m ainly associated with the increased w orkload associated w ith an efficient preservation
programme. F or example, the preservation o f sam ples on-site w ould result in an increased pre
sam pling preparation tim e and also an increased sam pling tim e as more sample containers may
be required to be labelled and filled. The keeping o f adequate records o f all preservation steps,
as required under ISO 5667, will also be time consum ing.
ISO 5667 —3 and ISO 5667-14 state that the preservation m ethod used must not result in dilution
o f the analyte or interfere w ith the subsequent analysis thereby influencing the final result. In
order to com ply with this requirement an appropriate QC procedure must be developed,
docum ented and im plem ented. Although this may result in a significant increase in the
laboratory analysts’ w orkload it should not result in a significant increase in the sam pler’s
w orkload, as no additional sampling is required. This corrective action could therefore be
im plem ented in the medium term at a medium cost (Table 3.4).
Com posite sam plers are currently used by LCC staff to sample w astew aters. These sam ples are
analysed for BOD, COD, suspended solids and nutrients. ISO 5667 -1 0 requires that when
com posite sam ples are collected over extended periods, preservation should be an integral part o f
the sam pling operation. The EPA recom mend the use o f autom atic samplers w ith built-in
refrigeration w hen sam pling w astew ater treatm ent plants, however, they have stated that an
acceptable com prom ise would be to protect the sam pling equipm ent from direct sunlight (EPA
1996). Preservation is required for a number o f param eters analysed in com posite w astew ater
samples taken by LCC environm ental staff e.g. sam ples undergoing analyses for B O D and
phosphate require preservation by refrigeration; sam ples analysed for am m onia m ust be
preserved by acidification. Com posite samplers that incorporate preservation facilities are
extrem ely expensive and may not be necessary i.e. due to the high levels o f the above pollutants
present in most w astew ater samples the non-preservation o f the sam ple may not significantly
affect the result obtained. This can only be ascertained by determ ining the stability o f the
param eters o f interest using a large number of representative w astew ater samples.
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4.2.4 Sam pling procedures
4.2.4.1 D rinking Water sam pling
The European C om m unities (Drinking W ater) Regulations, 2000, cam e into force in Ireland on
1st January, 2004. As a result o f this, the EPA has published a draft im plem entation handbook
for sanitary authorities entitled 'European Communities (D rinking Water) Regulations, 2000 - A
handbook on im plem entation fo r sanitary authorities D r a ft’ (Flanagan et al., 2003). The
requirem ents o f this handbook are very similar to those o f ISO 5667-5 (e.g. both require
sam pling procedures to be documented, sampling locations to be pre-determ ined and mapped
and correct and im m ediate sample preservation and storage)
The results o f the gap analysis carried out between ISO 5667- Parts 1, 2, 3, 5 and 14 and the
current drinking w ater sampling procedures at LCC revealed that a num ber o f the requirem ents
o f ISO 5667-5 are already being met by the laboratory. N evertheless, a significant num ber o f
requirem ents remain to be im plem ented (Table 3.5).
Each laboratory should produce a sampling manual (ISO 5667; Flanagan et al., 2003; Barron,
2001 and Clesceri et al., 1998). This manual should include the procedures and precautions to
be adopted for each param eter or group o f parameters. Sampling m anuals o f the environm ental
laboratory at LCC are in the form o f docum ented standard operating procedures (SO P) as shown
in A ppendix B.
SOP No. 6 relates to the sampling o f drinking w ater from consum er taps. This SOP gives details
on the sam pling equipm ent required, the need to sterilise and run the tap prior to sam pling and
the requirem ent to test for chlorine on-site. SOP No. 6 is not sufficiently com prehensive,
however, to meet the requirem ents o f ISO 5667, and in particular, Parts 1, 2, 3 and 5. A num ber
o f am endm ents m ust be made to SOP No. 6 in order to rectify this situation. These am endm ents
cover such areas as the nature o f sampling taps, sam pling containers, field meters, sample
volumes, filling, preservation and sealing o f samples, sam pling in low flow areas, QC measures,
sample storage and transportation, field records and safety precautions (Table 3.5 -C .A .2)
Some o f the am endm ents required o f SOP no. 6 are currently being carried out by LCC staff,
however, they fall short o f ISO 5667 requirem ents because they are not docum ented in the
appropriate SOP. For example, current drinking w ater sam pling practice at LCC is to;
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-m easure a num ber of param eters in-situ (using field equipm ent that has been
checked/cal ibrated);
-fill sample into sample container and seal;
-record results and other information into the appropriate field report sheet; and
-transport sam ples back to the laboratory in cooler boxes.
This inform ation is not, however, documented in SOP No. 6. To do so, would require little
effort and expense as outlined in Table 3.5-C.A.2.
Com prehensive details m ust be included in SOP No. 6 in relation to the selection o f sam pling
containers and the cleaning/preparation/sterilisation o f same. All physical/chem ical drinking
w ater samples taken by LCC environmental staff are currently collected in high-density
polyethylene (H D PE) bottles. Although this practice w as sufficient for the analysis o f m ost o f
the physical/chem ical param eters under the now revoked European Com m unities (D rinking
W ater) Regulations, 1988, the new European C om m unities (D rinking W ater) Regulations, 2000
(w hich cam e into force in January 2004) requires a w ider range o f param eters to be m onitored
and many o f these require the use o f specific containers for sample storage (e.g. pesticides and
trihalom ethanes). Therefore, the issue o f sampling containers needs to be urgently addressed.
This can be done in short term, however, the cost incurred may be low /m edium as the sam pling
time per sample will increase due to a larger num ber o f bottles requiring labelling and filling.
SOP No. 6 does not include details in relation to a num ber o f requirem ents o f ISO 5667. For
example, SOP No. 6 does not include details on the selection o f sam pling taps, the volum e o f
sample to be collected, param eters to be measured on-site, taking o f samples, sealing o f sam ple
bottles, preservation o f samples for various param eters, storage o f samples and safety
considerations. This inform ation is readily available in ISO 5667 and other publications
(Flanagan et a l 2003 and Anon, 1998) and therefore could be easily included in SOP N o. 6 in
the short term at a low cost (Table 3.5- C.A. 2). O ther details absent from SOP No. 6 (and that
are required under ISO 5667) include procedures for sam pling at different locations (e.g. from
reservoirs, w ater treatm ent plants and hydrants), procedures for sam pling in areas o f low flow (to
avoid disturbance o f sedim entary material) and procedures for taking QC samples. This
inform ation is also readily available in ISO 5667 and other publications (Flanagan et al., 2003
and Anon, 1998) and therefore could be easily included in SOP No. 6 in the short term at a low
cost (Table 3 .5 - C.A. 2).
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Results from the questionnaire revealed that, like LCC, most LA laboratories have docum ented
procedures in place for sampling drinking water. The level o f detail included in these procedures,
however, would appear to fall short o f ISO 5667 and EPA requirem ents particularly in relation to
sam pling container, sample labelling and preservation o f samples. EPA laboratories generally
seem to have m ore detailed docum ented procedures with regard to the above (Section 3.1,2).
The use o f the incorrect container type may affect the accuracy o f the result obtained. For some
analytes desorption o f constituents from the sample container w ould result in artificially elevated
results, w hile for others the adsorption o f constituents o f the sam ple onto the container would
result in artificially reduced results. I f the samples are not preserved or not preserved correctly,
the concentrations determ ined may be different from those existing at the tim e o f sampling.
(Flanagan et a l., 2003, Clesceri et al., 1998, NSAI, 1996, ISO 1987 and D epartm ent o f
Environm ent, 1981). The above may have a significant affect on the sample results obtained and
subsequently reported to members o f the public. If it w ere found that previous results reported
as com plying w ere in fact in breach o f legislation limits public confidence in drinking w ater
Certain requirem ents o f ISO 5667 require further investigation before details o f same can be
incorporated in SOP No. 6. For example, the need to m onitor taste on-site at a tim e w hen the
m icrobiological quality o f the w ater sample is unknow n and the requirem ent to disinfect using a
chlorine solution instead o f alcohol (which is currently being used). This could be assessed in
the short term at low cost by referencing relevant docum entation e.g. Flanagan et a l , 2003 and
Anon, 1998. Furtherm ore, ISO 5667 requires that a m ethod be developed and incorporated into
the sam pling program m e for investigating the dissolution o f m aterials (e.g. lead) from pipew ork
or the grow th o f m icroorganism s within the pipew ork (e.g. due to lack o f scouring). Either o f
the above may have a significant effect on w ater quality if present in excessive amounts. As
inform ation w ith regard to the above is not readily available, a com plete investigation w ould
have to be carried out. This could take a considerable period o f tim e and resources.
The requirem ent to record relevant drinking w ater field data on a field sheet is not only stated in
ISO 5667-5 but also by other w orkers (Flanagan et al, 2003; C lesceri et al, 1998; Bartram et al,
1996 and Crosby and Patel, 1995). LCC laboratory has a designated drinking w ater field sheet,
however, this is not sufficiently com prehensive to meet the requirem ents o f ISO 5667-5. The
drinking w ater field sheet used by LCC environm ental staff needs to be am ended to include
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details on w eather conditions, unusual observations and inform ation on sam ples taken for
specific reasons (Table 3.5- C.A. 11).
In summary, all o f the corrective actions with regard to drinking w ater sam pling can be
im plem ented using existing resources in a m edium /short period o f tim e and at a relatively low
cost. O btaining accreditation for drinking w ater sam pling (i.e. to ISO 5667-5) would be
particularly beneficial, as it would increase consum er confidence in the results obtained.
A gap analysis undertaken between ISO 5667- Parts 1, 2, 3, 6 and 14 and the current river w ater
sam pling procedures at LCC revealed that while some o f the requirem ents are currently being
met a significant num ber o f non conform ances still exist. The corrective actions required to
rem edy this situation are shown in Table 3.6.
SOP No. 8 relates to the sampling o f river w ater while SOP No. 47 relates to the sam pling o f
surface w aters used for the abstraction o f drinking w ater (A ppendix B). SOP No. 8 gives details
on the sam pling equipm ent required, the need to m easure dissolved oxygen and tem perature at
the sam pling site and the need to fill sampling bottles to overflow. SOP No. 47 also gives details
on the sam pling equipm ent required, where sam ples should be taken and sam ple transportation.
The details included in SOP N o .’s 8 and 47 are not sufficient to satisfy the requirem ents o f ISO
5667. The details that are lacking are similar to those m issing in SOP No. 6 for drinking w ater.
F or example, details w ith regard to sampling containers, sam pling equipm ent, calibration o f field
meters, volum e o f sam ple required, the filling o f the sam ple container and the preservation o f
sam ples (Table 3.6-C.A. 4).
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The am endm ents required to SOP N o.’s 8 and 47, in order to comply w ith ISO 5667, can be sub
divided into those am endm ents that can be achieved in the short term using existing resources,
those that can be achieved in the long term using existing resources and those that cannot be
achieved using existing resources thereby necessitating a long tim e scale for full implementation.
Short-term am endm ents relate to the inclusion into the SOP o f details w hich are readily available
in literature (and in particular ISO 5667) or are currently being carried out at LCC but not
docum ented. For example, current river water quality m onitoring practice is to;
-check/calibrate field m eters prior to and during sampling
-m easure a num ber o f param eters in situ e.g. dissolved oxygen, tem perature, pH and
conductivity;
The above practices are, however, not docum ented in SOP N o .’s 8 or 47. This could be
rem edied in the short term at relatively little expense.
As m entioned previously, some o f the detail lacking in SOP N o .’s 8 and 47 is readily available in
literature and its inclusion merely necessitates the review o f this literature, the incorporation o f
the relevant detail into the SOP and its im plem entation in current sampling practice. For
example, SOP N o .’s 8 and 47 does not include details in relation to sam pling containers and how
these are to be prepared prior to use. ISO 5667 contains a vast am ount o f inform ation on
sam pling containers and also on the preparation o f such containers. Inform ation in relation to
sam pling containers is also contained in Anon, 1998. The appropriate inform ation could easily
be incorporated into SOP N o .’s 8 and 47 from these sources.
Results o f the questionnaire revealed that 71% o f respondents docum ent the type o f sam pling
container to be used in their SOP. However, it appears that on som e occasions the details
included in the SOP are incorrect i.e. not one LA or EPA laboratory use glass bottles for
phosphate analysis. This highlights the need to docum ent correctly the type o f sam pling
container to be used. This could easily be incorporated into SOP N o .’s 8 and 47 in the short term
at relatively little expense.
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O ther inform ation lacking in SOP N o .’s 8 and 47 include details on sam pling equipm ent, volum e
o f sam ple to be collected for various parameters, fdling and sealing o f sample containers and
sample storage/transportation. This information is readily available in literature and could be
docum ented in SOP No. 8 in the short term at relatively little expense.
The gap analysis also revealed that SOP No. 8 does not include sufficient detail in relation to
sam pling during abnorm al conditions i.e. under flood conditions or during algal bloom s (Table
3.6-C.A. 9). I f sam pling is not carried out correctly under these conditions then the results
obtained will not be representative. In order to rectify this situation, possible abnormal
conditions m ust be identified and sampling requirem ents prepared for each o f these conditions.
This could be achieved in the short term, however, a medium cost may be incurred as additional
sam pling equipm ent may have to be purchased.
Sim ilar to the drinking w ater field report sheet, the report sheet used for river sam pling does not
provide for the recording o f all the necessary inform ation specified in ISO 5667-6. LCC does
not have a specific report sheet for sampling surface w aters used for abstraction o f drinking
water. This m ust be developed as per ISO 5667-6. This could be achieved in the short term at a
relatively low cost to the laboratory.
Some o f the corrective actions identified in the gap analysis may prove to be expensive and tim e
consum ing to im plem ent. For example, if an accurate m easurem ent o f dissolved oxygen (D O.)
is required (i.e. a m easurem ent o f D O . taken directly in the w ater-body as opposed to the current
approxim ate m easurem ent o f D O in the sampling bucket) then the existing short probes would
have to be replaced by long probes, thereby incurring a high cost (Table 3.6 - C.A. 10).
Some o f the proposed corrective actions required in order to fully com ply w ith ISO 5667 are
beyond the scope and capability o f the laboratory and therefore appropriate external consultants
would have to be engaged. Some exam ples are given below.
Pollutants present in a w aterbody may be distributed uniform ly throughout or they may, for
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determ ination o f the type o f distribution o f the pollutants o f interest in a w aterbody (i.e.
hom ogenous or non-hom ogenous) to be ascertained. The expertise necessary to carry out such a
study is not available in LCC and therefore im plem entation would be expensive and time
consuming.
‘I f significant stream ing or stratification exists at the sampling point a series o f transverse and
depth sam ples should be collected to determine the nature and extent o f any stream ing or
stratification’ (ISO 5667-1- Section 2.9.3.1). This would firstly involve identifying a m ethod to
assess stratification and then an assessment o f each river sampling site. Stratification is
im portant because it m eans that pollutants can be isolated in discrete areas o f a waterbody.
Sampling from stratified w aterw ays may miss pollutants altogether or result in exaggerated
pollutant concentrations.
In order to determ ine the im pact o f a discharge (w astew ater or adjoining tributary) on a river,
upstream and dow nstream sampling points m ust be accurately determ ined (NSAI 1994,
ISO, 1990). The location o f the downstream point is dependent on the particular river, the time
o f travel o f pollutants and the degree o f vertical, lateral and longitudinal mixing in the
waterbody. ISO 5667-6 (5.1.1.1) recom mends the use o f tracer techniques and conductivity
m easurem ents to determ ine the degree o f mixing in a river system. The expertise necessary to
carry out such a study is not available in LCC and therefore im plem entation w ould be expensive
and time consum ing.
4.2.4.3 W astewater
S taff o f L C C ’s environm ental laboratory m onitor all LA U rban w astew ater treatm ent plants in
the county in order to assess their operational efficiency as required under the E nvironm ental
Protection A gency Act, 1992 (Urban W aste W ater Treatm ent) Regulations, 1994. Industrial
discharges (to both w ater and sewer) licensed under the Local G overnm ent (W ater Pollution)
Act, 1977-1990 are also monitored.
The gap analysis undertaken between ISO 5667 - Parts 1, 2, 3, 10 and 14 and the current
w astew ater sam pling procedures at LCC revealed that while some o f the ISO 5667 requirem ents
in relation to w astew ater sampling are currently being met a significant num ber o f requirem ents
ill
have yet to be addressed. Table 3.7 details the corrective actions required in order to comply
w ith ISO 5667 with regard to w astewater sampling.
SOP No. 10 relates to sampling from urban W W TPs w hile SOP No. 11 relates to industrial
effluent sam pling (Appendix B). SOPs N o.’s 10 and 11 make reference to personal safety, give
details on the sam pling equipment required and list the sam pling locations. SOP No. 10 also
lists the param eters to be measured on-site The details included in SOPs N o .’s 10 and 11 are
not sufficient to fulfil all o f the requirements o f ISO 5667. The am endm ents required to rectify
this are sim ilar in nature to those required for drinking w ater and river water.
SOP N o .’s 10 and 11 do not document a num ber o f w astew ater sampling practices and
procedures already in place at LCC. For example, it is standard practice for L C C ’s
environm ental staff to attach a container to a long armed sam pling device to avoid contam ination
o f sam pling containers. In addition, sampling containers are not reused. These practices are not
docum ented in the appropriate SOPs. Temperature, pH and conductivity are m onitored in-situ
during industrial effluent sampling, using calibrated field meters. Again, this is not docum ented
in the appropriate SOPs. As these procedures are currently being carried out the inclusion o f
such details in the appropriate SOPs could take place in the short term.
As w as observed in the SOPs for drinking w ater and river w ater sampling, details regarding the
type o f sam pling container(s) to be used, the volum e o f sam ple(s) required and sample
preservation are not included in the w astew ater SOPs. This situation could be rectified in the
short term as the inform ation required is readily available. In fact, if a com prehensive SOP was
prepared for drinking water, river or w astew ater sam pling it could be used as a tem plate for the
other sam pling SO P’s as the type o f inform ation required is very sim ilar in all situations.
The gap analysis undertaken between L C C ’s current w astew ater sam pling procedures and ISO
5667-10 revealed that additional docum ented procedures are required in L C C ’s w astew ater
sam pling SOPs in order to comply with ISO 5667. These procedures (which relate to the
selection and purchase o f effective samplers and sam pling containers, the freezing and thaw ing
o f sam ples and sam pling o f storm sewage and surface run-off) must first be prepared using the
guidelines provided in ISO 5667. As the inform ation regarding the above is readily available
these procedures could be docum ented in the short term at a low cost to the laboratory.
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LCC do not, at present, have a specific field report form for sam pling w astewaters. Such a
report form is necessary to comply with the requirem ents o f ISO 5667, which also includes
details o f the inform ation to be included in these forms (ISO 5667-10:1992 (E-7). The
requirem ent to com plete this field report sheet must be included in SOP N o .’s 10 and 11. SOP
No. 11 must also include a requirement to note the operating procedures inside the plant at the
time o f sampling. This inform ation is necessary to allow the sample results obtained to be
com pared w ith the activity at the tim e o f sampling. The above corrective actions can be
im plem ented using existing resources over a relatively short time scale and at a relatively low
cost.
The requirem ent to prepare specific field report form s has been highlighted in the gap analyses
undertaken for drinking water, river w ater and w astew ater sampling. The questionnaire also
revealed the lack o f use o f specific field report sheet in other LA laboratories. Only 33% o f LA
laboratories, w hich responded to the questionnaire, have specific field report sheets. This is in
contrast to EPA laboratories, all o f w hom have specific field report forms.
U nder the EPA Act, 1992 (Urban W aste W ater Treatm ent) Regulations, 1994, 24 hour
com posite sam ples are required when sampling W W T P ’s. In LCC these com posite sam plers are
purchased and operated by the relevant County Council area offices. There are no docum ented
procedures, w ithin LCC, w ith regard to the purchasing o f such com posite samplers or the taking
o f com posite samples. The procedure for purchasing com posite samplers should take into
account the specifications given in ISO 5667-10, w hich are applicable to the specific use(s) o f
the sampler. In order to fulfil the requirem ents o f ISO 5667, the procedure for taking o f
com posite sam ples m ust include details on the type o f com posite sam ple required, the num ber o f
samples to be taken (w hich must be determ ined statistically) and the period over w hich the
sam ples are to be taken. D etails o f the param eters w hich cannot be m easured in a com posite
sample (e.g. tem perature and pH) must also be included. Although all o f the above corrective
actions can be im plem ented in-house, the period for im plem entation may be long-term if it is
found that the current com posite samplers do not meet the relevant specifications stated in ISO
5667. The purchase o f replacem ent com posite samplers w ould be very expensive.
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5.0 CONCLUSIONS
5.1 Q uestionnaire
From the questionnaire, it was concluded that:
1. N o laboratory in Ireland is currently accredited to ISO 5667 nor are any o f the
laboratories, w hich responded, in the process o f attaining accreditation to this standard.
26% o f laboratories, which responded, have considered accreditation to ISO 5667
how ever most o f these have found it to be very com plex and currently have it as part o f
their long-term plan.
2. The sam pling procedure used by environm ental laboratories is not generally questioned
during legal proceedings. This may be one o f the reasons why no laboratory is accredited
to ISO 5667.
3. O f the laboratories, which replied to the questionnaire, only 74% o f Local A uthority (LA)
and 60% o f EPA laboratories have docum ented sam pling procedures. The docum ented
sam pling procedures in EPA laboratories seem s to be m ore detailed than those in LA
laboratories, particularly with regard to the type o f sam pling container to be used and the
sam ples w hich are to be preserved.
4. The questionnaire indicated similar trends w ithin the various laboratory sectors. For
exam ple, LA laboratories generally do not preserve sam ples i.e. none preserve for oil and
grease w ith very few (5% ) preserving for am monia. Sim ilarly very few (27 % ) analyse
quality control field blanks or have considered obtaining accreditation specifically to ISO
5667. The trends in EPA laboratories are som ew hat different, from those in LA
laboratories, in that all EPA laboratories preserve sam ples for oil and grease and m ost
(67% ) preserve for ammonia. A higher percentage (60% ) also carry out quality control
field blanks and have considered obtaining accreditation specifically to ISO 5667.
5. Results o f the questionnaire revealed that all laboratories questioned use the incorrect
type o f sam pling container for w ater sam ples used for phosphate analysis. The Local
G overnm ent (W ater Pollution) Act, 1977 (W ater Q uality Standards for Phosphorus)
Regulations, 1998 specifies that phosphate levels >0.07m g/l are indicative o f a seriously
114
polluted river. This is a very low level in analytical term s and hence the im pact o f
absorption o f phosphate into the sampling container may be significant if the incorrect
being m onitored. This inform ation can be obtained from relevant leglisation and
associated im plem entation handbooks.
C om prehensive sampling procedures containing detailed inform ation in relation to
sam pling equipm ent (including sample containers and field m eters), sample volum es
required, filling of samples, sam ple preservation, sample storage, sample
transportation, maintenance o f records, quality control m easures and safety
precautions. This inform ation can be obtained from Standard M ethods (A .P.H .A
1998), relevant legislation and associated im plem entation handbooks.
2. The requirem ents o f ISO 5667 with regard to the detail required in the various sam pling
SOPS for river water, drinking w ater and w astew ater sam pling are sim ilar to one another.
If a com prehensive SOP was prepared for the sam pling o f one o f these w ater bodies it
could be used as a tem plate for the other sam pling S O P ’s. The situation is sim ilar for
field report forms.
3. A pproxim ately 80% o f the corrective actions required to bring LCC current sampling
procedure in line with ISO 5667 requirem ents could be im plem ented using current
laboratory resources and facilities. The tim e scale for im plem entation o f these corrective
actions varies. Total com pliance with all the relevant requirem ents o f ISO 5667 is
currently beyond the scope o f the environm ental laboratory at LCC. This is due to the
lack o f relevant in-house expertise and financial constraints with regard to such areas as
115
assessing sam pling sites for stratification, ensuring sufficient turbulence in the waterbody
being sampled and im plem enting measures to overcom e or m inim ize heterogeneity.
current annual budget provided adequate staff tim e is allocated. External consultants fees
could not be paid for from this budget since external consultant fees would very quickly
reach tens o f thousands o f euros.
5. The requirem ents with regard to the correct sampling and preservation o f samples are
becom ing m ore significant. This has been particularly noticeably in the E P A ’s draft
handbook on the im plem entation o f the European C om m unities (D rinking W ater)
Regulations, 2000 for sanitary authorities, w hich w as published in 2003. Several o f the
requirem ents specified are similar to those o f ISO 5667-5.
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6.0 RECOM M EN DATION S
1. The questionnaire return rate from the independent laboratory sector was very low (36%)
and w as therefore not truly representative o f w ater sampling practices in this sector.
M ore representative information regarding the independent laboratory sector therefore
needs to be obtained.
3. The Local G overnm ent (W ater Pollution) Act, 1977 (W ater Quality Standards for
Phosphorus) Regulations, 1998 required LAs to prepare and present to the EPA, a
Phosphate M easures Report by July 1999 and Im plem entation R eports every tw o years
thereafter. These reports incorporate results o f the m onitoring o f phosphate levels in
specified w aterbodies together with details o f phosphate reduction program m es. As no
laboratory, w hich responded to the questionnaire, use the correct type o f sam pling
containers w hen sam pling for phosphate it needs to be firstly determ ined if the phosphate
levels currently being measured by LA and E PA laboratories are accurate. I f it were
found that the phosphate levels have been underestim ated a review o f the phosphate
reduction program m es would then have to be undertaken.
4. U nder EU and Irish legislation all LA L aboratories are required to carry out similar w ater
quality m onitoring programmes. From the questionnaire, it becam e apparent that the
sam pling procedures and practices in LCC are sim ilar to those in other LA laboratories.
Therefore, the gap analysis carried out as part o f this dissertation could be used as a
117
tem plate in assessing the work required by other LA laboratories in obtaining
5. The gap analysis undertaken between practices and procedures carried out at LC C ’s
environm ental laboratory and ISO 5667 indicated that several o f the requirem ents o f this
standard could be implem ented in-house using existing facilities. Im plem entation o f
these m easures w ould be a positive step tow ards accreditation and w ould prepare
118
R EFEREN CES
1. Anon (1998), Standard M ethods fo r the Exam ination o f Water a n d Wastewater, 20th Edition,
2. Barron, J (2001), Good Laboratory Practice- Quality o f the A nalytical Result, Reagcon,
Shannon, Ireland.
3. Bartram, J., M akela, A. and Makela, E. (1996), Water Q uality M o n ito rin g - A p ra ctica l
guide to the design a n d implementation o f freshw ater quality studies a n d m onitoring
4. Butler, A., Carty, G , Kelly L. and Lehane M. (1995), L a n d fill m anuals- L andfill monitoring,
5. Carty, G., O ’Leary, G., Donlon, B and Henry, M. (1998), W astewater treatm ent m anua/s-
C haracterisation o f industrial wastewaters, Environm ental Protection Agency Ireland.
London.
7. Collins, M.F. (1997), The County Council o f the County o f Lim erick (com plainant) and
A .I.B.P Lim ited (accused) Rathkeale D istrict Court - 14th July 1997, The D istrict Court
Area o f Rathkeale.
8. Crosby, N T and Patel, I. (1995), General p rin cip les o f g o o d sam pling practice, The Royal
9. Crosby, N T., Day, J.A., Hardcastle, W.A., H olocom be, D.G. and Treble, R.D. (1999),
Q uality in the A nalytical Chemistry Laboratory, John W iley & Sons Chichester.
10. D epartm ent o f Environm ent (1992), Protection o f D rinking Water Supplies D raft G uidelines
119
11. Departm ent o f Environm ent (1981), Local G overnment (W ater P ollution) Act, 1977-
G uidelines on sam pling a n d analysis o f waters a n d effluents, Governm ent Publications
Office
12. E nvironm ental Protection A gency Act, 1992 (Urban Waste Water Treatment) Regulations,
1994 (S.I. No. 419 o f 1994), Government Supplies Agency.
14. EPA (1996), Environm ental Protection A gency Act, 1992 (Urban W asteW ater Treatment)
Regulations, 1994: A handbook on im plem entation fo r sanitary authorities. Environm ental
Protection Agency 1996, Environmental Protection Agency Ireland.
15. EPA (1995), EPA a n d the local authorities - sem inar proceedings, Environm ental Protection
A gency Ireland.
16. E uropean Com m unities (W ater Policy) Regulation 2003, (SI 722 o f 2003), G overnm ent
Supplies Agency
18. European C om m unities (Quality o f Surface Water In ten d ed f o r the Abstraction o f D rinking
Water) Regulations, 1989 (S.l. No. 294 o f 1989), G overnm ent Supplies Agency
20 Flanagan, P., O ’Leary, G , Crowe, M., Page, D. and Concannon, C. (2003) E uropean
C om m unities (D rinking Water) Regulations, 2000 - A handbook on im plem entation fo r
120
21. Flanagan, P., O ’Leary, G., Crowe, M., Page, D., Neill, M. and Concannon, C. (2002),
European C om m unities (Drinking Water) R egulations, 2000 - A handbook on
im plem entation f o r sanitary authorities DRAFT, Environm ental Protection Agency Ireland.
23. Flanagan, P.J. (1990b), European Communities (Q uality o f Surface Water Intended f o r the
Abstraction o f D rinking Water) Regulations, 1 9 8 9 -A handbook on im plem entation fo r
sanitary authorities, Environmental Research Unit, Departm ent o f Environm ent.
24. G alal-Gorchev, H. and Lewis, W M. (1984), G uidelines f o r drinking water quality- Vol. 1.
Recom m endations, WHO, Geneva, Switzerland.
25. Gray, N.F. (1999), Water Technology - An introduction f o r scientists a n d engineers, Arnold
Publishers, London
26. H am m er, M.J. (1986), Water a n d Wastewater Technology Seco n d Edition, Prentice Hall
Career & Technology, New Jersey, USA.
27. International Standard Organisation (1987), ISO 5667-4: Water quality - Sam pling- P art 4:
Guidance on sam pling fr o m lakes, natural a n d m an-made, International O rganisation for
Standardization, CH-1211 Geneva, Switzerland.
28. International Standard Organisation (1991), ISO 5667-5: Water quality ~ Sam pling- P art 5:
Guidance on sam pling o f drinking water a n d w ater u s e d fo r fo o d a n d beverage processing,
International O rganisation for Standardization, CH-1211 Geneva, Switzerland.
29. International Standard Organisation (1990), ISO 5667-6: Water quality - Sam pling- P art 6:
G uidance on sam pling o f rivers a n d streams, International O rganisation for Standardization,
CH-1211 Geneva, Switzerland
121
30. International Standard Organisation (1992), ISO 5667-10: Water quality - Sam pling- Part
10: G uidance on sam pling o f waste waters, International O rganisation for Standardization,
31. International Standard Organisation (1998), ISO 5667-14: Water quality - Sam pling- Part
14: G uidance on quality assurance o f environm ental water sam pling a n d handling,
International O rganisation for Standardization, CH-1211 Geneva, Switzerland.
32. Lehane, M., Le Bolloch, O. and Crawley, P. (2002), EPA E nvironm ent in Focus 2002,
Environm ental Protection Agency Ireland.
33. L o ca l G overnm ent (W ater Pollution) Act, 1977 (No. 1 o f 1977), G overnm ent Publications
Office
34. L ocal G overnm ent (W ater Pollution) Act, 1977 (W ater Q uality Standards f o r Phosphorus)
Regulations, 1998, (S.I. No. 258 o f 1998), G overnm ent Supplies Agency.
35. M cG arrigle, M L., Bowman, J.J., Clabby, K.J., Lucey, J., Cunningham , P., M acCarthaigh,
M ., K eegan, M., Cantrell, B., Lehane, M., Clenaghan, C. and Toner, P.F. (2002), Water
36. M etcalf and Eddy (1991), Wastewater Engineering, Treatment, D isposal a n d Reuse - Third
37. Miller, J.N. and M iller, J.C. (2000), Statistics a n d C hem om etrics f o r A nalytical Chem istry-
39. N ational Standards Authority o f Ireland (2000), I.S. E N IS O /IE C 17025: G eneral
requirem ents f o r the competence o f testing a n d calibration laboratories (ISO TE C
122
40. National Standards Authority o f Ireland (1994a), I.S. E N 25667-1: Water quality Sam pling-
Part 1: G uidance on the design o f sampling program m es (ISO 5667-1:1980), National
Standards A uthority o f Ireland, Dublin 9.
41. National Standards Authority o f Ireland (1994b), I.S. E N 25667-2: Water quality - Sam pling-
Part 2: G uidance on sam pling techniques (ISO 5667-2:1991), National Standards A uthority
o f Ireland, D ublin 9.
42. National Standards Authority o f Ireland (1996), I.S. E N 25667-3: Water quality - Sam pling-
Part 3: G uidance on the preservation and handling o f sam ples (ISO 5667-3:1994), National
Standards A uthority o f Ireland, Dublin 9.
43. O ’Leary, G, and Carty, G. (1998), Urban Waste Water discharges in Irela n d -A report fo r
the yea rs 1996 a n d 1997, Environmental Protection Agency Ireland.
44. Page, D., O ’Leary, G., Boland, A., Clenaghan, C. and Crow e, M. (2002) The quality o f
drinking w ater in Ireland - A report fo r the yea r 2001, Environm ental Protection Agency
Ireland.
45. Protection o f the Environm ent Act 2003 (No. 27 o f 2003), Governm ent Supplies Agency.
46. Smith, D. and O ’Leary, G. (2002), EPA Urban waste w ater discharges in Ireland- A n interim
report f o r the Year 2000, Environmental Protection Agency Ireland.
47. Stapleton, L., Lehane, M. and Toner, P.(2000), Ir e la n d ’s Environm ent A M illennium Report,
EPA 2000.
48. Treble, R. and N icholson, F., (2000), L egal aspects o f analytical m easurem ent - U ndertaking
analytical m easurem ent fo r court - a good practice guide f o r scientists, LGC (T eddington)
Lim ited 2000.
49. W orking G roup CITAC and EURACHEM (2002), G uide to Q uality in A n a lytica l Chem istry-
A n A id to Accreditation, CITAC and EU RA CH EM
123
APPENDIX A
THE DISTRICT COURT
BETWEEN/
Complainant.
AND/
A.I.B.P. LIMITED
Accused .
1. BACKGROUND:
• The eviden ce before the Court was that the samples were
acquired using a jug and lo ng -handled scoop which had
been used previously by the Officer in question and
which was stored in the back of his car. There were
further problems in that the samples of water obtained
were stored in plastic bottles instead of appropriately
A -l
-2 -
A-2
-3-
4. COMMENT:
A-3
-4 -
R o u t i n e D r in k in g W a t e r S u p p l y S a m p l e s .
• If possible obtain the sample from a shop / Co-op / Co. Council Office et......
• Identify yourself and state that you work for Limerick Co. Council.
• Inform them that you are taking a water sample as part o f a routine sam pling
program m e to assure water quality and request perm ission to take a sample.
• Enquire if there have been any problems with the water quality in the recent past.
Fill sterile bottle with water using aseptic technique. Rinse out plastic bottle and
fill to overflow ing.Thank supply user for their help, and clean your w ork area
• Return Equipm ent and samples to car, putting sterile bottle in cooler.
Co signed
B-l
L im e r i c k County Council L a b o r a t o r y
S t a n d a r d O p e r a t i n g P r o c e d u r e s No.8
R o u tin e R iver Sa mpling.
• D rop D.O. m eter probe into moving water and allow reading to settle.
• M ark bottle w ith location , D.O. (%), temp. (Deg C), and note anything unusual
w ith the river quality, height, weather et....
• Rinse sam pler and sample bottle. Fill sample bottle to overflow. Leave no air
spaces.
• Return to laboratory by 16:15 hours, and log samples and record pH.
Signed: Date:
B-2
L im e r i c k C ou n ty Co uncil l a b o r a t o r y
S t a n d a r d O p e r a t i n g P r o c e d u r e No.IO
S ew a g e T rea tm e n t P la n t S a m p lin g .
• W here a com posite sampler is available, contact the STP caretaker the evening
before, sam pling and requesting him / her to set the sam pler in motion.
• R equest that the sampling container is cleaned out carefully prior to the sam pler
being set in motion.
• Inform som eone at your base, o f the route you are taking.
• Clearly mark bottles giving the plant name , and the type o f sample.
• W here access is possible take samples from the influent and effluent.
• W here com posite sampler is unavailable take a grab from the m iddle channel.
• W here access is difficult use the long armed sampler, ensuring that it is rinsed out
well before each sample is taken.
• W here time allow s or where the effluent looks poor take both upstream and
dow nstream samples.
• At activated sludge plants where time allows take a m ixed liquor sam ple and
m easure the oxygen in the tank.
B-3
• W here possible rinse all equipment before returning to car.
• Return to the laboratory by 16:15 hours, log samples put on C.O.D. tests and store
samples.
Co sig n ed : C**
B-4
L im e r i c k C o u n t r Council l a b o r a t o r y
S t a n d a r d O p e r a t i n g P r o c e d u r e s N o.11
• Inform som eone at your base o f the route you are about to take.
• Inform yourself as to the nature o f the discharge and w hether the industry is
discharging to a sew er or to waters.
• Inform them that you are from the Co. Council and that you are there to take a
sam ple o f their industrial discharge. Ask if there is anyone from the com pany who
w ould like to accom pany you.
• Take a grab sam ple o f the discharge from the location indicated in the discharge
licence. Offer a split sample to the company.
• Rinse the sam pler and bottle out with the effluent before taking the sample.
• M ark the bottle w ith the name o f the company and the nature o f the sample.
• Return the laboratory before 16:15 hours to log samples and set up C .O .D .s’ and
record pH
Signed:
Co signed: 'X/'v-v
B-5
L im e ric k C ou n ty C ouncil
E n v iro n m e n t L aboratory
B a llyke effe
B-6
L im erick C ounty C ouncil
E nvironm ent Laboratory
Ballykeeffe
Sampling Procedure
2. N otify the sub-contracting laboratory prior to sam pling Salm onella O utline that
raw and treated sam ples will be delivered for each location. State that all sam ples
are to be analysed. State that positive results m ust be phoned to the Environm ent
L aboratory im m ediately.
The follow ing sam ple bottles m ust be taken for each site:
1. 2 No. 250m l sterile glass bottles (One for Total and Faecal Coliform s and
Streptococci and one for Clostridium). Sam ples to be taken o f raw w ater only.
2. 2 N o. 500 m l sterile glass bottles (For Salm onella analysis on raw w ater and
treated w ater)
3. 2 N o. 10 litre sterile plastic bottles ( One for C ryptosporidium on raw w ater
and one for Cryptosporidium on treated water)
4. 2 No. 1 litre plastic bottles (For chemical analysis including sub sam pling on
raw water)
All raw w ater sam ples should be taken at the abstraction point or if this is not feasible,
at the closest point to abstraction. All bacteriological sam ples w ill be taken aseptically
and all sam ples w ill be transported in cooler boxes containing ice packs.
The sam pler will return to base by 4pm to allow bacteriology analysis. Total and
Faecal Coliform s, Streptococci and Clostridium analysis should be carried out
im m ediately.
Log all sam ples in the Sam log system. A rrange for all sub contract w ork to be
collected/delivered.
Co. Signed:___C
B-7
APPENDIX C
T a b le C - l : S u m m a r y o f L o ca l A u th o r ity L a b o r a to r y r e p lie s to q u e s tio n n a ir e .
Q. Question: % Yes % No
No.
1. D oes the laboratory carry out its own sampling? 68 32
2. D oes the laboratory have personnel designated solely for sampling? 11 89
3. Are sam pling procedures documented? 74 26
4. Are there docum ented procedures for the training o f personnel involved 32 68
in sam pling?
5. Is the above training carried out in-house or by an independent outside
body?
A nsw er:
9 replied ‘in-house ’ none replied ‘independent outside b o d y '
6. Are sam pling training records maintained? 11 89
7. Has the laboratory ever considered obtaining accreditation specifically 16 84
for sam pling w ork carried out by the laboratory?
8. If Y ES to Q7please give brief details:
A n sw ers included:
>• A s p a rt o f M Sc. project
> A s p a rt o f overall accreditation
> M ore cost effective to contract out m ost work
9. D oes the laboratory use any o f the following as a guide w hen preparing
sam pling program m es and procedures?
ISO 5667 □ 11 89
LA Im plem entation handbooks □ 56 44
Standard M ethods (A.P.H.A) □ 83 17
10. Are sam ples taken/analysed by the laboratory used as evidence in court? 47 53
11. Have laboratory sampling procedures used by your laboratory ever been 16 84
questioned in court?
12. W hich o f the following samples are routinely sampled by your
laboratory: (Please tick)
River water: □ 72 28
W astew ater - Industrial effluent: □ 67 33
W astew ater - Sewage treatm ent plants: □ 72 28
D rinking water: □ 61 39
C-l
T a b le C - l (c td .)
Q. Question: % Yes % No
No.
13. Please list the param eters which are routinely m onitored at the following
sam pling locations;
17. W hat type o f sam pling containers does the laboratory use to sample the
following: % use the correct sampling container.
a) M icrobiological : 100% use sterile glass/plastic containers.
b) F lu o rid e: 100% use pla stic sam pling containers.
c) Oil and grease : 63% use glass sam pling containers.
d) Phosphate : 0% use glass sam pling containers.
e) M etals : 100% use glass/plastic sam pling containers.
18. Do the m ethod(s) docum ent what type o f sam pling container is to be 56 44
used?
19. A re field blanks analysed for each sample run? 27 73
C -2
T a b le C - l (c td .)
Q. Q u e stio n : % Y es % No
N o.
20 . Are any o f the following samples chem ically preserved prior to analysis:
Answ ers:
a) Ammonia: □ 5% chemically preserve fo r ammonia.
b) Phosphate: □ 6% chem ically preserve f o r phosphate
c) Total Phosphorus: □ 6% chem ically preserve f o r total phosphorus
d) Metals: □ 53% chem ically preser\’e f o r m etals
e) Oil and grease: □ 0% chem ically preserve fo r o il a n d grease
21. I f Y ES to Q20 - H ow soon after sampling are sam ples preserved?
Answ ers included:
a) Ammonia: same day
b) Phosphate: same day
c) Total Phosphorus: same day
d) Metals: same day, immediately, on receipt to lab,
e) Oil and grease: within 24hrs, within 5 days.
22 . D o the laboratory procedures document w hich sam ples are to be 64 36
preserved?__________________________________________________
23. Are records maintained o f the preservation carried out? 45 55
24. Are quality control tests carried out in order to ensure that the 18 82
preservatives used do not interfere with subsequent determ inations?
If Y ES please give brief details:
A n sw ers included:
'r Yes, by sub-contract laboratory,
y F ie ld blanks have been used.
> B la n k with preservative added is carried through analysis.
25. Is sodium thiosulphate (or similar chem ical) added to drinking w ater 100
sam pling bottles prior to sterilisation, in order to neutralise the effects o f
chlorine?
26. Are sam ples transported from the sampling site to the laboratory in a 68 32
refrigerated van or cooler box?___________________________________
27. Are there docum ented procedures with regard to the labelling o f 53 47
samples?___________________________________________________
28. Is inform ation regarding sample location and on-site analysis w ritten on
the sam pling bottle or on a field log-sheet?
A n sw ers included:
> 6 labs replied- on the sam pling bottle
> 3 labs replied - on a fie ld sheet.
F 3 labs rep lied - both
y 7 labs rep lied - yes______________________________________________
29. Are there standard field log-sheets for the various w ater bodies being 33 67
sampled?________________________________________________________
C-3
T a b le C - l (c td .)
Q. Question: % Yes % No
No.
30. Is the laboratory accredited to ISO 17025? 0 100
31. If Y E S to Q30 how many tests is the laboratory accredited for?
0% Y E S to 0 3 0
32. If N O to Q30 is the laboratory in the process o f attaining accreditation to 50 50
ISO 17025?
C-4
T a b le C -2 : S u m m a r y o f E P A L a b o r a to r y r e p lie s to q u e s tio n n a ir e .
Q. Question: % Yes % No
No.
1. D oes the laboratory carry out its own sampling? 83 17
2. D oes the laboratory have personnel designated solely for sampling? 80 20
3. Are sam pling procedures documented? 60 40
4. Are there docum ented procedures for the training o f personnel involved 20 80
in sampling?
5. Is the above training carried out in-house or by an independent outside
body?
A nsw er:
A l/ laboratories replied ‘in-house ’
6. Are sam pling training records maintained? 40 60
7. H as the laboratory ever considered obtaining accreditation specifically 60 40
for sam pling w ork carried out by the laboratory?
8. If YES to Q7 please give brief details:
A nsw ers included:
> L o n g term p la n but w ill probably not p ro ceed with it f o r several
years.
> C onsidered it but decided not to apply.
> A ccred ited fo r a num ber o f tests but d id not include sam pling as it is
m ore com plex a n d w ould require more time.
9. D oes the laboratory use any o f the following as a guide w hen preparing
sam pling program m es and procedures?
ISO 5667 □ 20 80
LA Im plem entation handbooks □ 20 80
Standard M ethods (A.P.H.A) □ 60 40
10. Are sam ples taken/analysed by the laboratory used as evidence in court? 100 0
11 . H ave laboratory sampling procedures used by your laboratory ever been 25 75
questioned in court?
12. W hich o f the following samples are routinely sampled by your
laboratory: (Please tick)
River water: □ 100 0
W astew ater - Industrial effluent: □ 100 0
W astew ater - Sewage treatm ent plants: □ 60 40
D rinking water: □ 40 60
C-5
T a b le C -2 (c td .)
Q. Q u e stio n : % Y es % No
N o.
13. Please list the param eters which are routinely m onitored at the following
sampling locations;
C-6
T a b le C -2 (c td .)
Q. Q u e stio n : % Y es % No
N o.
21. I f Y E S to Q20 - How soon after sampling are sam ples preserved?
Answers included:
a) Ammonia: On receipt at lab.
b) Phosphate: On receipt a t lab.
c) Total Phosphorus: On receipt a t lab.
d) Metals: On receipt a t lab a n d immediately.
e) Oil and grease: On receipt a t lab a n d immediately.
22 . D oes the laboratory procedures document which sam ples are to be 80 20
preserved?___________________________________________________
23. A re records m aintained o f the preservation carried out? 40 60
24. Are quality control tests carried out in order to ensure that the 80 20
preservatives used do not interfere with subsequent determ inations?
I f Y E S please give brief details:
A n sw ers included:
r Using fi e ld blanks.
25. Is sodium thiosulphate (or similar chem ical) added to drinking w ater 75 25
sam pling bottles prior to sterilisation, in order to neutralise the effects o f
chlorine?
26. Are sam ples transported from the sampling site to the laboratory in a 60 40
refrigerated van or cooler box?___________________________________
27. Are there docum ented procedures with regard to the labelling o f 60 40
samples?___________________________________________________
28. Is inform ation regarding sample location and on-site analysis w ritten on
the sampling bottle or on a field log-sheet?
A n sw ers included:
> 2 labs replied - on a fie ld sheet.
> 2 labs rep lied - y e s ______________________________________________
29. Are there standard field log-sheets for the various w ater bodies being 100
sam pled?_______________________________________________________
30. Is the laboratory accredited to ISO 17025? 60 40
31 I f Y E S to Q30 how many tests is the laboratory accredited for?
A n sw ers included:
> 18 tests
> 20 tests
> 22 tests
32. If N O to Q30 is the laboratory in the process o f attaining accreditation to 50 50
ISO 17025?
C-7
T a b le C -3: S u m m a r y o f In d e p e n d e n t L a b o r a to r y r e p lies to q u e stio n n a ir e .
Q. Question: % Yes % No
No.
1. D oes the laboratory carry out its own sampling? 75 25
2. D oes the laboratory have personnel designated solely for sampling? 100 0
3. Are sam pling procedures documented? 100 0
4. Are there docum ented procedures for the training o f personnel involved 33 67
in sampling?
5. Is the above training carried out in-house or by an independent outside
body?
A nsw er:
Two laboratories replied ‘in-house ’ the rem ainder d id not reply to the
question.
6. Are sam pling training records maintained? 50 50
7. H as the laboratory ever considered obtaining accreditation specifically 33 67
for sampling w ork carried out by the laboratory?
8. I f Y ES to Q 7please give brief details:
A n sw ers included:
> To ISO 5667
9. D oes the laboratory use any o f the following as a guide w hen preparing
sampling program m es and procedures?
ISO 5667 □ 0 100
LA Im plem entation handbooks □ 0 100
Standard M ethods (A.P H.A) □ 100 0
10. Are sam ples taken/analysed by the laboratory used as evidence in court? 100 0
11. Have laboratory sampling procedures used by your laboratory ever been 0 100
questioned in court?
12. W hich o f the following samples are routinely sam pled by your
laboratory: (Please tick)
River w ater: □ 67 33
W astew ater - Industrial effluent: □ 100 0
W astew ater - Sewage treatm ent plants: □ 67 33
D rinking water: □ 67 33
C-8
T a b le C -3 (c td .)
Q. Q u e stio n : % Y es % No
N o.
13. Please list the param eters which are routinely m onitored at the follow ing
sam pling locations;
17. W hat type o f sampling containers does the laboratory use to sample the
following: % use the correct sam pling container.
a) M icrobiological : 100% use sterile glass/plastic containers.
b) Fluoride : 100% use pla stic sam pling containers.
c) Oil and grease : 100% use glass sam pling containers.
d) Phosphate : 0% use glass sam pling containers.
e) M etals :_________ 100% use glass/plastic sam pling containers.
18. D o the m ethod(s) document what type o f sam pling container is to be 100
used 1*
19. Are field blanks analysed for each sample run? 67 33
20 . Are any o f the following samples chem ically preserved prior to analysis:
Answers:
f) A m m onia; □ 33% chem ically p r e s e n t f o r ammonia.
g) Phosphate: □ 0%> chem ically preserve f o r phosphate
h) Total Phosphorus: □ 0% chem ically preserve f o r total phosphorus
i) M etals: 6)7%> chem ically preserve f o r m etals
j) Oil and grease: □ 33% chem ically preserve f o r o il a n d grease
C-9
T a b le C -3 (c td .)
Q. Q u e stio n : % Y es % No
N o.
21. If Y E S to Q20 - How soon after sampling are sam ples preserved?
Armvers included:
f) Ammonia: On receipt at lab
g) Phosphate: 0% chemically preserve f o r phosphate
h) Total Phosphorus: 0% chemically preserve f o r total phosphorus
i) Metals. On receipt at lab, when subcontracting to ICP.
j) Oil and grease: On receipt at lab.___________________________
22 . D o the laboratory procedures document w hich sam ples are to be 100
preserved?__________________________________________________
23. A re records m aintained o f the preservation carried out? 100
24. Are quality control tests carried out in order to ensure that the 33 67
preservatives used do not interfere with subsequent determ inations?
I f Y E S please give brief details:
A nsw ers included:
> Preservation is perform ed as p e r Standard M ethods.
25. Is sodium thiosulphate (or similar chemical) added to drinking w ater 100
sam pling bottles prior to sterilisation, in order to neutralise the effects o f
chlorine?
26. Are sam ples transported from the sampling site to the laboratory in a 100 0
refrigerated van or cooler box?___________________________________
27. Are there docum ented procedures with regard to the labelling o f 100 T
samples?___________________________________________________
28. Is inform ation regarding sample location and on-site analysis w ritten on
the sampling bottle or on a field log-sheet?
A nsw ers included:
> I lab rep lied - m ostly on the bottle.
> / lab r e p lie d - y e s
> I lab rep lied - both_____________________________________________
29. Are there standard field log-sheets for the various w ater bodies being 33 67
sampled?________________________________________________________
30. Is the laboratory accredited to ISO 17025? 67 33
31. If Y E S to Q30 how many tests is the laboratory accredited for?
Answ ers included:
> 37 tests
> 40 tests
32. If N O to Q 30 is the laboratory in the process o f attaining accreditation to 100
ISO 17025?
C-10
APPENDIX D
DOCUMENT No. 1:
Gap Analysis results for I.S. E N 25667-1:1994 Water Quality - Sam pling - Part 1: G uidance
on the design o f sam pling program m es (ISO 5667-1:1980).
3. Introduction:
‘The sam ples collected should be as fu lly representative as possible o f the whole to be
characterized’
'All precautions sh o u ld be taken to ensure that, as f a r as possible, the sam ples do n o t undergo
any changes in the interval between sampling a n d analysis ’
‘Before any sam pling program m e is devised, it is very im portant that the objectives be
esta b lish ed ’
D -l
3. In tr o d u c tio n (c td ..):
'Some consideration shoidd also be given to the degree o f d etail a n d precision that w ill be
adequate. '
‘Som e consideration should also be given t o the m anner in which the results are to be
expressed a n d p resen ted e.g. max, min, median values, lo a d '
‘A dditionally a list o f param eters o f interest sh o u ld be com piled a n d the relevant analytical
procedure consulted since these w ill usually give guidance on precautions to be observed during
sam pling a n d subsequent handling '
D -2
3. Introduction (ctd..):
‘It m ay often be necessary to carry out a prelim inary sam pling a n d analysis program m e before
the fin a l objectives can be defined. ’
4. Requirem ents:
N ot applicable to gap analysis
5.1
‘Sam pling should be avoided at or near boundaries o f system s unless conditions are o f special
interest ’
5.3
‘Care should be taken to eliminate or minimize any changes in the concentration o f
determ inands o f interest that m ay be produced by the sam pling process itse lf a n d to ensure that
changes during the p e rio d between sampling a n d analysis are avoided or m inim ized ’
D -3
S E C T IO N 2: ID E N T I F IC A T IO N O F S A M P L IN G S I T U A T IO N S
7.2
‘Weather conditions sh o u ld be considered in order to ensure the safety o f personnel a n d
equipment. '
D -4
7.3
N ot applicable to gap analysis.
7.4
‘Sam pling from unsafe sites, such as unsafe banks, should be avoided i f possible. I f this is
unavoidable the operation shoidd be conducted by a team using appropriate precautions rather
than one operator. Sam pling fro m bridges shoidd be used when appropriate. ’
7.5
‘Reasonable access in a ll weather is important a n d it is essential f o r fre q u e n t routine sampling. ’
7.6
N ot applicable to gap analysis.
7.7
M a n y other situations arise during the sam pling o f water when special precautions have to be
taken to a vo id accidents. F or example, some industrial effluents m ay be corrosive or m ay
contain toxic or fla m m a b le materials. The dangers associated with sew age should n o t be
overlooked; these m ay be gaseous, microbiological, virological or zoological, such as fro m
am oebae o r helm inths.
D-5
7.8
N ot applicable to gap analysis.
7.9
N ot applicable to gap analysis.
7.10
N ot applicable to gap analysis.
7.11
N ot applicable to gap analysis.
‘I n designing quality sam pling networks it is usual to m ake provision f o r the m easurem ent o f
flow at key stations. ’
‘Identifying the sam pling location enables com parative sam ples to be taken a t other times. '
D -6
8 .3 C h a r a c te r o f flo w
'Ideally sam ples sh o u ld be taken from turbulent, w ell-m ixed liquids a n d whenever possible
turbulence should be induced in flo w s that are streamlined. ’
D -7
8 .7 N a tu r e o f liq u id
‘Solids m a y be d istributed anywhere throughout the depth o f a liquid. Adequate m ixing should be
carried out, i f possible, by m aintaining turbulent conditions. Ideally, the linear velocity should
be sufficient to induce turbulence a n d samples sh o u ld be taken under isokinetic conditions. I f this
is not possible, a series o f samples should be taken across a f u l l cross-section o f the flow . ’
D -8
8.10 Sam pling for volatile compounds content.
N ot applicable to gap analysis
9.1 Precipitation
N ot applicable to gap analysis.
D -9
9 .3 R iv e r s a n d S tre a m s.
9.3.1 M ixing
‘I f significant stream ing or stratification exists at the sam pling point, a series o f transverse a n d
depth sam ples sh o u ld be collected to determine the nature a n d extent o f any stream ing or
stratification. ’
‘ I f sam pling is intended to m onitor the effects o f a discharge, sam pling both upstream a n d
downstream sh o u ld be carried out, but careful consideration sh o u ld be given to the m ixing o f the
discharge a n d receiving water a n d its effects on the downstream samples. Sam pling should
extend f o r an appropriate distance downstream to assess the effects on the river. ’
D -10
9.4 Canals
Not applicable to gap analysis.
9.7 B ottom deposits in rivers, estuaries and the sea, lakes and reservoirs.
N ot applicable to gap analysis.
‘ The sam pling p o in t sh o u ld be selected so as to p erm it m onitoring o f residual disinfecting agents befo
any loss occurs but after a ll reactions are completed. ’
‘Sam pling f o r routine bacteriological exam ination is also required a n d suitable precautions,
including a ny national safety regulations, should be observed. ’
D-ll
9.8.1 Water being pum ped into supply (ctd.)
‘Sam pling tap should have no attachm ents and should be suitable f o r sterilization by flam ing.
The m aterial o f the sam ple p ip e shall be carefully chosen in relation to the test requirements. ’
‘I n order to m ake sure that the sample is drawn directly fr o m the tap into the container, the
sample container sh o u ld be p la ced immediately below the tap but not connected to it, nor in
direct contact with it. ’
‘Sam ples sh o u ld be taken fr o m a tap fitte d to the outlet m ain as close as possible to the
reservoir .Ensure the reservoir is em ptying at the time o f taking the sam ple ( if fillin g a n d
em ptying through sam e main).
D -12
9.8.3 Water in the distribution system
‘A nti-splash or sim ilar devices should be rem oved before sam pling; m ixer taps are not
recom m ended fo r sampling. ’
11 Trade Effluents.
11.1 Sites
‘The sam pling o f industrial effluents has to be considered in relation to the nature a n d location
o f each individual effluent ’
'The p o ssib ility o f dom estic sewage from the fa c to ry being co n tained in the sam ple sh o u ld also
be considered a n d the site should be chosen to exclude such wastes, i f necessary '
'If the effluent discharge is to a lagoon or holding tank, then the sam pling situation becom es
sim ilar to that f o r lakes. ’
D-13
11.1 S ite s (c td ..)
‘With m anhole sampling, it is preferable, fo r safety reasons, that the m anhole should be designed
so as to p erm it sam pling to take place without entry. ’
‘When effluents fr o m a variety o fp ro cesses discharge into a com m on main, adequate m ixing is
required in order to obtain satisfactory sample. ’
D -14
12 S e w a g e a n d S e w a g e E fflu en ts.
D -15
12.1.1 Liquid effluents (ctd .)
‘Crude sewage sam ples are freq u en tly taken after the prelim in a ry screening a n d com m inution
p rocesses so that adventitious inclusion o f large particles in the sam ple is avoided. ’
'In selecting a sam pling site fo r crude sewage a t the treatm ent p la n t, the inclusion o f
recirculated liquors within the p la n t should be considered. Ideally two samples, one including a ll
liquors representing the total load on the p lant a n d one excluding recirculated liquor to give a
m easure o f the loading from external sources, m ay be necessary ’
‘A utom atic sam pling devices that collect sam ples a t regidar intervals a n d w hich start at a
p rescrib ed flo w offer m any advantages. This equipm ent sh o u ld be installed in a p erm a n en t state
o f readiness. In m any instances, flow -proportional sam pling w ill be desirable.
Relevant precipita tio n a n d air temperature data sh o u ld be co llected throughout the p e r io d o f
investigation. '
D -16
S E C T IO N 3 T IM E A N D F R E Q U E N C Y O F S A M P L IN G
14. Introduction
N ot applicable to gap analysis.
'The times a n d freq u en c y o f sam pling in any program m e can be pro p erly decided only after
detailed prelim in a ry work, in which a high sam pling freq u en c y is necessary to provide the
inform ation to w hich statistical techniques are applied.
'Once the freq u en c y o f sam pling has been decided, the data obtained should be review ed
regularly so that changes can be made as required. ’
D -17
1 6 .4 D e te r m in a tio n o f c o n fid e n c e in terv a l an d n u m b e r o f sa m p les
D -18
17. A b n o r m a l V a r ia b ility .
18. D uration o f sam pling occasion and com posite sam ples.
‘ I f only the average quality during the p erio d is o f interest, a n d p ro vid ed the determ inand is
stable, it m ay be u se fu lfo r the duration o f collection o f sam ples to be long a n d preferably the
sam e as the p e rio d o f interest. ’
D -1 9
SEC TIO N 4 FLO W M EASUREM ENTS A ND SITUATIONS JU ST IFYIN G FLOW
M EA SU R EM EN TS FOR W ATER QUALITY PURPOSES.
19 Introduction
19.1 General
N ot applicable to gap analysis.
'In treatm ent processes, the pattern o f water m ovem ent in tanks affects the m ixing o f the contents
a n d the settling o f suspended m atter a n d should be considered to ensure representative sam ples
are collected. ’
D-20
20. J u s tific a tio n fo r flo w m e a su r em en ts in w a te r q u a lity co n tro l.
‘ A sam pling program m e fo r a river or estuary sh o u ld attem pt to sample the same body o f water
as it m oves along the watercourse. ’
D-21
D O U C M EN T No. 2:
Sum m ary o f the Corrective Actions required in order to com ply with:
I.S. E N 25667-1:1994 Water Quality - Sam pling - P a rt 1: G uidance on the design o f
sam pling program m es (ISO 5667-1:1980).
Note: F or the corrective actions to be im plem ented effectively s ta ff training shall have to be
p aram ount in a ll cases.
1. Identify and docum ent the preservation m ethod(s) required for the various samples.
Im plem ent preservation methods where required (ISO 5667-1:1980 Section 1 (3)).
3. State the objectives o f the sampling program m es (ISO 5667-1:1980 Section 1 (3)).
4. Identify and docum ent the degree o f detail and precision that will be adequate for analytical
field results. O utline the manner in which the results are to be expressed and presented, as
part o f the sam pling program m e (ISO 5667-1:1980 Section 1 (3)).
5. Com pile list o f param eters o f interest with reference to the relevant analytical procedure (ISO
5667-1:1980 Section 1 (3)).
7. A m end sam pling SOPs to include measures taken to elim inate or m inim ize any changes in
the concentration o f determ inands o f interest that may be produced by the sampling process
itself e.g.
a) Sam pling bottles are not reused
b) The sam pling bottle is attached to the long-arm sampler.
c) Sam ples are transported to the laboratory in a cooler box
(ISO 5667-1:1980 Section 1 (5.3)).
8. Identify and docum ent which samples are required to be chem ically preserved. Im plem ent
system o f chem ical preservation (ISO 5667-1:1980 Section 1 (5.3)).
10. A m end SOP N o .’s 8, 9,10 and 11 to include reference to the safety statem ent for the
environm ent section (ISO 5667-1:1980 Section 2 (7.1)).
11. A m end SOP No. 5 and 47 to include general reference w ith regard to safety and reference to
the safety statem ent for the environm ent section (ISO 5667-1:1980 Section 2 (7.1)).
12. A m end sam pling program m e to include how sam pling sites w ere selected e.g. access in all
w eather (ISO 5667-1:1980 Section 2 (7.5)).
D -22
13. Reassess river sam pling locations to take flow stations into account (ISO 5667-1:1980
Section 2 (8.1)).
14. R eview and am end, if required SOP N o .’s 8, 10, 11, and 47 with regard to ensuring sam ples
are taken from turbulent, well-m ixed liquids (ISO 5667-1:1980 Section 2 (8.3)).
15. Review and am end SOP N o .’s 10 and 11 to include details on how to handle liquids that may
be corrosive or abrasive (ISO 5667-1:1980 Section 2 (8.7)).
16. R eview w astew ater sampling locations to ensure sufficient turbulence is present at all sites.
Identify the sites w here there is not sufficient turbulence. D evelop and docum ent m ethod for
taking sam ples across the full cross-section o f the flow at these sites. Amend, if required,
SOP N o .’s 10 an d l 1 (ISO 5667-1:1980 Section 2 (8.9)).
17. Review and am end SOP N o .’s 6, 10, 11 or 47 and the field sheets to include requirem ent to
note m eteorological conditions (ISO 5667-1:1980 Section 2 (8.13)).
18. Identify appropriate m ethod to assess stratification at a river sam pling location. A ssess each
river sam pling location for stratification. Take appropriate m easures follow ing the results o f
the assessm ent (ISO 5667-1:1980 Section 2 (9.3.1)).
19. A ssess each river sam pling location for stratification (ISO 5667-1:1980 Section 2 (9.3.1)).
Take appropriate m easures following the results o f the assessm ent (ISO 5667-1:1980 Section
2 (9.3.1)).
20. Review river sam pling locations selected to ensure they provide representative sam ples i.e.
w here m arked quality changes are likely to occur or w here there are im portant river uses.
A m end sam pling program m es accordingly (ISO 5667-1:1980 Section 2 (9.3.2)).
21. Identify an appropriate m ethod to assess the effects o f a discharge on a river i.e. the selection
o f both upstream and dow nstream points. Document m ethod (ISO 5667-1:1980 Section 2
(9.3.2), (9.8.2)).
22. Prepare SOP detailing how samples are to be taken from storage reservoirs (ISO 5667-
1:1980 Section 2 (9.5)).
23. A m end s-ampling program m e detailing how the drinking w ater sam pling points are selected
(ISO 5667-1:1980 Section 2 (9.8.1)).
24. A m end SOP No. 6 to include details regarding selection o f drinking w ater sam pling taps (ISO
5667-1:1980 Section 2 (9.8.1)).
25. Identify the aspects w hich have to be considered w ith regard to the sam ple pipe and include
findings in SOP No. 6 (ISO 5667-1:1980 Section 2 (9.8.1)).
26. A m end SOP N o .6 to give precise details on the aseptic technique to be used w hen taking
m icrobiological sam ples (ISO 5667-1:1980 Section 2 (9.8.1)).
D -23
27. Include statem ent in SOP No. 6 stating that anti-splash devices should be rem oved before
sam pling and that m ixer taps are not recom mended for sam pling (ISO 5667-1:1980 Section 2
(9.8.3)).
29. Amend SOP No. 10 clearly stating exact location w here an influent sample should be taken
(ISO 5667-1:1980 Section 2 (12.1.1)).
30. Prepare SOP for sampling o f storm sewage and surface ru n -o ff taking the requirem ents o f
ISO 5667-1:1980 Section 2 (13) into account.
31. Amend sam pling program m e to clearly identify the source used to calculate the frequency o f
analysis (ISO 5667-1:1980 Section 3 (16.1)).
32. A scertain the need to statistically determ ine the num ber o f sam ples required for a given
confidence interval. I f required carry out statistical analysis, docum ent results and amend
sam pling program m e as required (ISO 5667-1:1980 Section 3 (16.4)).
33. Identify w hether the w ater bodies sampled have random o r system atic variations in quality.
D eterm ine statistically the number and times o f sam pling
(ISO 5667-1:1980 Section 3 (16.5)).
34 Prepare SOP detailing the procedure for sam pling during abnorm al conditions (ISO 5667-
1:1980 Section 3 (17)).
35. Amend SOP No. 49 to include details on the reporting o f the results from sam pling during
abnormal conditions (ISO 5667-1:1980 Section 3 (17)).
36. A m end SOP No. 10 to include details on the exact sam pling location from treatm ent aeration
tanks (ISO 5667-1:1980 Section 3 (19.2)).
D -24
D O C U M EN T No. 3:
Gap Analysis results for I.S. E N 25667-2:1994 Water quality - Sam pling- P art 2:
G uidance on sam pling techniques (ISO 5667-2:1991).
4.1 General
‘Certain param eters, such as the concentration o f dissolved gases, sh o u ld be m easured in situ i f
possible, to obtain accurate results. '
D -25
4.4 C ontinuous sam ples
N ot applicable to gap analysis.
Com posite sam ples are valuable in cases when com pliance with a lim it is based on the average
w ater quality. ’
D -26
5. Types of sam pling
‘ There are m any sam pling situations, some o f which can be satisfied by taking sim ple spot
sam ples w hereas others m ay require sophisticated instrum ental sam pling equipment. ’
6.1 M aterials.
6.1.1 General
‘The sam ple container has to presence the com position o f the sam ple from losses due to
adsorption a n d volatilization, or fro m contamination by fo re ig n substances. ’
‘The sam ple container used to collect a n d store the sam ple sh o u ld be chosen after considering,
fo r example, resistance to temperature extremes, resistance to breakage, ease o f g o o d sealing
a n d reopening, size, shape, mass, availability, cost, p o te n tia l f o r cleaning a n d re-use, etc. ’
D -27
6.1.1 General (ctd .)
'High density polyethylene is recom m end fo r silica, sodium, total alkalinity, chloride, specific
conductance, p H a n d hardness determ inations in water. ’
The sam ple containers used to collect a n d store the sam ples sh o u ld be selected by taking into
account the follow ing predom inant criteria:
a) M inim isation o f contam ination o f the water sam ple by the m aterial o f which the container or
its stopper is made.
b) A bility to clean a n d treat the walls o f the containers, to reduce surface contam ination by
trace constituents such as heavy metals.
c) C hem ical a n d biological inertness o f the m aterial o f which the container is made, in order to
p reven t or m inim ize reaction between constituents o f the sam ple a n d the container.
d) Sam ple containers m ay also cause errors by adsorption o f determ inands. Trace m etals are
p articularly liable to this effect but other determ inands (eg detergents, pesticides, phosphate)
m ay also be subject to error. ’
D -28
6.1.2 Sam pling lines
'The guidelines f o r the selection o f m aterials fo r sample containers also apply to sam pling lines. ’
6.2.1 General
’P olyethylene a n d borosi/icate glass bottles are suitable f o r conventional sam pling f o r the
determ ination o fp h y sic a l a n d chem ical param eters o f natural waters.
Screw cap, narrow -m outhed a n d wide-m outhed bottles sh o u ld be fitte d with inert plastics
stoppers/caps or g ro u n d glass stoppers.
I f the sam ples are transported in a case to a laboratory f o r analysis, the lid o f the case should be
constructed to p reven t loosening o f the stopper which co u ld result in spilling a n d or
contam ination o f the sample. ’
D-29
6.2.3 Trace organic contam inants
' The sam ple bottles sh o u ld be made o f glass as virtually a ll p la stics containers interfere with the
highly sensitive analysis. The closure should be o f glass or polytetrafluoroethylene ’.
‘The sam ples sh o u ld rem ain sealed until opened in the laboratory a n d should be co vered to
p revent contam ination. ’
D-30
6 .3 S a m p lin g e q u ip m e n t fo r p h y sic a l o r c h e m ic a l c h a r a c te r is tic s .
6.3.1 Introduction
‘ The volume o f sam ple collected should he sufficient f o r the required analyses a n d fo r any
repeat analyses. ’
D -3 1
6 .3 .2 E q u ip m e n t fo r sp o t sa m p lin g
6.3.2.1 G eneral
The simplest equipm ent for taking surface samples is a bucket or wide m outhed bottle dropped
into a body o f w ater and hauled out after sampling.
D -3 2
6.7 Equipm ent for sam pling o f dissolved gases (and volatile m aterials)
'Samples suitable f o r accurate determ inations o f dissolved gases sh o u ld only be obtained with
equipm ent which collects a sample by displacem ent o f water, rather than air, fr o m the sampler.
I f pum ping system s are u s e d fo r the collection o f dissolved g a s samples, it is essential that the
w ater be p u m p e d in such a way that the pressure a p p lied to it does not drop significantly below
atm ospheric pressure. The sample should be p u m p ed directly into the storage or analysis bottle,
which should be flu s h e d by an am ount equal to a t least 3 tim es its volume before starting
analysis or stoppering the bottle.
I f approxim ate results are acceptable, samples f o r dissolved oxygen determ inations m ay be
collected using a bottle or a bucket. The error introduced into these determ inations by contact
between the sam ple a n d the air varies with the degree o f saturation o f the g a s in the water. ’
‘Where sam ples are collected in a bottle from a tap or p u m p outlet, a flexib le inert tube which
delivers liquid to the bottom o f the bottle is recom m ended to ensure that liq u id is displaced from
the bottom o f the bottle a n d that m inim al aeration occurs. ’
D -33
7 I d e n tific a tio n a n d reco rd s
7.1 General
‘The source o f the sample a n d the conditions under which it w as collected sh o u ld be recorded
a n d attached to the bottle im m ediately after filling.
The results o f any on-site analyses carried out sh o u ld also be included in a report with the
sample. L abels a n d fo r m s should always be com pleted at the time o f sam ple collection. ’______
Findings N on-C onform ance C orrective Action
1. All bottles are labelled at time o f 1. As per findings No. 2 1. Am end SOP No. 47
sampling as required under SOP and 4. to include details
N o .’s 6, 8, 10 and 11 w ith regard to
2. SOP N o 47 does not include any labelling o f sample
details w ith regard to labelling o f bottles and
sample bottles. com pletion o f a
3. Results o f on-site analyses are sample report form.
included in a field report. There 2. Amend SOP No. 6,
are pre-prepared sample report 8, 10 and 11 to
forms for the various sample include details with
bodies. regard to recording
4. N o reference in SOP N o .’s 6, 8, on-site analyses on
10, 11 or 47 with regard to a sample report
recording on-site analyses on a form.
sam ple report form._____________
7.2 Reports.
‘A t least the fo llo w in g inform ation should be in clu d ed in the sam pling report:
a) L ocation (and name) o f sam pling site, with coordinates a n d any other relevant locational
inform ation.
b) D etails o f the sam pling point
c) D ate o f collection
d) M e th o d o f collection
e) Time o f collection
f) N am e o f collector
g) W eather conditions
h) N ature o f pretreatm ent
i) Preservative or stabiliser added
j ) D ata genera ted in the fie ld '
D -34
D O C UM ENT No.4:
Sum m ary o f the C orrective Actions required in order to com ply with: I.S. E N 25667-
2:1994 Water quality - Sam pling- Part 2: Guidance on sam pling techniques (ISO 5667-
2:1991).
Note: For the corrective actions to be im plem ented effectively s ta ff training sh a ll have to be
param ount in a ll cases.
1. Amend the relevant sampling SOPs to include details on the param eters to be m easured in
situ (ISO 5667-2:1991 (4.1)).
2. Amend sam pling program m e to include details on when spot sam ples are to be taken (ISO
5667-2:1991 (4.2), (5)).
3. Amend sam pling program m e to include details on when com posite sam ples are to be taken
(ISO 5667-2:1991 (4.6), (5)).
4. Develop, docum ent and implement method to determ ine w hether the param eters o f interest
vary significantly during the com posite sam pling period (ISO 5667-2:1991 (4.6)).
5. A m end SOP No. 6 to include details with regard to sam pling large volum es e.g. for
Cryptosporidium analysis (ISO 5667-2:1991 (4.7)).
6. D ocum ent in the relevant sampling SOPs the sam pling container to be used for various
analyses and record the type o f container used (ISO 5667-2:1991 (6.1.1)).
7. Develop and im plem ent system for selection and purchase o f sam pling containers, including
details on caps to be used for the various analyses (ISO 5667-2:1991 (6.1.1), (6.2.1), (6.2.3),
(6.5)).
8 Identify and docum ent the analytes which are light sensitive. Im plem ent system to ensure
the correct containers are used for sampling these analytes (ISO 5667-2:1991 (6.1.1)).
9. D ocum ent procedure for the selection o f sam pling lines (ISO 5667-2:1991 (6.1.2)).
10. A m end relevant sampling SOPs to include details w ith regard to filling the sam ple bottle
(ISO 5667-2:1991 (6.2.2)).
11 D ocum ent procedure for the selection o f sam pling containers for m icrobiological
exam ination (ISO 5667-2:1991 (6.2.4)).
12 A m end SOP N o .’s 6, 8, 10, 11 and 47 to include details on sealing the sam ple (ISO 5667-
2:1991 (6.2.4)).
13. Amend SOP N o ’s 6, 8, 10 and 11 to include details on the volum e o f sam ple(s) to be
collected for the determ ination o f various analytes (ISO 5667-2:1991 (6.3.1)).
14. D ocum ent a procedure for the selection o f effective sam plers (ISO 5667-2:1991 (6.3.1)).
D -35
15. Assess the accuracy required when determining dissolved gases. I f the current in-situ
analytical m ethods do not yield sufficient accuracy im plem ent appropriate m ethod (ISO
5667-2:1991 (6.7)).
16. Develop, docum ent and implement method with regard to the correct filling o f bottles from
taps or pumps, using flexible inert tubes (ISO 5667-2:1991 (6.7)).
17. Amend SOP No. 47 to include details with regard to labelling o f sam ple bottles and
com pletion o f sample report form (ISO 5667-2:1991 (7.1)).
18. Amend SOP No. 6, 8, 10 and 11 to include details with regard to com pletion o f sam ple report
forms (ISO 5667-2:1991 (7.1)).
19. Amend the field sample report forms to include the inform ation specified in ISO 5667-
2:1991 (7.2).
D -36
D O C U M E N T N o . 5:
ISO 5667-3:1994 W ater quality - Sampling- P art 3: G uidance on the preservation and
handling o f sam ples
D -3 7
3.1 General considerations (ctd..)
‘In every case, the m eth o d o f storage should be com patible with the various analytical
techniques f o r which it w ill be used. '
D -38
3.2.1 Filling the container (ctd..):
‘For m icrobiological examination, the sample container sh o u ld not be fille d to the brim so that
an air space is left after insertion o f the stopper. This aids m ixing before exam ination an d
avoidance o f accidental contamination. ’
D -3 9
3.2.2 Use o f appropriate containers (ctd..):
'It is preferable to reserve a set o f containers fo r a particular determinane!. ’
‘B lank sam ples containing distilled water should alw ays be taken, p reserved a n d analysed as a
check on the suitability o f the choice o f container a n d cleaning procedure. '
'For analysis o f trace quantities o f chem ical constituents o f surface or waste water, it is usual to
clean new containers thoroughly in order to m inim ize possible contam ination o f the sam ple ; the
type o f cleaner u sed a n d the container m aterial vary according to the constituents to be
analysed. '
D -4 0
3.2.3.1 For samples for chemical analysis (cld.)
'In general, new glassM are should be rinsed with w ater containing a detergent in order to
rem ove dust a n d residues o f packing material, fo llo w ed by through rinsing with distilled or
deionized water.
For general trace analysis, the bottles should be fille d with l m o l l solution o f nitric a cid or
hydrochloric a cid a n d left to soak fo r at least one day, fo llow ed by rinsing with distilled or
deionized water.
F or the determ ination o f phosphates, silicon, boron a n d surfactants, detergents should not be
used fo r cleaning purposes. ’
D -41
3.2.3.3 For sam ples f o r m icrobiological analysis
‘The container sh o u ld be able to withstand a sterilisation tem perature o f 1 75°C fo r 1 hour a n d
should not produce/release at this temperature any chem icals w hich w ould either inhibit
biological activity, induce m ortality or encourage growth. ’
D -42
3.2.4 Cooling or freezin g o f the samples
‘The sam ple sh o u ld be kept at a temperature lower than that du rin g fillin g . Containers should be
almost, but not completely, filled.
C ooling or fre e zin g o f sam ples is only truly effective i f it is app lied im m ediately after the
collection o f the samples.
C ooling cannot be considered as a m eans o f long-term storage, particularly in the case o f waste
w ater samples.
In general, fre e zin g allow s an increase in the p e rio d o f storage. Nevertheless, it is necessary to
control the fre e zin g a n d thawing technique fu lly in order to return the sample to its initial
equilibrium after thawing.
D -4 3
3.2.5 Filtration or centrifuging of samples
'Suspended mailer, sediment, algae and other m icro-organism s m ay be removed, either at the
time o f taking the sam ple or immediately afterwards, by filtration o f the samples, through filter
p a p er or m em brane filte r or by centrifuging.'
'It is essential that the filte r is not a cause o f contam ination a n d is carefully w ashed before use,
but in a m anner consistent with the fin a l m ethod o f analysis.
M em branes sh o u ld be used with caution as various heavy m etals a n d organic m aterial m ay be
adsorbed onto the m em brane surface a n d soluble com pounds w ithin the m em brane can be
leached out into the sample. ’
D -44
3.2.6 Addition of preservatives
'Certain preservatives n eed to be used with caution, considering the danger involved in their
handling. O perators should be w arned o f these dangers a n d the w ays o f pro tectin g themselves
fr o m them. ’
‘It is essential that the preservatives used do not interfere d u rin g the determ ination; tests
intended to check their com patibility are necessary in cases o f doubt. A n y dilution o f the sample
with a d d ed p reserva tives sh o u ld be taken into account during the analysis a n d calculation o f
result.
It is preferable that the addition o f preservatives be m ade using sufficiently concentrated
solutions so that only sm all volum es are necessary.
The addition o f these agents can also m odify the chem ical or p h ysica l nature o f the constituents
a n d it is therefore necessary that these m odifications are n o t incom patible with the objectives o f
later determ inations.
It is essential to carry out a blank test, particularly determ inations o f trace elements, to take into
account possible introduction o f an additional am ount o f the elem ent to be determ ined. ’
D -45
3 .3 R e c o m m e n d a tio n s
‘E ach analyst sh o u ld therefore verify, taking into account particularly the m ethod o f analysis
which he intends to use, whether the suggestions in table 1 to 5 are suitable f o r the sam ple with
which he is concerned. ’
‘C ontainers hold in g the sam ples should be m arked in a clear a n d durable m anner in order to
p erm it identification without am biguity in the laboratory. ’
‘A dditionally, it is necessary to note, a t the m om ent o f sampling, num erous details which w ill
p erm it a correct interpretation o f the inform ation obta in ed (date a n d hour o f sampling, nam e o f
person sampling, nature a n d am ount o f preservative added). ’
D -46
4 I d e n tific a tio n o f sa m p le s (c td ..)
‘Special sam ples o f anom alous m aterial should he clearly m a rked a n d accom panied by a
description o f the observed anomaly. It is essential that sam ples containing hazardous or
potentially hazardous materials, fo r example acids, are clearly identified as such. ’
5 Transport of samples
‘Containers hold in g sam ples m ust be p ro tected a n d sea led in such a w ay that they do not
deteriorate a n d do not lose any p a rt o f their contents during transport. P ackaging sh o u ld protect
the containers fr o m p ossible external contam ination a n d breakage, particularly near the
opening, a n d sh o u ld not itse lf be a source o f contamination. ’
D -47
5 T r a n s p o r t o f sa m p le s (c td ..)
‘D uring transportation, the sam ples should be kept as co o l a s practicable a n d p ro tected fro m
light, with each sam ple p la c ed inside an individual w a terp ro o f container i f possible. '
‘I f time o f travel exceeds the maximum recom m ended p resen ta tio n time before analysis then the
sam ples sh o u ld still be analysed a n d the time between sam pling a n d analysis reported a fter
consultation with the scientist interpreting the analytical results. ’
D -48
6 Reception of samples in the laboratory (ctd..)
‘It is recom m ended that the count o f sample containers received he verified against the record o f
the num ber o f sam ple bottles sent f o r each sample. ’
D -4 9
DOCUMENT No. 6:
Summary of the Corrective Actions required in order to comply with: ISO 5667-3:1994
Water quality - Sam pling- P art 3: Guidance on the presentation a n d handling o f sam ples
Note: F or the corrective actions to be im plem ented effectively s ta ff training shall have to be
param ount in a ll cases.
1. Amend SOP N o .’s 6, 8, 10, 11 and 47 to include field analyses, w hich are currently carried
out (ISO 5667-3:1994 (3.1)).
2. Assess the need to preserve samples and im plem ent appropriate m ethod if necessary (ISO
5667-3:1994 (3.1)).
3. Amend SOP N o .’s 6, 8, 10 and 11 to include details on the sam ple transportation from
sam pling site to laboratory in cooler boxes (ISO 5667-3:1994 (3.1), (3.2.4), (5)).
4. Amend SOP No. 43 to include details on the max. length o f sam ple storage for the various
analyses, m aking reference to guidelines in Standard M ethods (20th Ed.) (ISO 5667-3:1994
(3.1)).
5. A m end SOP N o .’s 10, 11 and 47 stating that the sam ple containers for physico-chem ical
param eters shall be filled com pletely and capped in such a w ay that there is no air above the
sample.
Amend SOP No. 6 stating that for microbiological exam ination, the sam ple container should
not be filled to the brim (ISO 5667-3:1994 (3.2.1)).
6. Amend SOP N o .’s 6, 8, 10, 11 and 47 stating that disposable H D PE sam pling bottles are to
be used for physico-chem ical param eters (ISO 5667-3:1994 (3.2.2)).
7. Amend SOP N o .’s 10 and 47 stating that sample containers, for physico-chem ical
m onitoring, shall be rinsed prior to filling (ISO 5667-3:1994 (3.2.2)).
8. Prepare SOP detailing the exact type o f sam pling container that is to be used for each analyte
o f interest (ISO 5667-3:1994 (3.2.2), (3.2.3.2), (3.2.3.3)).
9. Im plem ent system for the taking, preserving and analysing o f blank samples, to act as a
check on the suitability o f the choice o f container and cleaning procedure. A m end SOP
N o .’s 6, 8, 10, 11 and 47 accordingly (ISO 5667-3:1994 (3.2.2)).
10. Im plem ent and docum ent the method o f cleaning the various types o f sam ple containers, for
the various analytes o f interest (ISO 5667-3:1994 (3.2.3.1) (3.2.3.2) (3.2.3.3)).
11. Develop, docum ent and im plem ent a procedure for the freezing and thaw ing o f sam ples (ISO
5667-3:1994 (3.2.4)).
12. Identify and docum ent which sam ples are to be filtered or centrifuged. D evelop, docum ent
and im plem ent a procedure for the filtration/ centrifuging o f sam ples at the tim e o f taking the
sample o r im m ediately afterw ards (ISO 5667-3:1994 (3.2.5)).
D -50
13. Im plem ent a procedure for assessing w hether the filter type used to filter samples is a cause
o f contam ination (ISO 5667-3:1994 (3.2.5)).
15. Develop, docum ent and implement a procedure to verify w hether or not the preservation
suggestions in Table 1 to 5 o f ISO 5667-3:1994 are suitable for the sample w ith w hich it is
concerned (ISO 5667-3:1994 (3.3)).
16. A m end SOP N o.47 stating w hat details are required to be labelled on the sam pling bottles
(ISO 5667-3:1994 (4)).
17. Amend SOP N o .’s 6, 8, 10, 11 and 47 stating that the appropriate field sheet is to be
com pleted at the tim e o f sampling (ISO 5667-3:1994 (4)).
18. A m end field sheets to include details regarding tim e o f sam pling (ISO 5667-3:1994 (4)).
20. Develop, docum ent and implement a procedure for situations w here the tim e-of-travel
exceeds the max recom m end preservation tim e (ISO 5667-3:1994 (5)).
21. A m end SOP N o .’s 6, 8, 10, 11 and 47 stating that all sam ples are to be stored in a refrigerator
on arrival to the laboratory, if im m ediate analyses are not being carried out (ISO 5667-
3:1994 (6)).
22. Develop, docum ent and im plem ent procedure for verifying that the num ber o f sam ples
received at the laboratory coincides with the num ber recorded on the field sheet (ISO 5667-
3:1994 (6)).
D -5 1
DOCUMENT No. 7:
Gap Analysis results for: ISO 5667-5: 1991 Water quality - Sam pling- P art 5:Gui(lance on
sam pling o f drinking w ater and water used f o r fo o d an d beverage processing.
1. Scope.
‘I t is im portant that the sam pling purpose be defined as accurately as possible a n d that the
m easurem ents provide the required inform ation in the m ost efficient a n d statistically
representative manner. ’
3. Sampling Equipment.
M akes reference to ISO 5667-2 and ISO 5667-3.
4 Sampling procedure
D -52
4.1 S a m p lin g lo c a tio n (ctd ..)
'On-site analysis is recom m ended particularly f o r such determ inands as odour, taste, pH,
chlorine, ozone, dissolved oxygen, a cid (base) capacity, carbon dioxide, electrical conductivity
a n d f o r the assessm ent o f temperature. ’
‘Before transporting the sample to the laboratory, the appropriate p reservation technique has to
be applied. '
D -53
4.1.1 Service reservoir
‘Sam ples sh o u ld be collected fro m the inlet and outlet pipe, as d o s e as possible to the service
reservoir. G enerally 2 m in or 3 m in o ffre e flo w sh o u ld be allow ed to flu s h out any stale water
within the sam pling line before taking a sample.
I f it is essential to take dip samples (i.e. no sam pling valve on the outlet pipe), special care
should be taken to ensure that the sam pling operation does not introduce debris into the water
a n d that equipm ent is sterilized before sampling. ’
D -54
4.1.3 D isinfection plant
‘Sam ples from the influent to the disinfection/oxidation p ia n i should be taken as d o se as
possible to the plant. Sam ples o f the effluent should be collected after, allow ing fo r appropriate
contact p e r io d betw een w ater a n d disinfectant oxidant. ’
‘Sam pling from hydrants should be avoided wherever p o ssib le; i f this is unavoidable special
disinfection precautions are required. '
D -55
‘F or m icrobiological p w p o ses, sam pling taps should be sterilized by fla m e or alternative
m ethods o f equivalent efficiency. ’
‘When collecting a sam ple fr o m a distribution system the flu sh in g time should be in accordance
with the sam pling purpose, 2min. to 3min. being generally sufficient. Som etim es it m ay be
necessary to allow the w ater to flo w fr e e ly fo r a s long as 30 min. before collecting the sample. ’
D -56
‘I f dissolution o f m aterials fro m the pipework, or grow th o f m icro-organism s within the
pipew ork are being investigated, samples should be taken fr o m Ihe initial draw-off. ’
D -57
‘F or m icrobiological sampling, m etal taps should be fla m e d a n d p la stic taps should be
disinfected using an available chlorine solution. 'All fittin g s should be rem oved fro m the taps
prior to flu sh in g a n d sampling.
4.1.6 Sam pling o f bottled drinking w ater and w ater in tanks and containers for bulk storage on
trains, aircraft and ships.
N ot applicable to gap analysis.
D -58
5 S a m p lin g te c h n iq u e
D-59
5 .3 S a m p lin g fo r m ic r o b io lo g ic a l a n a ly sis (c td ..)
'The w ater should be allow ed to flo w fr e e ly fr o m the tap or the outlet. The sam pling container
should be fille d directly.
A fter sam pling the sam pling container should be closed tightly. C ontam ination o f the stopper
should be avoided. ’
'The sam pling outlet should, i f necessary, be sterilized by fla m e or other methods. ’
'W ide-mouth sam ple containers o f at least 300m l capacity with g ro u n d g la ss stoppers or screw
caps should be used. The sam ple containers should be sterilized f o r 20 m in a t 120° C a n d 200
kPa above am bient p ressure in a wet autoclave.
D uring sterilization a n d sample storage, the m aterials sh o u ld not p roduce or release chem icals
which inhibit or increase m icrobiological activity. ’
D -60
5.4 Sampling for virological analysis
N ot applicable to gap analysis.
6 Safety precautions
'Il is essential that p ersonnel responsible fo r the design o f sam pling program m es a n d fo r
carrying out sam pling operations ensure that the requirem ents o f relevant national safety
Regulations are taken into account a n d com plied w ith a n d that the sam pling p erso n n el are
inform ed o f the necessary precautions to be taken in sam pling operations.
D -61
7.2 Handling of samples
‘A s different analytical methods m ay require different m ethods o f preservation, distribution o f
the sam ple into several containers m ay be required. To m inim ize changes in the sam ple during
collection, storage a n d transport, these operations should be carried o u t in a s short a time
p e r io d a n d as soon after sam pling as possible. ’
‘I f contact o f the sam ple with air has to be avoided the sam ple container sh o u ld be fille d
com pletely a n d then im m ediately stoppered.
I f sam ples require vigorous m ixing before taking p o rtio n s f o r analyses, the sam ple container
should not be fille d com pletely or, i f air has to be avoided a fe w p ie c e s o f clean, sterile, inert
solids sh o u ld be p la c e d in the sam pling container, f o r exam ple so lid beads or a m agnetic
strirrer. ’
D -62
‘I f filtration is necessary the sample should be filte re d during or im m ediately after collection to
m inim ize any changes that m ay occur in the sample. ’
‘Contam ination o f the outside o f the sample containers, pa rticu la rly necks a n d stoppers sh o u ld
be avoided.
The sam pling containers should be secured fo r transport.
Unnecessary agitation or exposure to light during transport sh o u ld be avoided. ’
'The sam ples sh o u ld be stored in a clean room, w hich can be kept dark a n d co o l a n d in w hich no
chem ical reagents are used, separated from the laboratory. ’
D -63
8 S a m p le id e n tific a tio n an d record s
'Imm ediately after collection o f a sample, the container sh o u ld be labelled so that the sample is
easily identifiable. ’
‘D escribe each sam pling location. I f the same location is u sed perm anently, it is not necessary to
repeat a ll details every time. In this case only a statem ent o f the on-site m easurem ents a n d
variables such as w eather conditions a n d unusual observations n eed be recorded
When sam pling f o r specific reasons (e.g. customer com plaint) deta iled inform ation should be
given including the reasons f o r sampling. ’
D -64
9 Q u a lity a s su r a n c e o f sa m p lin g an d tr a in in g o f sa m p lin g p e r so n n e l
‘P ersonnel p erfo rm in g the sam pling should be instructed to cn’o id contam ination o f sam ples a n d
containers. Particular im portance should be given to the correct m easurem ent o f those
determ inands that are carried out on site, and to their correct recording. ’
D -65
D O C U M E N T No. 8:
Sum m ary o f the Corrective Actions required in order to com ply with: ISO 5667-5: 1991
W ater quality - Sam pling- P art 5:Guidance on sam pling o f drinking w ater and w ater used f o r
f o o d an d beverage processing.
Note: F or the corrective actions to be im plem ented effectively s ta ff training shall have to be
p aram ount in a ll cases.
1. D efine sam pling purpose in the sampling program m es (IS 0 5 6 6 7 -5 :1999 (1)).
2. A m end SOP No. 6 to include a list o f all the param eters, w hich are m easured on site
(ISO 5667-5.1999 (4.1)).
3. D evelop, docum ent and im plem ent method o f on-site analysis for odour (IS 0 5 6 6 7 -5 :1999
(4.1)).
4. Identify and docum ent which samples are to be preserved on-site. D ocum ent method o f
preservation and im plem ent system to record w hich sam ples w ere preserved (IS 0 5 6 67-
5:1999 (4.1), (7.2)).
5. D evelop, docum ent and implement procedure for sam pling from service reservoirs
(IS 0 5 667-5.1999 (4.1.1)).
6. Develop, docum ent and im plem ent procedure for sam pling from w ater treatm ent plants
(IS 0 5 6 6 7 -5 :1999 (4.1.2)).
7. Develop, docum ent and im plem ent procedure for assessing the efficiency o f the disinfection
plant at w ater treatm ent plants (1S05667-5:1999 (4.1.3)).
8. Identify and map predeterm ined sampling points for the various w ater supplies (IS 0 5 6 6 7 -
5:1999 (4.1.4)).
9. Develop, docum ent and im plem ent procedure for sam pling from hydrants (ISO 5667-5:1999
(4.1.4)).
10. A m end SOP No. 6 stating that w ater samples should be taken in the turbulent zone o f a pipe,
if possible W hen taking the sample w here there is a very low flow, care should be taken that
disturbance o f sedim entary material does not occur. I f this cannot be avoided, a sufficient
volum e o f w ater should be flushed or a sufficient tim e allow ed for a steady state to occur
(ISO566 7-5:1999 (4.1.4)).
11. D ocum ent the flushing period required for the various sam pling purposes (1S05667-5:1999
(4.1.5)).
12. A m end SQP No. 6 to include circum stances w here a system may have to be flushed for
extended periods (IS 0 5 6 6 7 -5 :1999 (4.1.4), (4.1.5))).
D -66
13. Develop, docum ent and implement procedure for investigating the dissolution o f m aterials
from pipew ork, or growth o f microorganisms w ithin pipew ork (IS 0 5 6 6 7 -5 :1999 (4.1.4),
(4.1.5)).
14. A ssess the need to disinfect using a chlorine solution versus alcohol. Amend SOP if
necessary (ISO S667-5:1999 (4.1.5)).
15. Am end SOP N o .6 to include the requirement to rem ove all fittings from taps prior to flushing
and sam pling (IS 0 5 6 6 7 -5 :1999 (4.1.5)).
16. Am end SOP No. 6 to include details on filling and sealing the sam ple container (IS 0 5 6 6 7 -
5:1999(5.1), (5.3)).
17. A m end SOP No. 6 to include circumstances w here sam ples may have to be taken from a
system that has been stagnant (1S05667-5:1999 (5.3)).
18. A m end SOP No. 6 to ensure that only bottles o f at least 300ml capacity are used (IS 0 5 6 6 7 -
5:1999 (5.3)).
19. Develop, docum ent and im plem ent SOP detailing how bottles are to be sterilized and a
m ethod to assess if materials used produce or release chem icals (1S05667-5:1999 (5.3)).
20. Amend drinking w ater SOP No. 6 to include reference to safety precautions required, w hen
sampling drinking w aters (ISO5667-5:1999 (6)).
21. Amend SOP No. 6 m aking reference to the volum e o f sample that is to be collected, for the
various param eters (IS 0 5 6 6 7 -5 :1999 (7.1)).
22. Develop, docum ent and implement method to ensure sam ples are stored in the correct
containers as soon as possible after sampling (ISO 5667-5:1999 (7.2)).
23. Identify and docum ent the samples with w hich contact with the air m ust be avoided and
those that require vigorous mixing before taking portions for analyses. D ocum ent procedure
for dealing w ith both types o f samples (IS 0 5 6 6 7 -5 :1999 (7.2)).
24. Identify the sam ples w hich are required to be filtered im m ediately after collection. D evelop,
docum ent and im plem ent procedure for filtering sam ples and train sam pling personnel
(ISO 5667-5:1999 (7.2)).
25. A m end SOP No. 6 to include details regarding the sealing o f sam ple containers and
transportation o f sam ples to the laboratory (IS 0 5 6 6 7 -5 :1999 (7.2)).
26. Amend SOP No. 6 to include details on storage o f sam ples in the laboratory (1S05667-
5:1999 (7.2)).
D -67
4. A m end SOP No. 6 to include requirement to com plete field sheet (1S05667-5:1999 (8)).
5. Develop, docum ent and implement quality assurance program m e including system o f blanks
(1805667-5:1999 (9)).
6. D ocum ent the procedure used for training sam pling personnel w ith regard to correct
sam pling techniques and on-site measurem ent techniques (IS 0 5 6 6 7 -5 :1999 (9)).
D -6 8
D O C U M E N T No. 9:
Gap Analysis results for ISO 5667-6: 1990 Water quality - Sam pling- Part 6: G uidance on
sam pling o f rivers a n d streams.
1. Scope:
‘A definition o f the p urpose o f sam pling is an essential prerequisite to identifying the principles
to be applied to a p a rticular sam pling problem . ’
3. D efinitions
N ot applicable to gap analysis.
4.1 M aterials
‘G lass containers sh o u ld be used when organic constituents are to be determined. '
‘Polyethylene containers are preferable f o r sam pling those determ inands that are m ajor
constituents o f glass (e.g. sodium, potassium , boron a n d silicon) a n d f o r sam pling o f trace
m etallic impurities.
D -69
4.1 M aterials (ctd..)
H ow ever polyethylene containers m ay not be suitable f o r collecting sam ples to be subjected to
som e trace m etallic analyses (e.g. mercury) a n d these containers sh o u ld only be used i f
prelim inary tests indicate acceptable levels o f contamination. ’
‘I f glass bottles are u s e d fo r storing w eakly buffered water, borosilicate rather than soda-glass
containers sh o id d be chosen. ’
D -70
4.1 M aterials (ctd..)
‘R efer to relevant standard analytical procedures fo r d etailed guidance on the type o f sam ple
container to be used. ’
M icrobiological sam pling bottles: ‘usually have a capacity o f a t least 250m l are fitte d with a
large screw caps, g ro u n d glass or other sterilizable stopper, co vered w ith alum inium fo il. I f
screw caps are used silicone rubber liners capable o f w ithstanding autoclaving at 121° C should
be used inside the cap.
D -71
4.2.1 Surface sam plers (ctd..)
‘I f bacteriological contam ination from the hand is a p o ten tia l problem , a clam p or p o le should
be attached to the bottle. ’
D -72
5 S a m p lin g p r o c e d u r e
D-73
5.1.1.1 Im p o rtan ce o f m ixing (ctd. )
D -74
5.1.2 Choice o f sam pling point
'Problems arise in selecting suitable sam pling sites w henever the determ inands are not
hom ogeneously distributed throughout the water body o f interest. In general, such sam pling sites
are best avoided. I f there is any possibility o f a non-hom ogeneous distribution o f the
determ inands o f interest at the chosen site, experim ental tests on the nature a n d m agnitude o f
any heterogeneity in a ll three dim ensions should be made. ’
D -7 5
5.2 Frequency o f sam pling (ctd..)
‘When using system atic sam pling it is essential to ensure that the freq u en c y o f sam pling does not
coincide with any natural cycle or some other tim e based effect.
It w ill usually be adequate to choose the sam pling tim es in a system atic m anner with sam ples
evenly distributed throughout the p e rio d o f interest. '
D -7 6
5,3.2 M icrobiological sam pling (ctd .)
‘The bottle is then fille d without rinsing a n d the stopper is replaced im m ediately
Sam ples should be taken by holding the bottle by the base a n d p lu n g in g it n eck down w ards to a
depth o f about 0.3m below the surface. The bottle should then be tilted so that the neck p o in ts
slightly upwards, the m outh being directed into the direction o f flow. ’
‘F or som e applications, sam pling w ill be concerned with an assessm ent o f soluble species (e.g.
trace m etals in river water). I f this is the case then it is necessary to separate the ‘d isso lv e d ’
fr o m the ‘u n d isso lved ’ m aterial as soon as practicable after sam pling (preferably a t the
sam pling site before transportation to the laboratory).
Whatever m edium is u sed f o r filtration, it is recom m ended that subsequent results be rep o rted as
‘filterable ' species (quoting the appropriate p o re size o f the filte r) rather than ‘d isso lve d ’
species. ’
D -77
Findings N on-C onform ance C orrective A ction
1. W hen sam pling for soluble 1. As per findings N o .’s 1 1. Develop, docum ent
species the ‘dissolved’ is not and 2. & im plem ent
separated from the ‘undissolved’ method for
m aterial as soon as practicable sampling o f soluble
after sampling. species.
2. Subsequent results are not 2. Im plem ent system
reported as ‘filterable’ species for the reporting o f
nor is the pore size o f the filter samples w hich are
recorded. filtered together
w ith the pore size o f
the filter used.
3. Train sam pling
personnel w ith
regard to sam pling
for soluble species.
'In all cases sam ple containers should be delivered to the laboratory tightly sealed a n d p ro tected
fr o m light a n d excessive heat. ’
D -7 8
5.4 Transport stabilization and storage of sam ples (ctd..)
‘The sam ples which cannot be analysed within a day should be stabilized or preserved in
accordance with the standard analytical method. ’
‘I n cases where p reservatives are used, the sample container cannot be p re-rin sed with the
m aterial to be collected. In all other sam pling circum stances p re-rin sin g o f sample containers
m ay be carried out, unless there are specific circum stances rendering this undesirable. ’
D -7 9
5.4 Transport stabilization and storage of sam ples (ctd..)
‘A llpreservation steps should be recorded in the report a n d the temperature m easured and
recorded on site, i f appropriate. Ideally other p h ysica l a n d chem ical param eters sh o u ld be
determ ined on site or as soon as possible afterwards. '
D -80
6 Safety precautions
‘Reasonable access to routine sam pling sites in a ll w eathers is particularly important.
When sam ples are to be taken by w ading into a river or stream , account should be taken o f the
possible presence o f soft mud, deep holes and sw ift currents. A w ading ro d or sim ilar probing
instrum ent is essential to ensure safe wading.
I f circum stances dictate that sam pling m ust take place at rem ote sites a n d in the vicinity o f deep
water, by a p erso n w orking alone, then it is recom m ended that a life ja c k e t be worn a n d an
appropriate system o f regular reporting to a central control p o in t be employed.
It sh o u ld be recognised that there m ay be bacteriological, virological a n d zoological hazards in
m any river or stream sam pling situations. ’
‘The d eta iled fo r m o f the sam pling report will d ep en d on the objectives o f sampling. M atters,
which could be c o n sid ered fo r inclusion, are:
a) nam e o f river or stream
b) sam pling site (description should be complete enough to allow another p erso n to f i n d the
exact location w ithout further guidance)
c) sam pling p o in t
d) date a n d tim e o f collection
e) nam e o f sam ple collector
f) w eather conditions a t the time o f sam pling and/or im m ediately p rio r to sam pling
D -8 1
7 S a m p le id e n tific a tio n an d reco rd s (ctd ..)
D -82
D O C U M E N T No. 10:
Sum m ary o f the C orrective Actions required in order to com ply with: ISO 5667: 1990
Water quality - Sam pling- P art 6: Guidance on sam pling o f rivers an d streams.
Note: F or the corrective actions to be im plem ented effectively s ta ff training shall have to be
param ount in a ll cases.
2. Identify and docum ent w hich samples are to be taken in glass containers (borosilicate glass if
used for storing w eakly buffered water) and w hich are to be taken in plastic containers.
A m end appropriate m ethods/SOPs (ISO 5667-6:1990 (4.1)).
3. Identify, docum ent SOP N o .’s im plem ent test to assess the suitability o f polyethylene
containers for collecting samples for trace m etallic analyses (ISO 5667-6:1990 (4.1)).
4. A m end SOP No. 8 to include details on the sam pling equipm ent to be used w hen sam pling
surface w ater (ISO 5667-6:1990 (4.2)).
6. A m end ‘sam pling program m e’ to include m ap o f the sam pling points used for the purpose o f
com pliance w ith the EC (Quality o f Surface W ater Intended for the A bstraction o f D rinking
W ater) Regulations, 1989 (ISO 5667-6:1990 (5.1.1)).
7. Identify, docum ent and im plem ent method fo r assessing the effects o f a tributary/effluent on
a main stream (ISO 5667-6:1990 (5.1.1.1)).
8. A ssess the need to ascertain the tim e-of-travel o f pollutants. I f required, identify, docum ent
and im plem ent m ethod for assessing the tim e-of-travel o f pollutants (ISO 5667-6:1990
(5.1.1.2)).
9. D eterm ine the possibility o f a non-hom ogeneous distribution o f the determ inands o f interest
at the various sam pling sites. If required identify, docum ent and im plem ent m ethod for
assessing the m agnitude o f any heterogeneity (ISO 5667-6:1990 (5.1.2)).
10. A m end SOP N o .’s 8 and 47 to include details on w hen the sam pling o f surface film s is
required and w hen it should be avoided (ISO 5667-6:1990 (5.3.1)).
11 D evelop, docum ent and im plem ent method for the sam pling o f soluble species. Im plem ent
system o f reporting on sam ples that are filtered and the pore size o f the filter used (ISO 5667-
6:1990 (5.4)).
D -83
12. A m end SOP No. 47 to include details on the sealing o f sam pling containers (ISO 5667-
6:1990 (5.4)).
13. A m end SOP N o. 8 to include details on sam ple transportation and the sealing o f sam pling
containers (ISO 5667-6:1990 (5.4)).
14. D evelop, docum ent and im plem ent m ethod for the preservation o f sam ples and develop
m ethod o f recording w hen samples are preserved (ISO 5667-6:1990 (5.4)).
15. A m end SOP N o .’s 8 and 47 to include details on w hen sam ple containers can/cannot be pre
rinsed (ISO 5667-6:1990 (5.4)).
16. A m end SOP N o .’s 8 and 47 to include param eters w hich are to be m easured and recorded on
site (ISO 5667-6:1990 (5.4)).
17. D evelop, docum ent and im plem ent m ethod(s) for periodically testing the sam pling m ethods
used i.e. field blanks, samples w ith added determ inands and/or duplicate sam ples (ISO 5667-
6:1990 (5.5)).
18. A m end SOP N o .’s 8 and 47 to include reference to the safety precautions necessary w hen
sam pling from river (ISO 5667-6:1990 (6)).
19. A m end SOP N o .’s 8 and 47 to include procedure for labelling sam ple containers and
com pleting field report forms (ISO 5667-6:1990 (7)).
20. D evelop appropriate field report sheet for sam pling surface w ater for abstraction, as per (ISO
5667-6:1990 (7)).
21. A m end river field report sheet to include all required details as per ISO 5667-6:1990 (7).
D -84
D O C U M E N T No. 11:
Gap A nalysis results for ISO 5667-10: 1992 Water quality - Sam pling- P art 10:G uidance on
sam plin g o f w aste waters.
1. Scope
‘This p a r t o f ISO 5667 contains details on the sam pling o f dom estic a n d industrial wastewater. It
covers w astew aters in a ll its fo r m s i.e. industrial w aste w ater a n d crude a n d treated dom estic
waste w a te r .'
1.1 O bjectives
‘When designing a w aste-w ater sam pling p r o g a m m e , it is essential fo r the objective o f the study
to be kep t in mind. ’
3. D efinitions.
N ot applicable to gap analysis.
D -85
4.1 S a m p le c o n ta in e r s (c td ..)
‘F or w astew ater sampling, pla stic containers are reco m m en d ed fo r m ost determinands. Some
exceptions exist w hen f o r example the fo llo w in g analyses are to be m ade:
oil a n d grease
hydrocarbons
detergents
- pesticides. ’
D -86
4.2.1 M anual sam pling equipm ent (ctd. )
‘When m anual sam ples are to be u sed fo r preparation o f com posite sam ples the volume o f the
bucket, ladle or bottle should be well defined a n d known to a precision o f w ithin +/-5%. ’
‘M an u a l sam pling equipm ent should be made o f an inert m aterial that does not influence the
analyses that w ill be carried out on the samples later.
B efore starting sampling, the equipm ent should be cleaned with detergent a n d water.
The sam pling equipm ent cannot be w ashed in the w aste stream when this w ill influence the
analysis carried out later (e.g. analysis f o r oil a n d grease a n d m icrobiological analysis) '
Additionally, the user sh o u ld also aim f o r the fo llo w in g attributes when choosing sam pling
equipment, unless the circum stances dictate that certain o f them m ay not be necessary.
(Refer to P3-4 ISO 5667-10: 1992 (E)) ’
D -87
4 .2 .2 A utom atic sam pling equipm ent (ctd. )
‘SA F E T Y PREC A U TIO N S - In a ll cases when selecting sam pling locations, safety and health
aspects should be observed.
D -88
5.1.1 General description (ctd..)
‘Subsequently, a site inspection, including the use o f chem ical tracer studies, as necessary,
should be conducted in order to ensure that the locations o f the sew ers a n d the p a th o f the waste
stream correspond to the draw ings a n d to make sure the selected location is representative fo r
the sam pling purpose. ’
'A location sh o u ld be chosen where the effluent has a high turbulent flow, to ensure g o o d mixing. ’
'In the absence o f a location with turbulent flo w conditions, such conditions sh o u ld be induced
by restricting the flo w e.g. with a baffle or a weir. ’
'The sam pling intake p o in t should always be located dow nstream fr o m the restriction and, as a
gen era l rule, it sh o u ld be located a t least three tim es the p ip e diam eter dow nstream o f the
restriction. The inlet o f the sam pling pro b e should p refera b ly fa c e the direction o f the flow but
m ay fa c e dow nstream i f too m any blockages result. ’
D -8 9
5.1.2 Sampling from sewers, channels and manholes (ctd .)
‘B efore p roceedin g w ith the sam pling o f industrial discharges, the conditions inside the p la n t
(e.g. p rocesses a n d production rates) should he n o ted a n d recorded along with p o ten tia l
hazards.
‘A s a g eneral rule the sam pling p o in t should be one-third o f the effluent w ater depth below the
surface o f the water. '
D -9 0
5.1.3 W astew ater treatm ent plants
‘When choosing sam pling locations fo r wastewater treatm ent plants, it is again im portant to
refer to objective o f the data collection program m e. ’
‘When sam pling a t the inlets ofplants, the objective o f the sam pling program m e should be
carefully coiisidered. In som e situations, there m ay be a n eed to sam ple crude sewage in the
m ixture w ith recirculated processing liquid. In other cases, it m ay be necessary to exclude the
effect o f these liquids. ’
‘F requent review s o f a p la n t's sam pling locations n eed to be made, to ensure that a n y relevant
changes in the operation o f unit processes are taken into account when sampling. ’
D -9 1
5.1.3 W astew ater treatm ent plants (ctd .)
'W henever sam pling wastewaters, great care sh o u ld be exercised to overcom e or m inim ize the
substantial heterogeneity caused by suspended solids that are often present. Similarly, therm al
stratification o f separate industrial effluent stream s m ay be fo u n d when sam pling effluents or
discharges fr o m industrial process a n d m easures have to be taken to p rom ote the m ixing o f such
stream s before sampling. ’
D -92
5.2.2 N um ber o f sam ples
‘Water analyses should be based on samples taken a t regular intervals during a certain period.
The sam ples sh o u ld be composite samples, unless the determ inations to be carried out p rohibit
the use o f a com posite sample. The necessary num ber o f sam ples taken during each com posite
sam ple should be decided on statistical techniques. '
'I f there is little or no diurnal variation, or day-to-day variations, then the p a rticular time o f day
or day o f the w eek f o r sam pling is relatively unim portant. The solution then is to sam ple evenly
throughout the year, but a t any time o f day and on any day o f the w eek (these being chosen at
convenience).
D -9 3
5.2.3 Sampling time (ctd. )
‘R elating the tim es o f sam pling to the particular p ro cess being m onitored m ay be very im portant
when considering industrial effluent discharges that are either seasonal or operated on a batch
basis. In either case, the discharge w ill not be continuous a n d the sam pling program m e w ill need
to take this fa c t into account. ’
Sam ples sh o u ld norm ally be taken a t fix e d inter\>als during the whole control period. The control
p e rio d m ay be one year, a num ber o f m onths or weeks, or even shorter p erio d s o f time.
I f the control p e r io d covers one year, the days o f sam pling m ay be d eterm ined fr o m the fo rm u la e
on P. 6 IS O 5667-10:1992.
Ensure that the sam pling does not lead to any risk o f system atic error f o r exam ple by alw ays
taking sam ples on one p a rticular day or week number. ’
D -9 4
5.2.3 Sampling time (ctd .)
D -95
5.3 Choice of sampling method
‘F or certain determ inations, only spot samples can be used. F or exam ple this is the case with oil
a n d grease, disso lved oxygen,, chlorine a n d sulfide. '
D -96
5.3.1.2 Com posite samples (ctd. )
‘I n both flo w -w eig h ted a n d tim e-w eighted composite sampling, each o f the spot sam ples should
be greater than 50m l in volume, often advisable that spot sam ples are 200-300m l in volume. ’
‘When collecting com posite sam ples during extended periods, preservation should be an integral
p a rt o f the sam pling operation. ’
D -9 7
6. Safety aspects of sampling.
'When w orking in sewers, cesspools, pum ping stations a n d w aste-w ater treatment p la n ts there
sh o u ld be an aw areness o f the follow ing:
danger o f explosion
risk o f p o iso n in g caused by toxic gases
risk o f suffocation caused by lack o f oxygen
risk o f diseases
risk o f p h ysica l injury
risk o f drow ning
risk o f im pact fr o m fa llin g objects. ’
‘In m any countries there are legal requirem ents on the vaccination o f people working in contact
with wastewater. Such requirem ents should be fu lfille d fo r p erso n n el involved in sam pling
wastewater. ’
D -9 8
6. Safety aspects of sampling (ctd..)
‘I f it is necessary to interfere with traffic it is essential that the appropriate w arning signs a nd
lights are used. ’
‘A p rin te d fo rm f o r the sam pling report should include the fo llo w in g inform ation where
appropriate:
- sam pling p o in t
abbreviated sam pling p o in t designation
- date, start a n d stop o f sam pling
time, start a n d stop o f sam pling
duration o f the sam pling p erio d
- purpose o f the sam pling
details o f the sam pling m ethod
details o f f i e l d tests.
The sam pling report sh o u ld apply to both perm anent a n d occasional sam pling points.
In appropriate cases, the sam pling report should be accom panied by a sketch identifying the site.
D -9 9
7. Sample identification and records (ctd..)
D -1 0 0
D O C U M EN T No. 12:
Sum m ary o f the C orrective Actions required in order to com ply with: ISO 5667-10: 1992
Water quality - Sam pling- Part 10:Gui(lance on sam pling o f w aste waters.
1. A m end sam pling program m e to define the objectives o f the w astew ater sam pling program m e
(ISO 5667-10:1992 (1), (5.1.3), (5.3.1.1)).
2. D evelop, docum ent and im plem ent procedure for the selection o f sam ple containers (ISO
5667-10:1992 (4.1)).
3. A m end SOPs N o 10 and 11 stating the type o f sam ple containers that are to be used for
various analyses (ISO 5667-10:1992 (4.1)).
5. Identify and docum ent criteria for the selection o f autom atic sam pling equipm ent, taking into
account the features and attributes stated in ISO 5667-10:1992 (4.2.1).
6. A m end sam pling program m e to include details on how sam pling sites w ere selected,
ensuring that safety and health aspects are considered (ISO 5667-10:1992 (5.1), (5.1.1)).
7. Identify the situations w here site inspection should be conducted in order to ensure that the
locations o f the sew ers and the path o f the w aste stream correspond to the draw ings and to
ensure the selected location is representative for the sam pling purpose. D evelop system o f
carrying out the site inspections using chem ical tracer studies o r other approved method.
D ocum ent results (ISO 5667-10:1992 (5.1.1)).
8 A scertain the need to clean the various sam pling locations prior to sam pling. This being done
in order to rem ove scale, sludge, bacterial film, etc. from the walls. Identify and docum ent
the sam pling locations that require to be cleaned (ISO 5667-10:1992 (5.1.2)).
10. Develop, docum ent and im plem ent procedure for noting and recording the conditions inside
a licensed industrial plant prior to sampling the discharge (ISO 5667-10:1992 (5.1.2)).
11. A m end SOPs No. 10 and 11 stating the depth at w hich the sam ples should be taken i.e. one-
third o fth e effluent w ater depth below the surface o f the w ater (ISO 5667-10:1992 (5.1.2)).
D-101
12. Identify and docum ent the exact sampling point for the influent and effluent for all
w astew ater plants, in the sampling program m e (ISO 5667-10:1992 (5.1.3)).
13. Develop, docum ent and im plem ent system for frequently review ing the plant’s sam pling
locations (ISO 5667-10:1992 (5.1.3)).
14. A scertain the possibility o f thermal stratification for all licensed industrial effluent
discharges. Identify, docum ent and im plem ent m easures to prom ote the m ixing o f these
stream s prior to sam pling (ISO 5667-10:1992 (5.1.3)).
15. Identify, docum ent and im plem ent measures to overcom e or m inim ize the substantial
heterogeneity caused by suspended solids in w astew ater treatm ent plants (ISO 5667-10:1992
(5.1.3)).
16. Identify and docum ent w hen and how em ulsified and floating material are to be sampled
(ISO 5667-10:1992 (5.1.4)).
17. D eterm ine statistically the num ber o f samples to be taken during each com posite sam ple
(ISO 5667-10:1992 (5.2.2)).
18. A scertain the need to take into account variations in industrial w astew ater quality w hen
sampling. I f required, identify the industrial variations in industrial w astew ater quality and
im plem ent appropriate sampling program m e (ISO 5667-10:1992 (5.2.3)).
19. A m end SOP No. 11 to include requirem ent to record tim e o f sam pling (ISO 5667-10:1992
(5.2.3)).
20. Identify and docum ent the sampling days required during the control period. A scertain if
there is system atic error in the sampling tim es selected. D ocum ent in the sam pling
program m e how th e specific sampling times w ere selected (ISO 5667-10:1992 (5.2.3)).
21. D evelop, docum ent and im plem ent a method for selecting the period over w hich a com posite
sam ple has to be taken, taking the following factors into account:
c) objective o f the sam pling program m e
d) the stability o f the sample
(ISO 5667-10:1992 (5.2.4))
22. Identify and docum ent when spot or com posite sam ples should be taken (ISO 5667-10:1992
(5.3.1.1)).
23. Identify and docum ent the param eters that can only be determ ined by taking spot sam ples
(ISO 5667-10:1992 (5.3.1.1)).
24. Identify and docum ent what type o f com posite sam ples are to be taken and w hen this should
occur (ISO 5667-10:1992 (5.3.1.2)).
25. D evelop and docum ent procedure for the taking o f com posite sam ples, including details on
the volum es to be taken (ISO 5667-10:1992 (5.3.1.2)).
D -102
26. Amend SOPs No. 10 and 11 to include details on sample preservation and storage (ISO
5667-10:1992 (5.4)).
27. A scertain the need to preserve samples during the collection o f com posite samples. I f
necessary, im plem ent system o f sample preservation (ISO 5667-10:1992 (5.4)).
28. Amend SOP No. 11 to include details on ensuring the sam pling location is safe to access
(ISO 5667-10:1992 (6)).
29. Develop, docum ent and im plem ent sampling report form for STP and industrial w astew ater
sam pling as per requirem ent 7 o f ISO 5667-10:1992 (E).
D -1 0 3
DO C UM ENT No. 13:
Gap Analysis results for ISO 5667-14:1998 Water quality - Sam pling- P a rt 14:G uidance on
quality assurance o f environm ental water sam pling an d handling
1. Scope
N ot applicable to gap analysis.
3. D efinitions.
N ot applicable to gap analysis.
D -104
The following quality control techniques are described in ISO 56 6 7 -1 4 :1998(E):
5.2 R eplicate quality control samples
D -105
6. Transport, stabilization and storage of sam ples (ctd...)
‘M easure a n d record the temperature o f the sample on-site. P hysical param eters (e.g. pH ,
dissolved gases, suspended solids) should be determ ined on site or as soon as possible
afterwards. '
‘I t is recom m ended that sample containers are tightly sea led a n d p ro tected fro m the effects o f
light a n d excessive heat, because the characteristics o f the sam ple m ay rapidly deteriorate due to
gas exchange, chem ical reactions an d the m etabolism o f organism s w hich m ay be present.
Ensure that samples, w hich cannot be analysed quickly, are stabilized. C ooling to 4 ° C m ay be
applied; f o r longer periods, freezin g to - 2 0 ° C as recom m ended in IS 0 5 6 6 7 -3 . ’
D -106
6. Transport, stabilization and storage o f sam ples (ctd...)
‘Sam ples m ay be p reserved by the addition o f chem icals o f suitable quality. Ensure that the
chosen m ethod o f preservation does n o t interfere w ith the subsequent exam ination or influence
results. R eco rd a ll preservation steps in the test report. '
D -107
8. Sample identification and records (ctd...)
‘When sam pling fo r special reasons, detailed inform ation should be given, including the reasons
f o r sam pling a n d any preservation steps taken. ’
D -1 0 8
D O C UM ENT No. 14:
Sum m ary o f the C orrective Actions required in order to com ply with: ISO 5667-14:1998
Water quality - Sam pling- Part 14:Guidance on quality assurance o f environm ental w ater
sam pling a n d handling
Note: F or the corrective actions to be im plem ented effectively s ta ff training shall have to be
param ount in a ll cases.
1. A m end SOP N o .’s 6, 8, 10, 11 and 47 to include details on the calibration and checking o f
field m eters prior to sampling and details on the transportation o f samples from the sam pling
site to the laboratory (ISO 5667-14:1998 (5.1)).
2. D ocum ent the sampling training procedure and develop detailed training records (ISO 5667-
14:1998 (5.1)).
3. Develop, docum ent and im plem ent analytical quality control program m e for sampling, as per
ISO 5667-14 :1998(E).
4. Identify and docum ent when and what preservatives are to be used, for the various analyses.
D ocum ent procedure for the preparation and use o f these preservatives. Im plem ent system o f
recording all preservation steps (ISO 5667-14:1998 (6)).
5. D ocum ent and im plem ent method for ensuring that the preservation used does not interfere
with the subsequent exam ination or influence results (ISO 5667-14:1998 (6)).
6. Amend SOP N o .’s 6, 8, 10, 11 and 47 detailing w hat param eters are to be m easured and
recorded on site (ISO 5667-14:1998 (6)).
7. Amend SOP N o .’s 6, 8, 10 11 and 47 to give details on the sealing, transportation and storage
o f sam ples prior to analyses (ISO 5667-14:1998 (6)).
8. Identify and docum ent what exact inform ation should be recorded when sam pling for special
reasons (ISO 5667-14:1998 (8)).
D -1 0 9
D O C U M E N T N o . 15:
N ote: F or the corrective actions to be im plem ented effectively s ta ff training shall have to be
param ount in a ll cases.
2. State the objectives o f the various sampling program m es (ISO 5667-1:1980 Section 1 (3)
e.g. drinking w ater m onitoring (IS 0 5 6 6 7 -5 :1999 (1)), w astew ater sam pling programm e. (ISO
5667-10:1992 (1), (5.1.3), (5.3.1.1)).
3. Identify and docum ent the degree o f detail and precision that will be adequate for analytical
field results. O utline the manner in which the results are to be expressed and presented, as
part o f the sam pling programme. Amend sam pling program m e to include definition o f the
m agnitude o f tolerable error in analytical field results (ISO 5667-1:1980 Section 1 (3)), (ISO
5667-6:1990 (1), (5.2)).
4. R eview the sam pling locations ensuring samples are taken from turbulent, well-m ixed liquids
(ISO 5667-1:1980 Section 2 (8.3)).
5. A m end sam pling program m e to give details on the introduction o f turbulent flow conditions,
w here necessary (ISO 5667-10:1992 (5.1.2)).
6. A scertain the need to statistically determ ine the num ber o f sam ples required for a given
confidence interval. I f required, carry out statistical analysis, docum ent results and amend
sam pling program m e as required (ISO 5667-1:1980 Section 3 (16.4)).
7. Identify and docum ent the w astew ater sampling tim es required. These can be ascertained
using the form ulae given in ISO 5667-10:1992 (5.2.3), w hich calculates the sam pling tim es
over a specified control period e.g. one year, a num ber o f m onths or weeks.
8. a) Identify w hether the w ater bodies sampled have random or system atic
variations in quality.
b) D eterm ine statistically the num ber o f sam ples required, to determ ine w hether random or
system atic variation occurs.
c) I f system atic variations in quality exist determ ine the tim es o f sam pling (these should be
spaced approxim ately equally over trend periods in w hich variations occur).
d) D ocum ent results and amend sampling program m e as required
(ISO 5667-1:1980 Section 3 (16.5))
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9. Com pile a list o f the param eters o f interest for each sample type e g w astew ater, river, etc.
w ith reference to the relevant analytical procedure used in the laboratory (ISO 5667-1:1980
Section 1 (3)).
10. A m end ‘sam pling program m e’ to include map o f surface w aters used for the abstraction o f
drinking w ater. Outline the various sampling points in these w ater bodies (ISO 5667-6:1990
(5.1.1)).
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D O C U M E N T No. 16:
Q u ality C o n tro l C o rre c tiv e A ctions
N ote: F o r the corrective actions to be im plem ented effectively s ta ff training shall have to be
p aram ount in a ll cases.
1. Im plem ent a procedure for assessing w hether the filter type used to filter samples is a cause
o f contam ination (ISO 5667-3:1994 (3.2.5)).
2. D evelop, docum ent and im plem ent a procedure for situations w here the tim e-o f -travel
exceeds the max recom m end preservation tim e (ISO 5667-3:1994 (5)).
3. Develop, docum ent and im plem ent procedure for verifying that the num ber o f samples
received at the laboratory coincides w ith the num ber recorded on the field sheet (ISO 5667-
3:1994 (6)).
4. Develop, docum ent and im plem ent method to ensure sam ples are preserved and stored in the
correct containers as soon as possible after sam pling (ISO 5667-5:1999 (7.2)).
5. Develop, docum ent and im plem ent analytical quality control (QC) program m e for
periodically testing the sampling methods used. This should include the use o f field blanks,
sam ples w ith added determ inands and/or duplicate sam ples (ISO 5667-6:1990 (5.5)), (ISO
5667-14:1998(E)).
6. Develop, docum ent and im plem ent procedure for training sam pling personnel w ith regard to
correct sam pling and on-site m easurem ent techniques (ISO 5667-5:1999 (9). D ocum ent the
sam pling training procedure and develop detailed training records (ISO 5667-14:1998 (5.1)),
(ISO 5667-3:1994 (3.2.1)).
7. Identify, docum ent and im plem ent a procedure to assess the suitability o f polyethylene
containers for th e collection o f samples for trace metal analyses (ISO 5667-6:1990 (4.1)).
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DOCUMENT No. 17:
P re se rv a tio n C o rrectiv e A ctions
N ote: F or the corrective actions to be im plem ented effectively s ta ff training shall have to be
param ount in a ll cases.
1. Identify and docum ent the preservation m ethod(s) required for the various samples.
Im plem ent preservation methods, w here required and develop m ethod o f recording when
sam ples are preserved (ISO 5667-1:1980 Section 1 (3), (5.3)), (ISO 5667-3:1994 (3.1)), (ISO
5667-14:1998 (6)).
2. A scertain the need to preserve samples during the collection o f com posite samples. If
necessary, im plem ent system o f sample preservation (ISO 5667-2:1991 (4.6)), (ISO 5667-
10:1992 (5.4)).
3. D ocum ent and im plem ent method for ensuring that the preservative used does not result in
dilution o f the analyte or interfere w ith the subsequent analysis thereby influencing the final
result (ISO 5667-3:1994 (3.2.6)), (ISO 5667-14:1998 (6)).
4. The efficiency o f the preservation process depends on the constituents w hich have to be
analysed, their levels and on the nature o f the sample. T herefore develop, docum ent and
im plem ent a procedure to verify w hether or not the preservation suggestions in Table 1 to 5
o f ISO 5667-3:1994 are suitable for the sample w ith w hich it is concerned (ISO 5667-3:1994
(3.3)).
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DOCUMENT No. 18:
D rin k in g W a te r C o rre c tiv e A ctions
N ote: F or the corrective actions to be im plem ented effectively s ta ff training shall have to be
param ount in a ll cases.
1. (a) M ap drinking w ater locations (ISO 5667-1:1980 Section 1 (3), Section 2 (8.2))
and predeterm ined sampling points for the various w ater supplies (IS 0 5 6 6 7 -
5:1999(4.1.4)).
(b) A m end sam pling programm e to include details on how the various drinking w ater
sam pling points are selected (ISO 5667-1:1980 Section 2 (9.8.1)).
3. Assess the need to use a flexible inert tube, to deliver liquid to the bottom o f the sam pling
bottle, w hen sam pling from a tap or pump outlet (ISO 5667-2:1991 (6.7)).
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4. Asses need to disinfect using a chlorine solution versus alcohol (w hich is currently being
used). Amend SOP if necessary (IS05 6 6 7 -5 :1999 (4.1.5)).
5. Develop, docum ent and im plem ent method o f on-site analysis o f odour and taste (IS05667-
5:1999 (4.1)).
7. Develop, docum ent and im plem ent SOP detailing how bottles are to be sterilized and a
m ethod to assess if the sampling container m aterials used produce or release chem icals
(ISO5667-5:1999 (5.3)).
8. Identify and docum ent samples w ith which contact with the air m ust be avoided and that
require vigorous m ixing before taking portions for analyses. D ocum ent procedure for dealing
with both types o f sam ples (ISO5667-5:1999 (7.2)).
9. Identify sam ples that require to be filtered/ centrifuged at the tim e o f taking the sample or
im m ediately afterwards. Im plem ent procedure for filtration/ centrifuging o f samples (ISO
5667-3:1994 (3.2.5)), (IS 0 5 6 6 7 -5 :1999 (7.2)).
10. Amend SOP No. 43 to include details on the max. length o f sam ple storage for the various
analyses, m aking reference to guidelines in Standard M ethods (A .P H.A. 20th Ed.) (ISO
5667-3:1994 (3.1)).
11. A m end field sheet to include details on w eather conditions, unusual observations and
inform ation on sam ples taken for a specific reason (ISO 5667-1:1980 Section 2 (8.13)), (ISO
5667-2:1991 (7.2), ISO 5667-3:1994 (4)), ( IS 0 5 667-5:1999 (8)).
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DOCUMENT No. 19:
R iver C o rre c tiv e A ctions
2. Identify appropriate method to assess each river sam pling location for stratification. Take
appropriate m easures following the results o f the assessm ent (ISO 5667-1:1980 Section 2
(9.3.1)).
3. Identify and docum ent an appropriate m ethod to assess the effects o f a discharge on a river
by selecting representative upstream and dow nstream locations (N ote: the discharge may be
a w astew ater discharge or an adjoining tributary) (ISO 5667-1:1980 Section 2 (9.3.2)), (ISO
5667-6:1990 (5.1.1.1)).
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5. A m end SOP No. 47 to include details on:
a) the type o f sam pling containers to be used for m icrobiological samples
b) the preparation o f microbiological sampling bottles
c) how m icrobiological samples are to be taken (ISO 5667-6:1990 (4.2), (5.3.2)).
6. D evelop appropriate field report sheet for sam pling rivers and surface w ater for abstraction
ISO 5667-1:1980 Section 2 (8.13)), (ISO 5667-2:1991 (7.2)), (ISO 5667-3:1994 (4)), (ISO
5667-6:1990 (7)).
7. Identify the sam ples w hich require to be filtered/centrifuged at the tim e o f taking the sample
or im m ediately afterwards. Im plem ent a procedure for the filtration/ centrifuging o f these
sam ples (ISO 5667-3:1994 (3.2.5)), (IS 0 5 6 6 7 -6 :1990 (5.4)).
8. D ocum ent and im plem ent procedures for the selection o f effective sam plers (ISO 5667-
2:1991 (6.3.1)) and containers. Include details on the cap types to be used for the various
param eters (ISO 5667-2:1991 (6.1.1), (6.2.1), (6.2.3), (6.2.4), (6.5)).
9. Identify abnorm al sam pling situations (e.g. flood conditions in a river or tim es o f an algal
bloom). Prepare SOP detailing the procedure for sam pling during these conditions and the
subsequent reporting o f these results (ISO 5667-1:1980 Section 3 (17), ISO 5667-14:1998
(8)).
10. A ssess w hether an accurate determ ination o f dissolved oxygen (D O .) is required i.e. a
m easurem ent o f D O. taken directly in the w ater-body as opposed to the current practice o f
m easuring D.O. in the sam pling bucket (ISO 5667-2:1991 (6.7)).
11. A ssess the need to ascertain the tim e-of-travel o f pollutants in rivers. I f required, identify,
docum ent and im plem ent method for assessing the tim e-of-travel o f pollutants in rivers {ISO
5667-6:1990 (5.1.1.2)).
12. D eterm ine the possibility o f a non-hom ogeneous distribution o f determ inands o f interest at
the various sam pling sites. Identify, docum ent and im plem ent m ethod for assessing same
IS O 5667-6:1990 (5.1.2).
13. A m end SOP No. 43 to include details on the m ax length o f sam ple storage fo r the various
analyses (ISO 5667-3:1994 (3.1)).
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DOCUMENT No. 20:
W astew ater C orrective Actions
Note: F or the corrective actions to be im plem ented effectively s ta ff training shall have to be
param ount in a ll cases.
2. Identify, docum ent and im plem ent measures to overcom e or m inim ize heterogeneity caused
by suspended solids and/or therm al stratification in w astew ater stream s (ISO 5667-10:1992
(5.1.3)).
3. Identify and docum ent when and how em ulsified and floating m aterial are to be sampled
(ISO 5667-10:1992 (5.1.4), ISO 5667-1:1980 Section 2 (12.1.1)).
5. Develop, docum ent and im plem ent system for frequently review ing the plan t’s sam pling
locations (ISO 5667-10:1992 (5.1.3)).
6. Prepare SOP for sampling o f storm sewage and surface ru n -o ff taking into account the
guidelines provided in ISO 5667-1:1980 Section 2 (13).
D -1 1 8
1) the sealing and transportation o f samples to the laboratory (ISO 5667-2:1991 (6.2.4), ISO
5667-3:1994 (3.1), (3.2.4), (5), ISO 5667-14:1998 (5.1),(6).
m) storage o f sam ples in a refrigerator on arrival to the laboratory, w here im m ediate
analyses is not being carried out (ISO 5667-3:1994 (6)).
n) Safety precautions necessary, (include details from the Laboratory Safety Statem ent)
(ISO 5667-1:1980 Section 2 (7.1)).
8. D evelop, docum ent and im plem ent sampling report form for STP and industrial w astew ater
sam pling as per ISO 5667. (ISO 5667-1:1980 Section 2 (8.13), ISO 5667-2:1991 (7.2), ISO
5667-3:1994 (4)), (ISO 5667-10:1992 (7))
9. Identify and docum ent whether sampling locations require to be cleaned (to rem ove scale,
sludge, bacterial film, etc. from the walls) prior to sam pling and detail how cleaning is to be
carried out (ISO 5667-10:1992 (5.1.2)).
10. Assess the need to use a flexible inert tube, to deliver liquid to the bottom o f the sam pling
bottle, when sam pling from a tap or pump outlet (ISO 5667-2:1991 (6.7)).
11. Identify the sam ples w hich require to be filtered/centrifuged at the tim e o f taking the sample
or im m ediately afterwards. Im plem ent a procedure for the filtration/ centrifuging o f these
samples (ISO 5667-3:1994 (3.2.5).
12. Develop, docum ent and im plem ent a procedure for the freezing and thaw ing o f sam ples (ISO
5667-3:1994 (3.2.4)).
13. A m end SOP No. 43 to include details on the max. length o f sam ple storage for the various
analyses, m aking reference to guidelines in Standard M ethods (A.P.H.A. 20th E d.) (ISO
5667-3:1994 (3.1)).
14. D ocum ent and im plem ent procedures for the selection o f effective samplers (ISO 5667-
2:1991 (6.3.1)) and the selection and purchase o f sam pling containers, including details on
the cap types to be used for the various param eters (ISO 5667-2:1991 (6.1.1), (6.2.1), (6.2.3),
(6.2.4), (6.5)), (ISO 5667-10:1992 (4.1)).
15. D ocum ent criteria for the selection o f autom atic sam pling equipm ent, taking into account the
features and attributes stated in ISO 5667-10:1992 (4.2.2).
16. D evelop, docum ent and im plem ent a m ethod for selecting the period over w hich a com posite
sam ple is to be taken, taking the objective o f the sam pling program m e and the stability o f the
sam ple into account (ISO 5667-10:1992 (5.2.4)).
17. Statistically determ ine the num ber o f samples to be taken during each com posite sam ple (ISO
5667-10:1992 (5.2.2)).
18. Identify and docum ent the param eters that can only be determ ined on spot or com posite
sam ples (ISO 5667-10:1992 (5.3.1.1)).
19. D evelop and docum ent procedure for the taking o f com posite samples, including the type o f
com posite sam ple & details on the volum es to be taken (ISO 5667-10:1992 (5.3.1.2)).
D -1 1 9
20. Im plem ent a procedure for:
dealing w ith sam ples o f anom alous material
identifying hazardous materials
(ISO 5667-3:1994 (4))
21. a) Identify areas w here a site inspection may be necessary in order to ensure the
locations o f the sewers and path o f the waste stream correspond to the site map
draw ings and the selected location is representative for sam pling purpose,
b) D evelop a system o f carrying out site inspections using chem ical tracer studies
or other approved method Develop an appropriate m ethod to docum ent results
o f same (ISO 5667-10:1992 (5.1.1)).
22. Develop, docum ent and im plem ent procedure for noting and recording conditions inside a
licensed industrial plant prior to sampling (ISO 5667-10:1992 (5.1.2))
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