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HJ 788-2016 English PDF

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HJ 788-2016: Water quality. Determination of Acetonitriie. Purge and Trap/Gas chromatography
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Basic data

Standard ID HJ 788-2016 (HJ788-2016)
Description (Translated English) Water quality. Determination of Acetonitriie. Purge and Trap/Gas chromatography
Sector / Industry Environmental Protection Industry Standard
Classification of Chinese Standard Z16
Word Count Estimation 10,122
Date of Issue 2016-03-29
Date of Implementation 2016-05-01
Quoted Standard HJ/T 91; HJ/T 164
Regulation (derived from) Ministry of Environmental Protection Announcement No
Issuing agency(ies) Ministry of Ecology and Environment

HJ 788-2016: Water quality. Determination of Acetonitriie. Purge and Trap/Gas chromatography

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Water quality.Determination of Acetonitriie.Purge and Trap/Gas chromatography National Environmental Protection Standard of the People 's Republic of China Determination of water quality of acetonitrile Purge trapping/gas chromatography Water quality-Determination of Acetonitrile-Purge And Trap/Gas chromatography 2016-03-29 released 2016-05-01 implementation release Ministry of Environmental Protection Directory Preface .ii

1 Scope of application

2 normative reference documents

3 Principle of the method

Interference and elimination 5 reagents and materials 1 6 instruments and equipment 2 7 Sample 2

8 Analysis steps

The results are calculated and expressed 10 precision and accuracy Quality assurance and quality control 12 Waste treatment 13 Precautions Appendix A (informative) method of precision and accuracy 7

Foreword

In order to implement the Environmental Protection Law of the People's Republic of China and the Law of the People's Republic of China on the Prevention and Control of Water Pollution, Protection of human health, regulate the determination of acetonitrile in water, the development of this standard. This standard specifies the purge and trapping/gas chromatography for the determination of acetonitrile in water. This standard is the first release. Appendix A to this standard is an informative appendix. This standard is organized by the Ministry of Environmental Protection Science and Technology Standards Division. The main drafting unit of this standard. Dalian Environmental Monitoring Center. The standard verification unit. Liaoning Province Environmental Monitoring Experimental Center, Shenyang City Environmental Monitoring Center Station, Jinzhou City Environmental Monitoring Central station, Tianjin Environmental Monitoring Center, Jiangsu Province Environmental Monitoring Center and Suzhou Environmental Monitoring Center Station. The environmental protection department of this standard approved on March 29,.2016. This standard has been implemented since May 1,.2016. This standard is explained by the Ministry of Environmental Protection. Water quality - Determination of acetonitrile - Purge and trap/gas chromatography Warning. The acetonitrile used in the experiment is harmful to human health. The standard solution preparation process should be carried out in the fume hood. Should be required to wear protective equipment, to avoid contact with skin and clothing.

1 Scope of application

This standard specifies the purge and trapping/gas chromatography for the determination of acetonitrile in water. This standard is applicable to the determination of acetonitrile in surface water, groundwater, industrial waste water and domestic sewage. When the hydrogen flame ionization detector was used, the detection limit of acetonitrile was 0.1 mg/L when the sample volume was 5.0 ml. Limited to 0.4 mg/L. When the nitrogen and phosphorus detectors were used, the detection limit of acetonitrile was 0.009 mg/L when the sampling volume was 5.0 ml The limit was 0.036 mg/L.

2 normative reference documents

The contents of this standard refer to the following documents or their terms. Those who do not specify the date of the reference file, the effective version of the appropriate For this standard. Technical specification for surface water and wastewater monitoring Technical specification for groundwater environmental monitoring

3 Principle of the method

The acetonitrile in the sample was purged with high purity nitrogen and adsorbed into the trap. The trap was heated and blown back with high purity nitrogen. The thermally desorbed acetonitrile is separated by gas chromatography and is detected by a hydrogen flame ionization detector or a nitrogen and phosphorus detector. To keep Qualitative and external standard method.

4 interference and elimination

Determination of acetonitrile in water by this method, dichloroethylene, methyl chloride, dichloroethane, dichloropropane, dichloropropene, tris Vinyl chloride, trichloropropane, trichloroethane, trichloromethane, tetrachlorethylene, tetrachloroethane, dibromoethane, bromochloromethane, bis Methyl bromide, monochloromethane, monochloromethane, monochloromethane, monochloromethane, monochloromethane, monochloroethane, monochloroethane, monochloromethane, Dibromochloropropane, dichlorodifluoromethane, trichlorofluoromethane, acetone, butanone, hexanone, carbon disulfide, monomethyl iodide, benzene, Toluene, chlorobenzene, bromobenzene, ethylbenzene, xylene, styrene, cumene, n-propylbenzene, dichlorobenzene, trichlorobenzene, chlorotoluene, Trimethylbenzene, butylbenzene, isopropyltoluene, hexachlorobutadiene, naphthalene, vinyl acetate, chloroethyl vinyl ether, methyl pentanone, Methanol, ethanol, acrylonitrile, acrolein, formaldehyde, acetaldehyde and other organic matter on the determination will not interfere. If there are other substances dry Interference, can be used with different polarity of the auxiliary column qualitative.

5 reagents and materials

5.1 Experimental water. secondary distilled water or water prepared by pure water equipment. Before use, subject to a blank test to confirm that there is no interference to the target compound in the retention time interval or target combination The detection concentration is lower than the method detection limit. 5.2 Acetonitrile (CH3CN). Chromatographic pure. 5.3 acetonitrile standard stock solution. ρ (CH3CN) ≈ 1 × 104 mg/L. Prepared with acetonitrile (5.2) at room temperature at 20 ° C. Remove the appropriate amount of test water (5.1) in a 10 ml volumetric flask, placed on a balance (5.2) to about 100 mg (accuracy to 0.1 mg), and weigh again; according to two The difference between the weight and the weight is determined by the exact quality of acetonitrile. With the experimental water (5.1) constant volume to the mark, shake, calculate the standard The exact concentration of the stock solution (accurate to 10 mg/L). Transfer to a brown reagent bottle with a Teflon screw cap at 4 ° C Under the cold storage, dark and sealed can be kept for 3 months. You can also purchase commercially available certified materials (in water as solvent). 5.4 acetonitrile standard use liquid I. ρ (CH3CN) = 100 mg/L. Remove the appropriate amount of test water (5.1) and a volume of acetonitrile standard stock solution (5.3) in 100 ml volumetric flask, Experimental water (5.1) constant volume to the marking, shake. Pro is now available. 5.5 acetonitrile standard use liquid Ⅱ. ρ (CH3CN) = 1.0 mg/L. Remove the appropriate amount of water (5.1) and 1.0 ml of acetonitrile in the order of liquid I (5.4) in 100 ml volumetric flask, Test water (5.1) constant volume to the mark, shake. Pro is now available. 5.6 high purity nitrogen. purity ≥ 99.999%. 5.7 Hydrogen. purity ≥99.95%. 5.8 Air. Dehumidified silica gel dehumidification and dehydrocarbon removal of hydrocarbons, or oil-free compressed air purified by 5 Å molecular sieve.

6 instruments and equipment

Unless otherwise stated, the use of the national standard A-class glass gauge is used for the analysis. 6.1 Gas Chromatograph. with capillary column shunt/splitless inlet, equipped with hydrogen flame ionization detector (FID) or nitrogen and phosphorus detection (NPD). 6.2 Purge and trap device. with 5 ml purge tube, the capture tube generally use 1/3Tenax, 1/3 silicone, 1/3 activated carbon mixed Adsorbents or other equivalent adsorbents. 6.3 Column. quartz capillary column, 30 m x 0.32 mm, film thickness 1.0 μm (polyethylene glycol -20 M fixative), or Other equivalent columns. 6.4 Air tightness syringe. 5 ml. 6.5 Reagent Bottle. 10 ml brown reagent bottle with polytetrafluoroethylene screw cap. 6.6 Sampling vials. 40 ml brown wide mouth sampling vial with PTFE cap screw cap. 6.7 balance. one thousandth of a balance. 6.8 Volumetric flask. Class A, 10 ml and 100 ml. 6.9 General laboratory equipment and equipment commonly used.

7 samples

7.1 Collection of samples Refer to the relevant provisions of HJ/T 91 and HJ/T 164. Use a 40 ml brown wide mouth with a Teflon screw cap Sampling bottle (6.6) Collect the sample and collect the sample should be filled with the sample bottle and stamped. Each batch of samples should be at least one full The procedure is blank (with the same batch of experimental water instead of the sample). 7.2 Transport and storage of samples After the collection of samples should be refrigerated below 4 ℃, dark, sealed and transported. If not timely analysis, should be below 4 ℃ Refrigerated, dark and sealed, the shelf life of not more than 6 d. There should be no organic interference in the sample storage area.

8 Analysis steps

8.1 Instrument reference conditions 8.1.1 Purge and trap Purge temperature of 35 ℃; purge time of 11 min; desorption temperature of 190 ℃; desorption time of 2 min; baking temperature The temperature is 220 ℃, the baking time is 7 min, the purge gas is high purity nitrogen and the purge flow rate is 40 ml/min. 8.1.2 Hydrogen Flame Ionization Detector Gas Chromatography The inlet temperature is.200 ℃, the split ratio is 7. 1, the oven temperature is 60 ℃, the column flow rate is 2.0 Ml/min; detector temperature of 230 ℃, hydrogen flow rate of 40 ml/min, air flow of 400 ml/min. 8.1.3 Nitrogen and Phosphorus Detector Gas Chromatography The inlet temperature is.200 ℃, the split ratio is 7. 1, the oven temperature is 100 ℃, the column flow rate is 2.0 Ml/min; detector temperature of 330 ℃, hydrogen flow rate of 3.5 ml/min, air flow rate of 60 ml/min. 8.2 Drawing of working curves 8.2.5 Hydrogen Flame Ionization Detector Remove the appropriate amount of water (5.1) in 5 100 ml brown volumetric flask, respectively, accurately add 0.5 ml, 1.0 ml, 2.0 ml, 3.0 ml, 5.0 ml acetonitrile standard liquid I (5.4), with the experimental water volume to the mark, shake. Formulated into acetonitrile quality concentrated Respectively, the standard series of 0.5 mg/L, 1.0 mg/L, 2.0 mg/L, 3.0 mg/L, 5.0 mg/L, respectively. From low to high concentrations Transfer the 5.00 ml standard series to the purge tube in turn, according to the instrument reference conditions (8.1). To the standard series of concentrations (Mg/L) as the abscissa, with the corresponding peak area (or peak height) as the vertical axis, the establishment of working curve. 8.2.2 Nitrogen and Phosphorus Detector Remove the appropriate amount of water (5.1) in 5 100 ml brown volumetric flask, respectively, accurately add 2.5 ml, 5.0 ml, 10.0 Ml, 20.0 ml, 50.0 ml acetonitrile standard liquid Ⅱ (5.5), with the experimental water volume to the mark, shake. Formulated into acetonitrile The concentration of 0.025 mg/L, 0.050 mg/L, 0.100 mg/L, 0.200 mg/L and 0.500 mg/L, respectively. From a low concentration to a high concentration, remove the 5.00 ml standard series from the purge tube in turn according to the instrument reference conditions (8.1). The concentration of the standard series (mg/L) as the abscissa, with the corresponding peak area (or peak height) as the vertical axis, Make a curve. 8.3 Standard reference chromatogram Under the instrument reference conditions (8.1) given in this standard, the acetonitrile standard gas chromatograms are shown in Figures 1 and 2. Figure 1 acetonitrile standard chromatogram (hydrogen flame ionization detector) Figure 2 acetonitrile standard chromatogram (nitrogen and phosphorus detector) 8.4 Determination of samples Remove the sample collected by 5.00 ml and follow the same instrument reference conditions (8.1) and (8.2) as the drawing work curve. To be measured. 8.5 blank test According to the same instrument reference conditions (8.1) and step (8.2), the corresponding volume of experimental water (5.1) for blank test.

9 Results calculation and representation

Qualitative analysis of acetonitrile The target is qualitatively based on the retention time of the target in the sample and the target in the standard series. Before the sample analysis, Create retention time window t ± 3s. T for the initial calibration, the concentration level of acetonitrile retention time average; s for the initial calibration of the Standard deviation of acetonitrile retention time at the concentration level. When the sample is analyzed, the target should peak within the retention time window. 9.2 Quantitative analysis of acetonitrile 9.2.1 Result calculation The concentration of acetonitrile is 1ρ from the working curve and the concentration of acetonitrile in the water sample is calculated according to the formula (1) F × = 1ρρ (1) Where. ρ - the mass concentration of acetonitrile in the sample, mg/L; 1ρ - the acetonitrile concentration obtained from the working curve, mg/L; F - sample dilution factor. 9.2.2 result representation Using hydrogen flame ionization detector, when the determination of less than 10 mg/L, the retention of a decimal point; when the determination of the results When you are greater than or equal to 10 mg/L, keep three significant digits. Using nitrogen and phosphorus detector, when the determination is less than 1 mg/L, the retention of three decimal places; when the determination is greater than or equal to 1 mg/L, retain three valid digits. 10 precision and accuracy Refer to Appendix A for precision and accuracy data. 11 quality assurance and quality control 11.1 calibration Each batch should be drawn with a working curve, the correlation coefficient should be ≥ 0.995. Otherwise you should find the reason to redraw the work curve. Every 20 samples or per batch (less than 20 samples) should be measured for a working curve intermediate concentration point standard solution The relative error between the result and the working curve should be ≤ ± 15%. Otherwise, the work curve must be redrawn. 11.2 blank test Every 20 samples or per batch (less than 20 samples) should analyze at least one lab blank and one full program blank. The determination of acetonitrile in the blank should be lower than the method detection limit. 11.3 spiked samples Every 20 samples or each batch (less than 20 samples) should be analyzed at least one blank plus standard and one sample plus standard, The recoveries should be in the range of 85% to 115%. 11.4 parallel samples Every 10 samples or each batch (less than 10 samples) should be analyzed for at least one parallel sample, parallel to the sample The deviation should be ≤ 15%. 12 Waste treatment The acetonitrile waste generated in the experiment should be collected and kept collectively and commissioned by qualified units for processing. 13 Precautions 13.1 When measuring acetonitrile in water, nitrogen and phosphorus detectors are preferred. 13.2 Glassware containing trace amounts of chromium will affect the determination of chromium and acetonitrile. Should use chrome-free sampling and Analytical containers. 13.3 to avoid nitrogen and phosphorus detector bead deliquescence, should be a week to run a run, so that nitrogen and phosphorus detector temperature. 13.4 If the baseline is unstable or there are other disturbances, the aging column needs to be heated.

Appendix A

(Informative) Method of precision and accuracy Table A.1 and Table A.2 show the precision and accuracy of the method, respectively. Table A.1 The precision of the method Analytical method Number of sample measurements Total mean (Mg/L) Laboratory relative standard deviation(%) Inter-laboratory relative standard deviation(%) Repetitive limit r (Mg/L) Reproducibility R (Mg/L) 6 0.5 2.3 to 5.7 1.7 0.1 0.1 6 2.4 1.8 ~ 4.9 1.9 0.3 0.3 blank plus standard 6 4.5 2.5 to 3.8 1.2 0.4 0.4 6 0.5 4.2 ~ 5.5 7.8 0.1 0.1 Surface water Plus standard 6 2.5 2.2 ~ 3.9 3.4 0.2 0.3 6 0.7 ~ 0.9 4.6 ~ 7.3 /// 6 1.7 ~ 2.2 3.1 ~ 6.7 /// FID Purge and trap method Waste water 6 3.6 ~ 4.7 2.9 ~ 4.2 /// 6 0.025 5.8 ~ 8.1 2.3 0.005 0.005 6 0.244 3.9 ~ 5.7 1.5 0.034 0.032 blank plus standard 6 0.445 2.4 ~ 3.9 2.2 0.039 0.044 6 0.025 3.6 ~ 7.4 5.0 0.004 0.005 Surface water Plus standard 6 0.247 3.0 ~ 5.0 4.2 0.027 0.038 6 0.017 ~ 0.021 7.8 ~ 13 /// 6 0.094 ~ 0.182 5.5 ~ 11 /// NPD Purge and trap method Waste water 6 0.415 ~ 0.440 2.5 ~ 5.7 /// Table A.2 The accuracy of the method Analytical method Number of sample measurements Plus scalar (Mg/L) Spiked recovery rate (%) (%) (%) ± 2 (%) 6 0.5 97.0 to 101 99.7 1.7 99.7 ± 3.4 6 2.5 94.0 to 99.2 97.5 1.8 97.5 ± 3.6 Blank spikes 6 4.5 99.6 to 103 101 1.2 101 ± 2.4 6 0.5 91.4 ~ 101 98.9 7.7 98.9 ± 15.4 Surface water 6 2.5 96.0 to 104 99.5 3.3 99.5 ± 6.6 6 1.5 94.1 to 105 97.9 4.1 97.9 ± 8.2 6 2.0 96.5 to 108 102 4.5 102 ± 9.0 FID Purge and trap method Waste water 6 4.5 96.0 to 102 99.8 2.1 99.8 ± 4.2 6 0.025 97.2 to 103 100 2.3 100 ± 4.6 6 0.250 95.2 ~ 99.6 97.7 1.4 97.7 ± 2.8 blank plus standard 6 0.450 97.3 ~ 103 98.8 2.1 98.8 ± 4.2 6 0.025 91.6 ~ 105 98.5 4.9 98.5 ± 9.8 Surface water 6 0.250 95.2 to 106 98.9 4.1 98.9 ± 8.2 6 0.025 92.8 ~ 109 100 6.5 100 ± 13.0 6 0.150 94.7 to 108 104 4.8 104 ± 9.6 NPD Purge and trap method Waste water 6 0.450 96.2 to 103 100 3.1 100 ± 6.2

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