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Basic dataStandard ID: HJ 1047-2019 (HJ1047-2019)Description (Translated English): Water quality - Determination of antimony - Graphite furnace atomic absorption spectrometry Sector / Industry: Environmental Protection Industry Standard Classification of Chinese Standard: Z16 Classification of International Standard: 13.060 Word Count Estimation: 13,140 Date of Issue: 2019 Date of Implementation: 2020-04-24 Issuing agency(ies): Ministry of Ecology and Environment HJ 1047-2019: Water quality - Determination of antimony - Graphite furnace atomic absorption spectrometry---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 antimony--Graphite furnace atomic absorption spectrophotometry) National Environmental Protection Standard of the People's Republic of China Determination of water quality antimony Graphite furnace atomic absorption spectrophotometry Water quality-Determination of antimony -Graphite furnace atomic absorption spectrometry 2019-10-24 released 2020-04-24 Implementation Released by the Ministry of Ecology and Environment ContentsForeword ... ii 1 Scope ... 1 2 Normative references ... 1 3 Terms and definitions ... 1 4 Methodology ... 1 5 Interference and cancellation ... 1 6 Reagents and materials ... 2 7 Instruments and equipment ... 2 8 Sample ... 3 9 Analysis steps ... 4 10 Calculation and Representation of Results ... 5 11 Precision and accuracy ... 5 12 Quality Assurance and Quality Control ... 6 13 Waste disposal ... 6 Appendix A (Normative Appendix) Matrix interference inspection methods ... 7 Appendix B (Normative) Standard Addition Method ... 8 Appendix C (Informative) Judgment on the Applicability of Standard Additions ... 9ForewordIn 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 Control", protect the ecology Environment, protect human health, standardize the determination method of antimony in water, and formulate this standard. This standard specifies graphite furnace raw materials for the determination of antimony in domestic sewage, industrial wastewater, certain contaminated surface water and groundwater Atomic absorption spectrophotometry. Appendix A and Appendix B of this standard are normative appendixes, and Appendix C is an informative appendix. This standard is issued for the first time. This standard is formulated by the Department of Eco-Environmental Monitoring, Laws and Standards Department of the Ministry of Ecology and Environment. This standard was drafted. Shanghai Pudong New Area Environmental Monitoring Station. Verification units of this standard. Shanghai Environmental Monitoring Center, Shanghai Minhang District Environmental Monitoring Station, Baoshan District, Shanghai Monitoring Station, Shanghai Jiading District Environmental Monitoring Station, Shanghai Qingpu District Environmental Monitoring Station, and Shanghai Huatest Label Testing Technology Limited the company. This standard was approved by the Ministry of Ecology and Environment on October 24,.2019. This standard will be implemented from April 24, 2020. This standard is explained by the Ministry of Ecology and Environment. Water quality-Determination of antimony-Graphite furnace atomic absorption spectrophotometry Warning. The antimony and its compounds used in the experiment are more toxic, hydrochloric acid is highly corrosive and volatile, and nitric acid is Strongly corrosive and oxidizing, reagent preparation and sample preparation should be carried out in a fume hood, and should be worn as required during operation Protective equipment to avoid contact with skin and clothing.1 ScopeThis standard specifies the graphite furnace atomic absorption spectrophotometry for the determination of antimony in water. This standard is applicable to the determination of antimony in domestic sewage, industrial wastewater, certain contaminated surface water and groundwater. When the injection volume is 20 μl, the detection limits of this standard for soluble antimony and total antimony are both 2 μg/L. The limits are all 8 μg/L.2 Normative referencesThis standard refers to the following documents or clauses therein. For undated references, the valid version applies to this standard. HJ/T 91 Technical specifications for surface water and sewage monitoring HJ/T 164 Technical Specifications for Groundwater Environmental Monitoring3 terms and definitionsThe following terms and definitions apply to this standard. 3.1 Soluble antimony Refers to antimony measured after a non-acidified sample is filtered through a 0.45 μm filter. 3.2 Total quantity of antimony Refers to antimony measured after acid filtration of an unfiltered sample.4 Method principleThe sample is filtered or digested and injected into a graphite furnace atomizer. The antimony element is dried, ashed, and atomized to form Selective atomic vapor of antimony in the ground state produces selectivity to the 217.6 nm characteristic line emitted by a light source (hollow cathode lamp or other light source) Absorption, within a certain range, its absorbance value is proportional to the mass concentration of antimony.5 Interference and cancellation5.1 When the mass concentrations of lead, zinc, cadmium, calcium, and aluminum are less than.200 mg/L,.200 mg/L, 250 mg/L, At 1000 mg/L and 1000 mg/L, it does not interfere with the determination of antimony. 5.2 When the mass concentration of nickel and iron is greater than 60 mg/L, 800 mg/L and SO4, respectively 2-, Cl- are greater than 160 mg/L, At 250 mg/L, it negatively interferes with the determination of antimony. Inspection of matrix interference is shown in Appendix A; it can be offset by standard addition method See Appendix B for interference; see Appendix C for applicability of the standard addition method.6 Reagents and materialsUnless otherwise specified, analytical reagents that meet national standards are used in the analysis, and the experimental water is newly prepared deionized water. Water or water of equivalent purity. 6.1 Hydrochloric acid. ρ (HCl) = 1.19 g/ml, excellent grade pure. 6.2 Nitric acid. ρ (HNO3) = 1.42 g/ml, excellent purity. 6.3 Palladium nitrate. 6.4 Magnesium nitrate. 6.5 Nitric acid solution. 1 + 1. 6.6 Nitric acid solution. 1 + 99. 6.7 Matrix modifier. ρ [Pd (NO3) 2] = 6.5 g/L, ρ [Mg (NO3) 2] = 2.0 g/L. Weigh 650 mg of palladium nitrate (6.3) into a beaker, add 1 ml of nitric acid (6.2) and 0.1 ml of hydrochloric acid (6.1) Dissolve, weigh.200 mg of magnesium nitrate (6.4), place in a beaker, add a small amount of water to dissolve, and mix the two reagents in one Transfer to a 100 ml volumetric flask, dilute with water to the mark, shake well, transfer to a polyethylene bottle, seal, and save 12 months. 6.8 Tartaric acid. w≥99.5%. 6.9 Metal antimony. spectrally pure, w≥99.99%. 6.10 Standard antimony stock solution. ρ (Sb) = 1000 mg/L. Accurately weigh 1.0 g (to the nearest 0.0001 g) metal antimony (6.9), place it in a beaker, and add 10 ml of hydrochloric acid (6.1) And 20 ml of nitric acid solution (6.5); add 100 ml of water and 1.5 g of tartaric acid (6.8) and warm to completely dissolve. cool down Then transfer it to a 1000 ml volumetric flask, dilute with water to the mark, shake well, transfer to a polyethylene bottle, and seal it. Months. Or use a commercially available certified antimony standard solution. 6.11 Standard antimony solution. ρ (Sb) = 100.0 mg/L. Accurately transfer 10.00 ml of standard antimony stock solution (6.10) into a 100 ml volumetric flask and dilute with a nitric acid solution (6.6) Make up to the mark, shake well, transfer to a polyethylene bottle and seal, and it can be stored for 6 months. 6.12 Standard antimony solution. ρ (Sb) = 10.0 mg/L. Accurately transfer 10.00 ml of standard antimony solution (6.11) into a 100 ml volumetric flask and dilute with a nitric acid solution (6.6) Set the volume to the mark, shake well, transfer to a polyethylene bottle and seal, and store it for half a month. 6.13 Carrier gas. Argon, purity ≥99.99%. 6.14 Filter. Acetate or PVC filter with a pore size of 0.45 µm.7 instruments and equipment7.1 Graphite furnace atomic absorption spectrophotometer. with background correction function. 7.2 Pyrolytic coated graphite tube. 7.3 Light source. Antimony hollow cathode lamp or other light source with 217.6 nm. 7.4 Microwave Digestion Apparatus. 7.5 Electric heating plate. The temperature control range is from room temperature to 300 ° C, and the temperature control accuracy is ± 5 ° C. 7.6 Sample vial. 500 ml, polyethylene or equivalent. 7.7 Instruments and equipment commonly used in general laboratories.8 samples8.1 Sample collection Collect samples in accordance with the relevant regulations of HJ/T 91 and HJ/T 164. Samples for the determination of soluble antimony and total antimony should be divided Don't collect. 8.2 Sample storage 8.2.1 Soluble antimony samples After the sample is collected, it should be filtered with a filter membrane (6.14) as soon as possible. The initial filtrate is discarded, and the required volume of filtrate is collected in a sample bottle. (7.6); 1 ml of nitric acid (6.2) is added to every 100 ml of the filtrate to acidify, and it is measured within 14 days. 8.2.2 Total antimony samples After sample collection, 1 ml of nitric acid (6.2) was added to every 100 ml sample to acidify it, and it was measured within 14 days. 8.3 Preparation of test specimens 8.3.1 Preparation of soluble antimony samples See 8.2.1. 8.3.2 Preparation of total antimony sample 8.3.2.1 Microwave Digestion Accurately measure 25.0 ml of the total antimony sample (8.2.2) in the digestion tank of the microwave digestion apparatus (7.4), add 2.0 ml Nitric acid (6.2) and 6.0 ml hydrochloric acid (6.1) (can reduce or increase the sampling volume and the amount of acid Product), microwave digestion at 170 ° C ± 5 ° C for 10 min. Digestion is complete, after cooling to room temperature, transfer to a 50 ml volumetric flask In water, dilute with water to the mark, shake well, and test. 8.3.2.2 Hot plate digestion method Accurately measure 25.0 ml of the total antimony sample (8.2.2) in a 250 ml Erlenmeyer flask and add 2.0 ml of nitric acid (6.2) And 6.0 ml hydrochloric acid (6.1) (can reduce or increase the sampling volume and the volume of the acid added in proportion to the actual needs), place Cover the watch glass or small funnel on the hot plate (7.5), keep it slightly boiling, and stop heating when the sample is uniform and clear, and wait for cooling After reaching room temperature, rinse the inner wall at least 3 times with appropriate amount of water, transfer to a 50 ml volumetric flask, dilute with water to the mark, and shake Uniform, to be tested. 8.4 Preparation of blank samples Use experimental water instead of the sample, and follow the same steps as the sample preparation (8.3) to prepare a laboratory blank sample Equipment.9 Analysis steps9.1 Reference measurement conditions The optimal working conditions of different models of instruments are different. You need to select the background correction and adjust the instrument to Best working condition. See Table 1 and Table 2 for reference measurement conditions. Table 1 Reference instrument measurement conditions Wavelength/nm Lamp current/mA Passband width/nm 217.6 10 0.2 Table 2 Reference heating program Temperature in heating phase/℃ time/s Drying 90 ～ 120 75 Ashing 1200 25 Atomic 1900 5 Clear 2100 3 9.2 Establishment of standard curve Pipette 0 ml, 0.05 ml, 0.10 ml, 0.20 ml, 0.40 ml, 0.50 ml, 0.75 ml of antimony standard use solution (6.12) respectively In a 50 ml volumetric flask, dilute to the mark with a nitric acid solution (6.6) and shake well. The mass concentration of this standard series are 0 μg/L, 10.0 μg/L, 20.0 μg/L, 40.0 μg/L, 80.0 μg/L, 100 μg/L, 150 μg/L. According to the reference measurement bar Piece (9.1), add 20 μl standard series solution and 2 μl matrix improver (6.7) to graphite tube (7.2) for each measurement Measure the absorbance in order from low concentration to high concentration, with the mass concentration of the standard series (μg/L) as the abscissa, and its corresponding The absorbance is the ordinate and a standard curve is established. 9.3 Sample measurement The measurement of the samples was performed in accordance with the same conditions and operating procedures as the standard curve establishment (9.2). If the measurement results Beyond the range of the standard curve, the sample should be diluted and re-measured with nitric acid solution (6.6). 9.4 Blank test The blank sample was measured under the same conditions and operating procedures as the sample measurement (9.3). 10 Calculation and representation of results 10.1 Calculation of results The mass concentration of antimony in the sample (μg/L) is calculated according to formula (1). 101 ) ( (1) In the formula. ρ--mass concentration of soluble antimony or total antimony in the sample, μg/L; ρ1--mass concentration of soluble antimony or total antimony in the sample obtained from the standard curve, μg/L; ρ0--mass concentration of soluble antimony or total antimony in blank sample obtained from the standard curve, μg/L; V1-constant volume of sample, ml; V--sampling volume, ml; D--sample dilution factor; 10.2 Results representation When the measurement result is less than 100 μg/L, the integer digits are retained; when the measurement result is greater than or equal to 100 μg/L, three digits are retained effective number. 11 Precision and accuracy 11.1 Precision Six laboratories performed uniform samples containing 10.0 μg/L, 40.0 μg/L and 100 μg/L of soluble antimony Six repeated determinations. The relative standard deviations in the laboratory ranged from 1.8% to 8.5%, 1.7% to 6.4%, and 1.7% to 9.7%; the relative standard deviations among the laboratories were 3.0%, 6.1%, and 3.4%; the repeatability limits were 0.9 μg/L and 4.5 μg/L, respectively. And 6.7 μg/L; the reproducibility limits were 1.1 μg/L, 7.8 μg/L, and 9.8 μg/L, respectively. Six laboratories have simulated uniform groundwater samples and surface with soluble antimony mass concentrations of 5.7 μg/L and 6.6 μg/L Water simulation samples were tested 6 times repeatedly. The relative standard deviations in the laboratory were 2.8% ～ 6.1% and 3.2% ～ 12%; relative standard deviations between laboratories are 5.6% and 6.5%; repeatability limits are 0.7 μg/L and 1.3 μg/L, respectively; Reproducibility limits were 1.1 μg/L and 1.7 μg/L, respectively. Six laboratories conducted microwave digestion of unified domestic sewage samples with a total concentration of 11.6 μg/L containing total antimony 6 repeated determinations. the relative standard deviation in the laboratory ranges from 2.3% to 9.0%; the relative standard deviation between laboratories is 9.5% The repeatability limit is 1.7 μg/L; the reproducibility limit is 3.6 μg/L. Six laboratories performed a hot plate digestion method for unified domestic sewage samples with a mass concentration of 13.4 μg/L containing total antimony 6 repeated determinations. the relative standard deviation in the laboratory ranges from 0.9% to 7.0%; the relative standard deviation between laboratories is 8.5%; repeatability limit is 1.6 μg/L; reproducibility limit is 3.5 μg/L. Six laboratories conducted microwave digestion of uniform industrial wastewater samples with a total concentration of 220 μg/L containing total antimony6 Repeated determination. the relative standard deviation in the laboratory ranges from 3.1% to 6.5%; the relative standard deviation between laboratories is 5.5%; The repeatability limit is 28.8 μg/L; the reproducibility limit is 44.0 μg/L. 11.2 Accuracy Six laboratories performed 6 times of certified standard samples (204906) of the mass concentration of antimony (1.52 ± 0.05) Repeated determination. The relative error range is -0.7% ～ 1.3%, and the final relative error value is 0.1% ± 1.5%. Six laboratories have a mass concentration of soluble antimony of 5.7 μg/L and 6.6 μg/L, respectively, and the spiked concentrations are 8.0 μg/L Of the unified groundwater simulation samples and surface water simulation samples were subjected to 6 repeated spiking analysis and determination. The difference is 91.0% ～ 106% and 86.8% ～ 101%; the final recoveries are 97.7% ± 11.2% and 93.0% ± 12.2%. Six domestic laboratories for a unified domestic sewage sample with a mass concentration of total antimony of 11.6 μg/L and a spiked concentration of 12.0 μg/L The product was analyzed and determined by microwave digestion for 6 times. The recovery range of standard addition was 95.0% ～ 104%. The final yield was 99.5% ± 7.4%. Six domestic laboratories for a unified domestic sewage sample with a mass concentration of total antimony of 13.4 μg/L and a spiked concentration of 15.0 μg/L The product was subjected to 6 repeated spiking analysis using a hot plate digestion method. the spiking recovery range was 91.3% -96.3%; spiking The final recovery was 94.5% ± 4.0%. Six industrial laboratories for a unified industrial wastewater sample containing a total concentration of total antimony of 220 μg/L and a spiked concentration of 100 μg/L The product was analyzed by microwave digestion with 6 repeated spike additions. The recoveries of the spikes ranged from 86.0% to 104%. The final yield was 93.2% ± 12.8%. 12 Quality Assurance and Quality Control 12.1 At least two laboratory blank samples shall be determined for each batch of samples, and the measurement results shall be lower than the detection limit of the method. 12.2 A standard curve should be established for each analysis sample, and the correlation coefficient should be ≥0.995. 12.3 Every 20 samples or each batch (≤20 samples/batch) should be analyzed at the middle concentration point of a standard curve. The relative error between the measurement result and the concentration at this point should be within ± 10%. 12.4 Every 20 samples or each batch (≤20 samples/batch) should be measured at least one parallel sample, the relative deviation of the measurement results Should be ≤20%. 12.5 Every 20 samples or each batch (≤20 samples/batch) should measure at least one matrix spiked sample, and the spiked recovery rate It should be controlled between 80% and 115%, or use a certified standard solution to control the accuracy of the measurement. 13 Waste treatment The waste liquid generated in the experiment should be collected separately, stored in a centralized manner, and properly labeled, and entrusted to a qualified unit for processing Management.Appendix A(Normative appendix) Matrix interference inspection method This method is suitable for samples with a certain concentration. Take two samples of the same sample, one of which is diluted 5 times (1 4), after dilution The measured value of the sample (not less than 10 times the detection limit) multiplied by the dilution factor is compared with the measured value of the undiluted sample. Differences within ± 10% are considered non-interfering. Otherwise, it indicates that interference exists and can be offset by dilution or standard addition method. When the diluted sample is less than 10 times the detection limit, the slope of the standard addition method curve can be compared with the slope of the standard curve. Relative deviations within ± 3% are considered non-interfering. Otherwise, matrix interference is present.Appendix B(Normative appendix) Standard addition method B.1 Establishment of calibration curve Add equal amounts of test samples to a blank of the same volume and three standard series of known different concentrations, assuming The concentration of the sample is Cx, the minimum concentration of the added standard is C0, C0≈0.5Cx, and the concentrations of...... |
