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GB/T 5121.27-2008: Methods for chemical analysis of copper and copper alloys - Part 27: The inductively coupled plasma atomic emission spectrometric method Delivery: 9 seconds. True-PDF full-copy in English & invoice will be downloaded + auto-delivered via email. See step-by-step procedure Status: Valid
Similar standardsGB/T 5121.27-2008: Methods for chemical analysis of copper and copper alloys - Part 27: The inductively coupled plasma atomic emission spectrometric method---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/GBT5121.27-2008 GB NATIONAL STANDARD OF THE PEOPLE’S REPUBLIC OF CHINA ICS 77.120.30 H 13 Methods for chemical analysis of copper and copper alloys - Part 27.The inductively coupled plasma atomic emission spectrometric method Issued on. JUNE 17, 2008 Implemented on. DECEMBER 01, 2008 Issued by. General Administration of Quality Supervision, Inspection and Quarantine; Standardization Administration of the People's Republic of China. Table of ContentsForeword... 3 1 Scope... 5 2 Method principle... 6 3 Reagents and materials... 6 4 Instruments... 11 5 Sample... 11 6 Analysis steps... 11 7 Calculation of analysis results... 16 8 Precision... 17 9 Quality assurance and control... 17ForewordGB/T 5121 “Methods for chemical analysis of copper and copper alloys” consists of 27 parts. - Part 1.The electrolytic method for the determination of copper content; - Part 2.Determination of phosphorus content; - Part 3.Determination of lead content; - Part 4.Determination of carbon and sulfur content; - Part 5.Determination of nickel content; - Part 6.Determination of bismuth content; - Part 7.Determination of arsenic content; - Part 8.Determination of oxygen content; - Part 9.Determination of iron content; - Part 10.Determination of tin content; - Part 11.Determination of zinc content; - Part 12.Determination of antimony content; - Part 13.Determination of aluminum content; - Part 14.Determination of manganese content; - Part 15.Determination of cobalt content; - Part 16.Determination of chromium content; - Part 17.Determination of beryllium content; - Part 18.Determination of magnesium content; - Part 19.Determination of silver content; - Part 20.Determination of zirconium content; - Part 21 - Determination of titanium content; - Part 22.Determination of cadmium content; - Part 23.Determination of silicon content; - Part 24.Determination of selenium and tellurium content; - Part 25.Determination of boron content; - Part 26.Determination of mercury content; - Part 27.The inductively coupled plasma atomic emission spectrometric method. This Part is Part 27. 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. Main drafting organizations of this Part. Chinalco Luoyang Copper Co., Ltd., Beijing Research Institute of Mining and Metallurgy, China Nonferrous Metals Industry Institute of Metrology and Quality. The drafting organization of this Part. Chinalco Luoyang Copper Co., Ltd. The participating drafting organizations of this Part. Design Institute of Daye Nonferrous Metals Co., Ltd., Guangzhou Nonferrous Metal Research Institute. Main drafters of this Part. Xia Qingzhu, Qin Shuping, Zhang Jinghua, Xie Liyun, Li Wei, Yao Qiaoping, Mei Hengxing, Gao Yu, Meng Huijuan, Yang Lijuan, Liu Aiju, Kou Zhilei. Main validators of this Part. Peng Jianjun, Dai Fengying, Shi Xiaoying, Xiong Xiaoyan, Wang Jin, He Mei, Yu Xuebing, Pan Xiaoling, Liu Tianping. Methods for chemical analysis of copper and copper alloys - Part 27.The inductively coupled plasma atomic emission spectrometric method1 ScopeThis Part specifies inductively coupled plasma emission spectrometric method for 25 elements of phosphorus, silver, bismuth, antimony, arsenic, iron, nickel, lead, tin, sulfur, zinc, manganese, cadmium, selenium, tellurium, aluminum, silicon, cobalt, titanium, magnesium, beryllium, zirconium, chromium, boron, mercury in copper and copper alloys. This Part is applicable to simultaneous determination of multiple elements of phosphorus, silver, bismuth, antimony, arsenic, iron, nickel, lead, tin, sulfur, zinc, manganese, cadmium, selenium, tellurium, aluminum, silicon, cobalt, titanium, magnesium, beryllium, zirconium, chromium, boron, mercury in copper and copper alloys. It is also applicable to independent determination of an element. See Table 1 for the determination range of each element. Table 1 -- Determination range of each element Element Mass fraction / % Element Mass fraction / %2 Method principleThe sample is decomposed with nitric acid and hydrochloric acid mixed acid or nitric acid. In acidic media, use inductively coupled plasma emission spectrometer to measure the mass concentration of each element at the corresponding wavelength. When the mass fraction of selenium and tellurium is not greater than 0.001%, use arsenic as a carrier to separate trace amounts of selenium, tellurium and matrix copper in co-precipitation. When the mass fraction of iron, nickel, zinc, and cadmium is not more than 0.001%, the separation and enrichment of copper is released by electricity.3 Reagents and materialsUnless otherwise specified, only reagents and distilled water or deionized water or equivalently pure water that are confirmed as analytically pure are used in the analysis. 3.1 Pure copper (the mass fraction of copper is not less than 99.99%, and the mass fraction of the element to be tested is not more than 0.00005%). 3.2 Sodium hypophosphite. 3.9 Nitric acid (1+1). 3.10 Nitric acid (1+5). 3.11 Nitric acid (1+100). 3.12 Hydrochloric acid (ρ1.19g/mL). excellent grade pure. 3.13 Hydrochloric acid (1+1). 3.14 Hydrochloric acid (1+120). 3.15 Mixed acid. 1 volume of hydrochloric acid (3.12), 3 volumes of nitric acid (3.8) and 4 volumes of water are mixed. 3.16 Manganese nitrate (1+10). excellent grade pure. 3.17 Boric acid saturated solution. 3.18 Sodium hydroxide solution (100g/L). 3.19 Lead nitrate solution (10g/L). excellent grade pure. 3.20 Phenolphthalein ethanol solution (10g/L). 3.26 Standard stock solutions of zinc, nickel, lead, cobalt and manganese. Respectively weigh 1.0000g of pure zinc, pure nickel, pure lead, pure cobalt, pure manganese (the mass fraction of which is not less than 99.95%) into a set of 150mL beakers. Respectively add 10mL of nitric acid (3.9). Heat to dissolve. Boil to remove oxides of nitrogen. Cool. Respectively move into a set of 1000mL volumetric flasks. Use water to dilute to the scale. Mix well. This set of solutions contains 1mg of zinc, 1mg of nickel, 1mg of lead, 1mg of cobalt, 1mg of manganese in 1mL. 3.30 Arsenic standard storage solution. Weigh 0.1320g of arsenic trioxide (As2O3) which has been pre-baked at 100°C~110°C for 2h and cooled to room temperature in a desiccator into a 150mL PTFE beaker. Add 10mL of sodium hydroxide solution (3.18). Heat to dissolve. Cool. Move into a 1000mL volumetric flask. Add water to 200mL~300mL. Add 2 drops of phenolphthalein ethanol solution (3.20). Use nitric acid (3.9) to neutralize until the solution changes from red to colorless. And excess by 10mL. Use water to dilute to the scale. Mix well. 1mL of this solution contains 100μg of arsenic. 3.31 Iron standard storage solution. Weigh 1.0000g of pure iron (the mass fraction of iron is not less than 99.95%) in a 150mL beaker. Add 40mL of hydrochloric acid (3.12). Heat till it is completely dissolved. Cool. Move into a 1000mL volumetric flask. Use water to dilute to the scale. Mix well. 1mL of this solution contains 1mg of iron.4 Instruments4.1 Inductively coupled plasma atomic emission spectrometer 4.2 Constant current electrolyzer equipped with automatic stirring device, with mesh platinum cathode and spiral platinum anode.5 SampleDebris not thicker than 1mm.6 Analysis steps6.1 Test material Weigh sample (5) according to Table 2, to the nearest of 0.0001g. 6.2 Determination times Make two determinations independently. Take the average value. 6.3 Blank test Conduct blank test with test material. 6.4 Preparation of test material solution Mass fraction / % Test material volume / g Dilution volume / mL 6.4.1 When the mass fraction of the element to be measured is greater than 0.001% to the upper limit of determination in Table 1 (Ni mass fraction is 0.001%~14%, lead mass fraction is 0.002%~7%) 6.4.1.1 Place the test material (6.1) in a 150mL beaker. Add 10mL~15mL of mixed acid (3.15). Cover the watch glass. Heat till the test material is completely dissolved. Use water to wash the watch glass and cup wall. Cool. Move to the volumetric flask according to Table 2.Use water to dilute to the scale. Mix well. 6.4.1.3 Samples containing chromium Place the test material (6.1) in a 150mL beaker. Add 5mL~10mL of nitric acid (3.9), 3mL~5mL of perchloric acid (3.6). Cover the watch glass. Heat to dissolve the sample and evaporate to perchloric acid smoke (about 1min~2min) to make the solution clear. Remove to cool. Use water to wash the watch glass and cup wall. Move to volumetric flask according to Table 2.Use water to dilute to the scale. Mix well. 6.4.2 When the mass score of the element to be tested is not greater than 0.001% 6.4.2.1 Selenium and tellurium Place the test material (6.1) in a 400mL beaker. Add 50mL of nitric acid (3.9). Cover the watch glass. Heat at low temperature until the sample is completely dissolved. Cool for a while. Add 10mL of perchloric acid (3.6). Heat up to emit white smoke 2min~3min. Use water to wash the watch glass and cup wall. Remove to cool. 6.4.2.2 Iron, nickel, zinc, cadmium Place the test material (6.1) in a 250mL high-shaped beaker. Add 40mL of nitric acid (3.9). Cover the watch glass. Heat till the test material is completely dissolved. Boil to remove nitrogen oxides. Use water to wash the watch glass and cup wall. 6.4.3 The mass fraction of lead is not greater than 0.002% In accordance with 6.4.2.3. 6.4.4 Samples with a mass fraction of nickel greater than 14% Place the test material (6.1) in a 150mL beaker. Add 10mL of mixed acid (3.15). Cover the watch glass. Heat until the test material is completely dissolved. Boil to remove nitrogen oxides. Use water to wash the watch glass and cup wall. Cool. Move to volumetric flask according to Table 2.Add 2.00mL of internal standard solution (3.25). Use water to dilute to the scale. Mix well. 6.5 Preparation of working curve solution 6.5.1 Working curve I - The mass fraction of the element to be tested is not more than 0.001% 6.5.2 Working curve II - The mass fraction of the element to be tested is 0.001%~0.1% 6.5.3 Working curve III - The mass fraction of the element to be tested is greater than 0.05% to the upper limit of determination in Table 1 (Ni mass fraction is 0.05%~14%) 6.6 Determination 6.6.1 For instrument determination conditions (recommended), see Table 3. When determining phosphorus and sulfur, the light chamber is ventilated with argon or nitrogen for more than 12h or evacuated.7 Calculation of analysis resultsCalculate the mass fraction w(X) of the determined element according to formula (1), in %.8 Precision8.1 Repeatability For measured values of two independent test results obtained under repeatability conditions, within the average range given in Table 5, the absolute difference between the two test results does not exceed the repeatability limit (r). The situation that exceeds the repeatability limit (r) does not exceed 5%. 8.2 Reproducibility For test values of two independent test results obtained under reproducible conditions, within the average range given in Table 6, the absolute difference between the two test results does not exceed the reproducibility limit (R).9 Quality assurance and controlApply national standard samples or industry standard samples (when the two are not currently available, control standard samples can also be used instead). Check the validity of this analytical method standard once a week or every two weeks. When the process is out of control, the cause shall be found out. ......Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al. 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