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HJ 599-2011 English PDF

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HJ 599-2011: Water quality. Determination of TNT. N-cetyl pridinium chloride. Sodium sulfite Spectrophotometric method
Status: Valid
Standard IDUSDBUY PDFLead-DaysStandard Title (Description)Status
HJ 599-2011239 Add to Cart 3 days Water quality. Determination of TNT. N-cetyl pridinium chloride. Sodium sulfite Spectrophotometric method Valid

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Basic data

Standard ID: HJ 599-2011 (HJ599-2011)
Description (Translated English): Water quality. Determination of TNT. N-cetyl pridinium chloride. Sodium sulfite Spectrophotometric method
Sector / Industry: Environmental Protection Industry Standard
Classification of Chinese Standard: Z16
Classification of International Standard: 13.060
Word Count Estimation: 9,944
Date of Issue: 2011-02-10
Date of Implementation: 2011-06-01
Older Standard (superseded by this standard): GB/T 13903-1992
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 N- cetyl pyridinium chloride sodium sulfite spectrophotometric method. This standard applies Ammunition industrial wastewater Determination of TNT. Using 30mm cuvette, the method detection limit of 0. 05mg/L, determination range of 0. 2 ~ 4mg/L. TNT measured concentration is higher than the upper limit of the sample may be measured after appropriate dilution.

HJ 599-2011: Water quality. Determination of TNT. N-cetyl pridinium chloride. Sodium sulfite Spectrophotometric method


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Water quality.Determination of TNT.N-cetyl pridinium chloride.Sodium sulfite Spectrophotometric method National Environmental Protection Standard of the People's Republic Replace GB/T 13903-92 Water quality - Determination of TNT - N-chlorohexadecyl Pyridine-sodium sulfite spectrophotometry Water quality-Determination of TNT -N-cetyl pridinium chloride -sodium sulfite spectrophotometric method 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); 4. Gas chromatographic method (HJ 600-2011) for the determination of water quality ladders, black ropes, and dien ladders; 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 interference and elimination.1 4 Reagents and materials.1 5 instruments and equipment. 2 6 samples. 2 7 Analysis steps..2 8 Results calculation and representation..3 9 precision and accuracy..3 10 Quality Assurance and Quality Control.3 11 Waste treatment 4 12 Notes 4 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 and standardization of TNT in water. This standard specifies the N-chlorohexadecylpyridine-sulfite spectrophotometric method for the determination of TNT in water. This standard is a revision of the "Measurement Spectrophotometric Method for Water Quality TNT" (GB/T 13903-92). This standard was first published in.1992. The original standard was drafted. Taiyang Jiangyang Chemical Plant. This standard is the first revision. Major repair The order is as follows. - The standard name was changed to "Determination of water quality TNT by N-chlorohexadecylpyridine-sodium sulfite spectrophotometry"; - increased interference and elimination clauses; -- Added blank test content; -- Added quality assurance and quality control regulations; -- Added provisions for 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 TNT's Determination Spectrophotometry (GB/T 13903-92) is abolished. 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., China Ordnance Industry Group Corporation and Liaoyang Qing Yang Special Chemical Co., Ltd. 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 ladder N-chlorohexadecylpyridine-sodium sulfite spectrophotometry

1 Scope of application

This standard specifies the N-chlorohexadecylpyridine-sulfite spectrophotometric method for the determination of TNT in water. This standard applies to the determination of TNT in the ammunition charging industrial wastewater. When using a 30 mm cuvette, the method detection limit is 0.05 mg/L and the measurement range is 0.2-4 mg/L. For samples with a TNT concentration higher than the upper limit of the method, the sample can be appropriately diluted and measured.

2 Principle of the method

The addition of TNT to the sodium sulfite in the sample is sensitized by N-chlorohexadecylpyridine to form a red complex. The absorbance was measured at a wavelength of 466 nm. Within a certain concentration range, the TNT concentration and absorbance values are in accordance with Lambert-Beer law.

3 interference and elimination

When the wastewater has a certain color, it will interfere with the measurement. Dilute to 25.0 ml by collecting 10.0 ml of sample as a sample blank. The absorbance was measured directly without any reagent. The absorbance of the sample blank is subtracted from the absorbance of the sample, and then calculated to eliminate the chromaticity pair The effect of the determination.

4 reagents and materials

Analytical purification reagents that meet national standards are used for analysis, unless otherwise stated. The experimental water is freshly prepared deionized water or steamed. Distilled water. 4.1 Concentrated hydrochloric acid. ρ(HCl) = 1.19 g/ml. 4.2 Hydrochloric acid solution. 1 1. 4.3 Concentrated ammonia. ρ(NH4OH) = 0.91 g/ml. 4.4 Ammonia solution. 1 1. 4.5 Ether. ρ(C2H5OC2H5) = 0.71 g/ml. 4.6 Anhydrous ethanol. ρ(C2H5OH) = 0.79 g/ml. 4.7 Sodium sulfite solution. ρ(Na2SO3) = 0.1 g/ml. Weigh 10.0 g of anhydrous sodium sulfite dissolved in an appropriate amount of water, dissolve and transfer to a 100 ml volumetric flask, add water to the mark, and mix. this The solution is valid for 3 days. 4.8 N-chlorohexadecylpyridine solution. ρ[C6H5N(CH2)15CH3Cl·H2O]=2.5 g/L. Weigh 0.500 g of cetylpyridinium chloride in an appropriate amount of water, dissolve it, transfer it to a.200 ml volumetric flask, add water to the mark, and mix. The solution was stored in a brown glass ground bottle and stored stably for 30 days at room temperature. 4.9 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 (4.6), and filter with medium-speed quantitative filter paper. Place the filtrate in a fume hood and allow it to dry naturally. Recrystallization twice, spare. 4.10 TNT standard stock solution. ρ(TNT) = 50.0 mg/L. Weigh 0.050 0 g TNT (4.9) in a 1 000 ml beaker, add about 800 ml of water preheated to 70 ° C, and place at 75-79 ° C. In a constant temperature water bath, stir while heating until completely dissolved. Remove, cool to room temperature and transfer to a 1 000 ml brown volumetric flask. Add water to the mark and mix. The solution is stored at 2 to 5 ° C in the dark, valid for 30 days, or purchased commercially available certified standards. 4.11 TNT standard use solution. ρ (TNT) = 10.0 mg/L. Measure 50.0 ml of TNT standard stock solution (4.10) in a 250 ml brown volumetric flask, add water to the mark and mix. When used Now equipped.

5 Instruments and equipment

5.1 Visible spectrophotometer. with 30 mm cuvette. 5.2 Constant temperature water bath. 5.3 Separating funnel. 50 ml. 5.4 Plug scale colorimetric tube. 50 ml. 5.5 Common instruments and equipment used in general laboratories.

6 samples

6.1 Sample collection and preservation Samples should be collected in brown glass bottles, stored at 0 to 4 ° C in the dark, and measured within 5 days. 6.2 Preparation of samples 6.2.1 When the pH value of the water sample is not 4~9, adjust the pH value with hydrochloric acid solution (4.2) or ammonia solution (4.4). 6.2.2 If there is more suspended matter in the water sample, it can be measured by filtration with quantitative filter paper or after extraction with ether. Extract with ether, the steps are as follows. Measure 25.0 ml of the sample in a 50 ml separatory funnel, add 15 ml of ether (4.5), vigorously shake Move for 2 min. After standing and layering, the water phase is discarded. The ether phase was transferred to a stoppered colorimetric tube and washed with 2 ml of diethyl ether (4.5). The funnel, washed ether was incorporated into a plug scale tube. Place the colorimetric tube in a constant temperature water bath (temperature does not exceed 40 ° C) and evaporate to no Ether smell, to be tested. 6.3 Preparation of blank samples A blank sample was prepared by replacing the sample with water and following the same procedure as in the preparation of the sample (6.2.2).

7 Analysis steps

7.1 Drawing of the calibration curve 7.1.1 Measure 0.00, 0.50, 1.00, 3.00, 5.00, 7.00, 10.00 ml TNT standard use solution (4.11) in 7 points The TNT content in the liquid funnel was 0.00, 5.00, 10.0, 30.0, 50.0, 70.0, 100 μg, respectively. Add water to 25 ml separately, according to 6.2.2 The same procedure is used for the extraction operation. 7.1.2 Add 2 ml of absolute ethanol (4.6) to the wall of the tube with a plug scale of the TNT standard series, add about 10 ml of water. Shake well. 7.1.3 Add 3 ml of sodium sulfite solution (4.7), mix, add 5 ml of N-chlorohexadecylpyridine solution (4.8), add water to 25 ml scribe line, shake well and let stand for 15 min. The absorbance was measured with a 30 mm cuvette at a wavelength of 466 nm using water as a reference. To suck The luminosity is the ordinate, and the corresponding TNT content (μg) is the abscissa, and a calibration curve is drawn. Note. When the TNT standard series is not directly extracted, only 0.00, 0.50, 1.00, 3.00, 5.00, 7.00, 10.00 ml TNT standard is used. The liquid (4.11) was placed in 7 plug-type colorimetric tubes, mixed, and the calibration procedure was drawn according to the same procedure as in 7.1.3. 7.2 Determination Measure 10.0 ml of the sample filtered by the quantitative filter paper in a stoppered colorimetric tube, and measure the absorbance according to the same procedure as in 7.1.3. Or a sample of 10.0 ml of diethyl ether extracted in a plug-type colorimetric tube, measured in accordance with the same procedure as in 7.1.2 and 7.1.3. Absorbance. Note. When the water sample is colorless and turbid, measure 10.0 ml of the sample in a stoppered colorimetric tube and measure the absorbance according to the same procedure as in 7.1.3. 7.3 Blank test The blank sample to be tested (6.3) was measured for absorbance according to the same procedure as in 7.2.

8 Calculation and representation of results

8.1 Calculation of results The mass concentration ρ of the TNT in the sample is calculated according to formula (1). 0m m ρ −= (1) Where. ρ--the mass concentration of TNT in the sample, mg/L; M--the TNT content of the sample obtained on the calibration curve, μg; M0--the TNT content of the blank sample found on the calibration curve, μg; V--sample volume, ml. 8.2 Representation of results When the measurement result is less than 1 mg/L, the two decimal places are retained, and when the measurement result is greater than or equal to 1 mg/L, the three significant numbers are retained. word.

9 Precision and accuracy

In the laboratory, six parallel determinations were made on the actual samples with TNT mass concentrations of 4.80 mg/L and 10.00 mg/L. The standard deviations were 1.10% and 0.65%, respectively, and the spiked recovery was 95.9% to 102%. Five laboratories measured and spiked the uniform samples with a TNT mass concentration of 2.00 mg/L. The standard deviation was 2.6%, and the spiked recovery was 95% to 110%. 10 Quality Assurance and Quality Control 10.1 At least one full program blank test shall be performed for each batch of samples, and the measured value shall not exceed the method detection limit. 10.2 The correlation coefficient of the calibration curve should be greater than or equal to 0.999. 10.3 Each batch of sample analysis shall have an intermediate checkpoint, and the relative deviation of the measured value from the corresponding point of the calibration curve shall not exceed 10%. 10.4 At least 10% of parallel samples should be determined for each batch of samples, and at least one parallel sample should be determined for less than 10 samples. The deviation should be less than 20%. 10.5 Each batch of samples should be tested by at least one spiked recovery analysis, and the actual sample spike recovery should be controlled at 90% to 110%. 11 Waste treatment The waste liquid generated during the test analysis and the remaining actual samples should be collected and disposed of properly. 12 Precautions 12.1 Ether should be stored at low temperature and protected from light. When a milky white precipitate appears when an appropriate amount of sodium sulfite solution (4.7) is added, the new ether should be replaced. 12.2 If there are more petroleum products in the water sample, it can be measured by filtering with double-layer quantitative filter paper.
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