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HJ 895-2017 English PDF

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HJ 895-2017: Water quality. Determination of methanol and acetone. Headspace gas chromatography
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Standard ID	Contents [version]	USD	STEP2	[PDF] delivered in	Standard Title (Description)	Status	PDF
HJ 895-2017	English	279	Add to Cart	3 days [Need to translate]	Water quality. Determination of methanol and acetone. Headspace gas chromatography	Valid	HJ 895-2017

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Basic data

Standard ID	HJ 895-2017 (HJ895-2017)
Description (Translated English)	Water quality. Determination of methanol and acetone. Headspace gas chromatography
Sector / Industry	Environmental Protection Industry Standard
Classification of Chinese Standard	Z16
Classification of International Standard	13.060
Word Count Estimation	12,151
Date of Issue	2017-12-21
Date of Implementation	2018-02-01
Quoted Standard	GB 17378.3; HJ/T 91; HJ/T 164
Regulation (derived from)	Ministry of Environmental Protection Announcement 2017 No. 77
Issuing agency(ies)	Ministry of Ecology and Environment
Summary	This standard specifies headspace/gas chromatography for the determination of methanol and acetone in water. This standard is applicable to the determination of methanol and acetone in surface water, groundwater, industrial wastewater, domestic sewage and seawater. When the sampling volume is 10 ml, the method detection limit of methanol is 0.2 mg/L, the lower limit of determination is 0.8 mg/L; the detection limit of acetone is 0.02 mg/L, and the lower limit of determination is 0.08 mg/L.

HJ 895-2017: Water quality. Determination of methanol and acetone. Headspace gas chromatography

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(Water quality - Determination of methanol and acetone - Headspace/gas chromatography) People's Republic of China national environmental protection standards Water quality - Determination of methanol and acetone Headspace/gas chromatography Water quality-Determination of methanol and acetone -Headspace gas chromatography 2017-12-21 Published 2018-02-01 implementation Ministry of Environmental Protection released i directory Foreword ..ii 1 scope of application .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 sample 2 8 Analysis steps .3 9 results calculated and said .4 10 precision and accuracy 11 Quality Assurance and Quality Control 6 12 Waste treatment .7 Appendix A (informative) method of precision and accuracy 8

Foreword

In order to implement the "Law of the People's Republic of China on Environmental Protection" and the "Law of the People's Republic of China on Prevention and Control of Water Pollution", protect the environment, Protection of human health, standardize the determination of methanol and acetone in water, the development of this standard. This standard specifies the determination of surface water, groundwater, industrial wastewater, domestic sewage and seawater methanol and acetone in the headspace / Gas chromatography. Appendix A of this standard is an informative annex. This standard is released for the first time. This standard by the Environmental Protection Department of Environmental Monitoring Division and Science and Technology Standards Division to develop. This standard was drafted. Jiangsu Provincial Environmental Monitoring Center. This standard verification unit. Taizhou Environmental Monitoring Center Station, Suzhou City Environmental Monitoring Center, Nanjing Environmental Monitoring Center Station, Dalian City Environmental Monitoring Center, Jinan City Environmental Monitoring Center and Shanghai Environmental Monitoring Center. This standard MEP approved on December 21,.2017. This standard since February 1,.2018 implementation. This standard is interpreted by the MEP. Water quality - Determination of methanol and acetone - Headspace/gas chromatography Warning. Chemicals used in the experiment, such as methanol and acetone, are harmful to human health. Solution preparation and sample pretreatment Procedures should be carried out in the fume hood, operation should be required to wear protective gear to avoid contact with the skin and clothing.

1 scope of application

This standard specifies the determination of methanol and acetone in water headspace/gas chromatography. This standard applies to the determination of methanol and acetone in surface water, groundwater, industrial wastewater, domestic sewage and sea water. When the sampling volume is 10 ml, the detection limit of methanol method is 0.2 mg/L, the lower limit of determination is 0.8 mg/L; the acetone The detection limit was 0.02 mg/L and the limit of determination was 0.08 mg/L.

2 Normative references

This standard references the following documents or the terms of them. For undated references, the effective version applies In this standard. GB 17378.3 Marine monitoring code - Part 3. Sample collection, storage and transport HJ/T 91 Technical Specifications for Surface Water and Sewerage Monitoring HJ/T 164 Groundwater Environmental Monitoring Technical Specifications

3 method principle

Under certain temperature conditions, the volatile components in the sample in the headspace bottle volatilize to the liquid space to generate the vapor pressure, After the two phases of the liquid reach the thermodynamic equilibrium, the volatile organic compounds in the gas phase are separated by gas chromatography and detected by hydrogen flame ionization Detector for testing. Chromatographic retention time qualitative, external standard method.

4 Interference and elimination

When using polyethylene glycol stationary phase column separation, when the sample concentration of ethyl acetate is higher than 25 mg/L methanol production Health interference, methyl acetate will interfere with acetone, you can use the stationary phase of 6% cyanopropyl benzene 94% Dimethylsiloxane color Column separation, if necessary, using gas chromatography - mass spectrometry for qualitative confirmation.

5 Reagents and materials

Unless otherwise stated, analytical grade reagents that meet national standards are used. 5.1 Experimental water. Double distilled water or pure water equipment for the preparation of water. The concentration of target compound in experimental water should be below the detection limit of the method, otherwise Should be pre-treatment, can be boiled by heating after 15 min stamped with cooling, or by purging the inert gas to go In addition to experimental water interference with methanol and acetone. 5.2 Hydrochloric acid (HCl). p = 1.19 g/ml. 5.3 hydrochloric acid solution. 1 1. 2 Measure 100 ml of hydrochloric acid (5.2) and add to 100 ml of experimental water (5.1) and mix well. 5.4 Sodium chloride (NaCl). excellent grade pure. Heat at 400 ° C for 2 h to remove any organic matter that may have adsorbed to the surface. After cooling, store in a clean reagent bottle. 5.5 Ascorbic acid (C6H8O6). 5.6 Methanol (CH3OH). pesticide residues. 5.7 acetone (CH3COCH3). pesticide grade. 5.8 Standard solution of methanol and acetone Ⅰ. ρ (CH3OH) ≈3 × 104 mg/L, ρ (CH3COCH3) ≈3 × 103 mg/L. Pipette appropriate amount of experimental water (5.1) in 100 ml volumetric flask, placed on a balance weighing. Carefully dropped a few drops of methanol (5.6) To weight gain of about 3.0 g (accurate to 0.1 mg), re-weighed, calculated according to the difference between the weight of two accurate accession of methanol the amount. Continue carefully dropping a few drops of acetone (5.7) to a weight gain of about 0.3 g (accurate to 0.1 mg), reweigh, according to the last two Calculate the exact mass of acetone added to the difference between the weighings. With experimental water (5.1) set the volume to the mark, shake, calculate a Alcohol and acetone standards using the exact concentration of liquid Ⅰ (accurate to 1 mg/L). Pro use now with. 5.9 Methanol and acetone standard solution Ⅱ. ρ (CH3OH) ≈ 300 mg/L, ρ (CH3COCH3) ≈ 30 mg/L. Accurate Pipette 1.00 ml methanol and acetone standard solution Ⅰ (5.8) in 100 ml volumetric flask, with the experimental water (5.1) Set the volume, shake well. 5.10 Nitrogen. Purity ≥99.999%. 5.11 Hydrogen. Purity ≥99.999%. 5.12 Air. Oil-free compressed air, 5Å molecular sieve purification.

6 instruments and equipment

6.1 Gas Chromatograph. Flame ionization detector (FID) with split/splitless inlet, oven programmed warming. 6.2 Automatic headspace sampler. heating temperature range controlled at room temperature to 250 ℃, temperature control accuracy. ± 1 ℃. 6.3 Column Ⅰ. Quartz capillary column, 30 m (length) × 530 m (ID) × 1.0 m (film thickness), fixed Phase is polyethylene glycol, or other equivalent capillary column. 6.4 Column II. Quartz capillary column, 30 m (length) × 530 m (ID) × 3.0 m (film thickness), fixed Phase 6% Cyanopropyl benzene 94% Dimethylsiloxane, or other equivalent capillary column. 6.5 Analytical Balance. a sense of the amount of 0.0001 g. 6.6 Headspace bottle. 22 ml glass headspace bottle with seal (Teflon/Silicone or Teflon/Butyl rubber Gland) (screw cap or disposable gland) or glass headspace compatible with the automatic headspace sampler (6.2) bottle. 6.7 Microprojectors. 5 μl, 10 μl, 25 μl, 100 μl, 250 μl, 1.0 ml injection needles. 6.8 Sampling bottle. 40 ml brown glass bottle with silicone rubber-teflon-lined screw cap. 6.9 General laboratory commonly used instruments and equipment.

7 samples

7.1 Sample Collection The samples were collected according to HJ/T 91, HJ/T 164 and GB 17378.3. 3 When collecting the sample, do not wash the sample with the sample. The sample should overflow in the sample bottle (6.8) without leaving space Sample should try to avoid or reduce the exposure of the sample in the air. All samples were collected parallel double sample. If the sample contains residual chlorine, Before sampling, 25 mg (accurate to 0.001 g) of ascorbic acid (5.5) should be added to the sampling bottle. If the sample exceeds the residual chlorine content 5 mg/L, the proportion of ascorbic acid should be increased proportionally, and for each additional 5 mg/L of residual chlorine, 25 mg Up to 0.001g) ascorbic acid. At the same time the laboratory water mounted in airtight glass bottles, taken to the sampling site, according to the above steps to collect the entire program blank Samples, each batch of samples should be filled with a full program blank. 7.2 Sample Storage After the sample is taken, immediately add the appropriate amount of hydrochloric acid solution (5.3), so that the sample pH ≤ 2, tighten the stopper, labeling, Immediately placed in the freezer in 4 ℃ below refrigerated transport. Samples shipped back to the laboratory, should be below 4 ℃ refrigeration, dark and Sealed, 14 days to complete the analysis and determination. Sample storage area should be free of volatile organic compounds interference. Note. If the sample was added to the hydrochloric acid solution after the bubble, to be resampled, re-collected samples without hydrochloric acid solution preservation, sample labels Must be marked on the acidification, analysis and determination within 24 h. 7.3 Sample Preparation After returning the sample to room temperature, accurately pipette 10.0 ml of sample into a vial pre-filled with 3.0 g of sodium chloride (5.4) (6.6), immediately stamped seal, shake to be measured. Note. When the actual sample concentration exceeds the working curve range, the sample can be properly reduced and volume to 10.0 ml after the determination. 7.4 blank sample preparation The experimental water (5.1) instead of the sample, according to the sample preparation (7.3) the same procedure to prepare a laboratory blank test kind.

8 Analysis steps

8.1 Instrument reference conditions 8.1.1 Headspace injection reference conditions Heating equilibrium temperature. 80 ℃; Heating balance time. 30 min; Sample needle temperature. 100 ℃; Transmission line temperature. 110 ℃; Injection volume. 1.0 ml. 8.1.2 GC reference analysis conditions Program temperature. the initial column temperature 50 ℃ for 6 min, 5 ℃/min rose to 100 ℃ for 2 min, then 5 ℃ / min to.200 ° C for 5 min; inlet temperature..200 ° C; split ratio 3. 1; carrier gas. nitrogen (5.10), Flow rate. 5.0 ml/min; Detector temperature. 280 ° C; Gas. Hydrogen (5.11), Flow rate 30 ml/min; Gas (5.12), flow rate 300 ml/min. 8.2 The establishment of working curve Take the headspace bottle (6.6) 7, were added 3.0 g sodium chloride (5.4), accurate removal of 10.00 ml of experimental water to each Vial, then add 0 μl, 25 μl, 50 μl, 100 μl standard solution II (5.9) and 5 μl, 10 μl, 15 μl 4 standard solution I (5.8), formulated into a standard series of methanol concentrations were 0 mg/L, 0.75 mg/L, 1.5 mg/L, 3.0 mg/L, 15.0 mg/L, 30.0 mg/L and 45.0 mg/L respectively. The standard series concentrations of acetone were 0 mg/L, 0.075 mg/L, 0.15 mg/L, 0.30 mg/L, 1.50 mg/L, 3.00 mg/L and 4.50 mg/L which are reference concentrations, Gland shake. According to the instrument reference conditions (8.1), from low concentration to high concentration followed by determination. The quality of the target concentration Degree (mg/L) for the abscissa, peak area or peak height for the vertical axis, the establishment of the working curve. 8.3 Sample Determination The sample was measured under the same conditions as in the working curve (8.2). Note. Alternate analysis of high and low concentration samples may cause interference, and a blank sample should be analyzed when analyzing a high concentration sample (7.4) to check for cross-contamination. 8.4 blank experiment The laboratory blank sample (7.4) is determined according to the same procedure as described in sample determination (8.3).

9 results calculated and expressed

9.1 The target compound is qualitative The target compound is characterized according to the retention time of the components. In this standard reference chromatographic conditions, methanol and acetone Standard chromatogram shown in Figure 1. When there is interference peak, column Ⅱ (6.4) can be used as a secondary qualitative column Ⅱ, methanol and The standard chromatogram of acetone is shown in Figure 2. Qualitative results should be confirmed by gas chromatography-mass spectrometry when necessary. Note. methanol tR = 3.4 min, concentration 39.5 mg/L; acetone tR = 2.5 min, concentration 3.94 mg/L Fig.1 Gas chromatogram of methanol and acetone on columnⅠ 5 Note. methanol tR = 1.7 min, the concentration of 39.5mg/L; acetone tR = 2.5 min, the concentration of 3.94 mg/L Figure 2 methanol and acetone in the chromatographic column Ⅱ gas chromatogram 9.2 quantitative results calculation Using external standard method, the concentration of methanol or acetone in the sample (mg/L) is calculated according to formula (1). ρi xif  (1) Where. ρi - sample mass concentration of methanol or acetone, mg/L; ρxi - the concentration of methanol or acetone from the working curve, mg/L; f - Sample dilution factor. 9.3 results show When the result of the determination of methanol in water is less than 10.0 mg/L, one digit after the decimal point is retained. When the result is equal to or greater than 10.0 mg/L, Keep 3 significant digits. When the result of determination of acetone in water is less than 1.00 mg/L, keep 2 digits after the decimal point. When the result is greater than or equal to 1.00 mg/L, Keep 3 significant digits. 10 precision and accuracy 10.1 Precision Six laboratories for the methanol concentration of 0.8 mg/L, 7.9 mg/L, 39.5 mg/L and acetone concentration of 0.08 mg/L, 0.79 mg/L, 3.94 mg/L of the uniform sample was repeated 6 times determination. methanol laboratory relative standard deviation were 1.2% -7.3%, 2.2% -4.4% and 1.5% -5.1%. The relative standard deviations (RSDs) were 1.8%, 0.8% and 1.0%, respectively. The reproducibility limits were 0.1 mg/L, 0.7 mg/L and 2.8 mg/L, respectively. The reproducibility limits were 0.1 mg/L, 0.7 mg/L and 2.9 mg/L. The relative standard deviations of acetone in the laboratory were 3.1% -8.6%, 1.4% -5.4% and 0.9% -2.1% respectively. The relative standard deviations of laboratory were 4.8%, 1.3% and 0.6%, respectively. The repeatability limits were 0.01 mg/L, 0.09 mg/L and 0.20 mg/L; reproducibility limits were 0.02 mg/L, 0.10 mg/L and 0.20 mg/L, respectively. Six laboratories spiked samples of surface water and seawater (methanol spiked at 7.9 mg/L, 39.5 mg/L, spiked with acetone Concentration of 0.79 mg/L, 3.94 mg/L) for 6 replicates. the relative standard deviation The differences were 2.2% ~ 11% and 1.4% ~ 5.1%, respectively. The relative standard deviations (RSDs) were 3.6% and 0.9%, respectively. The repeatability Respectively 1.1 mg/L and 3.1 mg/L; reproducibility limits were 1.3 mg/L and 3.2 mg/L, respectively. Sea water sample methanol in laboratory 6 relative standard deviations were 1.3% ~ 3.0% and 1.5% ~ 3.0%, respectively; relative standard deviations of laboratory were 3.1% and 2.1% respectively; The reproducibility limits were 0.5 mg/L and 2.4 mg/L, respectively. The reproducibility limits were 0.8 mg/L and 3.2 mg/L, respectively. Surface water samples acetone The relative standard deviations in the laboratory were 1.4% ~ 5.9% and 1.8% ~ 9.7%, respectively. The relative standard deviations 3.1% and 2.3%, respectively. The reproducibility limits were 0.08 mg/L and 0.54 mg/L, respectively. The reproducibility limits were 0.10 mg/L and 0.55 mg/L, respectively. The relative standard deviations (RSDs) of laboratory samples for seawater samples were 1.5% -3.7% and 1.6% -5.2% respectively. The relative standard deviation The quasi-deviations were 2.4% and 1.7% respectively. The repeatability was 0.06 mg/L and 0.41 mg/L, respectively. The reproducibility limits were 0.07 mg/L and 0.42 mg/L. Method precision summary data see Appendix A. 10.2 Accuracy Six laboratories spiked surface water, industrial wastewater and seawater samples (methanol spiked at a concentration of 7.9 mg/L, 39.5 mg/L, acetone spiked concentration of 0.79 mg/L, 3.94 mg/L). Surface water spiked sample recovery range of methanol, respectively The results showed that the final recoveries were 93.7% ± 6.8% and 95.4% ± 1.6%, respectively, from 87.3% to 97.1% and from 94.1% to 96.3% The recoveries of acetone ranged from 89.7% to 98.5% and from 90.4% to 97.0%, respectively. The final recoveries of acetone were 93.6% ± 5.8% and 94.3% ± 4.4%, respectively. The recoveries of methanol in industrial wastewater samples range from 77.2% to 110% and 81.2% to 102%, respectively, The final recoveries were 94.2% ± 24.4% and 94.7% ± 14.8%, respectively. The recoveries of acetone ranged from 85.0% 101% and 88.1% ~ 98.4% respectively. The final recoveries of spiked samples were 92.8% ± 12.4% and 92.7% ± 8.2%, respectively. Seawater samples The recoveries of methanol ranged from 92.3% to 101% and 94.5% to 100%, respectively. The final recoveries of methanol were 94.7% ± 6.0% and 96.4% ± 4.0% respectively. The recoveries of acetone were 93.1% -99.0% and 95.7% -100% The values were 94.6% ± 4.4% and 97.1% ± 3.2%, respectively. Method summary accuracy data, see Appendix A. 11 Quality Assurance and Quality Control 11.1 Blank Analysis Each batch of samples to do at least one laboratory blank test and the entire program blank test, the determination of the results shall not exceed the method of detection limit. Note. Methanol and acetone are commonly used laboratory solvents, attention should be paid to control the laboratory environment, cross-interference. 11.2 working curve Each batch of samples should be drawn working curve, the correlation coefficient should be ≥ 0.955, or to re-establish the working curve. For each 20 samples or each batch of samples (less than 20 samples) should be measured in a working curve intermediate concentration point standard solution, The measurement results and the relative concentration of the point of error should be within ± 20%, or to re-establish the working curve. 11.3 Determination of parallel samples Each sample should be collected parallel to the sample, every 20 samples or batches (less than 20 samples/batch) should be measured at least one A parallel sample, the relative deviation of parallel samples ≤ 20%. 11.4 Substrate spike determination For sample spiking, determine at least one spiked sample every 20 samples or batches (less than 20 samples/batch). 7 actual sample spike recovery between 70% to 120%. 12 Waste treatment The waste liquid and waste generated during the experiment shall be collected and stored in categories and correspondingly identified, commissioned by a qualified unit For processing.

Appendix A

(Informative) The precision and accuracy of the method Table A.1 six laboratories blank spiked determination of precision summary table Compound name average value (Mg/L) Laboratory relative standard deviation(%) Relative between laboratories standard deviation(%) Repeatability r (Mg/L) Reproducibility limit R (Mg/L) Methanol 0.8 1.2 ~ 7.3 1.8 0.1 0.1 7.8 2.2 ~ 4.4 0.8 0.7 0.7 36.9 1.5 ~ 5.1 1.0 2.8 2.9 acetone 0.08 3.1 ~ 8.6 4.8 0.01 0.02 0.78 1.4 ~ 5.4 1.3 0.09 0.10 3.83 0.9 ~ 2.1 0.6 0.20 0.20 Table A.2 six laboratory real sample spiked determination of precision summary table Compound matrix type Spiked concentration (Mg/L) average value (Mg/L) Laboratory Relative standard deviation(%) Laboratory Relative standard deviation(%) Repeatability r (Mg/L) Reproducibility limit R (Mg/L) Methanol Surface water 7.9 7.4 2.2 ~ 11 3.6 1.1 1.3 39.5 37.7 1.4 ~ 5.1 0.9 3.1 3.2 seawater 7.9 7.5 1.3 ~ 3.0 3.1 0.5 0.8 39.5 38.1 1.5 ~ 3.0 2.1 2.4 3.2 Industrial waste 7.9 - 0.7 ~ 3.8 - - - 39.5 - 0.5 ~ 2.1 - - - acetone Surface water 0.79 0.74 1.4 ~ 5.9 3.1 0.08 0.10 3.94 3.71 1.8 ~ 9.7 2.3 0.54 0.55 seawater 0.79 0.75 1.5 ~ 3.7 2.4 0.06 0.07 3.94 3.83 1.6 ~ 5.2 1.7 0.41 0.42 Industrial waste 0.79 - 0.4 ~ 12 - - - 3.94 - 0.3 ~ 2.0 - - - Table A.3 Accuracy of spiked determination of actual samples in six laboratories Compound name Sample type Spiked concentration (Μg/L) Recovery rate range (%) Methanol Surface water 7.9 87.3 ~ 97.1 93.7 ± 6.8 39.5 94.1 ~ 96.3 95.4 ± 1.6 Wastewater 7.9 77.2 ~ 110 94.2 ± 24.4 39.5 81.2 ~ 102 94.7 ± 14.8 seawater 7.9 92.3 ~ 101 94.7 ± 6.0 39.5 94.5 ~ 100 96.4 ± 4.0 acetone Surface water 0.79 89.7 ~ 98.5 93.6 ± 5.8 3.94 90.4 ~ 97.0 94.3 ± 4.4 Wastewater 0.79 85.0 ~ 101 92.8 ± 12.4 3.94 88.1-98.4 92.7 ± 8.2 seawater 0.79 93.1 ~ 99.0 94.6 ± 4.4 3.94 95.7 ~ 100 97.1 ± 3.2 (%) 2 _pSp 

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