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HJ 849-2017 English PDFUS$229.00 · In stock
Delivery: <= 3 days. True-PDF full-copy in English will be manually translated and delivered via email. HJ 849-2017: Water quality - Determination of ethylenethiourea - High performance liquid chromatography Status: Valid
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HJ 849-2017: Water quality - Determination of ethylenethiourea - High performance liquid 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 ethyl thiourea - Liquid chromatographic method) National Environmental Protection Standard of the People 's Republic of China Water quality - Determination of ethyl thiourea - Liquid chromatographic method Water quality - Determination of ethylenethiourea - High performance liquid chromatography 2017-08-28 released 2017-11-01 implementation Issued by the Ministry of Environmental Protection i directory Preface ..ii 1 Scope of application2 normative reference documents3 Principle of the method4 interference and elimination5 reagents and materials 1 Equipment and equipment 7 Sample 28 Analysis stepsThe results are calculated and expressed 10 Precision and Accuracy Quality assurance and quality control 12 Waste treatmentForewordIn 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 the Prevention and Control of Water Pollution, Barrier to human health, regulate the determination of water thiodide in water method, the development of this standard. This standard specifies the liquid chromatography for the determination of ethylene thiourea in water. This standard is the first release. This standard is organized by the Environmental Monitoring Department of the Ministry of Environmental Protection and the Department of Science and Technology Standards. The main drafting unit of this standard. Qingdao Environmental Monitoring Center Station and China Ocean University. The main verification unit of this standard. Ministry of Agriculture, Agricultural Product Quality Supervision, Inspection and Testing Center (Qingdao), Shandong Province Environmental Monitoring Central Station, Jinan City Environmental Monitoring Center Station, Tai'an City Environmental Protection Monitoring Station, Liaoning North Environmental Testing Technology Co., Ltd. and Green Island One Monitoring Co., Ltd. The environmental protection department of this standard approved on August 28,.2017. This standard has been implemented since November 1,.2017. This standard is explained by the Ministry of Environmental Protection. Determination of water quality of ethyl thiourea by liquid chromatography Warning. Ethylene thiourea is a carcinogen, the standard solution should be prepared in the operation of the fume hood, the operation should be required Wear protective equipment to avoid contact with skin and clothing.1 Scope of applicationThis standard specifies the liquid chromatography for the determination of ethylene thiourea in water. This standard is applicable to the determination of ethylene thiourea in surface water, groundwater, domestic sewage and industrial waste water. When the injection volume was 20 μl, the detection limit was 3 μg/L and the lower limit was 12 μg/L.2 normative reference documentsThe contents of this standard refer to the following documents or their terms. Those who do not specify the date of the reference file, the effective version of the appropriate For this standard. Technical specification for surface water and wastewater monitoring Technical specification for groundwater environmental monitoring3 Principle of the methodThe aqueous thiourea in water was injected directly by liquid chromatography with an ultraviolet detector. According to the retention time Qualitative and external standard method.4 interference and eliminationWhen the organic matter in the water sample interferes with the determination of ethylene thiourea, by changing the chromatographic conditions, so that the thiodide thiourea and dry Disassociation, or the water sample first with n-hexane extraction to remove part of the interference, take the water phase for analysis.5 reagents and materialsThe experimental water is pure water containing no organic matter. 5.1 methanol (CH3OH). liquid chromatography pure. 5.2 Ethylene thiourea. purity ≥ 98.5%. 5.3 Ethylene thiourea standard stock solution. ρ = 100 μg/ml. Weigh 0.010 g (accurate to 0.1 mg) ethylene thiourea (5.2), dissolved in water to 100 ml, frozen at 4 ° C, Dark and sealed can be kept for 3 months, or direct purchase of certified standard solution. 5.4 Ethylene thiourea standard use of liquid. ρ = 10.0 μg/ml. Accurately remove 1.00 ml of ethyl thiourea standard stock solution (5.3) and dilute to 10 ml with water.6 instruments and equipment6.1 Sampling vials. 100 ml brown glass jar with a mouth plug. 6.2 Liquid Chromatograph. with UV detector or diode array detector. 26.3 Column. Reagent column with 5 μm ODS, 25 cm in length and 4.6 mm in diameter, or other equivalent column. 6.4 Micro Samplers. 10 μl, 50 μl and 100 μl. 6.5 Filtration. 0.22 μm nylon filter or acetate filter. 6.6 Common laboratory equipment and equipment.7 samples7.1 Sample collection and storage Samples were collected according to the relevant regulations of HJ/T 91 and HJ/T 164. The collected water samples should be refrigerated at 4 ° C, protected from light and sealed Save, within 30 d analysis is completed. 7.2 Sample preparation The water sample was filtered through a 0.22 μm filter (6.5) and placed in a vial and tested. Note. For samples containing organic matter, take 10 ml of water samples, with 2 ml of n-hexane extraction, take the water phase for determination. 7.3 blank sample preparation The sample was prepared in the same manner as in Sample Preparation Step (7.2).8 Analysis steps8.1 Chromatographic reference conditions Mobile phase A. methanol; mobile phase B. water; flow rate. 0.8 ml/min; column temperature. 30 ℃; detection wavelength. 233 nm; Injection volume. 20 μl. The elution procedure is shown in Table 1. Table 1 elution program Time (min) A (%) B (%) Note. After 6 minutes elution, the cleaning column can be used to clean the column. The cleaning time can be adjusted according to the complexity of the actual sample. 8.2 Calibration curve establishment Respectively, take appropriate amount of thiodide standard use of liquid (5.4), diluted with water, the preparation of at least five concentrations of the standard series, The concentration of ethylene thiourea was 10.0, 50.0, 250, 500, 1000 μg/L (reference concentration). From low concentration to High concentration followed by the standard series of solution injection to the concentration of ethylene thiourea as the abscissa, the corresponding peak area or peak height Calculate the calibration curve. 8.3 Determination The sample to be tested (7.2) was subjected to the same conditions as the calibration curve. 38.4 blank test The blank sample to be measured (7.3) was measured under the same conditions as the sample.9 Results calculation and representation9.1 Qualitative analysis According to the samples in the ethylene thiourea and standard series of ethylene thiourea retention time for qualitative, if necessary, the standard sample Product addition method, absorption ratio at different wavelengths or scanning ultraviolet absorption spectroscopy and other methods to assist qualitative. Figure 1 shows the chromatograms of the thiourea thiourea under the chromatographic conditions recommended in this standard (8.1). Figure 1 Standard phase chromatogram of ethylene thiourea 9.2 Quantitative analysis The concentration of ethylene thiourea in water samples is calculated according to the following formula. A a (1) Where. - mass concentration of ethylene thiourea in water sample, μg/L; A - the peak area or peak height of ethylene thiourea; a - the intercept of the calibration curve; b - the slope of the calibration curve; f - the dilution factor of the water sample. 9.3 The result is shown When the determination result is greater than or equal to 100 μg/L, the data retained three significant digits; when the determination result is less than 100 μg/L, Reserved to integer bits. 10 precision and accuracy 10.1 precision Six laboratories were tested for white water thiazide with a concentration of 10.0 μg/L, 100 μg/L and 800 μg/L. The relative standard deviations in the laboratory were 3.0% ~ 9.0%, 0.8% ~ 3.1%, 0.3% ~ 1.1% respectively. The relative standard deviations were. 8.0%, 5.8%, 3.1%, and the repeatability r was 2 μg/L, 6 μg/L and 17 μg/L, respectively. The current limit R is. 3 μg/L, 18 μg/L, 72 μg/L. Six laboratories were tested for surface water spiked with thiodide concentrations of 5.0 μg/L, 10.0 μg/L and 50.0 μg/L for 6 The relative standard deviations in the laboratory were 2.0% ~ 7.5%, 2.7% ~ 9.0%, 0.6% ~ 4.8% respectively. The relative standard deviations were 8.4%, 10% and 4.6%, respectively. The repeatability r was 1 μg/L, 2 μg/L and 4 μg/L respectively. The limit R is. 1 μg/L, 3 μg/L, 8 μg/L. 6 laboratories were tested for samples of domesticated sulfur thiourea concentrations of 10.0 μg/L, 50.0 μg/L and 300 μg/L 6 times repeated determination. the relative standard deviation in the laboratory were. 4.0% ~ 9.4%, 0.4% ~ 3.8%, 0.4% ~ 4.1%; real The relative standard deviations were 12%, 9.5% and 12%, respectively. The repeatability r was 2 μg/L, 3 μg/L and 19 μg/L, respectively. Reproducibility R was. 4 μg/L, 13 μg/L, 107 μg/L. The concentration of thiourea in the two laboratories was 42 μg/L to 77 μg/L, 241 μg/L to 355 μg/L, 371 μg/L to 589 μg/L industrial wastewater samples were subjected to six repeated measurements. the relative standard devia...... |