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HJ 758-2015 English PDF

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HJ 758-2015: Water quality. Determination of haloacetic acids. Gas chromatography
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Basic data

Standard ID HJ 758-2015 (HJ758-2015)
Description (Translated English) Water quality. Determination of haloacetic acids. Gas chromatography
Sector / Industry Environmental Protection Industry Standard
Word Count Estimation 14,170
Date of Issue 2015-10-22
Date of Implementation 2015-12-01
Quoted Standard HJ/T 91; HJ/T 164
Regulation (derived from) Ministry of Environment Announcement 2015 No.62
Issuing agency(ies) Ministry of Ecology and Environment
Summary This standard specifies the determination of haloacetic acid compounds in water by gas chromatography. This standard applies to surface water, groundwater, sewage and industrial waste water in a acid, a bromine acetic acid, dichloroacetic acid, trichloroacetic acid, monochloroacetic a bromine, a bromine dichloroacetic acid, dibromo acetic acid, chlorodifluoromethane bromoacetate and three co-determination bromoacetate nine haloacetic acid compounds. When the sample volume is 40ml, the detection limit of this standard 2��g/L, detection limit of 8��g/L.

HJ 758-2015: Water quality. Determination of haloacetic acids. Gas chromatography

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Water quality.Determination of haloacetic acids.Gas chromatography National Environmental Protection Standard of the People's Republic Determination of water-based halogenated acetic acid compounds Gas chromatography Published on.2015-10-22 2015-12-01 Implementation Release Ministry i directory Preface II 1 Scope..1 2 Normative references..1 3 method principle..1 4 Interference and elimination.1 5 Reagents and materials.1 6 instruments and equipment.2 7 samples. 2 8 Analysis steps..3 9 result calculation and representation..4 10 precision and accuracy..5 11 Quality Assurance and Quality Control 5 12 Waste Treatment..6 13 Notes. 6 Appendix A (informative) method precision and accuracy 7 Appendix B (informative) internal standard and standard of nine haloacetic acid compounds and substitute derivatives on column 2 Chromatogram.9

Foreword

To implement the Environmental Protection Law of the People's Republic of China and the Law of the People's Republic of China on Water Pollution Prevention and Control, to protect the environment, This standard is formulated to ensure human health and to regulate the monitoring methods of halogenated acetic acid compounds in water. This standard specifies the gas phase color of haloacetic acid compounds in surface water, groundwater, domestic sewage and industrial wastewater. Spectral method. This standard is the first release. Appendix A and B of this standard are informative annexes. This standard was formulated by the Science and Technology Standards Department of the Ministry of Environmental Protection. This standard is mainly drafted by. Qingdao Environmental Monitoring Center Station, Qingdao Technological University. This standard is verified by the Agricultural Products Supervision and Inspection Center of the Ministry of Agriculture (Qingdao) and the National Urban Water Supply and Water Quality Monitoring Network. Station, Zibo Environmental Monitoring Station, Weifang Environmental Monitoring Center Station, Zibo Anrui Water Quality Testing Center, Qingdao Economic Technology Development zone water supply and drainage monitoring station. This standard was approved by the Ministry of Environmental Protection on October 22,.2015. This standard has been implemented since December 1,.2015. This standard is explained by the Ministry of Environmental Protection. 1 Determination of water-halogenated acetic acid compounds - Gas chromatography Warning. The solvents, internal standards, substitutes and standard samples used in the experiments are all toxic and harmful compounds. The system shall be carried out in a fume hood, and protective equipment shall be worn as required to avoid contact with skin and clothing.

1 Scope of application

This standard specifies gas chromatography for the determination of haloacetic acid compounds in water. This standard applies to surface water, groundwater, domestic sewage and industrial wastewater, monochloroacetic acid, monobromoacetic acid, dichloroacetic acid, Nine halogenated groups of trichloroacetic acid, monobromo-chloroacetic acid, monobromodichloroacetic acid, dibromoacetic acid, monochlorodibromoacetic acid and tribromoacetic acid Determination of acetic acid compounds. When the sample volume is 40 ml, the detection limit of this method is 2 μg/L, and the lower limit of determination is 8 μg/L.

2 Normative references

The contents of this standard refer to the following documents or their terms. For undated references, the valid version is appropriate. Used in this standard. HJ/T 91 Surface Water and Wastewater Monitoring Technical Specifications HJ/T 164 Technical Specifications for Groundwater Environmental Monitoring

3 Principle of the method

Under acidic conditions (pH < 0.5), the water sample was extracted with methyl tert-butyl ether, and the extract was derivatized with a solution of sulfuric acid in methanol. The haloacetic acid compound is formed into methyl haloacetate, separated by gas chromatography, and determined by an electron capture detector (ECD). Take The retention time is qualitative, and the working curve is quantified by the internal standard method.

4 interference and elimination

When there are interfering substances in the sample, you can adjust the pH of the water sample to >12, extract once with 20 ml of n-hexane, and discard the organic The phase is determined by the preparation and analysis steps of the sample.

5 reagents and materials

Unless otherwise stated, analytical analytical reagents in accordance with national standards were used for the analysis, and experimental water was used for the fresh preparation. Sub-water or distilled water. 5.1 ammonium chloride (NH4Cl). 5.2 Sodium chloride (NaCl). excellent grade pure. Bake in a muffle furnace at 450 °C for 2~3 h before use. 5.3 sodium bicarbonate (NaHCO3). 5.4 Ammonium chloride solution. ρ(NH4Cl) = 10 mg/ml. Weigh 1.0 g of ammonium chloride (5.1) and add to 100 ml of water. 5.5 Sodium chloride solution. ρ (NaCl) = 250 g/L. Weigh 25 g of sodium chloride (5.2) and add to 100 ml of water. 5.6 Saturated sodium bicarbonate (NaHCO3) solution. Weigh more than 10 g of sodium bicarbonate (5.3) and dissolve it in a 100 ml reagent bottle with water, keeping the bottom of the bottle with sodium bicarbonate crystals. 25.7 Sulfuric acid. ρ(H2SO4) = 1.84 g/ml. 5.8 Methyl tert-butyl ether (CH3OC(CH3)3, abbreviated MTBE). pesticide residue grade. 5.9 Methanol (CH3OH). pesticide residue grade. 5.10 Sulfuric acid-methanol solution. 19. Pipette 10 ml of sulfuric acid (5.7) and slowly drip into a 150 ml beaker pre-filled with 90 ml of methanol (5.9) until the temperature is cold. It is used after room temperature. Available now. 5.11 Internal standard solution. 1,2,3-trichloropropane solution, ρ=1.0 mg/ml. Purchase a commercially available certified standard solution. 5.12 Substitute criteria. 2-bromobutyric acid, liquid, purity >97%. 5.13 Alternative stock solution. ρ = 10.0 mg/ml. Weigh the substitute standard (5.12) 0.100 g (accurate to 0.1 mg) and add 10 ml containing the appropriate amount of MTBE (5.8) In the volumetric flask, use MTBE (5.8) to bring up to the mark. Store at 4 °C in the dark and protected from light. 5.14 Alternative use solution. ρ = 40.0 mg/L. Take.200 μl of the alternative stock solution (5.13) and add it to a 50 ml volumetric flask containing the appropriate amount of MTBE (5.8). Then use MTBE (5.8) to bring up to the mark. 5.15 Halogenated acetic acid mixed standard solution. ρ = 2.00 mg/ml. A commercially available certified standard solution containing nine haloacetic acids was purchased. Store at 4 °C in the dark and protected from light. 5.16 Halogenated acetic acid mixed standard use solution. ρ = 40.0 mg/L. Take 20 μl of the haloacetic acid mixed standard solution (5.15) and dilute to 1.0 ml with MTBE (5.8). Available now. 5.17 carrier gas. high purity nitrogen, purity ≥ 99.999%.

6 Instruments and equipment

6.1 Sampling bottle. 100 ml brown glass bottle. 6.2 Gas Chromatograph. with split/splitless inlet with electronic capture detector. 6.3 Column 1. Quartz capillary column, length 30 m, inner diameter 0.32 mm, film thickness 0.25 μm, stationary phase 14% cyanopropyl Phenyl (of which 7% cyanopropyl 7% phenyl)/86% dimethylpolysiloxane. Column 2. quartz capillary column, 30 m long, 0.32 mm internal diameter, 0.25 μm film thickness, 5% phenyl/95% stationary phase Dimethylpolysiloxane. 6.4 Electric constant temperature water bath. Temperature accuracy ± 2 °C. 6.5 separatory funnel. 125 ml with a Teflon piston. 6.6 10 ml with a colorimetric tube. 6.7 Common instruments and equipment used in general laboratories.

7 samples

7.1 Acquisition and preservation Sample collection was performed in accordance with the requirements of HJ/T 91 and HJ/T 164. According to the ratio of 1.0 ml ammonium chloride solution (5.4) per 100 ml water sample, the ammonium chloride content in the water sample is about 100 mg/L. 3 After adding the water sample, cover the stopper and mix by shaking. At least one full program blank should be collected for each batch of samples. The sample should be extracted and analyzed as soon as possible. If it cannot be analyzed in time, it should be stored in a refrigerator at 4 °C, protected from light, and extracted within 14 days. The product extraction derivative should not be stored in the refrigerator at 4 ° C for more than 7 days. 7.2 Preparation of samples Add 40.0 ml of water sample to the separatory funnel (6.5), add 50.0 μl of the alternative solution (5.14), and add 2 ml. Sulfuric acid (5.7), shake well and quickly add 8 g of sodium chloride (5.2) to dissolve and dissolve. Add 4 ml of MTBE (5.8) and extract for 5 min. Allow to stand for 5 min. The lower aqueous phase was collected and extracted once with 4 ml of MTBE (5.8). Combine the extracts twice. Accurate shift Take 3.0 ml of the extract into a 10 ml colorimetric tube (6.6), add 6.0 μl of the internal standard solution (5.11), and add 3 ml of new preparation. Sulfuric acid-methanol solution (5.10), mix, derivatize in a 50 (±2) °C hot water bath for 120 (±10) min, remove the colorimetric tube and cool But at room temperature, add 7 ml of sodium chloride solution (5.5), tighten the cap and shake well, then remove the lower layer with a 10 ml graduated pipette. Aqueous phase (residual aqueous phase < 0.3 ml). Slowly add 1 ml of saturated sodium bicarbonate solution (5.6), tighten the cap and vent the gas intermittently. Pipette 1.0 ml of the upper extract into a 2 ml brown injection vial for analysis. 7.3 Preparation of blank samples The sample was replaced with experimental water, and a blank sample was prepared according to the preparation method (7.2) of the sample.

8 Analysis steps

8.1 Gas Chromatography Reference Conditions Inlet temperature. 210 ° C; temperature program. initial temperature 40 ° C for 5 min, 2.5 ° C/min rose to 65 ° C, Then increase to 85 ° C at 10 ° C/min, then rise to 205 ° C at 20 ° C/min for 5 min; detector temperature. 300 ° C; Gas. nitrogen (5.17); carrier gas flow rate. 2.0 ml/min, tail gas flow rate. 60 ml/min; injection method. splitless injection; Injection volume. 1.0 μl. 8.2 Establishment of the working curve Add 40.0 ml of experimental water to 5 separatory funnels (6.5), respectively, and mix the haloacetic acid with a micro-syringe. Standard use solution (5.16) and alternative use solution (5.14) 10 μl, 20 μl, 50 μl, 100 μl,.200 μl, in turn Into 5 separatory funnels (6.5), according to the same procedure as sample preparation (7.2), extract, add internal standard, derivatization, Standards to target compounds and surrogate concentrations of 10.0 μg/L, 20.0 μg/L, 50.0 μg/L, 100 μg/L,.200 μg/L Column. The measurement was then carried out in accordance with the gas chromatographic reference conditions (8.1). Taking the concentration of the target (ρx) as the abscissa, the product of the ratio of the peak area of the target to the internal standard and the concentration of the internal standard (Axρis/ Ais) establishes a working curve for the ordinate. 8.3 Standard Reference Chromatogram Under the chromatographic conditions (8.1) given in this standard, the internal standard and nine haloacetic acid compounds and substitute derivatives are colored. Standard chromatogram in column 1. Methyl 41-monochloroacetate, methyl 2-bromoacetate, methyl 3-chloroacetate, methyl 4-trichloroacetate, 5-1,2,3-trichloropropane (internal standard), 6-Methyl monobromochloroacetate, methyl 7-2-bromobutyrate (alternative), methyl 8-bromodichloroacetate, methyl 9-dibromoacetate, 10-chlorodichloride Methyl bromoacetate, methyl 11-tribromoacetate Figure 1 Standard chromatogram of the internal standard and nine haloacetic acid compounds and substitute derivatives in column 1. 8.4 Sample determination After the sample was treated according to the preparation method of the sample (7.2), it was measured according to the gas chromatography reference condition (8.1). 8.5 Blank test The blank sample (7.3) was measured in accordance with the gas chromatographic reference conditions (8.1).

9 Calculation and representation of results

9.1 Target compound characterization The target compound is characterized according to the retention time of the component. Column 2 can be used as an auxiliary qualitative if necessary. Column 2 See Appendix B for the peak sequence of the target compound. 9.2 Target compound quantification 9.2.1 Calculation of results Calculate the mass concentration of haloacetic acid in the water sample according to formula (1). aAA isis   x (1) Where. ρx-haloacetic acid concentration, μg/L; Peak area of Ax-target compound; Peak area of the Ais-internal standard; Concentration of ρis-internal standard, μg/L; The intercept of the a-work curve, μg/L; The slope of the b-work curve. 9.2.2 Results Representation When the measurement result is less than 100 μg/L, the result is retained to an integer; when the measurement result is greater than or equal to 100 μg/L, the result is Keep three significant digits. 510 precision and accuracy 10.1 Precision Six laboratories with nine haloacetic acid standards for concentrations of 10.0 μg/L, 80.0 μg/L, and 160 μg/L The uniform sample was tested in parallel for 6 times. The relative standard deviations in the laboratory were. 1.3%~15%, 1.2%~8.4%, 0.8%~11%; the relative standard deviations between laboratories are. 10%~16%, 7.2%~15%, 6.6%~14%; reproducibility The limits r are. 2 μg/L ~3 μg/L, 11 μg/L ~15 μg/L, 21 μg/L ~33 μg/L; the reproducibility limit R is. 3 μg/L ~5 μg/L, 20 μg/L ~34 μg/L, 33 μg/L ~70 μg/L. See Appendix A, Table A.1. 10.2 Accuracy 6 laboratories added 30.0 actual samples of surface water, domestic sewage and industrial wastewater to 10.0 μg/L and 80.0 respectively. At μg/L and 160 μg/L, the recoveries of the nine haloacetic acids were in the range of 88.8%~102%, 93.6%~107%, 90.8%~97.6%. The recovery rate of the surrogate in the actual sample ranged from 91.2% to 108%. See appendix A table A.2. 11 Quality Assurance and Quality Control 11.1 Blank test At least one laboratory blank and one full program blank should be made for each batch of samples. The measured value of the target compound in the blank should be low The method detection limit. 11.2 parallel sample At least 10% of parallel samples should be determined for each batch of samples. When the number of samples is less than 10, at least one parallel sample should be measured. The relative deviation of the results of the sample measurement should be ≤ 30%. 11.3 Calibration The correlation coefficient of the curve should be ≥0.995 for the initial calibration, otherwise the calibration curve should be redrawn. 11.4 Continuous calibration For each 20 samples measured, a calibration curve intermediate concentration standard solution should be determined, and the relative error between the measurement result and the initial calibration. The difference should be within ±30%. Otherwise, the calibration curve needs to be redrawn. 11.5 internal standard If the calibration curve is not the first calibration, the internal standard peak area should be within ±50% of the internal standard peak area at the initial calibration, otherwise Should be recalibrated. 11.6 Alternative recovery rate Substitutes should be added to all samples and blanks. The same procedure as the sample should be used to analyze the spiked recovery of the surrogate. Within 70.0%~130%. 11.7 matrix addition and recycling Each batch of samples should be subjected to at least one matrix spike analysis. The recoveries of the nine haloacetic acids in the sample should be 70.0%~ Within 130%. 612 Waste Treatment The organic waste liquid generated in the experiment shall be collected, stored in a centralized manner, and entrusted to a qualified unit for processing. 13 Precautions 13.1 The interference of this method mainly comes from the long-term exposure of the glass instruments and reagents used in the operation to the air. In order to eliminate this interference, the glass instrument should be cleaned before use, and the chemical reagent should use the newly opened reagent. 13.2 Derivative time and derivatization temperature should be strictly controlled in the preparation method of sample (7.2). 13.3 If the sample concentration exceeds the curve range, an appropriate amount of sample can be prepared and measured after dilution with experimental water to 40.0 ml.

7 Appendix A

(informative appendix) Method precision and accuracy Tables A.1 and A.2 give the precision and accuracy of the method, respectively. Table A.1 Precision of the method Serial number compound average value (μg/L) Relative standard in the experimental room Quasi-bias (%) Relative standard between laboratories Quasi-bias (%) Repeatability limit r (μg/L) Reproducibility limit R (μg/L) Monochloroacetic acid (MCAA) 10 4.8~13 14 2 4 81 1.4~7.7 12 11 29 156 2.1~10 9.8 26 49 Monobromoacetic acid (MBAA) 10 2.4~12 10 2 4 84 2.2~6.5 7.2 12 20 156 1.9~87 11 27 54 Dichloroacetic acid (DCAA) 10 2.7~12 10 2 4 85 1.4~8.4 8.8 12 24 165 3.5~10 14 30 70 Trichloroacetic acid (TCAA) 10 2.4~15 12 2 4 89 1.2~7.0 8.7 13 25 154 3.1~11 12 27 58 Monobromo-chloroacetic acid (BCAA) 10 1.7~12 12 2 4 84 1.0~7.0 9.4 12 25 155 1.1~10 11 26 52 Monobromodichloroacetic acid (BDCAA) 9 1.3~13 10 2 3 82 1.8~7.5 13 13 32 150 1.3~15 7.2 33 42 Dibromoacetic acid (DBAA) 10 1.3~13 16 2 5 84 2.8~7.2 8.4 12 23 155 0.8~11 11 31 55 Monochlorodibromoacetic acid (CDBAA) 9 1.7~11 12 2 3 80 2.1~8.2 12 14 29 152 1.2~10 6.7 28 38 Tribromoacetic acid (TBAA) 9 5.6~15 12 3 4 75 1.9~7.7 15 13 34 145 3.6~6.3 6.6 21 33 8 Table A.2 Method accuracy Serial number compound sample Types of Standard concentration (μg/L) Spike recovery range (%) Addition to recover the final value 2P PS (%) Monochloroacetic acid (MCAA) Surface water 10.0 76.0~108 94.726.2 Domestic sewage 80.0 78.6~114 10124.6 Industrial wastewater 160 82.5~109 97.519.0 Monobromoacetic acid (MBAA) Surface water 10.0 84.0~111 10120.6 Domestic sewage 80.0 91.4~112 10415.2 Industrial wastewater 160 78.1~106 97.221.6 Dichloroacetic acid (DCAA) Surface water 10.0 84.0~118 10121.2 Domestic sewage 80.0 87.8~113 10618.6 Industrial wastewater 160 75.2~119 97.630.6 Trichloroacetic acid (TCAA) Surface water 10.0 83.0~111 97.822.8 Domestic sewage 80.0 87.8~115 10720.0 Industrial wastewater 160 77.5~109 96.123.4 Monobromo-chloroacetic acid (BCAA) Surface water 10.0 83.0~118 10225.2 Domestic sewage 80.0 85.6~112 10519.8 Industrial wastewater 160 79.4~109 96.620.6 Monobromodichloroacetic acid (BDCAA) Surface water 10.0 83.0~106 93.519.6 Domestic sewage 80.0 76.8~115 10226.2 Industrial wastewater 160 85.6~103 93.913.4 Dibromoacetic acid (DBAA) Surface water 10.0 74.0~114 97.731.8 Domestic sewage 80.0 89.0~113 10517.8 Industrial wastewater 160 80.4~109 96.921.0 Monochlorodibromoacetic acid (CDBAA) Surface water 10.0 82.0~111 90.821.2 Domestic sewage 80.0 78.8~114 99.523.0 Industrial wastewater 160 88.8~103 95.212.6 Tribromoacetic acid (TCAA) Surface water 10.0 82.0~107 88.820.6 Domestic sewage 80.0 75.9~115 93.628.4 Industrial wastewater 160 83.8~99.4 90.812.0 substitution (SUR) 2-bromobutyric acid Surface water 50.0 91.6~108 97.011.6 Domestic sewage 91.2~97.0 94.45.2 Industrial wastewater 91.6~96.2 94.03.4

9 Appendix B

(informative appendix) Standard chromatogram of internal standard and nine halogenated acetic acid compounds and substitute derivatives on column 2 Methyl 1-chloroacetate, methyl 2-bromoacetate, methyl 3-chloroacetate, methyl 4-trichloroacetate, methyl 5-bromochloroacetate, 6-1, 2, 3- Trichloropropane (internal standard), methyl 7-2-bromobutyrate (alternative), methyl 8-dibromoacetate, methyl 9-monobromodichloroacetate, 10-chlorodibromoethane Methyl ester, methyl 11-tribromoacetate Figure B.1 Standard chromatogram of the internal standard and nine halogenated acetic acid compounds and substitute derivatives in column 2.

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