CN103149286A - Method for detecting chloroacetic acid in seawater desalting strong brine - Google Patents
Method for detecting chloroacetic acid in seawater desalting strong brine Download PDFInfo
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Abstract
The invention discloses a method for detecting chloroacetic acid in seawater desalting strong brine. The method comprises the steps: firstly filtering a water sample, then carrying out acidification and esterification under the condition of heating in a water bath, directly placing a derivative bottle containing the water sample into a blowing and trapping automatic sample injector, and measuring the content of the chloroacetic acid in the seawater desalting strong brine through a gas chromatography electron capture detector. In the process of operation, usage amount of organic solvent is little, operational steps are simple, the esterification reaction of dichloroacetic acid and trichloroacetic acid in the water sample is conducted in the derivative bottle, samples are not needed to be transferred, and finally the derivative bottle containing the esterified water sample is directly placed into the blowing and trapping automatic sample injector to conduct the enrichment sample injection. The detection method is quick, simple and convenient to achieve, low in detection limit, high in degree of precision and high in recovery rate, and can satisfy the requirements of quantitative determination of target compound in the seawater desalting strong brine.
Description
Technical field
The present invention relates to by means of the chemistry of measuring material or physical property is tested or the method for amalyzing substances, specifically, relate to for the chloroacetic detection method of seawer system.
Background technology
The biocides such as liquid chlorine commonly used, sodium hypochlorite in the desalinization preprocessing process; these biocides are when bacterium in water, algae and other marine organism are killed in chlorination; usually can with seawater in the soil ulmin reaction; produce a series of chlorinated secondary products; these chlorinated secondary products and excessive biocide can be along with the strong brine discharge into seas; although its concentration due to the degraded and the physical dilution process decrease; but also can certain harm be arranged to hydrobiont, have a strong impact on the local ecologic environment in ocean through the long-term accumulation meeting.Therefore wherein, chloroacetic toxicity is larger, is one of important indicator of water quality monitoring in the world, carries out that in sea water desalinization strong brine, the chloroacetic acid monitoring has important practical significance.
Chloroacetic acid in water environment adopts vapor-phase chromatography to measure usually, and sample-pretreating method has that liquid-liquid extraction is derivative, head space, purge and trap etc.The people such as Qiu Fen are in " chloroacetic acid in the gas chromatography determination Drinking Water " literary composition, with reference to the drinking water standard method of inspection (GB/T5750-2006), water sample through sulfuric acid acidation, is extracted to contain interior target methyl tert-butyl ether, carry out again esterification derivative, measure through GC-ECD.The people such as Zhang Jian adopt Solid-Phase Extraction-purge and trap-gas chromatography mass spectrometry method to divide the content of the chloroacetic acid in bleed in " purge and trap-GC-MS measures the chloroacetic research of underwater trace " literary composition, first pass through Solid-Phase Extraction, then carry out derivative reaction.Above-mentioned these methods need to consume a large amount of organic solvents, complex operation step, time and effort consuming; And because the salinity of sea water desalinization strong brine is higher, be subjected to the impact of salting-out effect, the above-mentioned detection method that these are applicable to the fresh water system can not the Accurate Determining sea water desalinization strong brine in chloroacetic content.
In recent years, fast development along with Seawater Desalination Project, the dense salt waste water of its discharging receives publicity day by day on the impact of marine environment, in strong brine, the detection method research of organic contaminant still is in the starting stage, at present, have not yet to see chloroacetic detection method research report in relevant sea water desalinization strong brine.
Summary of the invention
What the present invention will solve is can not accurately detect chloroacetic technical matters in sea water desalinization strong brine at present, chloroacetic detection method in a kind of sea water desalinization strong brine is provided, and detection limit is low, and precision is high, operation steps is simple, need not to shift sample in testing process.
In order to solve the problems of the technologies described above, the present invention is achieved by following technical scheme:
Chloroacetic detection method in a kind of sea water desalinization strong brine, the method is carried out according to following steps:
(1) water sample to be measured filters, and filtrate is packed in clean Brown Glass Brown glass bottles and jars only;
(2) add the concentrated sulphuric acid to regulate its pH value to 0.1 ~ 0.5;
(3) 2 ~ 4 ℃ of stored refrigerated;
(4) get cryopreserved liquid within 24h and be placed in derivative bottle, adding percent by volume is 10% ~ 20% sulfuric acid methanol solution, and the volume ratio of described filtrate and described sulfuric acid methanol solution is 1: 0.02 ~ 0.2;
(5) with described derivative bottle in 40 ~ 60 ℃ of water bath with thermostatic control 40 ~ 120min;
(6) described derivative bottle is put into the purge and trap automatic sampler, by the gas chromatography electron capture detector, chloroacetic acid in sea water desalinization strong brine is measured;
(7) density of scawater preparation chloroacetic acid standard serial solution, carry out pre-treatment according to step (2) to step (5), measure with the gas chromatography electron capture detector under the condition identical with step (6), take chloroacetic mass concentration as horizontal ordinate, peak area is as ordinate drawing standard curve, obtains the typical curve regression equation;
(8) obtain chloroacetic peak area according to step (6), utilize the chloroacetic typical curve regression equation of step (7) gained, calculate chloroacetic mass concentration in water sample to be analyzed.
Chloroacetic acid described in the present invention refers to dichloroacetic acid (DCAA) and/or trichloroacetic acid (TCAA).
Preferably, in step (1), water sample to be measured filters and adopts filter paper or filter membrane.Described filter paper is the middling speed qualitative filter paper.Described filter membrane aperture is 0.45 μ m.
Preferably, the pH value in step (2) is 0.1.
Preferably, in step (4), the percent by volume of sulfuric acid methanol solution is 10%.
Preferably, described in step (4), the volume ratio of filtrate and described sulfuric acid methanol solution is 1: 0.12.
Preferably, the bath temperature in step (5) is 60 ℃.
Preferably, the water-bath time in step (5) is 60min.
Usually, the salinity of the density of scawater in step (7) is 40.
The present invention is under strong acid and heating condition, make trace amounts of chlorine acetic acid and the corresponding methyl esters of excessive methanol reaction generation in sea water desalinization strong brine, then utilize the gas chromatography electron capture detector to measure, carry out qualitative, peak area calibration curve method with retention time and carry out quantitatively.
The reaction equation of methyl dichloroacetate:
The reaction equation of methyl trichloroacetate:
The invention has the beneficial effects as follows:
Density of scawater (salinity 40) the preparation chloroacetic acid standard serial solution that use of the present invention is close with the sea water desalinization strong brine salinity, and according to chloroacetic mass concentration and peak area drawing standard curve, obtain the typical curve regression equation, can reduce the sea water desalinization strong brine salting-out effect to the impact of testing result, improve detection accuracy.First the suspension in sea water desalinization strong brine and finely ground particle substance are filtered out before sample detection, then under condition of water bath heating, carry out the acidifying esterification, the derivative bottle that above-mentioned water sample directly will be housed is again put into the purge and trap automatic sampler, and the gas chromatography electron capture detector is measured chloroacetic content in sea water desalinization strong brine.
In operating process of the present invention, the organic solvent use amount is few, operation steps is simple, in water sample, the esterification of dichloroacetic acid and trichloroacetic acid is carried out in derivative bottle, need not to shift sample, the derivative bottle of water sample directly will be housed after esterification at last put into the purge and trap automatic sampler and carry out the enrichment sample introduction.
Adopt detection method of the present invention to detect that in sea water desalinization strong brine, the detection limit of dichloroacetic acid and trichloroacetic acid is respectively 0.15 ~ 0.79 μ gL
-1With 0.84 ~ 1.35 μ gL
-1, precision RSD is respectively 1.26% ~ 7.33% and 1.01% ~ 8.10%, and average recovery rate is respectively 82.3% ~ 112.4% and 80.4% ~ 110.6%.Detection method of the present invention is quick, easy, and detection limit is low, and precision is high, and the recovery is high, can satisfy target compound quantitative measurement requirement in sea water desalinization strong brine.
Description of drawings
Fig. 1 is that concentration is 36.0 μ gL
-1Standard model gained standard colors spectrogram;
Fig. 2 is the chromatogram that the embodiment of the present invention 1 detects water sample.
Embodiment
The present invention is described in further detail below by specific embodiment, and following examples can make those skilled in the art more fully understand the present invention, but do not limit the present invention in any way.
The material that uses in each embodiment is as follows:
Density of scawater (salinity 40), standard substance dichloroacetic acid (DCAA), trichloroacetic acid (TCAA), State Standard Matter Research Centre;
The concentrated sulphuric acid is that top grade is pure, and mass concentration is 98.3%, Tianjin Kermel Chemical Reagent Co., Ltd.;
Methyl alcohol is chromatographically pure, Tianjin Concord Technology Co., Ltd.;
The sulfuric acid methanol solution: add 50mL methyl alcohol (chromatographically pure) in beaker, then shift 10 ~ 20mL concentrated sulphuric acid (top grade is pure) with transfer pipet, liquid to be mixed reaches room temperature, transfers in the 100mL volumetric flask, dilutes constant volume with methyl alcohol.
Each embodiment instrument is as follows:
The 7890A gas chromatograph of being furnished with electron capture detector (μ ECD), U.S. Agilent company;
The Stratum PTC device of being furnished with the AQUATek70 automatic sampler, U.S. Teledyne Tekmar company;
Thermostat water bath.
Embodiment 1
(1) water sample preparation
A. get the water sample that 30mL sea water desalinization strong brine floss hole gathers, sample is top layer and bottom mixed sample.
B. water sample to be measured filters with the middling speed qualitative filter paper, and filtrate is packed in clean Brown Glass Brown glass bottles and jars only;
C. add the concentrated sulphuric acid in filtrate, regulate its pH value to 0.1;
D. Brown Glass Brown glass bottles and jars only is positioned over 4 ℃ of refrigerator and cooled and hides preservation;
E. refrigerate and get the above-mentioned filtrate of 25mL within 24h and be placed in the derivative bottle that capacity is 40mL, adding the 3.0mL percent by volume is 10% sulfuric acid methanol solution, and mixes;
F. the water-bath of above-mentioned derivative bottle being put into 60 ℃ is incubated 60min;
G. will derive bottle and put into the purge and trap automatic sampler, by the gas chromatography electron capture detector, chloroacetic acid in sea water desalinization strong brine be measured;
(2) gas chromatography arranges condition
Described gas chromatography adopts HP-5(30m * 0.32mm * 0.25 μ m) quartz capillary column; Carrier gas used is high pure nitrogen; Injector temperature is 200 ℃; Detecting device (ECD) temperature is made as 250 ℃; Adopt temperature programme: the column temperature initial temperature is 35 ℃, keeps 7min, then with 5 ℃ of min
-1Heating rate is warming up to 70 ℃, then with 30 ℃ of min
-1Heating rate is warming up to 250 ℃, keeps 5min; The post flow is 1mL min
-1, tail blows 60mLmin
-1The split ratio 5:1 of capillary column; External standard method is quantitative;
Purge sample size 20mL; Purge time 12min; Sweep gas flow velocity 30mLmin
-1, purge 40 ℃ of temperature; Desorption time 2min, 280 ℃ of baking temperatures; Stoving time 12min.
(3) preparation of standard sample and mensuration
With density of scawater (salinity 40) preparation chloroacetic acid standard serial solution, chloroacetic mass concentration is respectively: 0.0,12.0,24.0,36.0,60.0,120.0 μ gL
-1
According to the pre-treating method in the water sample preparation, the chloroacetic acid standard serial solution is similarly processed, and measure with the gas chromatography electron capture detector under identical condition with water sample, take its mass concentration as horizontal ordinate, peak area is ordinate drawing curve, obtain the working curve regression equation, dichloroacetic acid working curve equation is y=436x-133, and linearly dependent coefficient is 0.9992; Trichloroacetic acid working curve equation is y=968x-410, and linearly dependent coefficient is 0.9990; Wherein, mass concentration is 36.0 μ gL
-1Standard model gained standard colors spectrogram see Fig. 1.
(4) result and data
A. the chromatogram of water sample that the present embodiment detects is seen Fig. 2, according to obtaining chloroacetic peak area, utilizes the typical curve regression equation calculation to go out chloroacetic mass concentration in water sample to be analyzed, and test result sees Table 1.
B. detection sensitivity: the present embodiment is measured blank solution 11 times, obtains average signal-to-noise ratio, and the detection limit that calculates dichloroacetic acid and trichloroacetic acid according to signal to noise ratio (S/N ratio) S/N=3 is respectively 0.15 μ gL
-1With 0.84 μ gL
-1
C. the accuracy of detection method: the mode that this enforcement adopts mark-on to reclaim has been verified the accuracy that detects, and does recovery experiment take sea water desalinization strong brine as background solution, adds the standard model of known quantity, replication 6 times.This enforcement average recovery rate and accuracy the results are shown in Table 1.
Table 1 average recovery rate and accuracy determination result (n=6)
Embodiment 2
(1) water sample preparation
A. get the water sample that 30mL sea water desalinization strong brine floss hole gathers, sample is top layer and bottom mixed sample.
B. water sample to be measured is with the membrane filtration of 0.45 micron, and filtrate is packed in clean Brown Glass Brown glass bottles and jars only;
C. add the concentrated sulphuric acid in filtrate, regulate its pH value to 0.5;
D. Brown Glass Brown glass bottles and jars only is positioned over 2 ℃ of refrigerator and cooled and hides preservation;
E. refrigerate and get the above-mentioned filtrate of 25mL within 24h and be placed in the derivative bottle that capacity is 40mL, adding the 0.5mL percent by volume is 20% sulfuric acid methanol solution, and mixes;
F. the water-bath of above-mentioned derivative bottle being put into 40 ℃ is incubated 40min;
G. will derive bottle and put into the purge and trap automatic sampler, by the gas chromatography electron capture detector, chloroacetic acid in sea water desalinization strong brine be measured;
(2) that condition is set is identical with embodiment 1 for gas chromatography.
(3) preparation of standard sample and mensuration
With density of scawater (salinity 40) preparation chloroacetic acid standard serial solution, chloroacetic mass concentration is respectively: 0.0,12.0,24.0,36.0,60.0,120.0 μ gL
-1
According to the pre-treating method in the water sample preparation, the chloroacetic acid standard serial solution is similarly processed, and measure with the gas chromatography electron capture detector under identical condition with water sample, take its mass concentration as horizontal ordinate, peak area is ordinate drawing curve, obtain the working curve regression equation, dichloroacetic acid working curve equation is y=620x-75, and linearly dependent coefficient is 0.9975; Trichloroacetic acid working curve equation is y=310x-27, and linearly dependent coefficient is 0.9981.
(4) result and data
A. according to obtaining chloroacetic peak area, utilize the typical curve regression equation calculation to go out chloroacetic mass concentration in water sample to be analyzed, test result sees Table 2.
B. detection sensitivity: the present embodiment is measured blank solution 11 times, obtains average signal-to-noise ratio, and the detection limit that calculates dichloroacetic acid and trichloroacetic acid according to signal to noise ratio (S/N ratio) S/N=3 is respectively 0.40 μ gL
-1With 1.09 μ gL
-1
C. the accuracy of detection method: the mode that this enforcement adopts mark-on to reclaim has been verified the accuracy that detects, and does recovery experiment take sea water desalinization strong brine as background solution, adds the standard model of known quantity, replication 6 times.This enforcement average recovery rate and accuracy the results are shown in Table 2.
Table 2 average recovery rate and accuracy determination result (n=6)
Embodiment 3
(1) water sample preparation
A. get the water sample that 30mL sea water desalinization strong brine floss hole gathers, sample is top layer and bottom mixed sample.
B. water sample to be measured filters with the middling speed qualitative filter paper, and filtrate is packed in clean Brown Glass Brown glass bottles and jars only;
C. add the concentrated sulphuric acid in filtrate, regulate its pH value to 0.3;
D. Brown Glass Brown glass bottles and jars only is positioned over 3 ℃ of refrigerator and cooled and hides preservation;
E. refrigerate and get the above-mentioned filtrate of 25mL within 24h and be placed in the derivative bottle that capacity is 40mL, adding the 5.0mL percent by volume is 15% sulfuric acid methanol solution, and mixes;
F. the water-bath of above-mentioned derivative bottle being put into 50 ℃ is incubated 50min;
G. will derive bottle and put into the purge and trap automatic sampler, by the gas chromatography electron capture detector, chloroacetic acid in sea water desalinization strong brine be measured;
(2) that condition is set is identical with embodiment 1 for gas chromatography.
(3) preparation of standard sample and mensuration
With density of scawater (salinity 40) preparation chloroacetic acid standard serial solution, chloroacetic mass concentration is respectively: 0.0,12.0,24.0,36.0,60.0,120.0 μ gL
-1
According to the pre-treating method in the water sample preparation, the chloroacetic acid standard serial solution is similarly processed, and measure with the gas chromatography electron capture detector under identical condition with water sample, take its mass concentration as horizontal ordinate, peak area is ordinate drawing curve, obtain the working curve regression equation, dichloroacetic acid working curve equation is y=257x-104, and linearly dependent coefficient is 0.9981; Trichloroacetic acid working curve equation is y=528x-227, and linearly dependent coefficient is 0.9985.
(4) result and data
A. according to obtaining chloroacetic peak area, utilize the typical curve regression equation calculation to go out chloroacetic mass concentration in water sample to be analyzed, test result sees Table 3.
B. detection sensitivity: the present embodiment is measured blank solution 11 times, obtains average signal-to-noise ratio, and the detection limit that calculates dichloroacetic acid and trichloroacetic acid according to signal to noise ratio (S/N ratio) S/N=3 is respectively 0.79 μ gL
-1With 1.35 μ gL
-1
C. the accuracy of detection method: the mode that this enforcement adopts mark-on to reclaim has been verified the accuracy that detects, and does recovery experiment take sea water desalinization strong brine as background solution, adds the standard model of known quantity, replication 6 times.This enforcement average recovery rate and accuracy the results are shown in Table 3.
Table 3 average recovery rate and accuracy determination result (n=6)
Embodiment 4
(1) water sample preparation
A. get the water sample that 30mL sea water desalinization strong brine floss hole gathers, sample is top layer and bottom mixed sample.
B. water sample to be measured is with the membrane filtration of 0.45 micron, and filtrate is packed in clean Brown Glass Brown glass bottles and jars only;
C. add the concentrated sulphuric acid in filtrate, regulate its pH value to 0.1;
D. Brown Glass Brown glass bottles and jars only is positioned over 4 ℃ of refrigerator and cooled and hides preservation;
E. refrigerate and get the above-mentioned filtrate of 25mL within 24h and be placed in the derivative bottle that capacity is 40mL, adding the 2.0mL percent by volume is 10% sulfuric acid methanol solution, and mixes;
F. the water-bath of above-mentioned derivative bottle being put into 60 ℃ is incubated 90min;
G. will derive bottle and put into the purge and trap automatic sampler, by the gas chromatography electron capture detector, chloroacetic acid in sea water desalinization strong brine be measured;
(2) that condition is set is identical with embodiment 1 for gas chromatography.
(3) preparation of standard sample and mensuration
With density of scawater (salinity 40) preparation chloroacetic acid standard serial solution, chloroacetic mass concentration is respectively: 0.0,12.0,24.0,36.0,60.0,120.0 μ gL
-1
According to the pre-treating method in the water sample preparation, the chloroacetic acid standard serial solution is similarly processed, and measure with the gas chromatography electron capture detector under identical condition with water sample, take its mass concentration as horizontal ordinate, peak area is ordinate drawing curve, obtain the working curve regression equation, dichloroacetic acid working curve equation is y=114x-41, and linearly dependent coefficient is 0.9990; Trichloroacetic acid working curve equation is y=210x-34, and linearly dependent coefficient is 0.9988.
(4) result and data
A. according to obtaining chloroacetic peak area, utilize the typical curve regression equation calculation to go out chloroacetic mass concentration in water sample to be analyzed, test result sees Table 4.
B. detection sensitivity: the present embodiment is measured blank solution 11 times, obtains average signal-to-noise ratio, and the detection limit that calculates dichloroacetic acid and trichloroacetic acid according to signal to noise ratio (S/N ratio) S/N=3 is respectively 0.32 μ gL
-1With 0.97 μ gL
-1
C. the accuracy of detection method: the mode that this enforcement adopts mark-on to reclaim has been verified the accuracy that detects, and does recovery experiment take sea water desalinization strong brine as background solution, adds the standard model of known quantity, replication 6 times.This enforcement average recovery rate and accuracy the results are shown in Table 4.
Table 4 average recovery rate and accuracy determination result (n=6)
Embodiment 5
(1) water sample preparation
A. get the water sample that 30mL sea water desalinization strong brine floss hole gathers, sample is top layer and bottom mixed sample.
B. water sample to be measured filters with the middling speed qualitative filter paper, and filtrate is packed in clean Brown Glass Brown glass bottles and jars only;
C. add the concentrated sulphuric acid in filtrate, regulate its pH value to 0.3;
D. Brown Glass Brown glass bottles and jars only is positioned over 3 ℃ of refrigerator and cooled and hides preservation;
E. refrigerate and get the above-mentioned filtrate of 25mL within 24h and be placed in the derivative bottle that capacity is 40mL, adding the 5.0mL percent by volume is 15% sulfuric acid methanol solution, and mixes;
F. the water-bath of above-mentioned derivative bottle being put into 50 ℃ is incubated 120min;
G. will derive bottle and put into the purge and trap automatic sampler, by the gas chromatography electron capture detector, chloroacetic acid in sea water desalinization strong brine be measured;
(2) that condition is set is identical with embodiment 1 for gas chromatography.
(3) preparation of standard sample and mensuration
With density of scawater (salinity 40) preparation chloroacetic acid standard serial solution, chloroacetic mass concentration is respectively: 0.0,12.0,24.0,36.0,60.0,120.0 μ gL
-1
According to the pre-treating method in the water sample preparation, the chloroacetic acid standard serial solution is similarly processed, and measure with the gas chromatography electron capture detector under identical condition with water sample, take its mass concentration as horizontal ordinate, peak area is ordinate drawing curve, obtain the working curve regression equation, dichloroacetic acid working curve equation is y=147x-52, and linearly dependent coefficient is 0.9987; Trichloroacetic acid working curve equation is y=256x-88, and linearly dependent coefficient is 0.9991.
(4) result and data
A. according to obtaining chloroacetic peak area, utilize the typical curve regression equation calculation to go out chloroacetic mass concentration in water sample to be analyzed, test result sees Table 5.
B. detection sensitivity: the present embodiment is measured blank solution 11 times, obtains average signal-to-noise ratio, and the detection limit that calculates dichloroacetic acid and trichloroacetic acid according to signal to noise ratio (S/N ratio) S/N=3 is respectively 0.22 μ gL
-1With 0.86 μ gL
-1
C. the accuracy of detection method: the mode that this enforcement adopts mark-on to reclaim has been verified the accuracy that detects, and does recovery experiment take sea water desalinization strong brine as background solution, adds the standard model of known quantity, replication 6 times.This enforcement average recovery rate and accuracy the results are shown in Table 5.
Table 5 average recovery rate and accuracy determination result (n=6)
Although the above is described the preferred embodiments of the present invention; but the present invention is not limited to above-mentioned embodiment; above-mentioned embodiment is only schematic; be not restrictive; those of ordinary skill in the art is under enlightenment of the present invention; not breaking away from the scope situation that aim of the present invention and claim protect, can also make the concrete conversion of a lot of forms, within these all belong to protection scope of the present invention.
Claims (10)
1. chloroacetic detection method in a sea water desalinization strong brine, is characterized in that, the method is carried out according to following steps:
(1) water sample to be measured filters, and filtrate is packed in clean Brown Glass Brown glass bottles and jars only;
(2) add the concentrated sulphuric acid to regulate its pH value to 0.1 ~ 0.5;
(3) 2 ~ 4 ℃ of stored refrigerated;
(4) get cryopreserved liquid within 24h and be placed in derivative bottle, adding percent by volume is 10% ~ 20% sulfuric acid methanol solution, and the volume ratio of described filtrate and described sulfuric acid methanol solution is 1: 0.02 ~ 0.2;
(5) with described derivative bottle in 40 ~ 60 ℃ of water bath with thermostatic control 40 ~ 120min;
(6) described derivative bottle is put into the purge and trap automatic sampler, by the gas chromatography electron capture detector, chloroacetic acid in sea water desalinization strong brine is measured;
(7) density of scawater preparation chloroacetic acid standard serial solution, carry out pre-treatment according to step (2) to step (5), measure with the gas chromatography electron capture detector under the condition identical with step (6), take chloroacetic mass concentration as horizontal ordinate, peak area is as ordinate drawing standard curve, obtains the typical curve regression equation;
(8) obtain chloroacetic peak area according to step (6), utilize the chloroacetic typical curve regression equation of step (7) gained, calculate chloroacetic mass concentration in water sample to be analyzed.
2. chloroacetic detection method in a kind of sea water desalinization strong brine according to claim 1, is characterized in that, in step (1), water sample to be measured filters and adopts filter paper or filter membrane.
3. chloroacetic detection method in a kind of sea water desalinization strong brine according to claim 2, is characterized in that, described filter paper is the middling speed qualitative filter paper.
4. chloroacetic detection method in a kind of sea water desalinization strong brine according to claim 2, is characterized in that, described filter membrane aperture is 0.45 μ m.
5. chloroacetic detection method in a kind of sea water desalinization strong brine according to claim 1, is characterized in that, the pH value in step (2) is 0.1.
6. chloroacetic detection method in a kind of sea water desalinization strong brine according to claim 1, is characterized in that, in step (4), the percent by volume of sulfuric acid methanol solution is 10%.
7. chloroacetic detection method in a kind of sea water desalinization strong brine according to claim 1, is characterized in that, described in step (4), the volume ratio of filtrate and described sulfuric acid methanol solution is 1: 0.12.
8. chloroacetic detection method in a kind of sea water desalinization strong brine according to claim 1, is characterized in that, the bath temperature in step (5) is 60 ℃.
9. chloroacetic detection method in a kind of sea water desalinization strong brine according to claim 1, is characterized in that, the water-bath time in step (5) is 60min.
10. chloroacetic detection method in a kind of sea water desalinization strong brine according to claim 1, is characterized in that, the salinity of the density of scawater in step (7) is 40.
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| CN105241967A (en) * | 2015-07-22 | 2016-01-13 | 厦门谱尼测试有限公司 | Measurement method of residual quantity of chloroacetic acid compounds in cosmetics |
| CN106525670A (en) * | 2017-01-24 | 2017-03-22 | 淄博市环境监测站 | Method for simultaneously detecting nine haloacetic acids in PM2.5 fine particulate matters in air |
| CN107422053A (en) * | 2017-07-04 | 2017-12-01 | 苏州出入境检验检疫局检验检疫综合技术中心 | A kind of method of trichloroacetic acid in LC-MS detection cosmetics |
| CN108008061A (en) * | 2017-12-06 | 2018-05-08 | 湖北省兴发磷化工研究院有限公司 | A kind of method of chloroacetic acid in ion chromatography detection monoxone, dichloroacetic acid, trichloroacetic acid and sulfate radical |
| CN109406690A (en) * | 2018-11-25 | 2019-03-01 | 山东达因海洋生物制药股份有限公司 | A kind of method in relation to substance in detection chloraldurate |
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| CN101131381A (en) * | 2007-09-27 | 2008-02-27 | 上海交通大学 | Method for detecting halogen acetic acid in drinking water |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105241967A (en) * | 2015-07-22 | 2016-01-13 | 厦门谱尼测试有限公司 | Measurement method of residual quantity of chloroacetic acid compounds in cosmetics |
| CN106525670A (en) * | 2017-01-24 | 2017-03-22 | 淄博市环境监测站 | Method for simultaneously detecting nine haloacetic acids in PM2.5 fine particulate matters in air |
| CN106525670B (en) * | 2017-01-24 | 2019-03-12 | 肖洋 | The method for measuring nine kinds of halogen acetic acids in air PM2.5 fine particle simultaneously |
| CN107422053A (en) * | 2017-07-04 | 2017-12-01 | 苏州出入境检验检疫局检验检疫综合技术中心 | A kind of method of trichloroacetic acid in LC-MS detection cosmetics |
| CN107422053B (en) * | 2017-07-04 | 2020-08-21 | 苏州出入境检验检疫局检验检疫综合技术中心 | Method for detecting trichloroacetic acid in cosmetics by liquid chromatography-mass spectrometry |
| CN108008061A (en) * | 2017-12-06 | 2018-05-08 | 湖北省兴发磷化工研究院有限公司 | A kind of method of chloroacetic acid in ion chromatography detection monoxone, dichloroacetic acid, trichloroacetic acid and sulfate radical |
| CN108008061B (en) * | 2017-12-06 | 2020-11-10 | 湖北省兴发磷化工研究院有限公司 | Method for detecting monochloroacetic acid, dichloroacetic acid, trichloroacetic acid and sulfate radical in chloroacetic acid by ion chromatography |
| CN109406690A (en) * | 2018-11-25 | 2019-03-01 | 山东达因海洋生物制药股份有限公司 | A kind of method in relation to substance in detection chloraldurate |
| CN109406690B (en) * | 2018-11-25 | 2022-02-25 | 山东达因海洋生物制药股份有限公司 | Method for detecting related substances in chloral hydrate |
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