CN101776606A - Method for analyzing total carbon and total organic carbon in liquid - Google Patents
Method for analyzing total carbon and total organic carbon in liquid Download PDFInfo
- Publication number
- CN101776606A CN101776606A CN201010110736A CN201010110736A CN101776606A CN 101776606 A CN101776606 A CN 101776606A CN 201010110736 A CN201010110736 A CN 201010110736A CN 201010110736 A CN201010110736 A CN 201010110736A CN 101776606 A CN101776606 A CN 101776606A
- Authority
- CN
- China
- Prior art keywords
- total
- carbon
- organic carbon
- total organic
- liquid
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Images
Landscapes
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention provides a method for analyzing total carbon and total organic carbon in liquid, which relates to the technical field of detection of components. An atomic emission spectrum is used for analyzing the total carbon and the total organic carbon. By regulating the pH value of a solution and blowing and removing CO2 in the solution with gas which does not contain CO2, the method of the invention can be used for respectively analyzing the total carbon and the total organic carbon. The analyzing method of the invention can overcome the influence of high salt and strong acid and has the advantages of small error, high accuracy, simplicity and convenience.
Description
Technical field
The present invention relates to the detection technique field of composition, particularly the method that total carbon in the liquid and total organic carbon are analyzed.
Background technology
Chemical oxygen demand cod is the important indicator that tradition is estimated the contaminated degree of water body, but because the assay method of COD is no matter be the potassium permanganate high-temperature oxidation, the potassium permanganate low-temperature oxidation method still is the problem that all there is the oxygenation efficiency of organic substance in potassium dichromate oxidation, the general potassium permanganate high-temperature oxidation of using, its oxygenation efficiency is 50～60%, use potassium dichromate oxidation, its oxygenation efficiency is 80～90%, under acid potassium dichromate condition, even the catalytic action of silver sulfate is arranged, the straight chain fatty compound can be oxidized effectively, it is oxidized that yet aromatic hydrocarbons and pyridine are difficult to, and its oxygenation efficiency is lower.Therefore, chemical oxygen demand cod can not reflect total amount of organic fully.
The measurement of total carbon (TC) and total organic carbon (TOC) is used more and more extensive at aspects such as environment monitoring, quality controls, adopt TOC analyzer method at present, is that the carbon compound in the sample (organic and inorganic) is converted into CO by catalytic oxidation
2, detect CO with the non-dispersion infrared detector
2, but when the high salt of this type of methods analyst, strong acid sample, problem such as the ubiquity catalyzer is easily poisoned, reburner is perishable.
Summary of the invention
The object of the present invention is to provide a kind of method that total carbon and total organic carbon in the liquid such as water, waste water, strong acid, salt solution are analyzed.
The present invention adopts Atomic Emission Spectral Analysis total carbon and total organic carbon.
The method of analyzing total carbon content is: the pH value of adjusting liquid is 0～12; The emissive power of adjusting CID CCD detecting device is that 650～1750W, secondary air amount are that 0～1.5L/min, atomizer pressure are that 0～0.4Mpa, pump speed are that 0～150rpm, integral time are 0～120 second; Adopt high purity water and Potassium Hydrogen Phthalate preparation standard specimen, carry out the matrix coupling; Under the identical spectra condition, adopt calibration curve method that the total carbon of liquid is carried out quantitative test.
The method of analyzing total organic carbon content is: the pH value of adjusting liquid is 0～12; The emissive power of adjusting CID CCD detecting device is that 650～1750W, secondary air amount are that 0～1.5L/min, atomizer pressure are that 0～0.4Mpa, pump speed are that 0～150rpm, integral time are 0～120 second; Adopt high purity water and Potassium Hydrogen Phthalate preparation standard specimen, carry out the matrix coupling; Earlier with not containing CO
2Gas purging remove CO in the solution
2, under the identical spectra condition, adopt calibration curve method that the total organic carbon of sample is carried out quantitative test again.
Because the matrix effect difference of water, waste water, strong acid, salt solution is very big, need adopts the matrix coupling with Atomic Emission Spectral Analysis, and will guarantee the purity (not containing carbon) of the reagent that added.And atomic emission spectrum can be measured water, waste water, strong acid, the various matrix sample of salt solution, so the present invention selects Atomic Emission Spectral Analysis.
The inventive method adopts the pH value of adjusting solution, with not containing CO
2Gas purging remove CO in the solution
2So, can analyze total carbon and total organic carbon respectively, analytical approach of the present invention can overcome the influence of high salt, strong acid, and this method error is little, precision is high, simple and convenient.
Description of drawings
Fig. 1 is the atomic emission spectrum spectrogram of embodiment 1.
Fig. 2 is the atomic emission spectrum canonical plotting of embodiment 1.
Embodiment
Take the representational uniform liquid sample of 100mL (water, waste water, strong acid, salt solution), with Atomic Emission Spectral Analysis total carbon and total organic carbon.
Embodiment 1
Analyze total carbon and total organic carbon amount in the brine sample.
Total carbon is analyzed: the emissive power of adjusting CID CCD detecting device: 1350W, and secondary air amount: 1.0L/min, atomizer pressure: 0.2MPa, pump speed: 80rpm selects 10 seconds integral time.Adopt with high purity water, Potassium Hydrogen Phthalate preparation standard specimen, carry out the matrix coupling with high pure sodium chloride, the pH value of adjusting sample is 7, under the identical spectra condition, the total carbon emission spectrogram of sample and the emission spectrogram of standard specimen are contrasted, carry out qualitative analysis; Adopt calibration curve method that the total carbon of sample is carried out quantitative test, total carbon is 203mg/L, and its error is analyzed, and it the results are shown in Table shown in 1: total carbon relative standard deviation 0.017896% in the sample.
Total organic carbon is analyzed: the emissive power of adjusting CID CCD detecting device: 1350W, and secondary air amount: 1.0L/min, atomizer pressure: 0.2MPa, pump speed: 80rpm selects 10 seconds integral time.Adopt with high purity water, Potassium Hydrogen Phthalate preparation standard specimen, carry out the matrix coupling with high pure sodium chloride, the pH value of adjusting sample is 2, with nitrogen purging 20 minutes, under the identical spectra condition, the total organic carbon emission spectrogram of sample and the emission spectrogram of standard specimen are contrasted, carry out qualitative analysis; Adopt calibration curve method that the total organic carbon of sample is carried out quantitative test, total organic carbon is 150mg/L, and its error is analyzed, and it the results are shown in Table shown in 1: total organic carbon relative standard deviation 0.020588% in the sample.
The standard specimen stacking diagram of atomic emission spectrum embodiment 1 as shown in Figure 1.Among the figure, horizontal ordinate is a wavelength, and unit is nm; Ordinate is signal intensity (a no unit), and foreign language is expressed as: S (IR).To represent blank, low mark and high standard respectively be the spectrogram at 193.091nm place at wavelength for three standard specimens among the figure.
The atomic emission spectrum standard specimen match linear graph of embodiment 1 as shown in Figure 2.
Total carbon and total organic carbon amount in the wastewater sample.
Total carbon is analyzed: the emissive power of adjusting CID CCD detecting device: 950W, and secondary air amount: 0.5L/min, atomizer pressure: 0.1MPa, pump speed: 100rpm selects 5 seconds integral time.Adopt with high purity water, Potassium Hydrogen Phthalate preparation standard specimen, the pH value of adjusting sample is 5, under the identical spectra condition, the total carbon emission spectrogram of sample and the emission spectrogram of standard specimen is contrasted, and carries out qualitative analysis; Adopt calibration curve method that the total carbon of sample is carried out quantitative test, total carbon is 341mg/L, and its error is analyzed, and it the results are shown in Table shown in 2: total carbon relative standard deviation 0.011721% in the sample.
Total organic carbon is analyzed: the emissive power of adjusting CID CCD detecting device: 950W, and secondary air amount: 0.5L/min, atomizer pressure: 0.1MPa, pump speed: 100rpm selects 5 seconds integral time.Adopt with high purity water, Potassium Hydrogen Phthalate preparation standard specimen, the pH value of adjusting sample is 1, uses nitrogen purging 15 minutes, under the identical spectra condition, the total organic carbon emission spectrogram of sample and the emission spectrogram of standard specimen is contrasted, and carries out qualitative analysis; Adopt calibration curve method that the total organic carbon of sample is carried out quantitative test, total organic carbon is 251mg/L, and its error is analyzed, and it the results are shown in Table 2: total organic carbon relative standard deviation 0.014102% in the sample.
Embodiment 3
Total carbon and total organic carbon amount in the hydrochloric acid sample.
Total carbon is analyzed: the emissive power of adjusting CID CCD detecting device: 1150W, and secondary air amount: 0.5L/min, atomizer pressure: 0.15MPa, pump speed: 75rpm selects 15 seconds integral time.Adopt with high purity water, Potassium Hydrogen Phthalate preparation standard specimen, carry out the matrix coupling with high purity hydrochloric acid, the pH value of adjusting sample is 1, under the identical spectra condition, the total carbon emission spectrogram of sample and the emission spectrogram of standard specimen is contrasted, and carries out qualitative analysis; Adopt calibration curve method that the total carbon of sample is carried out quantitative test, total carbon is 105mg/L, and its error is analyzed, and it the results are shown in Table shown in 3: total carbon relative standard deviation 0.010491% in the sample.
Total organic carbon is analyzed: the emissive power of adjusting CID CCD detecting device: 1150W, and secondary air amount: 0.5L/min, atomizer pressure: 0.15MPa, pump speed: 75rpm selects 15 seconds integral time.Adopt with high purity water, Potassium Hydrogen Phthalate preparation standard specimen, carry out the matrix coupling with high purity hydrochloric acid, the pH value of adjusting sample is 1, with nitrogen purging 10 minutes, under the identical spectra condition, the total organic carbon emission spectrogram of sample and the emission spectrogram of standard specimen are contrasted, carry out qualitative analysis; Adopt calibration curve method that the total organic carbon of sample is carried out quantitative test, total organic carbon is 100mg/L, and its error is analyzed, and it the results are shown in Table 3: total organic carbon relative standard deviation 0.012081% in the sample.
The relative standard deviation of total carbon and total organic carbon in table 1 salt solution
| Analysis times | Total carbon (mg/L) | Total organic carbon (mg/L) |
| ??1 | ??200 | ??150 |
| ??2 | ??201 | ??148 |
| ??3 | ??205 | ??147 |
| ??4 | ??203 | ??150 |
| ??5 | ??209 | ??152 |
| ??6 | ??199 | ??153 |
| ??7 | ??198 | ??155 |
| ??8 | ??203 | ??147 |
| ??9 | ??206 | ??145 |
| ??10 | ??207 | ??151 |
| Relative standard deviation (%) | ??0.017896 | ??0.020588 |
The relative standard deviation of total carbon and total organic carbon in table 2 waste water
| Analysis times | Total carbon (mg/L) | Total organic carbon (mg/L) |
| ??1 | ??342 | ??256 |
| ??2 | ??341 | ??254 |
| ??3 | ??344 | ??248 |
| ??4 | ??337 | ??246 |
| ??5 | ??335 | ??248 |
| ??6 | ??339 | ??247 |
| ??7 | ??342 | ??252 |
| ??8 | ??336 | ??255 |
| ??9 | ??345 | ??251 |
| ??10 | ??347 | ??249 |
| Relative standard deviation (%) | ??0.011721 | ??0.014102 |
The relative standard deviation of total carbon and total organic carbon in table 3 hydrochloric acid
| Analysis times | Total carbon (mg/L) | Total organic carbon (mg/L) |
| ??1 | ??105 | ??100 |
| ??2 | ??104 | ??99 |
| ??3 | ??106 | ??100 |
| ??4 | ??104 | ??98 |
| ??5 | ??105 | ??101 |
| ??6 | ??107 | ??99 |
| ??7 | ??106 | ??97 |
| ??8 | ??104 | ??98 |
| ??9 | ??104 | ??99 |
| Analysis times | Total carbon (mg/L) | Total organic carbon (mg/L) |
| ??10 | ??104 | ??100 |
| Relative standard deviation (%) | ??0.010491 | ??0.012081 |
Claims (3)
1. the method that total carbon in the liquid and total organic carbon are analyzed is characterized in that adopting Atomic Emission Spectral Analysis total carbon and total organic carbon.
2. according to the described method that total carbon in the liquid and total organic carbon are analyzed of claim 1, it is characterized in that the method for analyzing total carbon content is: the pH value of adjusting liquid is 0～12; The emissive power of adjusting CID CCD detecting device is that 650～1750W, secondary air amount are that 0～1.5L/min, atomizer pressure are that 0～0.4Mpa, pump speed are that 0～150rpm, integral time are 0～120 second; Adopt high purity water and Potassium Hydrogen Phthalate preparation standard specimen, carry out the matrix coupling; Under the identical spectra condition, adopt calibration curve method that the total carbon of liquid is carried out quantitative test.
3. according to the described method that total carbon in the liquid and total organic carbon are analyzed of claim 1, it is characterized in that the method for analyzing total organic carbon content is: the pH value of adjusting liquid is 0～12; The emissive power of adjusting the CIDCCD detecting device is that 650～1750W, secondary air amount are that 0～1.5L/min, atomizer pressure are that 0～0.4Mpa, pump speed are that 0～150rpm, integral time are 0～120 second; Adopt high purity water and Potassium Hydrogen Phthalate preparation standard specimen, carry out the matrix coupling; Earlier with not containing CO
2Gas purging remove CO in the solution
2, under the identical spectra condition, adopt calibration curve method that the total organic carbon of sample is carried out quantitative test again.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201010110736A CN101776606A (en) | 2010-02-05 | 2010-02-05 | Method for analyzing total carbon and total organic carbon in liquid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201010110736A CN101776606A (en) | 2010-02-05 | 2010-02-05 | Method for analyzing total carbon and total organic carbon in liquid |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101776606A true CN101776606A (en) | 2010-07-14 |
Family
ID=42513120
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201010110736A Pending CN101776606A (en) | 2010-02-05 | 2010-02-05 | Method for analyzing total carbon and total organic carbon in liquid |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101776606A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103080683A (en) * | 2010-08-27 | 2013-05-01 | 朗盛德国有限责任公司 | High-temperature furnace, use of a spinel ceramic and method for carrying out T(O)C measurements of samples |
| CN103196896A (en) * | 2013-04-16 | 2013-07-10 | 四川大学 | Continuous flow analysis method for detecting total organic carbon in water sample |
| CN105705943A (en) * | 2013-10-23 | 2016-06-22 | 哈希公司 | Carbon analysis using ferrate oxidation |
| CN111351783A (en) * | 2018-12-20 | 2020-06-30 | 上海宝钢工业技术服务有限公司 | Method for detecting content of organic matters in soil |
-
2010
- 2010-02-05 CN CN201010110736A patent/CN101776606A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103080683A (en) * | 2010-08-27 | 2013-05-01 | 朗盛德国有限责任公司 | High-temperature furnace, use of a spinel ceramic and method for carrying out T(O)C measurements of samples |
| CN103196896A (en) * | 2013-04-16 | 2013-07-10 | 四川大学 | Continuous flow analysis method for detecting total organic carbon in water sample |
| CN105705943A (en) * | 2013-10-23 | 2016-06-22 | 哈希公司 | Carbon analysis using ferrate oxidation |
| CN105705943B (en) * | 2013-10-23 | 2019-06-14 | 哈希公司 | Carbon analysis is carried out using ferrate oxidation |
| CN111351783A (en) * | 2018-12-20 | 2020-06-30 | 上海宝钢工业技术服务有限公司 | Method for detecting content of organic matters in soil |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US9791430B2 (en) | Measurement of total organic carbon | |
| Ma et al. | Determination of nanomolar levels of nutrients in seawater | |
| Mertes et al. | Development of a sensitive long path absorption photometer to quantify peroxides in aerosol particles (Peroxide-LOPAP) | |
| Zhang et al. | An automatic gas-phase molecular absorption spectrometric system using a UV-LED photodiode based detector for determination of nitrite and total nitrate | |
| CN113218902B (en) | Method and device for automatically monitoring residual concentration of hydrogen peroxide on line | |
| CN101776606A (en) | Method for analyzing total carbon and total organic carbon in liquid | |
| CN107655875B (en) | Total organic carbon analysis method based on high-intensity ultraviolet light oxidation and point discharge | |
| JP5282204B2 (en) | Formaldehyde measuring method and formaldehyde measuring device | |
| CN108982379A (en) | The methods and applications of NO3-N and NO2-N nitrogen total amount in a kind of measurement sample | |
| CN101825641A (en) | Water quality total nitrogen on-line automatic monitoring device | |
| CN105675763A (en) | Multifunctional chromatographic apparatus and method for measuring chloridion and total organic carbon | |
| Tue-Ngeun et al. | Determination of dissolved inorganic carbon (DIC) and dissolved organic carbon (DOC) in freshwaters by sequential injection spectrophotometry with on-line UV photo-oxidation | |
| CN201662575U (en) | On-line automatic monitoring device for water quality total nitrogen | |
| CN202119742U (en) | Chemical oxygen demand (COD)/total organic carbon (TOC)/twisted nematic (TN) online automatic monitor using high temperature burning oxidation method | |
| CN113065095B (en) | Ultraviolet spectrum-based detection algorithm for nitrogen content in water | |
| US20140057360A1 (en) | Arrangement and method for detecting hydrogen peroxide | |
| Yang et al. | Miniature microplasma carbon optical emission spectrometry for detection of dissolved oxygen in water | |
| CN110146487B (en) | In-situ determination of total SO in food2Method (2) | |
| CN112666151A (en) | Method for rapidly, qualitatively and quantitatively analyzing trace bromide ions | |
| Zheng et al. | Development of trichloroethylene gaseous sensor utilizing ZnO–Y 2 O 3 as nanocatalyst based on thermal desorption/cataluminescence | |
| Zhao et al. | An environment-friendly device for rapid determination of chemical oxygen demand in waters based on ozone-induced chemiluminescence technology | |
| CN215115863U (en) | Detection apparatus for antioxidant content in transformer plant insulating oil | |
| Santos et al. | Sequential injection methodology for carbon speciation in bathing waters | |
| Chen et al. | Determination of total mercury and methylmercury in human hair by graphite-furnace atomic absorption spectrophotometry using 2, 3-dimercaptopropane-1-sulfonate as a complexing agent | |
| JP2002205053A (en) | System for monitoring raw water and method for controlling operation of concentrating/separating apparatus using the same |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Open date: 20100714 |