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GB/T 14849.3-2020: Methods for chemical analysis of silicon metal - Part 3: Determination of calcium content Delivery: 9 seconds. True-PDF full-copy in English & invoice will be downloaded + auto-delivered via email. See step-by-step procedure Status: Valid GB/T 14849.3: Historical versions
Similar standardsGB/T 14849.3-2020: Methods for chemical analysis of silicon metal - Part 3: Determination of calcium content---This is an excerpt. Full copy of true-PDF in English version (including equations, symbols, images, flow-chart, tables, and figures etc.), auto-downloaded/delivered in 9 seconds, can be purchased online: https://www.ChineseStandard.net/PDF.aspx/GBT14849.3-2020 GB NATIONAL STANDARD OF THE PEOPLE’S REPUBLIC OF CHINA ICS 77.040.30 H 17 Replacing GB/T 14849.3-2007 Methods for chemical analysis of silicon metal - Part 3.Determination of calcium content Issued on. MARCH 06, 2020 Implemented on. FEBRUARY 01, 2021 Issued by. State Administration for Market Regulation; Standardization Administration of the People's Republic of China. Table of ContentsForeword... 3 1 Scope... 5 2 Normative references... 5 3 Flame atomic absorption spectrometry... 5 4 Chlorophosphonazo I spectrophotometry... 9 5 Quality assurance and control... 13 6 Test report... 13ForewordGB/T 14849 “Methods for chemical analysis of industrial silicon” consists of the following 11 parts. - Part 1.Determination of iron content; - Part 2.Determination of aluminum content - Chrome azurol S spectrophotometric method; - Part 3.Determination of calcium content; - Part 4.Determination of elements content Inductively coupled plasma atomic emission spectrometric method; - Part 5.Determination of elements content—Analysis using an X-ray fluorescence method; - Part 6.Determination of carbon-Infrared absorption method; - Part 7.Determination of phosphorus content - Phosphorus molybdenum blue spectrophotometry; - Part 8.Determination of copper content - Atomic absorption spectrometric method; - Part 9.Determination of titanium content - Diantipyryl methane spectrophotometry; - Part 10.Determination of mercury content - Atomic fluorescence spectrometric method; - Part 11.Determination of chromium content - Diphenylcarbazide spectrophotometric method. This Part is Part 3 of GB/T 14849. This Part was drafted in accordance with the rules given in GB/T 1.1-2009. This Part replaces GB/T 14849.3-2007 “Methods for chemical analysis of silicon metal - Part 3.Determination of calcium content”. Compared with GB/T 14849.3-2007, in addition to editorial modifications, the main technical changes are as follows. - added warning; - modified range of determination from 0.020%~0.30% to 0.0050%~0.55% (see Clause 1 of this Edition, Clause 1 of Edition 2007); - added normative references (see Clause 2 of this Edition); - modified method summary (see 3.1 and 4.1 of this Edition, Clause 2 and Clause 11 of Edition 2007); - added requirements for analysis reagents and water (see 3.2 and 4.2 of this Edition); - modified precision (see 3.7 and 4.7 of this Edition, Clause 8 and Clause 17 of Edition 2007); - added test report (see Clause 6 of this Edition). This Part was proposed by China Nonferrous Metals Industry Association. This Part shall be under the jurisdiction of National Technical Committee on Non-ferrous Metals of Standardization Administration of China (SAC/TC 243). The drafting organizations of this Part. Aluminum Corporation of China Zhengzhou Nonferrous Metal Research Institute Co., Ltd., Kunming Metallurgical Research Institute, Guangdong Industrial Analysis and Testing Center, Guizhou Institute of Analysis and Testing, South China University of Technology, Xi'an Hantang Analysis and Testing Co., Ltd., Changsha Research Institute of Mining and Metallurgy Co., Ltd., Chinalco Shanxi New Materials Co., Ltd., Chinalco Luoyang Copper Processing Co., Ltd., North Mine Testing Technology Co., Ltd., Chinalco Mining Co., Ltd., Shenzhen Zhongjin Lingnan Nonferrous Metals Co., Ltd., Baotou Aluminum Industry Co., Ltd., Shandong Nanshan Aluminum Industry Co., Ltd. Main drafters of this Part. Shi Lei, Huang Puying, Liu Yingbo, Cui Hao, Hu Zongxi, Zhang Xiaoping, Wang Zhengqiang, Dai Fengying, Han Xiao, Yang Xin, Li Shaowen, Zhang Yingying, Wang Huihui, Yang Binghong, Gu Li, Cui Junfeng, Zhang Xiaoguang, Wang Xue. Versions of standard substituted by this Part are. - GB/T 14849.3-1993, GB/T 14849.3-2007. Methods for chemical analysis of silicon metal - Part 3.Determination of calcium content Warning - The personnel using this Part shall have practical experience in formal laboratory work. This Part does not point out all possible security issues. The user is responsible for taking appropriate safety and health measures and ensuring compliance with the conditions stipulated by relevant national laws and regulations.1 ScopeThis Part of GB/T 14849 specifies the method for determination of calcium content in silicon metal. This Part is applicable to determination of calcium content in silicon metal. The range for determination is. 0.0050%~0.55%.2 Normative referencesThe following referenced documents are indispensable for the application of this document. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies. GB/T 8170, Rules of rounding off for numerical values & expression and judgement of limiting values3 Flame atomic absorption spectrometry3.1 Method summary Use hydrofluoric acid and nitric acid to dissolve test material. Perchloric acid smokes to remove silicon and fluorine. Use nitric acid to dissolve the residue. Use lanthanum salt to suppress aluminum interference. At a wavelength of 422.7nm of flame atomic absorption spectrometer, use air-acetylene flame to measure the absorbance of calcium. Calculate the mass fraction of calcium. 3.2 Reagents and materials Unless otherwise specified, in the analysis, it shall only use the confirmed analytically-pure reagent AND distilled water or deionized water or equivalent- pure water. 3.2.1 Perchloric acid (ρ=1.67g/L). 3.2.7 Calcium standard solution. Pipette 25.00mL of calcium standard stock solution (3.2.6) in a 250mL volumetric flask. Use water to dilute to the scale. Mix well. 1mL of this solution contains 50μg of calcium. 3.3 Instruments 3.3.1 Atomic absorption spectrometer, attached with calcium hollow cathode lamp. Under the best working conditions of the instrument, any atomic absorption spectrometer that can achieve the following indicators can be used. 3.3.2 Platinum dish, 100mL. 3.3.3 Teflon beaker, 250mL. 3.4 Specimen The specimen shall be able to pass through a 0.149mm standard sieve. Use magnet to remove iron. 3.5 Test steps 3.5.1 Test material Weigh 0.50g of specimen (3.4), to the nearest of 0.0001g. 3.5.2 Number of determinations Do two tests in parallel. 3.5.3 Blank test Conduct blank test with test material (3.5.1). 3.5.4 Determination 3.6 Processing of test data Calculate the mass fraction of calcium wCa according to formula (1). 3.7 Precision 3.7.1 Repeatability Obtain the measured value of two independent test results under repeatability conditions. Within the average range given in Table 2, the absolute difference between the two test results does not exceed the repeatability limit (r).4 Chlorophosphonazo I spectrophotometry4.1 Method summary Use hydrofluoric acid and nitric acid to decompose the test material. Perchloric acid smokes to remove silicon and fluorine. Use hydrochloric acid to dissolve the residue. Use triethanolamine, 1,10-phenanthroline, and acetylacetone to mask interference elements. At pH10~pH10.5, calcium and chlorophosphonazo I form a colored complex. Take the faded solution of EGTA-Pb as a reference. 4.2 Reagents and material Unless otherwise specified, in the analysis, it shall only use the confirmed analytically-pure reagent AND distilled water or deionized water or equivalent- pure water. 4.2.1 Hydrofluoric acid (ρ=1.14g/mL). 4.2.2 Nitric acid (1+1). 4.2.3 Perchloric acid (1+1). 4.2.4 Hydrochloric acid (1+1). 4.2.5 Triethanolamine (1+3), stored in polyethylene bottles. 4.2.11 Calcium standard stock solution. Weigh 2.4970g of calcium carbonate that has been dried at 105°C and cooled to room temperature in a dryer (reference reagent, ≥99.95%). Place in a beaker. Add about 200mL of water. Then add hydrochloric acid (4.2.4) dropwise to completely dissolve. 4.3 Instruments 4.4 Specimen The specimen shall be able to pass a 0.149mm standard sieve. Use magnet to remove iron. 4.5 Test steps 4.5.1 Test material Weigh 1.0g of specimen (4.4), to the nearest of 0.0001g. 4.5.5 Drawing of working curve 4.5.5.1 Pipette 0mL, 0.50mL, 1.00mL, 2.00mL, 3.00mL, 4.00mL, 5.00mL, 6.00mL of calcium standard solution (4.2.12) to respectively place in a set of 50mL volumetric flasks. The following shall be carried out according to 4.5.4.4~4.5.4.5.5 Quality assurance and controlIn analysis, use standard sample or control sample to verify. Or at least use standard sample or control sample to verify the analysis method once every year.6 Test reportThe test report shall give at least the following information. ......Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al. 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