HOME   Cart(0)   Quotation   About-Us Tax PDFs Standard-List Powered by Google www.ChineseStandard.net Database: 189759 (2 Feb 2025)

HJ 680-2013 PDF English


Search result: HJ 680-2013 English: PDF
Standard IDContents [version]USDSTEP2[PDF] delivered inName of Chinese StandardStatus
HJ 680-2013English330 Add to Cart 0-9 seconds. Auto-delivery. Soil and sediment. Determination of mercury, arsenic, selenium, bismuth, antimony. Microwave dissolution/Atomic Fluorescence Spectrometry Valid
BUY with any currencies (Euro, JPY, GBP, KRW etc.): HJ 680-2013     Related standards: HJ 680-2013

PDF Preview: HJ 680-2013


HJ 680-2013: PDF in English

HJ 680-2013 HJ NATIONAL ENVIRONMENTAL PROTECTION STANDARD OF THE PEOPLE’S REPUBLIC OF CHINA Soil and sediment - Determination of mercury, arsenic, selenium, bismuth, antimony - Microwave dissolution/Atomic Fluorescence Spectrometry ISSUED ON: NOVEMBER 21, 2013 IMPLEMENTED ON: FEBRUARY 01, 2014 Issued by: Ministry of Environmental Protection Table of Contents Foreword ... 5 1 Scope of application ... 6 2 Normative references ... 6 3 Principle of the method ... 6 4 Reagents and materials ... 7 5 Instruments and devices ... 10 6 Samples ... 10 7 Analysis steps ... 12 8 Calculation and presentation of results ... 14 9 Precision and accuracy ... 15 10 Quality assurance and quality control ... 16 11 Waste disposal ... 16 12 Precautions ... 16 Appendix A (informative) Summary data of precision and accuracy ... 18 Soil and sediment - Determination of mercury, arsenic, selenium, bismuth, antimony - Microwave dissolution/Atomic Fluorescence Spectrometry 1 Scope of application This Standard specifies the microwave dissolution/atomic fluorescence spectrometry for the determination of mercury, arsenic, selenium, bismuth, and antimony in soil and sediment. This Standard applies to the determination of mercury, arsenic, selenium, bismuth, and antimony in soil and sediment. When the sample size is 0.5 g, for mercury, the detection limit of this method is 0.002 mg/kg, and the lower limit of determination is 0.008 mg/kg; for arsenic, selenium, bismuth, and antimony, the detection limit is 0.01 mg/kg, and the lower limit of determination is 0.04 mg/kg. 2 Normative references This Standard refers to the following documents or their clauses. For undated references, the latest edition applies to this Standard. GB 17378.3 The specification for marine monitoring - Part 3: Sample collection storage and transportation GB 17378.5 The specification for marine monitoring - Part 5: Sediment analysis GB/T 21191 Atomic fluorescence spectrometer HJ/T 166 Technical specification for soil environmental monitoring HJ 613 Soil - Determination of dry matter and water content - Gravimetric method 3 Principle of the method After the sample is dissolved by microwave, the test solution enters the atomic fluorescence spectrometer; under the reducing action of potassium borohydride solution, arsine, bismuth hydrogen, antimony hydrogen and hydrogen selenide gas are generated, and mercury is reduced to atomic state. Ground-state atoms are formed in the hydrogen- hydrogen flame, and atomic fluorescence is generated under the excitation of light emitted by element lamps (mercury, arsenic, selenium, bismuth, antimony). The atomic fluorescence intensity is proportional to the element content in the test solution. 4 Reagents and materials Unless otherwise specified, the analysis is performed using guarantee reagents that comply with national standards, and the experimental water is freshly prepared distilled water. 4.1 Hydrochloric acid (HCl), ρ = 1.19 g/ml. 4.2 Nitric acid (CHNO3), ρ = 1.42 g/ml. 4.3 Potassium hydroxide (KOH). 4.4 Potassium borohydride (KBH4). 4.5 Hydrochloric acid solution: 5 + 95. PIPETTE 25 ml of hydrochloric acid (4.1) and DILUTE to 500 ml with experimental water. 4.6 Hydrochloric acid solution: 1 + 1. PIPETTE 500 ml of hydrochloric acid (4.1) and DILUTE to 1000 ml with experimental water. 4.7 Thiourea (CH4N2S): analytical reagent. 4.8 Ascorbic acid (C6H8O6): analytical reagent. 4.9 Reducing agents: 4.9.1 Potassium borohydride solution A: ρ = 10 g/L. WEIGH 0.5 g of potassium hydroxide (4.3); PUT it in a beaker containing 100 ml of experimental water; STIR with a glass rod until completely dissolved; ADD 1.0 g of potassium borohydride (4.4); STIR to dissolve. This solution is prepared on the day of use for the determination of mercury. 4.9.2 Potassium borohydride solution B: ρ = 20 g/L. WEIGH 0.5 g of potassium hydroxide (4.3); PUT it in a beaker containing 100 ml of experimental water; STIR with a glass rod until completely dissolved; ADD 2.0 g of potassium borohydride (4.4); STIR to dissolve. This solution is prepared on the day of use for the determination of arsenic, selenium, bismuth, and antimony. 4.13.3 Arsenic standard use solution: ρ = 100.0 μg/L. PIPETTE 10.00 ml of arsenic standard intermediate solution (4.13.2); PLACE it in a 100 ml volumetric flask; ADD 20 ml of hydrochloric acid solution (4.6); DILUTE to the marked line with experimental water; MIX well. Prepare before use. 4.14 Selenium (Se) standard solution. 4.14.1 Selenium standard stock solution: ρ = 100.0 mg/L. PURCHASE commercially available certified reference materials/certified reference samples, or WEIGH 0.1000 g of high-purity selenium powder; PLACE it in a 100 ml beaker; ADD 20 ml of nitric acid (4.2); HEAT at low temperature until dissolved; COOL to room temperature; TRANSFER to a 1000 ml volumetric flask; DILUTE to the marked line with experimental water; MIX well. 4.14.2 Selenium standard intermediate solution: ρ = 1.00 mg/L. PIPETTE 5.00 ml of selenium standard stock solution (4.14.1); PLACE it in a 500 ml volumetric flask; DILUTE to the marked line with experimental water; MIX well. 4.14.3 Selenium standard use solution: ρ = 100.0 μg/L. PIPETTE 10.00 ml of selenium standard intermediate solution (4.14.2); PLACE it in a 100 ml volumetric flask; DILUTE to the marked line with experimental water; MIX well. Prepare before use. 4.15 Bismuth (Bi) standard solution. 4.15.1 Bismuth standard stock solution: ρ = 100.0 mg/L. PURCHASE commercially available certified reference materials/certified reference samples, or WEIGH 0.100 0 g of high-purity metal bismuth; PLACE it in a 100 ml beaker; ADD 20 ml of nitric acid (4.2); HEAT at low temperature until completely dissolved; COOL; TRANSFER to a 1000 ml volumetric flask; DILUTE to the marked line with experimental water; MIX well. 4.15.2 Bismuth standard intermediate solution: ρ = l.00 mg/L. PIPETTE 5.00 ml of bismuth standard stock solution (4.15.1); PLACE it in a 500 ml volumetric flask; ADD 100 ml of hydrochloric acid solution (4.6); DILUTE to the mark line with experimental water; MIX well. 4.15.3 Bismuth standard use solution: ρ = 100.0 μg/L. PIPETTE 10.00 ml of bismuth standard intermediate solution (4.15.2); PLACE it in a 100 ml volumetric flask; ADD 20 ml of hydrochloric acid solution (4.6); DILUTE to the marked line with experimental water; MIX well. Prepare before use. 4.16 Antimony (Sb) standard solution. 4.16.1 Antimony standard stock solution: ρ = 100.0 mg/L. PURCHASE commercially available certified reference materials/certified reference samples, or WEIGH 0.1197 g of antimony trioxide (Sb2O3) that has been dried at 105 °C for 2 h; DISSOLVE it in 80 ml of hydrochloric acid (4.1); TRANSFER to a 1 000 ml volumetric flask; ADD 120 ml of hydrochloric acid (4.1); DILUTE to the marked line with experimental water; MIX well. 4.16.2 Antimony standard intermediate solution: ρ = 1.00 mg/L. PIPETTE 5.00 ml of antimony standard stock solution (4.16.1); PLACE it in a 500 ml volumetric flask; ADD 100 ml of hydrochloric acid solution (4.6); DILUTE to the marked line with experimental water; MIX well. 4.16.3 Antimony standard use solution: ρ = 100.0 μg/L. PIPETTE 10.00 ml of antimony standard intermediate solution (4.16.2); PLACE it in a 100 ml volumetric flask; ADD 20 ml of hydrochloric acid solution (4.6); DILUTE to the marked line with experimental water; MIX well. Prepare before use. 4.17 Carrier gas and shielding gas: argon (purity ≥ 99.99 %). 4.18 Slow quantitative filter paper. 5 Instruments and devices 5.1 Microwave dissolution instrument with temperature control and temperature programming functions, and the temperature accuracy can reach ±2.5 °C. 5.2 The atomic fluorescence spectrometer shall comply with the provisions of GB/T 21191, with elemental lamps of mercury, arsenic, selenium, bismuth, and antimony. 5.3 Constant temperature water bath apparatus. 5.4 Analytical balance: the accuracy is 0.000 1 g. 5.5 Common laboratory equipment. 6 Samples 6.1 Collection of samples Collect soil samples according to the relevant provisions of HJ/T 166; collect sediment samples according to the relevant provisions of GB 17378.3. Respectively PIPETTE 0, 0.50, 1.00, 2.00, 3.00, 4.00, 5.00 ml of arsenic standard solution (4.13.3); PLACE them in 50 ml volumetric flasks; respectively ADD 5.0 ml of hydrochloric acid (4.1) and 10.0 ml of thiourea and ascorbic acid mixed solution (4.10); PLACE at room temperature for 30 min (when the room temperature is lower than 15 °C, place in a 30 °C water bath for 20 min); DILUTE to the marked line with experimental water; MIX well. (3) Calibration series for selenium Respectively PIPETTE 0, 0.50, 1.00, 2.00, 3.00, 4.00, 5.00 ml of selenium standard solution (4.14.3); PLACE them in 50 ml volumetric flasks; respectively ADD 10.0 ml of hydrochloric acid (4.1); PLACE at room temperature for 30 min (when the room temperature is lower than 15 °C, place in a 30 °C water bath for 20 min); DILUTE to the marked line with experimental water; MIX well. (4) Calibration series for bismuth Respectively PIPETTE 0, 0.50, 1.00, 2.00, 3.00, 4.00, 5.00 ml of bismuth standard solution (4.15.3); PLACE them in 50 ml volumetric flasks; respectively ADD 5.0 ml of hydrochloric acid (4.1) and 10.0 ml of thiourea and ascorbic acid mixed solution (4.10); DILUTE to the marked line with experimental water; MIX well. (5) Calibration series for antimony Respectively PIPETTE 0, 0.50, 1,00, 2.00, 3.00, 4.00, 5.00 ml of antimony standard solution (4.16.3); PLACE them in 50 ml volumetric flasks; respectively ADD 5.0 ml of hydrochloric acid (4.1) and 10.0 ml of thiourea and ascorbic acid mixed solution (4.10); PLACE at room temperature for 30 min (when the room temperature is lower than 15 °C, place in a 30 °C water bath for 20 min); DILUTE to the marked line with experimental water; MIX well. See Table 4 for the concentrations of the calibration series solutions of mercury, arsenic, selenium, bismuth, and antimony. 7.3 Plotting of calibration curve Using potassium hydride solution (4.9.1 or 4.9.2) as the reducing agent and 5 + 95 hydrochloric acid solution (4.5) as the carrier, determine the atomic fluorescence m - the mass of the sample to be weighed, g; wdm - the dry matter content of the sample, %. 8.1.2 Calculation of results for sediment samples The element (mercury, arsenic, selenium, bismuth, antimony) content w2 (mg/kg) in the sediment is calculated according to formula (2): where: w2 - the element content in the sediment, mg/kg; ρ - the mass concentration of the element in the test solution, obtained from the calibration curve, μg/L; ρ0 - the determined mass concentration of the element in the blank solution, μg/L; V0 - the constant volume of the test solution after microwave dissolution, ml; V1 - the volume of the divided test solution, ml; V2 - the constant volume of the test solution determined after being divided, ml; m - the mass of the sample to be weighed, g; f - the moisture content of the sample, %. 8.2 Result presentation When the determination result is less than 1 mg/kg, the number after the decimal point shall be reserved up to three digits; when the determination result is greater than 1 mg/kg, three significant figures shall be reserved. 9 Precision and accuracy 9.1 Precision Determined the reference samples of mercury, arsenic, selenium, bismuth, and antimony by six laboratories, and the inner-laboratory relative standard deviations are 1.44 % ~ 11.7 % for mercury, 0.67 % ~ 8.91 % for arsenic, 0.79 % ~ 23.1 % for selenium, 1.47 % ~ 19.4 % for bismuth, and 1.83 % ~ 11.7 % for antimony; inter-laboratory relative standard deviations are 3.42 % ~ 11.2 % for mercury, 3.14 % ~ 4.44 % for arsenic, 3.92 % ~ 9.46 % for selenium, 4.92 % ~ 7.59 % for bismuth, and 3.35 % ~ 9.95 % for antimony; repeatability limits are 0.003 ~ 0.006 mg/kg for mercury, 0.298 ~ 3.03 mg/kg for arsenic, 0.013 ~ 0.025 mg/kg for selenium, 0.019 ~ 0.299 mg/kg for bismuth, and 0.049 ~ 0.363 mg/kg for antimony; reproducibility limits are 0.003 ~ 0.007 mg/kg for mercury, 0.320 ~ 3.55 mg/kg for arsenic, 0.017 ~ 0.029 mg/kg for selenium, 0.019 ~ 0.485 mg/kg for bismuth, and 0.068 ~ 0.655 mg/kg for antimony. The summary results of precision tests are detailed in Appendix A. 9.2 Accuracy Determined the reference samples of mercury, arsenic, selenium, bismuth, and antimony by six laboratories, and the relative errors are -12.5 % ~ 12.5 % for mercury, -7.5 % ~ 4.7 % for arsenic, -25.0 % ~ 8.6 % for selenium, -12.7 % ~ 8.8 % for bismuth, and -15.8 % ~ 11.1 % for antimony. The summary results of accuracy tests are detailed in Appendix A. 10 Quality assurance and quality control 10.1 Measure at least 2 whole-process blanks for each batch of samples. The blank samples shall use the same dissolution procedure as the samples, and the determination results shall be lower than the lower limit of the method. 10.2 According to the batch size, for each batch of samples, it shall determine 1 ~ 2 reference material(s) containing target elements, and the determination results shall be within the controllable range. 10.3 In each batch (less than 10) or every 10 samples, at least 10 % of the samples shall be repeatedly dissolved. 10.4 If the sample dissolution process produces excessive pressure and causes pressure release and destroys its closed system, the data of this sample shall not be used. 10.5 This Standard specifies that the correlation coefficient of the calibration curve shall not be less than 0.999. 11 Waste disposal The waste liquid generated during the experiment cannot be dumped at will, and shall be entrusted to a qualified organization for disposal according to the provisions. 12 Precautions 12.1 Nitric acid and hydrochloric acid are highly corrosive, so the sample dissolution process shall be carried out in a fume hood, and experimenters shall wear protective devices. ......
Source: Above contents are excerpted from the PDF -- translated/reviewed by: www.chinesestandard.net / Wayne Zheng et al.