HJ 895-2017_English: PDF (HJ895-2017)
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Water quality. Determination of methanol and acetone. Headspace gas chromatography
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| 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 | 12,131 | | 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 | | 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)
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 dete......
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