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HJ 598-2011 English PDF

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HJ 598-2011: Water quality. Determination of TNT. Sodium sulfite spectrophotometric method
Status: Valid
Standard IDUSDBUY PDFLead-DaysStandard Title (Description)Status
HJ 598-2011209 Add to Cart 3 days Water quality. Determination of TNT. Sodium sulfite spectrophotometric method Valid

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Basic data

Standard ID: HJ 598-2011 (HJ598-2011)
Description (Translated English): Water quality. Determination of TNT. Sodium sulfite spectrophotometric method
Sector / Industry: Environmental Protection Industry Standard
Classification of Chinese Standard: Z16
Classification of International Standard: 13.060
Word Count Estimation: 8,898
Date of Issue: 2011-02-10
Date of Implementation: 2011-06-01
Older Standard (superseded by this standard): GB/T 13905-1992
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 sodium sulfite TNT spectrophotometry. This standard applies to the production and use of powdered ammonium nitrate explosive discharge of industrial process wastewater Determination of TNT. When the sample volume was 10. 0ml, using 30mm cuvette, the method detection limit of 0. 1mg/L, determination range of 0. 4 ~ 10mg/L. TNT measured concentration is higher than the upper limit of the sample may be measured after appropriate dilution.

HJ 598-2011: Water quality. Determination of TNT. Sodium sulfite spectrophotometric method

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Water quality.Determination of TNT.Sodium sulfite spectrophotometric method National Environmental Protection Standard of the People's Republic Replace GB/T 13905-92 Determination of water quality ladder Sodium sulfite spectrophotometry Water quality-Determination of TNT -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); 3. Determination of water quality ladders N-chlorohexadecylpyridine-sodium sulfite spectrophotometry (HJ 599-2011); 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 3 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 sodium sulfite spectrophotometric method for the determination of TNT in water. This standard is a revision of the "Sodium Sulfite Spectrophotometric Method for the Determination of Water Quality TNT" (GB/T 13905-92). This standard was first published in.1992. The original standard drafting unit was the Fifth Design and Research Institute of China Ordnance Industry. This is the first revision. The main revisions are as follows. - increased interference and elimination clauses; -- Increased preparation of the sample; -- Added quality assurance and quality control regulations; -- Added waste disposal provisions. 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. Determination of TNT's Sodium Sulfite Spectrophotometry (GB/T 13905-92) was 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. Water quality - Determination of TNT - Sodium sulfite spectrophotometric method

1 Scope of application

This standard specifies the sodium sulfite spectrophotometric method for the determination of TNT in water. This standard is applicable to the determination of TNT in industrial wastewater discharged during the production and use of powdered ammonium ladder explosives. When the sample volume is 10.0 ml and the 30 mm cuvette is used, the detection limit is 0.1 mg/L and the measurement range is 0.4-10 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

At room temperature, the TNT in the sample reacts with anhydrous sodium sulfite to form yellow trinitrotoluenesulfonate, which is measured at a wavelength of 420 nm. The amount of absorbance. Within a certain concentration range, the TNT concentration and absorbance values are in accordance with Lambert-Beer law.

3 interference and elimination

3.1 When the wastewater has a certain color, it will interfere with the measurement. It is advisable to dilute the water sample of the same volume as the sample to 25 ml as a sample blank. The absorbance was measured directly without the addition of sodium sulfite solution. The absorbance of the sample blank is subtracted from the absorbance of the sample, and then calculated to eliminate the color The effect of degree on the determination. 3.2 When the hardness of the sample is greater than 600 mg/L, it will interfere with the measurement results. Add 1.0 ml of ethylenediamine tetraacetate to 10.0 ml of sample The acid disodium salt solution (4.3) and 1-3 drops of sodium hydroxide solution (4.4) are used to make the pH of the water sample in the range of 10-11. Amount of reagent added Should be included in the calculation of the results.

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 sulfuric acid. ρ(H2SO4) = 1.84 g/ml. 4.2 Anhydrous ethanol (C2H5OH). 4.3 EDTA-2Na solution. ρ(C10H14N2Na2O8·2H2O)=0.1 g/ml. Weigh 10 g of disodium edetate dissolved in 100 ml of water and shake well. 4.4 Sodium hydroxide solution. ρ (NaOH) = 0.2 g/ml. Weigh 20 g of sodium hydroxide in 100 ml of water and shake well. 4.5 Aluminum sulfate solution. ρ[Al2(SO4)3] = 0.18 g/ml. Weigh 18 g of aluminum sulfate dissolved in 100 ml of water and mix. 4.6 Sodium carbonate solution. ρ(Na2CO3) = 0.16 g/ml. Weigh 16 g of sodium carbonate dissolved in 100 ml of water and mix. 4.7 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 (4.2), and filter with medium-speed quantitative filter paper. Place the filtrate in a fume hood and allow it to dry naturally. Recrystallization twice, spare. 4.8 TNT standard solution. ρ (TNT) = 50.0 mg/L. Accurately weigh 0.050 g of TNT (4.7) dissolved in 3 ml of concentrated sulfuric acid (4.1), slowly add water to dissolve, and then transfer to a 1 000 ml volumetric flask. In the middle, add water to the marking line and mix. 4.9 Anhydrous sodium sulfite solution. ρ(Na2SO3) = 0.2 g/ml. Weigh 20.0 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.

5 Instruments and equipment

5.1 Visible spectrophotometer. with 30 mm cuvette. 5.2 Plug scale colorimetric tube. 25 ml. 5.3 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 Measure 100 ml of water in an Erlenmeyer flask, add 0.5 ml of aluminum sulfate solution (4.5), and add 0.5 ml of sodium carbonate solution (4.6). After taking the supernatant, take the supernatant and test it. 6.3 Preparation of blank samples The sample was replaced with experimental water, and a blank sample was prepared in the same manner as in the preparation of the sample (6.2).

7 Analysis steps

7.1 Calibration 7.1.1 Measure 0.00, 0.50, 1.00, 1.50, 2.00, 2.50, 3.00 ml TNT standard solution (4.8) placed in 7 pieces respectively In the colorimetric tube, water was added to a 10 ml engraved line, and the TNT contents were 0.00, 25.0, 50.0, 75.0, 100, 125, and 150 μg, respectively. 7.1.2 Add 5 ml of anhydrous sodium sulfite solution (4.9) to the above-mentioned stoppered colorimetric tube, dilute to 25 ml with water, and shake. Evenly, color development for 5 min. The absorbance was measured with a 30 mm cuvette at a wavelength of 420 nm using water as a reference. Taking the absorbance as the ordinate, A calibration curve is drawn with the corresponding TNT content (μg) as the abscissa. 7.2 Determination Take 10.0 ml of the sample (6.2) in a stoppered colorimetric tube and measure the absorbance according to the same procedure as in 7.1.2. 7.3 Blank test Measure 10.0 ml blank sample (6.3) in a stoppered colorimetric tube and analyze according to the same procedure as in measurement (7.2). Absorbance.

8 Calculation and representation of results

8.1 Calculation of results The mass concentration ρ (mg/L) of the TNT in the sample is calculated according to formula (1). 0m mf 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--10 ml, sample volume; F--dilution ratio. 8.2 Results representation 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

Six times of the actual samples with TNT mass concentrations of 2.46 mg/L, 4.65 mg/L, 6.18 mg/L and 9.99 mg/L were applied. The relative standard deviations were 1.83%, 1.70%, 1.15%, and 0.64%, respectively. When the spiked amount was 20 μg, the spiked recovery was 94.4% to 102.4%. 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 and waste water generated during the test should be collected and disposed of properly.
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