LS 17614 (Part 3) 2021 - ISO 5667-3 2018
LS 17614 (Part 3) 2021 - ISO 5667-3 2018
LS 17614 (Part 3) 2021 - ISO 5667-3 2018
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NATIONAL FOREWORD
This lndian Standard (Part 3) whicfi is identical with ISO 5667-3 : 2018 'Whter quality
Sampling Part 3: Preservation and handling of water samples' issued by the lntemational-
-
Organization for Standardization (lSO) was adopted by the Bureau of lndian Standards on
recommendation of the Water Quality Seclional Committee and approval of the Chemical Division
Council.
'under the general title 'WATER QUALIry SAMPLING" this standard is being published in several
- 5667-3
other parts. This part is an adoption of ISO : 2018 which specifies general requirements for
sampling, preservation, handling, transport and storage of all water samples induding those for
biological analyses.
The other parts ot this lndian Standard are:
lS 17614 (Part 1) :2021 \Iater quality Sampling : Part 1 Guidance on the design of sampling
-
programmes and sampling techniques (under pint)
lS 17614 (Part 4) : 2021 \/ater quality Sampling : Part 4 Guidanc€ on sampling from lakes,
-
natural and man-m ade (under pint)
lS 17614 (Part 5) : 2021 Vlhter quality Sampling : Part 5 Guidance on sampling of drinking
-
waterfrom treatrnent works and piped distribution systems (under ptint\
lS '17614 (Part 6) : 2021 \ hter quality Sampling : Part 6 Guidance on sampling of rivers and
sveams (under - pintl
lS 176'14 (Part 7) : 2021 \ hterquality Sampling : Part 7 Guidance on sampling of water and
-
steam in boiler planls (under pint)
lS 17614 (Part 8) : 2021 Water quality Sampling : Part
- I Guidance on the samding of wet
deposition (under pin|
lS 17614 (Part 9) : 2021 Vlhter quality Sampling : Part 9 Guidance on sampling from marine
waters (under pnnt) -
lS 17614 (Part 10) :2021 Water quality Samding : Part 10 Guidance on sampling of waste
waleB (under pintl -
lS '17614 (Part 12) : 2021 Water quality :
Sampling Part 12 Guidance on sampling of bottom
-
sediments from rivers, lakes and estuarine areas (under pintl
lS 17614 (Part 131 :2021 Vlhter quality Sampling : Part 13 Guidance on sampling of sludges
(under pin0 -
lS 17614 (Part 14\'. 2021 Vlhter quality Sampling : Part 14 Guidance on quality assurance and
-
quality control of environmental water sampling and handling (under
pnnl
lS 17614 (Part 151 :2021 \ryater quality Sampling : Part 15 Guidance on the preseNation and
-
handling of sludge and sediment samples lunder pint)
lS 17614 (Part 16\ .2021 Water quality Sampling : Part 16 Guidanc€ on biotesting of samples
(under pint) -
lS 17614 (Part 17) . 2021 \A,bter quality
- Sampling . Pad '17 Guidance on sampling of bulk
suspended solids (under pnno
lS 17614 (Part 19\ : 2021 Water quality Sampling : Part'19 Guidance on sampling of marine
-
sediments(under print)
lS 17614 (Pan 2Ol :2021 \ hterquality-Samding : Part20Guidanceontheuseof sampling data
for decision making Compliance with thresholds and classification
systems (underpnnt)-
Introduction
This document is intended to be used in conjunction with ISO 5667-1, which deals with the design of
sampling programmes and sampling techniques.
Where possible this document has been brought into line with current standards. Where new research
or validation results have provided new insights, the tatest knowledge has been used.
ISO 5567-3 provides in Table A.1 validated preservation times and/or conditions as well as descriptions
of best practice. Table A-1 also refers, for each analyte, to those ISO standards available at the date of
publication ofthis ISO 5667-3. This is however not an exhaustive lisL Other methods may be used when
they have been validated. However, it is strongly recommended that where a method validation is not
available, the preservation times for the analyte as listed in Table A.1 for ISO test methods be followed.
The preservation and storage conditions and maximum storage times per analyte as listed in Table A.1
should be regarded as default conditions to be applied in the absence of any other information,
However, if validation of preservation techniques and holding times has been carried out, relative
to specific circumstances and matrices, by a laboratory, then, provided that it can produce evidence
of this validation where they differ from those set out in Tahlsj-l of this standard, these validated
preservation and storage conditions and maximum storage times are deemed acceptable for use by the
validating laboratories.
Attention is drawn to the proposed development of a new part in the ISO 5667 series, which further
elaborares on ISO 5667-3:2018, Annex C, and which will contain guidelines and the elaboration of the
required techniques of how to validate new storage times or preservative methods and details of the
techniques described.
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lndian Standard
WATER QUALITY _ SAMPLING
PART 3 PRESERVATION AND HANDLING OF WATER SAMPLES
1 Scope
This document specifies general requirements for sampling, preservation, handling, transport and
storage ofall water samples including those for biological analyses.
It is not applicable to water samples intended for microbiological analyses as specified in ISO 19458,
ecotoxicological assays, biological assays and passive sampling as specified in the scope oflSO 5667-23.
This document is particularly appropriate when spot or composite samples cannot be analysed on site
and have to be transported to a laboratory for analysis.
2 Normative references
The following documents are referred to in the text in such a way that some or all of their content
constitutes requirements of this documenL For dated references, only the edition cited applies. For
undated references, the latest edition ofthe referenced document (including any amendmentsl applies.
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ISO 5667.3 : 2018
3.2
saDple preservation
any procedure used to stabilize a sample in such a way that the properties
under examination are
maintained stable from the collection step until preparation for analysii
ry9F I to entry: Different analytes may require several samples from the same source that
are stabilized by
different procedures.
[SOURCE: ISO 11074:2015, 4.4.20, modified Note 1to entry has been addedl
-
3,3
sample storage
process, andthe result ofkeeping a sample available under predefined conditions, usually for a specified
time interval between collection and further treatment ofa sample
[SOURCE: ISO 11074:2015, 4.4.22, modified Note 1 to entry has been added; "soil sample" has been
changed to "samplel -
3.4
storagc time
period of time between filling of t}le sample container and further treatment of the sample in the
laboratory, if stored under predefined conditions
Not€ 1 to entry: Sampling finishes as soon as the sample container has been fllled with the sample. Storage time
ends when the sample is taken by the analyst to start sample preparation prior to analysis.
Note 2 to entry: Further treatmentis, for most analytes, a solvent extraction or acid destruction. The inital steps
of sample preparation can be steps complementary to the storaSe conditions for the maintenance of anal)rte
concentrations.
4 Samplingand chainofcustody
If there is a need to take samples, this is done according to a sampling programme. The first step is to
design a sampling programme. Guidance on this topic is given in ISO 5667-1.
Depending on the sample type and matrix, the guidelines found in ISO 19458 and in the relevant part(s]
oflSO 5557 shall be consulted.
The process of preservation and handling of water samples consists of several steps, During this
process, the responsibility for the samples might change. To ensure the integrity of the samples, all
steps involving the sample shall be documented.
AII preparation procedures shall be checked to ensure positive or negative interferences do not occur.
As a minimum, this shall include the analysis ofblanks (e.g. field blank or sample container) or samples
containing known levels of relevant analytes as specified in ISO 5667-74.
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All reagents shall be labelled with a "shelf-life", The shelf-life represents the period for which the
reagent is suitable for use, ifstored correctly. This shelflife shall not be exceeded. Any reagents that are
not completely used by the expiry of the shelf-life date shall be discarded.
Check reagents periodically, e.g. by field blanks, and discard any reagent found to be unsuitable.
Between on-site visits, reagents shall be stored separately from sample containers and other equipment
in a clean, secure cabinet in order to prevent contamination,
Each sample shall be labelled accordingly, after the addition ofthe preservative, Otherwise, there could
be no visible indication as to which samples have been preserved, and which have not.
5.1 Solids
5.1.5 Hexamethylenetetramine (hexamine, urotropine), CoH rzN+, w(Ce H pNa') > 99 Vo.
5,2 Solutions.
Dissolve 10,0 g of zinc acetate in. -100 ml of water . Dilute to 100 ml with water. Store the solution in a
polypropylene or glass bottle for a maximum period of 1 a.
5,2.2 Orthophosphoric acid {p = 1,7 E/mlJ, H3POa, w[H3POaJ > 85 %, c[H3POa] = 15 mol/I.
s.2.3 Hydrochloric acid (p = 1,2 g/mll, HCl, l,[HCl] > 36 %, c(HCl) = 12,0 mol/.
s,2,4 Nitric acld (p = 1,42 g/mlJ, HNO3, w(HNO3) > 65 %, c(HNOrl = 15,8 mol/|.
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lS '17614 (Part 3l : 2021
ISO 5667-3 : 2018
WARNING Adding the concentrated acid to the water caD give violent reactions because ofan
exothermic- reaction.
WARNING Beware of formaldehyde vapours. Do not store large numbers of samples in small
work areas.-
5.2,10 AJkaline Lugol's solution, 100 g potassium iodide (5.1.61, 50 g iodine (5.1.71, and 250 g sodium
acetate [5^13] in 1 000 ml water to pH 10.
5.2.11 Acidic Lugol's solution, 100 g potassium iodide (5.r.6J,50 g iodine (5.1.71 and 100 ml glacial
acetic acid (5.2.17) in 1 000 ml water to pH 2.
5,2,12 Neutralized formaldehyde solution, formaldehyde solution (5.2.71 neutralized with sodium
tetraborate (5.1.41 or hexamethylenetetramine (5.1.51. Formalin solution at 100 g/l gives a final solution
of 9(CH2OJ = 3,7 o/o to 4,0 o/o.
WARNING Beware offormaldehyde vapours. Do not store large numbers of samples in small
work areas.-
5.2.14 Sodium hypochlorite NaOCl, w{NaOCll = 10 %. Dissolve 100 g sodium hypochlorite (NaOClJ in
1 000 ml of water.
5.2.15 Potassium iodate KlO3, w(KIO3l = 10 %. Dissolve 100 g potassium iodate IKI03] in 1 000 ml
of water.
5.3 Materials.
I.3.2 Filter, pore size 0,40 [m to 0,45 pm, unless a different filter size is specified in the analytical
Internati onal Stan dard.
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6 Containers
DetailsofthetypeofcontainerusedforthecollectionandstoraqeofsamplesareBiveninTablesA.l
shall also be given
to tL3. The same considerahons ffi ; ;; ;"b;ilri;uitable;onhineimaterial
to if,e selection of cap liner materials'
Samplecontainersshallbemadeofamaterialappropriateforpreservingthenaturalpropertiesofboth
the samole and the expected *"g. "i ir"i"r"ln'r'niti
sri,"Uf. iypes of cJntainers for each analyte to be
."r.r."d are given in Tab!rl\' ! to A'3'
prescribed can be different from those used for
NoTE For very low concenEations of metals' containers
in thi analytical lnternational standards'
higher concentrations, Details canle-i;";; i;-13lrGAL rr
as polyethylene (PE) or polytetrafluoroethylene
lfthe samples are to be frozen, suitable containers,such
(PTFEl, shall be used to prevent breakage'
containers with a certificate of
The use of disposables is preferred' Some manufacturers supply
cleanliness. lf such a certiticate oicie"niin".r ir supplied, it
is-nlt necessary to clean or rinse the
containers before use.
If immediate filtration on site is impossible, then the reason and the time between sampling and
filtration shall be added to the test report.
7.1 Sample handling and presersadon for physical and chemlcal examlnadon
Waters, particularly fresh waters, waste waters and groundwaters, are susceptible to changes
as a result of physical, chemical or biological reactions which may take place between the time of
sampling and the commencement of analysis. The nature and rate of these reactions are often such
that, if precautions are not taken during sampling, transport and storage (for specific analytes), the
concentrations determined are different to those existing at the time of sampling.
The extent of these changes is dependent on the chemical and biological nature of the sample, its
temperature, its exposure to light, the type of the container in which it is placed, the hme between
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sampling and analysis, and the conditions to which it is subiected, e.8. agitation during transporL
Further specific causes ofvariation are Iisted in a) to f).
a]
- The presence of bacteria, algae and other organisms can consume certain constituents of
the simples. These organisms can also modify the nature of the constituents to produce new
constitu;nts. This biological activity affects, for example, the concentrations of dissolved oxygen,
carbon dioxide, compounds of nitrogen, phosphorus and, sometimes, silicon.
b] Certain compounds can be oxidized either by dissolved oxygen present in the samples, or by
atmospheric oxygen [e.g. organic compounds, FeIll) and sulfides].
cJ Certain substances can precipitate out of solution, e.g. calcium carbonate, metals, and metallic
compounds such as Al(OH]3, or can be lostto thevapourphase (e.g. oxygen, cyanides, and mercuryJ.
d) Absorption of carbon dioxide from air can modify pH, conductivity, and the concentration of
dissolved carbon dioxide. Passage of compounds like ammonia and silicon fluoride through some
types ofplastics may also affect pH or conductivity.
eJ Dissolved metals or metals in a colloidal state, as well as certain organic compounds, can be
irreversibly adsorbed on to the surface ofthe containers or solid materials in the samples.
fl Polymerized products can depolymerize, and conversely, simple compounds can polymerize.
Changes to particular constituents vary both in degree and rate, not only as a function of the type of
water, but also, for the same water type, as a function ofseasonal conditions.
These changes are often sufficiently rapid to modify the sample considerably in a short time. In all
cases, it is essential to take precautions to minimize these reactions and, in the case of many analytes,
to analyse the sample with a minimum of delay. If the required precaution for changes is filtration on
site, then a filter (5.3.2J shall be used.
al the effect of the fixative, and/or preservative, on the loss of the organism shall be known
beforehand;
b) the fixative or preservative shall effectively preventthe biological degradation of organic matter at
least during the storage period ofthe samples;
c) the fixative, and/or preservative, shall enable the biological analyte (e.g. organisms or taxonomical
groups) to be assessed during the storage period of the samples.
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The delay between sampling and measurement has to be consistent with the radioactive halHife of
the radionuclides of interest. The conditions to be taken for adequate storage are independent of the
radioactive half-life, but identical to those required for the corresponding stable isotope.
NOTE Cooling radiological samples is primarily used to prevent algal growth and biological spoilage. It is
not a necessary preservation step for radiochemical analyses, These samples are often combined with those for
physical, chemical or biological analysis.
I Sample transport
Cooling or freezing procedures shall be applied to bamples to increase the time period available for
transport and storage and if required by Tables A.1 to A.3. When transport takes place, the sampling
plan (e.g.lSO 5667-11 shall consider:
If the maximum storage time cannot be met, then the sampling plan shall be reformulated to allow
these requirements to be accommodated.
A cooling temperature of the device during transport of (5 t 3) 'C has been found suitable for many
applications, Cooling and freezing procedures applied shall be in line with instructions from the
analytical laboratory. Freezing especially requires detailed control of the freezing and thawing process
in order to return the sample to its initial equilibrium after thawing.
Containers holding samples shall be protected and sealed during transport in such a way that the
samples do not deteriorate or lose any part of their content. Container packaging shall protect the
containers from possible external contamination, particularly near the opening, and should not itself
be a source of contamination.
Glass containers shall be protected from potential breakage during transport by appropriate packaging.
Samples shall be transported as soon as possible after sampling and with cooling ifnecessary according
to Tables A.1 to A.3.
Laboratory samples for dispatch or transport by third parties and preserved Iaboratory samples should
be sealed in such manner that the integrity of the sample can be maintained.
Samples required for (potential] regulatory investigations should be sealed to a level that meets the
requirements of the authorities or other organization[s] concerned with the transport of the sample.
During transportation samples shall be stored in a cooling device capable of maintaining a temperature
of [5 t 3) "C. For proper evaluation ofthe conditions during transport, a device capable ofrecording the
[maximum) temperature ofthe air surrounding the sample may be used.
NOTE Devices capable of logging of the air temperature during the transportation are available, but their
use and adequate calibration can be costly.
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9 Identification of samples
Container labels should withstand wetting, drying and freezing without detaching or becoming
illegible. The labelling system shall be waterproof to allow use on site.
The exact information given in the sampling report and on the sample labels depends on the objectives
of the particular measurement programme. In all cases, an indelible label shall be secured to the sample
container.
All other information is supplementary and should be detailed in the sample report.
10 Sample reception
All information regarding sample, handling and storage shall be included in a sampling reporL
Laboratory staff shall receive and check information on sample preservation and sample transport
conditions,
In all cases, and especially when a "chain of custody" process needs to be established, the number of
sample containers received in the laboratory shall be verified against the number of sample containers
submitted.
11 Sample storage
The storage duration of the water samples within the laboratory is specific to the analyte(s] to be
analysed. Samples shall be stored no longer than the maximum storage period given in Tables A.1 to
A.3. The maximum storage time includes the time of transport to the laboratory (3f$.
The refrigeration conditions within the laboratory shall be [3 t 2J "C. Where samples are frozen for
preservation, unless otherwise specified, the temperature shall be maintained below -18'C. Exceptions
to these refrigeration conditions are listed in Tables A.1 to 43.
When thawing frozen samples, it is recommended that each sample container be placed in a separate
secondary container to minimize the risk of liquid loss, should a split become apparent during the
thawing process or a rupture occur during initial freezing and storage. A mild impact can cause splitting
of some plastics at low temperatures.
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With respectto thawing, itis recommended thatthis be done under ambient conditions, unless specified
otherwise in Tables A.1 to A.3 or the analytical International Standard being used.
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AnnexA
(informativeJ
A,1 General
This document and the analytical International Standards listed in this annex are complementary. See
the Notice on page 1.
In some cases the alternative preservation techniques listed contradict each other. It is intended that
where an existing analytical International Standard is used, the preservation technique described in
that method applies. However, alternative preservation techniques given in this document can also be
appropriate. Where no preservation method is described in the analytical International Standard, or no
analytical International Standard is used, the technique(s) listed in this document shall be used.
A validation protocol used for validation studies can be found in Annex C. Reports and data regarding
validation are listed in the bibliography,
A.4 Biologicalanalysis
The following general remarks should be noted in relation to use ofTable A.2.
Plastics used for containers in the laboratory are for instance pE, pTFE, pEI pB pFA, and FEp.
-
- lf a preservation period is not specified, it is generally unimportant The indication "1 month"
represents preservations without particular difficulty.
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Contamination of the sample should be avoided, especially if the sample activity is very low Some
- sample sites can have measurable activity in the soil or air, or in waters other than those being
sampled. Laboratories, as well as some items of domestic equipment, can contain radioactive
material. When sampling precipitation, any special requirements in this table are additional to
those given in ISO 5667-8. As the collection of sufficient sample can require a period of days, both
the starting and finishing times and dates should be recorded. A record of precipitation collection
for the sample station for the appropriate period should be appended. Stabilizer or carrier may be
added, ifappropriate for the analytes being measured.
- Plastics used for containers in the laboratory are for instance PE, PTFE, PET, PP, PFA, and FEP.
NOTE Some plastics bottles slowly concentrate samples over a period ofmany months by being very slightly
permeable to water. Also see the comments for e.g, radon.
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Table A.1 Technlques for sample preservation Physicochemlcal and chemical analysls -o6
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Reference lnternatlonal Preservatlon and storage condltions Maxlmum validated or I q,*
Analyte to be studied
Standard
Type of container
additional to Clauses I and L[ storage times Best practice 3I
qr!
For samples high in dissolved gases, an- .. t,
alyse preferably on site. Reduction and NJ
Plastics or glass
oxidation during storage can change 9 r.r
Acidity and alkalinity t+d Best practice o..
the sample. N
cN
IS0 9963-1:1994 For samples high in dissolved gases,
PE, borosilicate glass
No reference to ISO 5667-3 analys€ preferably on site.
Acidify to pH 1 to pH 2 with HNO3
Plastics or glass [52,4). Store samples in the dark or use
IS0 9562:2004 Glass is required if dark-coloured bottles, 5d Best practice
Adsorbable organlc No reference to ISO 5667-3 the concentration is
halides IAOX) suspected to be low Ifsamples are chlorinated, Note c
applies.
Plastics Freeze to b€low -18 'C. l month Best practice
ISO 12010:2012
Alkanes, Naphthalene Short- refers normatively to Glass Rinse bottles with 2 ml isooctane
chaln ISO 5667-3
polychlorinated
(sccPs) ISO 18635r2016 Glass Store samples in the dark or use
No reference to ISO 5657-3 dark-coloured bottles.
ISO 15586:2003 PE, PP, FEP
refers normatively to
tso 5667-3
IS0 11885:2007 For normal
Acidify to pH 1to pH 2 with HNO3
Aluminium refers normatively to concentrationsl
(s.2.4).
l month Best practice
ISO 5667-3 PE.HD, PTFE
ISO 17 294-2:20'16 For low
refers normatively to concentrations:
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Anions: see the individual anions [Br, F-, Cl-, Nor, Not, soi-,-and Po;)
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Reference International Preservation and storage conditions Maximum Validated or Ba*
Analyte to be studied
Standard
Type of container
additional to Clauses 8 and Ll storage times Best practlce sI
(.,
!
Boron ISO 11885:2007 For normal .. ,
refers normatively to concentrations: Nl
ISO 5667-3 PE.HD, PTFE 9ar
Acidify to pH 1 to pH 2 with HNO3
6 months Validatedlt(It] o..
ISO L7 294-2:2016 For low (s.2.4). N
cN
refers normatively to concentrations:
IS0 5667-3 PFA, FEP
IS0 15061:2001 Remove any ozone from the sample, for
refers normatively to example, add 50 mg of ethylenediamine
Bromate
ISO 5667-3:1994
PE
(5.1-9) to 1 I of sample immediately
l month Best practice
after sampling.
lS0 10304-1:2007
Bromlde and bromlne l month Best practice
refers normatively to PE or glass
compounds rso 5667-3
Plastics or glass,
Bromine residual Analyse on site 5 min Best practice
dark coloured
ISO 15586:2003
refers normatively to PE, PP, FEP
ISO 5667-3
ISO 5961:1994
refers normatively to PE, borosilicate glass
rso 5667-3 Acidify to pH 1 to pH 2 with HN03
Cadmium 6 months Val idate d [l.illl
ISO 11885:2007 For normal (s.2.4).
refers normatively to concentrationsi
tso 5667-3 PE.HD, PTFE
ISO L7 294-2:2076 For low
refers normatively to concentrationsl
rs0 5667-3 PFA, FEP:
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analyse within I h.
Freeze to below -18 'C
Waters shall be filtered before
ISO 8245:1999 acidifyingto pH 1to pH 2 with H2S0a 7d Best practice
Carbon, dissolved
organic (DOCJ refers normatively to Plastics or glass (s.2.s) or H3Poa.(s.2.2).
ISO 5667-3
Freeze to below -18 oC. l month Best practice
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@ Table A.1 (continued)
o-
Reference International Preservation and storage conditions Maximum Validated or sd
Analyte to be studied
Standard
IYpe ofcontainer
additional to Cla_uses I and 11 storage tlmes Best practice 3i
9r!
Plastics or glass Acidify to pH I to pH 2 with H2S0a Validatedtull
,. s
ISO 15705;2002 6 months Nf
Chemical oxygen demand PP, glass (s.2.s). 9qr
refers normatively to o..
{CoDcr) lSo 5667-3:1994 Plastics
Freeze to below -18 'C. 6 months Validatedlltul N
Plastics o
N
Chloramine Plastics or dark glass Analyse on site. 5 min Best practice
ISO 10304-4:1997
Chlorate Add NaOH (5.1.3. or 5.2.61 to
refers normatively to Plastics or glass 7d Best practice
pH 10 t 0,5
IS0 5667-3:1994
ISO 15682:2000
PE or glass
refers to ISO 5667-3
None required, common techniques do
IS0 10304-4:1997 1 month Best practice
not have an adverse effect
Chloride refers normatively to Plastics or glass
ISO 5667-3;1994
ISO 15923-1:2013
refers normatively to
rs0 5667-3
Chlorinated solvents]. See Volatile org anic compounrls
Chlorine dioxide Plastics or dark glass None required, analyse on site 5 min Best practice
Chlorine, residual Plastics or dark glass Analyse on site, 5 min Best practice
ISO 70304-4:7997
Chlorite refers normatively to Plastics or dark glass Add Na0H (5.1.3 or s.2.6) to pH 10 r 0,5 7d Best practice
IS0 5667-3:1994
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Analyte to be studied
Reference lnternational Preservatlon and storage condltlons Maximum Validated or
Type ofcontainer
Standard additional to Clauses I and LL storage times Best practice
ISO 14403-1:2012 and Add NaOH (5J-3 or 5-?-o) to adiust the 7d
lSO 74403 -212072 pH to 12. 1d if sulfide is Best practice
Cyanide, easlly ltberated Plastics or glass present
refer normatively to Store samples in the dark or use
ISO 5667-3 dark-coloured bottles. 3d Best practice
Add NaOH (5.1.3 or 52,6) to 6d
IS0 17690r2015
Cyanide, free (pH = 6) pH=11 t 0,1.
refers normatively to < 1d ifsulfide Best practice
Store samples in the dark or use
ls0 5667-3 is present
dark-coloured bottles.
t4d
1d if sulfide ls validatedtllql
Add NaoH (sJJ or 5^2,6J to adiust the present
pH to 12.
Cyanide, total IS0 14403-1:2012 and Plastics or glass
Store samples in the dark or use
ISO L4 403-2:2OL2 dark coloured bottles.
refer normatively to
7d Best practice
ISO 5667-3
Cyanochloride Plastics 1d Best practice
Detergents: See Surfactants
Dissolved solids (dry residue): See Totql solids (total residues)
Extractable organic
halldes IEOX) ln surface lfsamples are chlorinated, Note c
Glass
applies.
4d Validated[']11
and waste water
Extractable organic
halides (EOX) in If samples are chlorinated, Note c
groundwater and Glass
applies.
l month validatedteil
drinking water
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N
Table A.1 (continued) 66
o-l
Reference lnternational Preservation and storage conditions Maximum Validated or Bd
Analyte to be studied
Standard
Iype ofcontainer
additional to Clirusclg and aL storage times Best practice sI
qr!
Extractable organic Ifsamples are chlorinated, Note c .. D
Glass applies, Acidify to pH 1 to pH 2 with 14d Best practice Na
halldes (EOX) P r.r
HN03 (5.2.4) or H2so* [52.5]. o..
N
IS0 10304-1:2007 cN
refers normatively to
rso 5667-3
ISO 10359-1:1992
refers normatively to
ISO 5667-3
Fluorides
ISO 10359-2:1994 Plastics but not PTFE l month Best Practice
refers normatively to
IS0 5667-3:1994
lS0/TS 17951-1:2016
ISO/TS 17951-2:2016
refer to ISO 5667-3
Acidify with HCI (5.2.3J to 1 mol/l.
Hydrazine Glass Store samples in the dark or use 1d Best practice
dark-coloured bottles.
Acidify to pH 1 to pH 2 with HCI (s.2-3), 1 month Best practice
Glass
HN03 (s.2.a) or H2S04 (5,Z5).
Glasswith ground
ISO 9377-2:2000
refers normatively to
glass stopper, orwith 4d Best practice
screw cap, lined with
Hydrocarbons ISO 5657-3:1994
PTFE
Plastics or
Iron(ll) borosilicate glass
Acidify to pH 1 to pH 2 with HCI (5.2.3). 7d Best practice
ISO 15586:2003
refers normatively to PE, PP, FEP
ISO 5657-3
I5O 11885:2007 For normal
concentrations: Acidifyto pH 1to pH 2 with HNo3
Iron refers normatively to 1 month Best practice
(sJ,41.
IS0 5657-3 PE.HD, PTFE
ISO 77294-2:2016 For low
refers normatively to concentrations:
IS0 5667-3 PFA, FEP
Plastics or glass or
Freeze to below -18 "C. 6 months Validatedtrl].i]
borosilicate glass
Kleldahl nitrogen
lS0 5663:1984 Plastics orglass or Acidify to pH 1 to pH 2 wlth H2S0a
No reference to ISO 5667-3 borosilicate glass (s.2. s).
l month Best practice
N
o, Table A.1 (continued) 66
or
Reference lnternational Preservation and storage conditions Maximum Validated or $c-
Analyte to be studied Type ofcontainer
Standard addltlonal to Clausesj and 11 storage times Best practlce 3i
(,,
ISO 13395:1996 PE or glass 1d Best practice .-al!
refers normatively to Nf
ISO 5667-3:L994 PE or glass Freeze to below -18'C. 8d Best practice I r,r
Nltrate all waters
o.,
- IS0 15923-1:2013 Plastics or glass 1d Best practice N
e
refers normatively to Plastics or glass Acidifyto pH 1to pH 2 with HCI (s.2.3). 7d Best practice N
ISO 5667-3 l
Plastics Freeze to below -18 "C. month Best practice
Nitrate in waste water and Plastics or glass Waters shall be filtered on site, 4d validatedt9zl
surface water {ro11
ISo 13395:1996
Analysis should preferably be carried
refers normatively to Plastics or glass
out on site.
1d Best practice
ISO 5667-3:1994
Nitrite all waters
- IS0 15923-1:2013
refers normatively to
rso 5667-3
Nltrlte ln waste water and Plastics or glass Waters shall be filtered on site. 4d Validated[92]
surface water t10.tl
Analyte to be studied Reference lnternational 'Iype ofcontainer Preservation and storage conditions Maximum Validated or
Standard additional to Clause$.8 and lL storage times Best practice
Orthophosphates, dissolved: See Plr osphorus, dissolved
Fix the oxygen on site. Store samples in
Plastics or glass 4d Best practice
the dark or use dark-coloured bottles.
IS0 5814:2012 The electrochemical method may be
No reference to IS0 5667.3 used as well and can be carried out on
Oxygen Plastics or glass 1d Best practice
site, Store samples in the dark or use
dark-coloured bottles.
ISO 17289:2014
Plastics or glass None required, analyse on site.
No reference to ISO 5667-3
Acidifyto pH 1to pH 2 with HzSO+
2d Best practice
Plastics or glass
Permanganate index ISO 8467:1993 t5r.5).
(CODMn) No reference to ISO 5667-3 Plastics or glass Store samples in the dark. 2d Best practice
Plastics Freeze to below -18'C, 1 month Best practice
lfsamples are chlorinated, Note c t4d Best practice
Glass
Pesticides, carbamates applies.
Plastics Freeze to below -18'C. 1 month Best practice
Acidify to pH 1 to pH 2 with HCI [5.2.3J,
Pesticides, phenoxyalkanoic Glass with PTFE cap HNO3 (5.2.4) or HzSO+ (52.5)c.
herbicidesa 14d
liner or septum Acidify to between pH 3 to 4 witb
alkylhalogenated phenoxy methanoic acid (5216)c. Best practice
acids, hydroxybenzonitriles IS0 15913:2000
and bentazone refers normatively to Glass, dark coloured 3d
ISO 5667-3:1994
-a6
OJ
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GIass
Acidify to pH <4 with HgPo+ (5.2.2) or 27d Best practice
H25oa (5.2.5).
Phenol index ISO 74402:7999 Acidify to pH < 4 with H3P04,( l-2)
refers normatively to PTFE, glass or H2SOa (5.2"5). Store samples in the 2Ld Best practice
lS0 5667-3:1994 dark or use dark-coloured bottles.
ISO 8165-1:1992 Glass or borosilicate
refers normatively to glass with PTFE cap
Acidify to pH < 4 with H:P0+ (5.2.2) or 27d Best practice
HzSo+ (5-iLE)c.
ISO 5667-3:1985 liner
Phenols
IS0 8165-2:1999
refers normatively to Glass, dark coloured pH<2 7d Best practice
I5O 5667-3:1994
ISO 18857-1:2005
Glass
refers normatively to
IS0 5667-3 Glass with ground Acidify to pH 2 with HCI (5.2.3) or
Phenols, alkylated glass stoppet or with H2s0a (5.2.s). 14d Best practice
ISO 18B 57-2r2009
refers normatively to screw cap, lined with
PTFE.
ISO 5667-3
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(,,
N Table A.l (continued) 66
O-r
Reference International Preservation and storage conditions Maximum Validated or sd
Analyte to be studied
Standard
Iype ofcontainer addltional to Llalrses,8 and -l-1
storage times Best practlce 3I
9t!
.. ,l
Plastics, glass or
Na
borosilicate glass 9cr
IS0 15681-1:2003 o..
N
refers normatively to o
N
ISO 5667-3 Plastics, glass or
IS0 15681-2:2003 borosilicate glass
refers normatively to
ISO 5667-3 Acidify to pH I to pH 2 with H2S0a 1 month Best Practice
Phosphorus, total IS0 11885:2007 For normal (s.2.s) or HNo3 [s.2.aJ.
refers normatively to concentrations:
ISO 5667-3 PE.HD, PTFE
$A 17294-2:2016 For low
refers normatively to concentrations:
ISO 5667-3 PFA, FEP
IS0 6878:2004 Preferably glass,
No reference to ISO 5667-3 otherwise PE, PVC
6 months validate d t 10ll
Plastics Freeze to below -18 'C,
lS0 18856:2004
Phthalates Store samples in the dark or use 4d Best practice
refers normatively to Glass
dark-coloured bottles.
rso 5667-3
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a
o Table A.2 [continued) 6d
o-.
Organism group to Tlpe of Preservation technique
Maximum recommended se-
be studled contalner withln the laboratory
preservation time before
analysis
Comments 3I
t,!
"tl
Nl
Macrophytes Glass or plastics Add ethanol [5-?9) to the 6 months Fill bottle to -90 %0, Leave sufficient headspace to allow
with tight sample to give a final volume homogenization, 9or
o,.
fitting lid fraction of 7 0 o/o to 75 o/o
N
year
o
N
Freeze to below -18'C 7 Special procedures may be necessary with groups
which are changed by standard applied preservation
methods.
Benthic diatoms Glass or plastics Addition of 0,5 partto 1 part by 6 months Store samples in the dark. Alkaline Lugol's solution
with tight volume of [acid (5JJ-0] or alka- [5J-1-I) is generally applicable in fresh water and acidic
fitting lid line (5.2.11)l Lugol's solution to Lugol's solution (5.2.10) in marine water with delicate
200 parts by volume ofsample. flagellates. For specific determination see specific
Cool to (3 r 2) "C standard. Addition ofmore Lugol's solution maybe nec-
essary if decolourization occurs. Over saturation [deep/
brown colouring) should be avoided, yet enough Lugol's
solution (5.2.10 or 52-L[) should be added to turn the
sample to a cognac or straw coloul,
Fill bottle to -90 0/0, Leave sufficient headspace to allow
homogenization.
Add ethanol (SJ!J to the 6 months Fill bottle to -90 0/0, Leave sufficient headspace to allow
sample to give a final volume homogenization.
fraction of 7O o/o to 7 5 o/o
Pelagic diatoms Glass or plastics Addition of0,5 partto l part by 6 months Store samples in the dark. Alkaline Lugol's solution
with tight volume of [acid (5.2.10J or alka- (5,2.10 is generally applicable in fresh water and acidic
fitting lid line (5.2.r1)l Lugolt solution to Lugol's solution (5.2.10) in marine water with delicate
200 parts by volume ofsample. flagellates. For specific determination see specific
cool to (3 r 2) "c standard. Addition ofmore Lugol's solution may be nec-
essary if decolourization occurs. Over saturation (deep/
brown colouring) should be avoided, yet enough Lugol's
solution (5.2.10 or 5-jl"11J should be added to turn the
sample to a cognac or straw colour.
Fill bottle to -90 %, Leave sufficient headspace to allow
homogenization.
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Table A,3
- Techniques for sample preservation
- Radiochemical analytes and activities 66
o-
Analyte or Maximum recommended Be*
Type of
activity to be
container Preservation technique preservation time before Comments 3E
studied analysis 9r!
"lr
r.r A
Acidify to pH <2 with HN03 Do notacidify ifthe sample is evaporated immediately on
Gross alpha
(s.2.4)
l month
a planchette for analysis. without acidification, however,
Q r.r
activity Plastics Ga ,.
7d store samples in the dark and cool to (3 t 2)'C ifpossible. N
None cN
Gross beta- Acidify to pH < 2 with HN03 Do notacidify ifthe sample is evaporated immediately on
1 month
activity [except io- Plastics (s.2.4) a planchette for analysis. Without acidification, however,
dine radioisotopes) None 7d store samples in the dark and cool to (3 t 2) "C if possible.
Acidify to pH < 2 with HNO3 If possible, store samples in the dark and cool to
(sJ.4) l month
Gamma-emitters Plastics [3 r 2) 'c.
lfa sample is notacidified, stora8e maybe shorter if
None 7d metal present are easily hydrolysed.
Actinides Acidify to pH <2 wtth HN03
2 months
(52A)
[alpha-emitters lfpossible, store samples in the dark and cool to
such as uranium, Plastics
plutonium, [3 12) "C.
None td
americium, curium)
Add NaOH (s.2.4) to pH > 10 l month Fill bottle completely,leave no headspace and do not stir
Ifpossible, store samples in the dark and cool to
(3 t 2) "c.
r4c Plastics None 5d 0nly ifpH > 7, fill the container completely to avoid any
exchange between sample and the air above.
Ifpossible, store samples in the dark and cool to
(3 r 2) "C.
Acidify to pH < 2 with HNO3 7d For gamma-spectrometry, acidification is sufficient.
(s-2-4). For gross beta-determination, acidify to pH < 1 with
Iodine Where iodine-isotopes are meas- HN03 [5.2.4); add 2 ml to 4 ml ofNaOCl [5.2.14J per litre
(radioisotopes] Plastics
ured with gross-beta-detection ofsample, ensuring an excess offree chlorine.
techniques, add KIO3 (5.2.15) to Ifpossible, store samples in the darkand cool to
prevent losses during evaporation (3 r 2) "c.
Fill bottle completely, leave no headspace and do not stir,
Radon isotopes Glass cool to [3 r 2) "c 1d If possible, store samples in the dark.
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Annex B
[informativeJ
Container preparation
8.1 Reagents
Unless otherwise stated, use only reagents ofrecognized analytical grade and distilled or demineralized
water or water of equivalent purity.
8.2 Solvent-washedglasscontainers
WARNING Organic solvents can be hazardous. Provide suitable handling facilities and handle
with care, -
Non-disposable sample containers and lids for semi-volatile analysis should be washed with a
phosphate-free detergent solution, followed by thorough rinses with hot tap-water and analyte-free
water. The last step should be an acetone rinse. The lids should be in place on the container during the
rinse step (solvent in the container with the lid tightly screwed down] because the solvents can rinse
plastic from the interior screw threads on to the PTFE lining.
For analysis of volatile organic compounds, sample containers, screw caps, and septa (silicone vapour
barriersJ should be washed with a phosphate-free detergent, rinsed once with tap-water, rinsed at least
twice with analyte-free water, then dried at greater than 105 oC. A solvent rinse should generally be
avoided because it can interfere with the analysis, although a methanol rinse is acceptable.
Alternatively, single use disposable containers and lids may be used for both sample types.
8.3 Acid-washedcontainers
For trace metal analysis, new sample containers should always be used, Sample containers and lids
should be thoroughly cleaned with a phosphate-free detergent solution, thoroughly rinsed with metal-
free water, soaked for 24 h in -10 % volume fraction HNO: or -25 % volume fraction HCl, and rinsed
with metal-free water.
44
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Annex C
IinformativeJ
C.1 General
Studies of the preservation of water samples were carried out in the Netherlands between 2003 and
2011. The studies were performed bylaboratories associated with the Federation ofDutch laboratories,
calibration and inspection bodies (FeNeLabJ. The obiective was to establish preservation times for
a number of critical analyses in the most relevant types of water: groundwater, surface water, and
waste water.
A fixed protocol was used, which distinguished between four types of water: groundwater or eluate;
surface water or etTluent; food industry waste water; chemical industry waste water.
C.2 Protocol
Within each study, a minimum of between 6 and 12 different samples were used, at low and high
concentration levels. Samples were obtained and divided over various bottles on day 0 and ifnecessary
spiked. Day 0 is defined as the sampling date and date ofarrival in the laboratory.
On day 0, analyses of eight test portions [bottles] were performed and the mean, i1, of each analyte
was calculated.
Subsequent measurements ofthree test portions were carried out each day in sequence, e.g. at 1 d, 2 d,
4 d,7 d, 14 d, and 28 d. From the analytical results obtained, the mean of each analyte, fg, was
calculated.
Once the difference between the mean test results of the stored test portions and the mean test results
on day 0 was more than twice the standard deviation, q established by method validation, i.e.
f6 -x-a > 2s
45
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Additionally data provided by individual members of FeNeLab were evaluated. These data were
obtained in stability studies for interlaboratory comparisons or for validation of procedures of
sampling, transport and analysis ofa specific laboratory.
C.4 Evaluations
The following analyses and matrices were evaluated:
All reports and data involved are listed in the bibliography {References [81] to 805]J and are available
from The Netherlands Standardization Institute [NEN], except for References IBB1, t89l, t961 and U.esl.
46
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tP fi'B2@.1a2.124.21E -d 21112t2@3 15:a72.1ldit 1'15-?,231227-25
Bibliography
t1l ISO 5663:1984, Woter quality Determination ofKjeldahl nitrogen Method after mineralization
with selenium - -
lSo 58t4:2012, water quolity
Lzl
- Determination ofdissolved oxygen - Electrochemical probe method
ISO 5951:1994, Water quality
t31
- Determinotion ofcadmium by atomic absorption spectrometry
t4l ISO 6468:1996,Water quality Determination ofcertain orgonochlorine insecticides, potychlorine
biphenyls and chlorobenzenes
- Gas-chromatogrophic method after liquid-liquid extraction
-
ISO 6878:200d Woter quality
tsl
spectrometric method - Determinotion of phosphorus - Ammonium motybdate
l6l ISO 7027-1:2016, Woter quality Determination of turbidity Part 1: Quantitative methods
- -
17l ISO 7150-1:1984, Water quality Determination of ommonium Port 7: Monual spectrometric
method - -
ISO 7887:2011, Water quality
t8l - Exomination ond determination of colour
ISO 7888:1985, Wa ter quality
tel - Determination of electrical conductivigr
ISO 7980:1986, Water quality
[10]
spectrometric method
- Determination of calcium and magnesium - Atomic obsorption
[11] ISO 8165-1:1992, Water quality Determination of selected monovalent phenols Port 1: Gas-
chromdtogmphic
-
method ofter enrichment by extroction
-
UZ] ISO 8165-2:1999, Water quolity Determination olselected monovolent phenols Part 2: Method
by ilerivatization ond gas chromotogrophy
- -
[13] $O a245:1999, Water quality Guidelines lor the determination of total organic corbon ITOC) and
dissolved organic carbon (DOC)
-
I14l ISO 8467:1993, Water quality Determination ofpermanganote index
-
ISO 9377-2:2OOO, Woter quolity
[1s] - Determination of hydrocarbon oil index
solvent extraction and gas chromatography
- Part 2: Method using
u6l ISO 9439:1999, Woter quality Evaluation of ultimate oerobic biodegradobility of organic
compounds in aqueous medium
- Carbon dioxide evolution test
-
[17] lSO 9552:2004, Water quol@ Determination olodsorboble orgonically bound halogens (AOX)
-
ISo 9963-1:1994, Woter quality Determination of alkalinity Part 1: Determination oI total
[18]
and com p o site a I ko I i n i ty - -
ISO 9964-3:1993, Woter quality Determinotion ofsodium and potassium Port3: Determination
[1e]
of sodium anil potossium by flame emission spectrometry
- -
- Measurement of biochemical
ISO 10260:1992, Water quality parameters Spectrometric
t20l
determination of the chlorophyll-o concentration
-
ISO 10304-1:2002 Water qualigt of
12tl
ions
- Determinotion of dissolved onions by liquid chromatogrophy
Port 7: Determination of bromide, chloride, fluoride, nitrate, nitrite, phosphate and sulfate
-
122) ISO 10304-3:1997, Water quolity Determination of dissolved anions by liquid chromatography of
ions
-
Part 3: Determination of chromate, iodide, sulfite, thiocyanate ond thiosulfate
-
47
SupdLd !, BSB Edge u.da t'rE lirc tm BIS td olrFs. CoBLnl SdvioE - t.el. ({ura<*'.pdr.81&ml.M) -
lP d.42O2.112.1?a21A - @d 27n!2@3 15:17:22 q.hd EIS-20231227-25
[23] ISO 10304-4:1997, Water qualitlt Determination of dissolved anions by liquid chromatography
- of
ions Port 4: Determination of chlorate, chloride ond chlorite in woter with low contaminotion
-
t24) ISO 10359-1:1992, Water quality Determinotion of fluoride
- - Port 7: Electrochemical probe
method for potable and lightly polluted water
t28l ISO 10695:2000, Water quality Determination of selected organic nitrogen and phosphorus
-
compounds Gas chromatographic methods
-
l29l ISO 11074:2015, Soil quality
- Vocabulary
[30] ISO 11369:1992 Water quality Determination of seleAed plont treotment agents
- Method
-
using high performance liquid chromatography with UV detection after solid-kquid extroction
t31l ISO 11423-1:1992 Water quality Determination of benzene and some derivatives
- - Part 1:
H ead-space gas chromatographic method
[32] ISO 11423-2:1997, Water quality Determinotion of benzene and some derivatives
- - Part 2:
Method using extraction and gas chromatography
t35l ISO 12010:2012, Water quality Determination of short-choin polychlorinated alkanes (SCCPs) in
-
woter Method using gas chromatogrophy-moss spectromew $C-MS) and negotive-ion chemical
-
ionization (NCI)
48
Sl+dLd bt ESB Eda€ ordd tlE aod's rM ats ld ODg. CdE n:m Sdi- - lolir. (rNddh.9.E l4eg@d.Gm)
tP &t62tE. t12.12121E - &d 2Um2315.a7 22 .t*td AE-20231227-25
tssl ISO L7034, Generol requirements for the competence ofreference materiol producers
ts6l SO fi2a9:2014, Water quality Determinotion of dissolved oxygen Optical sensor method
- -
ISO 17294-2:2O16, Water quality
ts 7l
(ICP-MS) - Applicotion of inductively coupled plasmo mass spectrometry
Part 2: Determination of selected elements including uronium isotopes
-
tssl ISO 17353:2004 Water quolity Determination of selected organotin compounds Gas
chrom o togra p h i c m ethod
- -
Ise] ISO 17378-1:2014,Water quolity Determination of arcenic ond antimony Part 7: Method using
-
hydride generation atomic fluorescence spectrometry (HG -AFS)
-
ISO 17378-2:2Ol4,Water quality
[60] - Determinotion oforcenic ond antimony
hydride generution otomic absorption spectrometry (H G -AAS) - Part 2: Method using
ISO 17690:2015, Water quolity of available free cyanide (pH 6) using flow
[63] - Determination
injection onalysis [FIA), gas-dilfusion and amperometric detection
164) ISO 17852:2006, Woter quality Determination of mercury Method using atomic fluorescence
spectrometry - -
49
$rp-d b, EsB Ed!6 qds itE b..B t m BtS fo. Oi.e. CoErt nt S6ivb6 - rohi. (rudr.rdE0lomt.dn) _
tp ,,,dra2@,_112j2121E _ @27n2r2@.315[t7e q*.1g ?,,z3I?2i-15
lS 17614 {Prn 3) : 2021
ISO 5aB7-3 : 2018
167) ISO/TS 17951-2:2016, Water quality Determination offluoride using flow anolysis (FIA and CIA)
-
Port 2: Method using continuous flow analysis ICFA) with qutomated in-line distillaiion
-
[68] ISO 17993:2O02, Water quolity Determination of 15 polycyclic oromatic hydrocarbons (PAH) in
-
woter by HPLC with fluorescence detection after liquid-liquid extroction
[70] ISO 18635:2016, Water quolity Determination of short-chain polychlorinoted alkanes (SCCPs) in
-
sedimenl sewage sludge and suspended (particulate) matter Method using gas chromatography- *
moss spectrometry (GC-MS) and electron capture negative ionization (ECNI)
l74l ISO 20595:2018, Water quolity Determination of selected easily volatile organic compounds in
-
water Method using gas chromatography and mass spectrometry by static headspace technique
-
(HS-GC.MS)
[76] ISO 23913:2006, Water quolity Determinotion of chromium(Vl) Method using flow analysis
(FlA and CFA) and spectrometric detection
- -
1771 ISO 28540:2011, Woter quality Determination of 75 polycyclic aromatic hydrocarbons (PAH) in
water
-
Method using gas chromatography with mass spectrometric detection (GC-MS)
-
t78l ISO 29441:2010, Water quality
- Determination of totol nitrogen after UV digestion
using flow analysis (CFA and FIA) and spectometric detection
- Method
I79l EN 15204:2006, Woter quality Guidonce stondard on the enumeration of phytoplankton using
inverted microscopy (U termdhl
-
technique)
t80] APHA, AWWA, WEF, Standard methods for the examination of water and waste water. American
Public Health Association. American Water Works Association. Water Environment Federation,
Z?nd edition,2Ol2
[81] Baiema B.L. Evoluatie van de pH metingen 2005-2007 met betekking tot monsterneming,
conservering en meetonzekerheid lEvaluotion of pH meosurements 2005-2007 with respect to
sampling, preservation and uncertaintyl. Vitens Laboratorium Rapportcode: VL-IO-AC0702-2,
January 2008
50
S!9dbd b, as8 Eds€ (nd- 0. liEE t m BIS b. olrl.!. CorrLnt sdYi6 - t&L (r@dEcdigl8i.l.co.n) -
lP &4 2@-L2.121 21C - *d 2l12J&7 15:11 2.t]*|e 815-20?3127-25
t82l Bafema B.L. Onderzoek naar de houdbaarheid von ammonium in aongezuurde en niet aangezuurde
monsters, [Aquakem600J fResearch on moximum storage times of ammonium in acidiJied and non'
aciitifieil samplesl. Vitens Laboratorium Rapportcode: VL-lO-AC0521, December 2005
[83] Van Bakergem E., Validation oI the preservation time of organochlorine pesticides (OCP),
polychlorinated biphenyls {PCB) and non-volotile chlorobenzenes (NCBZ) rn B,aste woters. Al-West,
April 2011
[S4] Broer W. Volidotion "Preservation time organochlorine pesticides, PCB and tri-, tetra-, pento- ond
hexachlorobenzenes in gmundwoter". ALcontrol, October 2008
t85] De long G., Van Berkel E. Validotie ringonderzoek VGK en VAK in afvalwoter lValidation ofVGK and
VAK intralaboratory trails on surfoce waterl.Kiwa,proiectnummer 630000.162.001 April 2003
[87] FeNeLab. Conservering van tin in woter met solpeterzuur lPreservation of tin in water with nitric
acrdl. FeNeLab, lune 2008
[88] G6mez-Ariza f.L., Girildez I., Morales E., Ariese F,, Cofino W. Queuauviller P., Stability and storage
problems in organotin speciation in environmental sarnples. f. Environ. Monil 1999, I pp,l97-2O2
t89] Haney f.F., Hall D.J. Sugor-cooted Daphnia: A preservation technique for Clodocero. Limnol.
Oceanogr. 1973, 18 pp. 331-333
[90] KIWA. Validatie van (nieuwe) pardmeters en/of matices [Validotion of [new) parometers dnd
matricesl, Kiwa, KHRO-5.0.8, August 2003
t9U KIWA. Validatie t,b,v. ringonderzoeken onionen lValidotion for anions interlaboratory comparisonl,
Kiwa,2003
[93] KlWA.Validatie t.b.v. ringonderzoeken metalen lvalidation for metals interlaboratory comparisonf.
Kiwa, 2003
[94] Landwehr f.L., Tukker l, Volidatie van conserveringstermijn ONB en OPB in afiolwoter lValiilation
of storoge times of ONBs ond OPBs in waste waterl SIKB prolect 55 Versie 1, October 2003
t95] Landwehr I,L. Validotie van conserveringstermijnen in Afvalwaten Houdbaarheid van OCB, PCB en
CB (chloorbenzenes) fValidation of storoge times in waste waten Preservotion of OCBs, PCBs, anil
CBsl. Omegam, fuly 2009
[96] Schoerbel l, Methoden der Hydrobiologie: S sswasserbiologie fHydrobiology methods: Fresh woter
biologyl. Stuttgart: Fischec 3rd Edition, 1980
[99] Van Den Berg W., Yedema E, Validatie conserveertermijn EOX in water {Vatidation storage time
EOX in waterl, Dienst waterbeheer en riolering, ingenieursbureau, Rapportnummer O3.780225,
November 2003
51
SupdLd b, ASB EQ6 undq th6 lirc rM Bls fd orFsp Co@Lnt Sdi- - rot tr (@!.dttaFl'3ea@mrdn) -
tP .d@2@.112-12l21A - dM 27112t2@3 15:a1:22 Erh.l als-2023r227-25
[100] Van Den Berg W.A.l. Onderzoek op conserveringstermijn van afvalwatermonsters voor de pH
bepaling |nvestigation into the storoge time of woste woter samples for pH determinationl.
Waterproef proiect 2007-109, September 2007
[10q Van Kranenburg P. Validatie van conserver@stermijn van oromaten en CKW in water lValidation
of the stomge time of aromatics and chlorinated hydrocarbons in water). Analytico milieu BV,
october 2003
[102] Van Den Berg M.A.E. ANVM project 209 Evaluation of preservation methods and moximum storage
times for woter somples. Delft: NEN, 2002
[103] Van Den Berg M.A,E. STOWA report 2000-26. Evaluatie van conserveringstechnieken lEvoluation
of preservation metiods]. Utrecht STOWA, 2000
[104] Waterschap Groot Salland. Validatie van conserveringstermijn van nitrite en nitraat+nitrite in
oppervlaktewater en afvalwater lYalidotion of preservation times of nitrite and nitrate+nitrite in
surfoce water and waste woterl.Waterschap Groot Salland, October 2003
[1os] Werres F., Balsaa P., SchmidtT.C. Total concentration analysis of polycylic aromatic hydrocarbons
in aqueous samples with high suspended particulote matter content,l, Chromatogr. A. !216,2009,
pp.2235-2240
52
SlpfE br BSB EdlE (ns tE bD nw AEi ld Oi.qE Co@la.l Sdvir - tol6t ( Edr.fd.6a]&maff) -
tP .d@ 2@.112.12121a - (dod 27h2t82315:172 q/8ilat 8ts"frZ312?-25
(Continued ttom *@nd @vei
lS 17614 (Pat121) . 2021 \ hter quality Sampling : Part 21 Guidance on sampling of drinking
- by tankers or means other than distribution pipes
water distributed
(under pnnq
lS 17614 (Pan 22\ '. 2021 Water quality Sampling : Pafi 22 Guidance on the design and
-
installation of groundwater monitoring points (under pdnt\
lS 17614 (Paftz3\:2021 Vlhter quality Sampling : Part 23 Guidance on passive sampling in
-
surface waters (under pint\
lS 17614 (Pan 24\ : 2021 \ hler quality Samding : Parl 24 Guidance on the auditing of water
-
quality sampling (under pint)
lS 17614 (Part 25) : 2021 \ hter quality Sampling : Part 25 for microbiological analysis (under
pnn0' -
The lndian Standard lS 3025 (Part 1) : 1987 'Method of sampling and test (Physacal and Chemical)
for water and wastewater: Part 1 Sampling' prescribes the methods of sampling of water and
waslewater for physical and chemical examinalions. This is a very old slandard and hence it is not
exhaustive. The Committee responsible for formulating this standard has decided to harmonize the
method of sampling prescribed in lS 3025(Part 1) with those prescribed in lS 17614 (Patl1) : 20211
ISO 5667-1 :2020 and 17614 (Part 3) : 2021llSO 5667-3 : 2018. Hence, lS 3025 (Part'l) : '1987 will be
withdrawn afler the public€tion of these two standards.
The text of the ISO Standard has been approved as suitable for publication as an lndian Standard
without deviations. Certain terminologies and conventions are, however, not identical to those used in
lndian Standards. Attenlion is partiorlarly drawn to the following:
a) V\iherever the words 'This doarment' appear refening to this standard, they should be read as
'This lndian Standard'.
b) Comma (,) has been used as a decjmal marker, while in lndian Standards, the cunent practice
is to use a point (.) as the decimal marker.
ln this adopted standard, reference appears to certain lntemational Standards where the standard
atrnospheric conditions to be obseNed are stipulated which are not apdicable to tropical/subtropical
countries. The applicable standard atmospheric conditions for lndian conditions arc 27 r 2 "C and
65 + 5 percent relative humidi$ and shall be observed while using this standard.
ln this adopted standard, references appearto certain lntemational Standards for which lndian Standards
also exist. The conesponding lndian Standards, which are to be substituted in their respedive places,
are listed below along with their degree of equivalence for the editions indicated:
ISO 3696 vllater for analytical lS 1070 : 1992 Reagent grade water
-
Not Equivalent
laboratory use Specification and Specification (t hid rev i sio n\
test methods
-
ISO 19458 V1/ater quality lS 17614 (Part 25) : 2021llSO 19458 : ldentical with
- Sampling
for microbiological analysis 2006 \ hter quality Sampling for lso 19458:
-
microbiological analysis (under pnnt) 2006
The tectlnical committee has reviewed the provisions of the following lntemational Standards refened
in this standard and has dec.ided that they are acceptable for use in conjugation with this standard:
1) ISO ha6 puui6hed 24 parts of ISO 5667 6erie6 wtrile the other parts of ISO 5667 serie6 are uhder developrnent lndia ha6
adopted ISO 5667 series from Pan I to Part 24.
S'rpdin by BS8 Edo€ u.tdr db titE fm Bts fd on g. Co@t nt sdvba - rot i. ( ure.Ir.pdrEaaOsm..d,) _
tP a&.@ 2q2..112_121.21E _ ffi 2t12tZV3 1s1t.A eg*trt BtS-2oAi 227-2s
BIS is a statutory institution established under the Bureau of lndian Standards Act,2Oi6 to promote
harmonaous development of the activities of standardization, marking and quality certification of goods
and attending to conneded matters in the country.
Copyrlght
BIS has the copyright of all its publications. No part of these publications may be reproduced in any
form without the prior permission in writing of BlS. This does not predude the free use, in the course of
implementing the standard, of necessary details, sucfi as symbols and sizes, type or grade designations.
Enquiries relating to copyright be addressed to the Darecior (Publications), BlS.
Amendments are issued to standards as the need arises on the basis of comments. Standards are also
reviewed periodically; a standard along with amendments is reafrirmed when sucfl revlew indicates that
no changes are needed; if the review indicates that changes are needed, it is taken up for revision.
Users of lndian Standards should ascertain that they are in possession of the latest amendments or
edition by refening to the latesl issue of 'BlS Catalogue' and 'Standards: Monthly Additions'.
This lndian Standard has been developed from Doc No-r CHD 36 (15787).
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