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HJ 600-2011: Water quality. Determination of TNT, RDX, DNT. Gas chromatography
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Water quality. Determination of TNT, RDX, DNT. Gas chromatography
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HJ 600-2011
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Standard similar to HJ 600-2011 GB 5085.7 GB 5085.1 HJ 609 HJ 598 HJ 597 Basic data | Standard ID | HJ 600-2011 (HJ600-2011) | | Description (Translated English) | Water quality. Determination of TNT, RDX, DNT. Gas chromatography | | Sector / Industry | Environmental Protection Industry Standard | | Classification of Chinese Standard | Z16 | | Classification of International Standard | 13.060 | | Word Count Estimation | 12,196 | | Date of Issue | 2011-02-10 | | Date of Implementation | 2011-06-01 | | Older Standard (superseded by this standard) | GB/T 13904-1992 | | Regulation (derived from) | Department of Environmental Protection Notice No. 9 of 2011 | | Issuing agency(ies) | Ministry of Ecology and Environment | | Summary | This standard specifies the determination of TNT, RDX and DNT by gas chromatography. This standard applies to industrial wastewater Ammunition TNT, RDX and DNT determination. | HJ 600-2011: Water quality. Determination of TNT, RDX, DNT. Gas chromatography---This is a DRAFT version for illustration, not a final translation. Full copy of true-PDF in English version (including equations, symbols, images, flow-chart, tables, and figures etc.) will be manually/carefully translated upon your order.
Water quality.Determination of TNT, RDX, DNT.Gas chromatography
National Environmental Protection Standard of the People's Republic
Replace GB/T 13904-92
Determination of water quality TNT, Hessian and Dien
Gas chromatography
Water quality-Determination of TNT, RDX, DNT
-Gas chromatography
Published on.2011-02-10
2011-06-01 Implementation
Ministry of Environmental Protection released
Ministry of Environmental Protection
announcement
No. 9 of.2011
In order to implement the "Environmental Protection Law of the People's Republic of China", protect the environment, protect human health, and standardize environmental monitoring, the water is now approved.
The determination of total mercury is determined by the Cold Atomic Absorption Spectrophotometry and other nine standards for national environmental protection standards.
The standard name and number are as follows.
I. Determination of total mercury in water - Cold atomic absorption spectrophotometric method (HJ 597-2011);
2. Determination of water quality ladders by sodium sulfite spectrophotometry (HJ 598-2011);
3. Determination of water quality ladders N-chlorohexadecylpyridine-sodium sulfite spectrophotometry (HJ 599-2011);
5. Determination of water quality of formaldehyde - Acetylacetone spectrophotometry (HJ 601-2011);
6. Determination of water quality 石墨 Graphite furnace atomic absorption spectrophotometry (HJ 602-2011);
VII. Determination of water quality 火焰 Flame atomic absorption spectrophotometry (HJ 603-2011);
VIII. Determination of total hydrocarbons in ambient air - Gas chromatography (HJ 604-2011);
IX. Determination of Volatile Organic Compounds in Soils and Sediments Purge and Trap/Gas Chromatography-Mass Spectrometry (HJ 605-2011).
The above standards have been implemented since June 1,.2011 and published by the China Environmental Science Press. The standard content can be found on the website of the Ministry of Environmental Protection.
From the date of implementation of the above standards, the following seven national environmental protection standards approved and issued by the former National Environmental Protection Agency shall be abolished.
The name and number are as follows.
1. Determination of total mercury in water quality by cold atomic absorption spectrophotometry (GB 7468-87);
2. Determination of water quality ladders by sodium sulfite spectrophotometry (GB/T 13905-92);
3. Determination of water quality ladders by spectrophotometry (GB/T 13903-92);
4. Determination of water quality TNT, Hessian and Dien, gas chromatography (GB/T 13904-92);
V. Determination of water quality formaldehyde acetylacetone spectrophotometry (GB 13197-91);
VII. Determination of total hydrocarbons in ambient air Gas chromatography (GB/T 15263-94).
Special announcement.
February 10,.2011
Content
Foreword..iv
1 Scope..1
2 Method principle..1
3 reagents and materials.1
4 instruments and equipment. 2
5 samples. 2
6 Analysis steps..3
7 Calculation and representation of results..5
8 precision and accuracy..5
9 Quality Assurance and Quality Control 6
10 Waste treatment 6
11 Note 6
Appendix A (informative appendix) Determination of precision and accuracy data of the target.7
Iv
Foreword
To protect the environment and protect the human body 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 Water Pollution Prevention and Control
This standard is formulated for the determination of health, standardization of TNT, Hessian and Dien.
This standard specifies the gas chromatographic method for the determination of TNT, Hessian and Dient in water.
This standard is a revision of the "Gas Chromatography Method for the Determination of Water Quality, Esso, and Dien" (GB/T 13904-92).
This standard was first published in.1992. The original standard drafting unit was the Sixth Design and Research Institute of China Ordnance Industry. This is the first revision.
The main revisions are as follows.
- increased the principle of the method;
-- Increased capillary column content;
-- Added blank test content;
-- Added quality assurance and quality control regulations;
-- Increased waste disposal and precautions.
The national environmental protection standard “Water quality approved and issued by the former National Environmental Protection Agency on December 2,.1992 since the implementation of this standard.
The gas chromatography method for the determination of TNT, Hessau, and Dienction (GB/T 13904-92) is abolished.
Appendix A of this standard is an informative annex.
This standard was formulated by the Science and Technology Standards Department of the Ministry of Environmental Protection.
This standard is mainly drafted by. Beijing Zhongbing North Environmental Technology Development Co., Ltd., Nanjing University of Science and Technology, School of Chemical Engineering and Chinese soldiers.
Industrial Group Corporation.
This standard is verified by. Taizhou University of Science and Technology, Nanjing University of Science and Technology, Changzhou Environmental Monitoring Center Station, Jiangsu University of Science and Technology, Taizhou City Ring
Environmental Monitoring Center Station, National Civil Blasting Equipment Quality Supervision and Inspection Center and Nanjing Police Dog Research Institute of the Ministry of Public Security.
This standard was approved by the Ministry of Environmental Protection on February 10,.2011.
This standard has been implemented since June 1,.2011.
This standard is explained by the Ministry of Environmental Protection.
Determination of water quality TNT, Hessian and Dien, gas chromatography
1 Scope of application
This standard specifies the gas chromatographic method for the determination of TNT, Hessian and Dient in water.
This standard is applicable to the determination of TNT, Hesuojin and Dien ladder in the industrial wastewater of ammunition.
When the sampling volume is 10.0 ml, the packed column is used. The detection limit is. TNT 0.02 mg/L, Black Sox 0.1 mg/L, Dion
Ladder 0.01 mg/L; the lower limit of determination. TNT 0.08 mg/L, black soda 0.4 mg/L, Dien ladder 0.04 mg/L.
When the sampling volume is 10.0 ml, the capillary column is used. The detection limit is 0.02 mg/L for TNT and 0.05 mg/L for black cable.
Dien ladder 0.01 mg/L; the lower limit of determination. TNT 0.08 mg/L, black soda 0.2 mg/L, Dien ladder 0.04 mg/L.
2 Principle of the method
Extract the TNT, Hessian and Dien ladder in the sample with benzene, and then take a certain volume of benzene extract under the selected chromatographic conditions.
It was separated by chromatography and detected by an electron capture detector. The retention time was qualitative and the peak area (or peak height) was quantified by internal standard method.
3 reagents and materials
Unless otherwise stated, chromatographic purification reagents conforming to national standards were used for the analysis, and the experimental water was newly prepared deionized water or steamed.
Distilled water.
3.1 Acetone (CH3COCH3).
3.2 Anhydrous ethanol (C2H5OH).
3.3 Benzene (C6H6). There is no interference peak at the target position by chromatography, otherwise it should be re-distilled through a full glass distiller.
3.4 Internal standard. 1,5-dinitronaphthalene (1,5-DNN), ρ[C10H6(NO2)2]=10.0 mg/L
Accurately weigh 0.025 0 g 1,5-dinitronaphthalene dissolved in acetone (3.1), and after dissolving, move to a 25 ml volumetric flask with acetone (3.1)
Dilute to the mark and shake well. Pipette accurately 10.0 ml, place in a beaker containing 500 ml of water, and remove the acetone on a 50 ° C water bath.
After cooling to room temperature, transfer to a 1 000 ml brown volumetric flask, add water to the score line, and shake well. Stored in a refrigerator at 0 to 4 ° C in the dark, it is effective
The period is 30 days.
3.5 Internal standard. 1,5-dinitronaphthalene (1,5-DNN), ρ[C10H6(NO2)2]=1.0 mg/L
Measure 10.0 ml of internal standard (3.4) into a 100 ml brown volumetric flask, add water to the score line, and shake well. Stored in ice at 0 to 4 ° C in the dark
In the box, it is valid for 30 days.
3.6 TNT. 2,4,6-trinitrotoluene [CH3C6H2(NO2)3]
Weigh 1.0 g of TNT (industrial product) in a small beaker, dissolve it with 10 ml of absolute ethanol (3.2), and filter with medium-speed quantitative filter paper.
Place the filtrate in a fume hood and allow it to dry naturally. Recrystallization twice, spare.
3.7 Hessian (RDX). 1,3,5-trinitrohexahydro-symmetric triazabenzene or 1,3,5-trinitro-1,3,5-trinitrohexane (C3H6O6N6 )
Weigh 1.0 g of Hessau (industrial product) in a small beaker, dissolve it with 10 ml of acetone (3.1), and filter with medium-speed quantitative filter paper.
The filtrate was placed in a fume hood and protected from light and dried naturally. Recrystallization twice, spare.
3.8 Dint ladder (DNT). 2,4-dinitrotoluene [C6H3CH3(NO2)2], or purchase commercially available certified reference materials.
3.9 TNT standard stock solution. ρ(TNT)=100.0 mg/L
Weigh 0.100 0 g TNT (3.6) in a small beaker, dissolve it with 20-50 ml of acetone (3.1), and transfer to a 500 ml water.
In the cup, remove the acetone on a 50 ° C water bath, cool to room temperature, transfer to a 1 000 ml brown volumetric flask, add water to the line and shake. The
The solution is stored in a refrigerator at 0 to 4 ° C in the dark, and is valid for 30 days.
3.10 Hessian standard stock solution. ρ(RDX)=20.0 mg/L
Weigh 0.020 0 g RDX (3.7) in a small beaker, dissolve it with 20-50 ml of acetone (3.1), and transfer to a 500 ml water.
In the cup, remove the acetone on a 50 ° C water bath, cool to room temperature, transfer to a 1 000 ml brown volumetric flask, add water to the line and shake. The
The solution is stored in a refrigerator at 0 to 4 ° C in the dark, and is valid for 30 days.
3.11 Dien ladder standard stock solution. ρ(DNT)=100.0 mg/L
Weigh 0.100 0 g DNT (3.8) in a small beaker, dissolve it with 20-50 ml of acetone (3.1), and transfer to a 500 ml water.
In the cup, remove the acetone on a 50 ° C water bath, cool to room temperature, transfer to a 1 000 ml brown volumetric flask, add water to the line and shake. The
The solution is stored in a refrigerator at 0 to 4 ° C in the dark, and is valid for 30 days.
3.12 anhydrous sodium sulfate (Na2SO4). excellent grade pure
Bake at 350 ° C for 4 h before use, cool to room temperature in a desiccator, and store in a sealed glass bottle.
3.13 Organic phase filter. 0.45 μm.
3.14 Carrier gas. high purity nitrogen, purity (volume fraction) ≥ 99.999%.
4 Instruments and equipment
4.1 Gas Chromatograph. with an electron capture detector.
4.2 Column
4.2.1 Packed column. made of quartz glass, 1.5 m long, inner diameter 2 to 3 mm; carrier. Chromosorb G AW-DMCS 60-80
Fixative solution. trifluoropropylmethylpolysiloxane (QF-1); liquid phase loading. 3% QF-1.
Method of coating fixed liquid. Weigh 0.3 g of fixative QF-1 in a small beaker, dissolve it with acetone (3.1), and the amount of acetone should be just soaked.
No 10 g of the carrier, volatilized to dryness at normal temperature, and dried at 180 ° C for 2 h, ready for use.
Aging of the packed column. Install the filled column on the chromatograph inlet, the outlet is not connected to the detector, and is ventilated with a small carrier gas flow. column
The box was maintained at 230 ° C, aged for 48 h, and the detector continued to age until the baseline was straight.
4.2.2 Capillary column. 30 m × 0.25 mm (inside diameter) × 0.25 μm (film thickness), stationary phase. trifluoropropylmethylpolysiloxane (QF-1),
Load capacity. 50% QF-1, or other equivalent capillary column.
4.3 Microinjector. 1 μl, 5 μl.
4.4 Constant temperature water bath.
4.5 separatory funnel. 60 ml.
4.6 Reciprocating Oscillator.
4.7 Common instruments and equipment used in general laboratories.
5 samples
5.1 Sampling and preservation
Collect 500 ml samples in brown glass bottles, store them in the dark at low temperature (0~4 °C), and extract the water samples within 7 days. The extract should be at 4
Store in the dark at °C and analyze within 30 days.
5.2 Preparation of samples
Take 10.0 ml of the sample and place it in a separatory funnel. Add an appropriate amount of internal standard, shake well, and add 5 ml of benzene (3.3) to oscillate on the shaker.
2 min, let stand for 15 min. The aqueous phase was placed in another separatory funnel and the organic phase was placed in a 10 ml volumetric flask. Repeat extraction once, merge
The extract was dehydrated with 1 g of anhydrous sodium sulfate (3.12) and made up to 10 ml with benzene (3.3) for testing.
Note 1. When using a capillary column, add 0.1 ml internal standard (3.4); when using packed column, add 0.1 ml internal standard (3.5).
Note 2. If there are particulate matter in the sample, the above test sample should be filtered through the organic phase filter membrane (3.13).
5.3 Preparation of blank samples
A sample of 10.0 ml of water was taken instead of the sample, and a blank sample was prepared in the same manner as in the preparation of the sample (5.2).
6 Analysis steps
6.1 Reference chromatographic conditions
6.1.1 packed column
Vaporization chamber temperature. 210 ~ 220 ° C; oven temperature. 180 ~ 190 ° C; detector temperature. 250 ~ 270 ° C (detector outlet export room
Outside); carrier gas flow rate. 100 ~ 120 ml/min; supplementary carrier gas flow rate. 30 ~ 50 ml/min; recorder attenuation. according to the baseline and the sample is
Measurement of sample content; injection volume. 1 ~ 2 μl.
6.1.2 Capillary column
Vaporization chamber temperature. 220 ° C; oven temperature..200 ° C; detector temperature. 300 ° C (detector outlet is exported outside); carrier gas flow 2
Ml/min; split ratio. 20.1 ~ 50.1 (can be adjusted according to peak conditions and injection volume); injection volume. 0.5 ~ 1 μl.
6.2 Calibration
6.2.1 Drawing a calibration curve
Measure a certain volume of TNT standard stock solution (3.9), black soda standard stock solution (3.10) and Dien ladder standard stock solution (3.11)
Into 6 100 ml volumetric flasks, add water to the engraved line to prepare standard series of different concentration levels (see Table 1 for specific mass concentration levels). again
Pipette 10.0 ml of the standard series into 6 separatory funnels and follow the same procedure as in 5.2. From low mass concentration to high quality
Degree is injected into the chromatograph for analysis, and the ratio of the target peak area to the internal standard peak area (or the ratio of the target peak height to the internal standard peak height) is vertical.
Coordinates, with the mass concentration (mg/L) as the abscissa, draw a calibration curve.
Table 1 Calibration Series Mass Concentration Unit. mg/L
Target mass concentration 1 mass concentration 2 mass concentration 3 mass concentration 4 mass concentration 5 mass concentration 6
TNT 0.1 0.5 1.0 5.0 10.0 20.0
Hessian today 0.2 0.4 1.0 2.0 4.0 5.0
Dien ladder 0.1 0.5 1.0 5.0 10.0 20.0
6.2.2 Standard chromatogram
The standard chromatograms of TNT, Hessian and Dient are shown in Figure 1 and Figure 2 under the reference chromatographic conditions of this standard.
Injection
1-DNT; 2-TNT; 3-internal standard; 4-RDX
Figure 1 Standard chromatogram of a packed column
RDX
DNT TNT
1,5-DNN
ECD 7.29
Figure 2 Standard chromatogram of a capillary column
6.3 Determination
Take a small amount of the sample to be tested (5.2) with a micro-injector, analyze according to the reference chromatographic conditions (6.1), and record the peak area (or peak).
high).
6.4 Blank test
Use a micro-injector to take an appropriate amount of the blank sample to be tested (5.3), and analyze it according to the same procedure as in the measurement (6.3) to record the peak area (or
Peak height).
7 Calculation and representation of results
7.1 Calculation of results
The mass concentration iρ (mg/L) of the component to be tested (TNT, RDX or DNT) in the sample is calculated according to formula (1).
Ρρ ×= standard (1)
Where. iρ - the mass concentration of the component i to be tested in the sample, mg/L;
V1--extraction volume, ml;
V--water sample volume, ml.
7.2 Results representation
When the measurement result is less than 1 mg/L, the result remains two decimal places. When the measurement result is greater than or equal to 1 mg/L, the result is retained
Three significant figures.
8 precision and accuracy
8.1 Precision
8.1.1 packed column
The relative standard deviation of repeatability is not greater than. TNT 2.1%, Hessian 4.4%, Dien ladder 2.8%; Reproducibility relative standard deviation
Not more than. 3.1% for TNT, 7.4% for Hessian, and 5.0% for Dien.
8.1.2 Capillary column
Six laboratories measured the uniform standard samples containing TNT, Hessian and Dien, respectively, and the relative standards in the laboratory.
The deviation range is from 1.06% to 8.70%, the relative standard deviation between laboratories ranges from 0.51% to 7.80%, and the repeatability limit ranges from 0.001 to ～.
0.39 mg/L, the reproducibility limit ranged from 0.01 to 0.57 mg/L.
8.2 Accuracy
8.2.1 packed column
A water sample with a TNT concentration of 2.71 mg/L, a black sputum concentration of 1.26 mg/L, and a Diento concentration of 0.72 mg/L was performed.
According to the spiked analysis, the recoveries ranged from 97.1% to 104.0% for TNT, 90.0% to 95.7% for Hessian, and 99.0% for Dien.
107.0%.
8.2.2 Capillary column
Six laboratories tested the uniform standard samples containing TNT, Hessian and Dien, respectively, with a relative error range of
−13.3% to 10.9%.
A summary of the precision and accuracy data for capillary column measurements is provided in Appendix A.
9 Quality Assurance and Quality Control
9.1 There is a difference in structure and performance between each detector, and the linear range is also different. The quantification should be within the linear range.
A retention time window of t ± 3 s should be established prior to sample analysis. When the sample is analyzed, the target compound retention time should be within the retention time window.
9.2 Perform a reagent blank test for each batch of reagents. The reagent blank test results should be lower than the method detection limit. At least one whole process for each batch of samples
In the blank test, the target compound concentration should be below the detection limit.
9.3 The correlation coefficient of the calibration curve should be greater than or equal to 0.995.
9.4 A continuous calibration analysis should be performed every working day. Continuous calibration should be prior to blanking and sample analysis. Continuous calibration of the concentration
A concentration point of the quasi-curve, the relative deviation of the concentration of the target compound continuously calibrated from the concentration of the most recent calibration curve shall not be greater than
20%. If several consecutive calibrations are outside the allowable range, the calibration curve should be redrawn.
9.5 Each batch of samples should be tested at least 10% of parallel samples, and the relative deviation of parallel sample analysis results should be less than 20%.
9.6 Each batch of samples should be tested by at least one spiked recovery analysis, and the actual sample spike recovery should be controlled at 80% to 120%.
10 Waste treatment
The waste liquid and waste water generated during the test should be collected and disposed of properly.
11 Precautions
11.1 The glassware used in the experiment should be cleaned and dried. If necessary, use potassium dichromate washing solution to soak in tap water and distilled water.
Rinse and dry.
11.2 The electron capture detector has high sensitivity, narrow linear range and easy contamination. Care should be taken to keep the detector clean.
Appendix A
(informative appendix)
Measuring the precision and accuracy data of the target
Table A.1 Summary of precision data for TNT, Hessian and Dien
Target TNT (Black Line) RDX (DTX)
Sample mass concentration /
(mg/L) 0.08 0.5 10 0.8 3.0 10.0 0.1 0.5 10.0
Relative standard in the experimental room
deviation/%
1.06~
4.72
2.69~
5.10
2.33~
3.57
1.27~
2.15
3.99~
5.46
2.87~
4.73
2.06~
4.85
3.65~
8.70
2.42~
5.11
Relative standard between laboratories
Deviation /% 7.80 0.94 0.51 0.76 1.52 0.77 2.24 2.13 2.07
Repeatability limit/(mg/L) 0.001 0.02 0.28 0.02 0.15 0.39 0.002 0.02 0.28
Reproducibility limit/(mg/L) 0.02 0.02 0.29 0.03 0.19 0.42 0.01 0.04 0.57
Table A.2 Summary of Accuracy Data for TNT, Hessian and Dien
Target TNT (Black Line) RDX (DTX)
Sample mass concentration /
(mg/L) 0.08 0.5 10.0 0.8 3.5 10.0 0.1 0.5 10.0
Relative error /% −12～10.9 0.6～3.6 −0.5～1.0 −0.75～
1.25
−1.67～
2.17
−1.9～0 3.75～
10.0
−2.8～3.8 −13.3～−8.3
Relative error final value /% 3.96 ±17.9 2.23 ±4.87 0.05±1.02 0.73±2.48 −0.81±
3.94
−1.02±
2.34
7.52±17.2 0.17±4.17 −11.5±
23.7
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