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Delivery: <= 3 days. True-PDF full-copy in English will be manually translated and delivered via email. HJ 674-2013: Water quality. Determination of hydrazine and monomethyl hydrazine by p-Dimethylaminobenzaldehyde spectrophotometric method Status: Valid
Basic dataStandard ID: HJ 674-2013 (HJ674-2013)Description (Translated English): Water quality. Determination of hydrazine and monomethyl hydrazine by p-Dimethylaminobenzaldehyde spectrophotometric method Sector / Industry: Environmental Protection Industry Standard Classification of Chinese Standard: Z16 Classification of International Standard: 13.060 Word Count Estimation: 13,18 Older Standard (superseded by this standard): GB/T 15507-1995; GB/T 14375-1993 Quoted Standard: GB/T 14376 Regulation (derived from): Department of Environmental Protection Notice No. 70 of 2013 Issuing agency(ies): Ministry of Ecology and Environment Summary: This standard specifies the Determination of hydrazine and monomethyl hydrazine dimethylaminobenzaldehyde spectrophotometry. This standard is divided into two parts: the first part is the spectrophotometric determination of hydrazine on dimethylaminobenza HJ 674-2013: Water quality. Determination of hydrazine and monomethyl hydrazine by p-Dimethylaminobenzaldehyde spectrophotometric method---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 hydrazine and monomethyl hydrazine by p-Dimethylaminobenzaldehyde spectrophotometric method National Environmental Protection Standard of the People's Republic Replace GB/T 15507-1995, GB/T 14375-1993 Water quality and determination of methylhydrazine - Dimethylaminobenzaldehyde Water quality-Determination of hydrazine and monomethyl hydrazine by p-Dimethylaminobenzaldehyde spectrophotometric method Released on.2013-11-21 2014-02-01 implementation Release Ministry table of ContentsPreface II The first part of the determination of 肼 1 1 Scope 1 2 Principle of the method 1 3 interference and elimination 1 4 reagents and materials 1 5 Instruments and equipment 2 6 samples. 2 7 Analysis step 2 8 result calculation 3 9 Precision and accuracy 4 10 Quality Assurance and Control 4 11 Waste Disposal 4 The second part of the determination of methyl hydrazine 4 1 Scope .4 2 Reference Standard 5 3 Principle of the method 5 4 interference and elimination..5 5 reagents and materials..5 6 Instruments and equipment 6 7 samples.6 8 Analysis steps..6 9 result calculation 7 10 precision and accuracy..7 11 Quality Assurance and Quality Control..8 12 Waste disposal 8ForewordTo 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, to protect the environment, To ensure human health, standardize the monitoring and analysis methods for strontium and methyl hydrazine in water, and develop this standard. This standard specifies the p-dimethylaminobenzaldehyde spectrophotometric method for the determination of hydrazine and methylhydrazine in water. This standard applies to the determination of bismuth and methyl hydrazine in surface water, groundwater, domestic wastewater and industrial wastewater. This standard is for the determination of water quality 对 dimethylaminobenzaldehyde spectrophotometry (GB/T 15507-1995) and "water Determination of quinone monomethyl hydrazine, revision of dimethylaminobenzaldehyde spectrophotometry (GB/T 14375-1993), original standard for the first time Published in.1995 and.1993. The main drafting units of the original standard are respectively, GB/T 15507-1995. Dandong City, Liaoning Province Bao Institute, the 7th Design and Research Institute of the former Aerospace Department, Xi'an Qinghua Electrical Appliance Factory of the former Ministry of Weapons Industry; GB/T 14375-1993. The Seventh Design and Research Institute of the former Aerospace Department. This standard is divided into two parts. the first part is the determination of hydrazine by p-dimethylaminobenzaldehyde spectrophotometry; the second part is the second part Methylaminobenzaldehyde spectrophotometric determination of methyl hydrazine. This standard is the first revision, the main revisions are as follows. Divided into the determination of bismuth, the second part is the determination of methyl hydrazine; - Modification of the method for eliminating nitrite interference by substituting p-diaminosulfonic acid for sodium azide; -- Revised the editorial errors and formats that appeared in the original standard. From the date of implementation of this standard, "Determination of water quality 对 dimethylaminobenzaldehyde spectrophotometry" (GB/T 15507-1995) and "Determination of water-methyl hydrazine by p-dimethylaminobenzaldehyde spectrophotometry" (GB/T 14375-1993) Abolished. This standard is revised by the Science and Technology Standards Department of the State Environmental Protection Administration. The main revision unit of this standard. National Environmental Analysis and Testing Center, China Aerospace Science and Technology Group Sixth Institute 101 (China Airlines Day Liquid Propellant Research Center). The units that participate in the verification of this standard are. National Environmental Analysis and Testing Center, China Aerospace Liquid Propellant Research Center, North Beijing Municipal Environmental Protection Monitoring Center, Beijing Physical and Chemical Testing Center, Propellant Testing and Protection Center of the General Armament Department, Army of General Equipment Department Equipment research and ordering department anti-chemical metering station. This standard was approved by the Ministry of Environmental Protection on November 21,.2013. This standard has been implemented since February 1,.2014. This standard is explained by the Ministry of Environmental Protection. Water quality and determination of methylhydrazine - dimethylaminobenzaldehyde spectrophotometric method This standard specifies the p-dimethylaminobenzaldehyde spectrophotometric method for the determination of hydrazine and methylhydrazine in water. This standard is divided into two parts. The first part is spectrophotometric determination of hydrazine with p-dimethylaminobenzaldehyde, and the second part is p-dimethylaminobenzaldehyde spectrophotometry. The methyl hydrazine was measured. The first part of the determination of 肼1 Scope of applicationThis standard specifies the p-dimethylaminobenzaldehyde spectrophotometric method for the determination of hydrazine in water. This standard applies to the determination of bismuth in water and industrial wastewater. According to the water sample 50mL, using the 5cm absorption pool calculation, the detection limit of this method is 0.003 mg/L, the quantitative measurement The circumference is (0.012~0.240) mg/L. If a 1cm absorption cell is used, the detection limit is 0.015 mg/L, and the quantitative determination range is (0.060~1.00) mg/L. When the concentration of strontium in the water sample is greater than 1.00 mg/L, it can be determined after dilution.2 Principle of the methodUnder acidic conditions, hydrazine reacts with p-dimethylbenzaldehyde to form p-dimethylaminobenzyl nitrogen yellow compound. in The absorbance is measured at a wavelength of 458 nm, and its absorbance is proportional to the content of germanium in a certain concentration range.3 interference and eliminationInterference determination of semicarbazide, thiourea and urea at 20 mg/L, 50 mg/L and.200 mg/L respectively; methyl hydrazine is strontium content There is interference when 3 times. When the water sample contains chromium, add 2mL HCl (4.2) to 10mL water sample, add 0.4mL 1% potassium iodide, shake Evenly, let stand for 10 minutes. When the NO2 ̄ in the water sample is greater than 1 mg/L, it will have negative interference with the determination. When the concentration of NO2 ̄ in the water sample is 1.0mg/L~4.5mg/L, Add 1.0 mL of ammonium sulfamate or sulfamic acid solution (4.5) to 10 mL of water and shake well to complete the reaction. To eliminate interference. For different NO2 concentration, adjust the amount of sulfamic acid added in the above ratio.4 reagents and materialsThe reagents used in this standard are analyzed using analytical analytical reagents in accordance with national standards, unless otherwise stated. The water is freshly prepared deionized or distilled water. 4.1 Hydrochloric acid (HCl). ρ = 1.19 g/mL. 4.2 Hydrochloric acid solution. c (HCl) = 0.12 mol/L. Take 250mL beaker, add.200 water, hydrochloric acid (4.1) 5.0mL, stir evenly, transfer to 500mL volumetric flask, use water Dilute to the mark and shake well. Transfer to a 500mL reagent bottle for later use. 4.3 Ethanol (95%). 4.4 p-Dimethylaminobenzaldehyde solution Weigh 4.0 g of p-dimethylaminobenzaldehyde in.200 mL of 95% ethanol and 20.0 mL of hydrochloric acid (4.1) and store in brown. Keep it in the bottle and protect it from light. 4.5 Ammonium sulfamate or sulfamic acid solution. ρ = 5.0 mg/mL. 0.50 g of ammonium sulfamate (NH4SO3NH2) or sulfamic acid (NH2SO3H) was weighed and dissolved in 100 mL of water. 4.6 肼 standard stock solution. ρ (N2H4) = 100 mg/L. Weigh 0.3280g of guanidine hydrochloride (N2H4·2HCl) or 0.4060g of barium sulfate (N2H4 H2SO4) in a beaker and add HCl to dissolve. Solution (4.1) 10.0mL was dissolved, quantitatively transferred into a 1000 mL volumetric flask, diluted with water to the mark line for use. Can also use the certificate Quasi sample. 4.7 肼 standard use solution. ρ (N2H4) = 1.00 mg/L. Pipette 10.0 mL of standard stock solution (4.6) into a 1000 mL volumetric flask, add HCl solution (4.1) 10.0 mL, and use water. Dilute to the mark.5 Instruments and equipmentUnless otherwise stated, the analysis used a Class A glass gauge in accordance with national standards. 5.1 Spectrophotometer. with 1 cm and 5 cm absorption cells. 5.2 with colorimetric tube. 50mL, 100mL. 5.3 Laboratory general instruments.6 samples6.1 Acquisition and preservation Glass bottles were used for sampling and storage of samples. After sampling, the water sample was immediately acid or alkali to neutral and measured within 24 hours. 6.2 Water sample pretreatment If the water sample (6.1) contains tiny solid particles, it can be filtered with a quick filter paper, and a few milliliters of water that has started to be filtered out is discarded. After the sample, the filtrate is ready for use or centrifuged. 6.3 Sample preparation Take 100mL colorimetric tube, add water sample to 50mL mark, add HCl solution (4.1) 1.0mL, dilute with water to 100mL Marking.7 Analysis steps7.1 Determination of radon in surface water and groundwater 7.1.1 Calibration Take 5 50mL plug colorimetric tubes and add 肼 standard solution (4.7), 0, 0.50, 1.00, 1.50, 2.00, 3.00 mL, Dilute to 50 mL mark with HCl solution (4.2), add 10.0 mL of p-dimethylaminobenzaldehyde solution, mix and let stand for 20 min. Using a 5 cm absorption cell at a wavelength of 458 nm with distilled water as a reference, measure the absorbance, and take the barium content as the abscissa, deduct the test. The absorbance of the blank standard solution is plotted on the ordinate and a calibration curve is drawn. Linear regression analysis method is used to determine the slope for the sample. Product content calculation. 7.1.2 Sample determination Take water sample (6.3) in a 50 mL dry plug colorimetric tube and carefully add water to the 50 mL mark. Add 10.0mL Mix p-dimethylaminobenzaldehyde solution (4.4). After 20 minutes, use a 5 cm absorption cell at 458 nm wavelength with distilled water as reference. Ratio, measure absorbance. 7.2 Determination of high concentration bismuth 7.2.1 Calibration Take 5 50mL plug color tubes and add 肼 standard solution (4.7), 0, 2.00, 4.00, 6.00, 8.00, 10.0 mL, Dilute to 25 mL with HCl solution (4.2), add 5.0 mL of p-dimethylaminobenzaldehyde solution, mix and let stand for 20 min. Using a 1 cm absorption cell at a wavelength of 458 nm with distilled water as a reference, measuring the absorbance, taking the yttrium content as the abscissa, deducting the test The absorbance of the blank standard solution is plotted on the ordinate and a calibration curve is drawn. Linear regression analysis method is used to determine the slope for the sample. Product content calculation. 7.2.2 Sample determination Take water sample (6.3) in a 25mL dry colorimetric tube and carefully add to the 25mL mark (if industrial wastewater The concentration is higher, you can take water sample (6.3) 1.0mL, 5.0mL or 10.0mL as needed, then dilute with HCl solution (4.2) Up to 25mL mark). Add 5.0 mL of p-dimethylaminobenzaldehyde solution (4.4) and mix. Use a 1 cm absorption tank after 20 minutes The absorbance was measured at 458 nm using distilled water as a reference.8 Calculation of results8.1 Calculation of results The 肼 content ρ (mg/L) in the sample is calculated as follows. ρ = Vb AAk × −× )( 0 Where. A - absorbance of the sample solution; A0 - reagent blank liquid absorbance; b -- the slope of the calibration curve obtained by linear regression analysis; V -- Analyze the sample volume (for example, surface water, ground water is 50mL, industrial wastewater is the actual sample body) Product, such as 1.0, 5.0, 10.0 or 25.0mL); k -- dilution factor (where k=2). If the measurement result is in hydration enthalpy, multiply the result by 1.56. Because 1.56 parts of N2H4·H2O contains 1 part of N2H4. 8.2 Results representation When the result is greater than or equal to 0.100 mg/L, the calculation results take 3 significant figures; when the result is less than 0.100 mg/L, Leave to the third digit after the decimal point.9 Precision and accuracy9.1 precision Six laboratories measured the uniform water samples with a concentration of 0.021 mg/L, 0.152 mg/L, and 0.392 mg/L. The relative standard deviations in the laboratory are 0.5-6.1 (%), 0.6-5.7 (%), 0.3-2.5 (%); the relative standard between laboratories The deviations were 13.1%, 7.0%, and 5.0%, respectively. The repeatability limits were 0.0019 mg/L, 0.011 mg/L, and 0.017 mg/L, respectively. Reproduce The sexual limits were 0.0078 mg/L, 0.031 mg/L, and 0.057 mg/L, respectively. 9.2 Accuracy Six laboratories added 0.020 mg/L and 0.10 mg/L to surface water and 0.10 mg/L and 0.40 mg/L for industrial wastewater. The four samples were measured separately, and the recoveries (%) of the spiked results ranged from 96.9 to 102.2; 98.6 to 103.0; 95.5 ~ 101.6; 98.1 ~ 103.7. The recoveries were 101.2 ± 8.6; 100.2 ± 3.0; 98.7 ± 4.4; 103.0 ± 4.4. 10 Quality Assurance and Control 10.1 The standard addition method can be used to compare the results of the standard working curve method to determine whether matrix interference exists in the sample. The relative deviation between the two results is within 10%, and the matrix interference is negligible. If it is greater than 10%, it can be judged that the base exists in the sample. Body interference. In the same way, the calibration curve method was used to prepare and process the sample, and ammonium sulfamate was added to eliminate the interference. 10.2 There should be one full procedural blank for each batch (≤10) of samples analyzed. 10.3 Each batch (≤10) of samples must have a blank spike and the recovery rate is between 90% and 110%. 10.4 There should be one parallel sample for each batch (≤10) of samples analyzed. When the quantity is large, the number of parallel samples should be selected in proportion to 10%. The relative deviation of the parallel sample results should be less than 10%. 10.5 The correlation coefficient of the calibration curve regression equation developed each time should be greater than 0.999. 11 Waste disposal The waste liquid generated in the experiment should be collected regularly and safely treated according to laboratory waste. Entrust qualified units when necessary Dispose of. The second part of the determination of methyl hydrazine1 ScopeThis standard specifies the p-dimethylaminobenzaldehyde spectrophotometric method for the determination of methylhydrazine in water. This standard applies to the determination of methyl hydrazine in water and industrial wastewater. Calculated according to the use of 2cm absorption tank and 15 mL of surface water. The detection limit of methyl hydrazine is 0.015 mg/L. It is (0.060~1.50) mg/L. When the methyl hydrazine content in the water sample is greater than 1.50 mg/L, it can be determined after dilution.2 Reference standardThe contents of this standard refer to the following documents. For undated references, the valid version applies to this standard. GB/T 14376 Determination of dimethyl hydrazine in water - Amino ferrocyanide spectrophotometric method3 Principle of the methodUnder acidic conditions, methyl hydrazine reacts with p-dimethylaminobenzaldehyde to form a yellow condensate, which is measured at a wavelength of 470 nm. The amount of absorbance. The absorbance is proportional to the content of methyl hydrazine in a certain concentration range.4 interference and elimination肼 Interfering with the determination of methyl hydrazine. When the content of dimethyl hydrazine is higher than that of methyl hydrazine, it can be corrected by a calibration curve.5 reagents and materialsThe reagents used in this standard are analyzed using analytical analytical reagents in accordance with national standards, unless otherwise stated. The water is freshly prepared deionized or distilled water. 5.1 Sulfuric acid. ρ = 1.84 g/mL. 5.2 Ethanol. 95% or more. 5.3 Methyl hydrazine (CH3NHNH2). purity 98% or more. 5.4 Sulfuric acid solution. c(H2SO4) = 1.0 mol/L. Add 50 mL of water to a 500 mL beaker, slowly inject 27.8 mL of sulfuric acid (5.1), and transfer to a 500 mL capacity after stirring. Dilute the bottle to the mark with water and shake well. Transfer to a 500mL reagent bottle for later use. 5.5 Sulfuric acid solution. c(H2SO4) = 0.050 mol/L. Add 100 mL of water to a 1000 mL beaker, slowly inject 50 mL of sulfuric acid (5.4), and mix to transfer to 1000 mL capacity. Dilute the bottle to the mark with water and shake well. Transfer to a 1000mL reagent bottle for later use. 5.6 p-Dimethylaminobenzaldehyde solution. Weigh p-dimethylaminobenzaldehyde [(CH3)2NC6H4CHO] 5.0g, add 20mL sulfuric acid Solution (5.4), mix and add 100 mL of ethanol (5.2) to dissolve. 5.7 Ammonium sulfamate or sulfamic acid solution. ρ = 10 g/L. 1.0 g of ammonium sulfamate (NH4SO3NH2) or sulfamic acid (NH2SO3H) was weighed and dissolved in 100 mL of water. 5.8 methyl hydrazine standard stock solution. ρ = 10.0 mg/mL. Pipette 5 mL~10 mL sulfuric acid solution (4.4) into a 25 mL volumetric flask. The volumetric flask was weighed and weighed to 0.0001 g. Pipette approximately 0.25 mL to 0.30 mL of methyl hydrazine (4.3), pipette into the volumetric flask, and gently shake the bottle. Weighed again, weighed to 0.0001 g, and the amount of methyl hydrazine (4.3) added was 0.2500 g. Dilute to the mark with sulfuric acid solution (4.4). Or calculate the standard stock concentration based on the actual amount of methyl hydrazine (0.245~0.255) g added. 5.9 methyl hydrazine standard intermediate solution. ρ =.200 mg/L. Pipette 2.0 mL of methyl hydrazine stock solution (5.8), transfer to a 100 mL volumetric flask, and dilute to the mark with sulfuric acid solution (4.5). Store at 2 ° C ~ 5 ° C. 5.10 Standard solution for methylhydrazine. ρ=2.00 mg/L. Pipette 5.00mL of methyl hydrazine solution (5.9), transfer it to a 500mL volumetric flask, dilute to the mark with sulfuric acid solution (5.5), and mix. Prepared on the same day before use.6 Instruments and equipment6.1 Spectrophotometer. with 2 cm absorption cell. 6.2 General laboratory equipment. 6.2.1 Colorimetric tube. 25 mL, 100 mL. 6.2.2 Volumetric flask. 25mL, 100mL, 500mL.7 samples7.1 Acquisition and preservation Glass bottles were used for sampling and storage of samples. After sampling, the water sample was immediately acid or alkali to neutral and measured within 24 hours. 7.2 Water sample pretreatment If the water sample (7.1) contains tiny solid particles, it can be filtered with a quick filter paper, and a few milliliters of water that has started to be filtered out is discarded. After the sample, the filtrate is ready for use or centrifuged. 7.3 Sample preparation 7.3.1 Industrial wastewater. Take a 100 mL dry colorimetric tube and add the pretreated water sample (7.2) to the vicinity of the 50 mL mark. Carefully ad......Tips & Frequently Asked Questions:Question 1: How long will the true-PDF of HJ 674-2013_English be delivered?Answer: Upon your order, we will start to translate HJ 674-2013_English as soon as possible, and keep you informed of the progress. The lead time is typically 1 ~ 3 working days. 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