GB/T 20975.23-2020 English PDFUS$189.00 · In stock
Delivery: <= 3 days. True-PDF full-copy in English will be manually translated and delivered via email. GB/T 20975.23-2020: Methods for chemical analysis of aluminium and aluminium alloys - Part 23: Determination of antimony content Status: Valid GB/T 20975.23: Historical versions
Basic dataStandard ID: GB/T 20975.23-2020 (GB/T20975.23-2020)Description (Translated English): Methods for chemical analysis of aluminium and aluminium alloys - Part 23: Determination of antimony content Sector / Industry: National Standard (Recommended) Classification of Chinese Standard: H12 Classification of International Standard: 77.120.10 Word Count Estimation: 10,174 Date of Issue: 2020-06-02 Date of Implementation: 2021-04-01 Older Standard (superseded by this standard): GB/T 20975.23-2008 Quoted Standard: GB/T 8005.2; GB/T 8170-2008 Issuing agency(ies): State Administration for Market Regulation, China National Standardization Administration Summary: This standard specifies the potassium iodide spectrophotometric method and the cerium sulfate titration method for the determination of antimony content in aluminum and aluminum alloys. This standard applies to the arbitration determination of antimony content in aluminum and aluminum alloys. Determination range of potassium iodide spectrophotometry: 0.004 0%��0.25%; Determination range of cerium sulfate titration method: 4.00%��16.50%. GB/T 20975.23-2020: Methods for chemical analysis of aluminium and aluminium alloys - Part 23: Determination of antimony content---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. Methods for chemical analysis of aluminium and aluminium alloys--Part 23.Determination of antimony content ICS 77.120.10 H12 National Standards of People's Republic of China Replace GB/T 20975.23-2008 Chemical analysis methods of aluminum and aluminum alloys Part 23.Determination of Antimony Content 2020-06-02 released Implementation on 2021-04-01 State Administration for Market Regulation Issued by the National Standardization Management Committee ForewordGB/T 20975 "Methods for Chemical Analysis of Aluminum and Aluminum Alloys" is divided into 37 parts. ---Part 1.Determination of mercury content; ---Part 2.Determination of arsenic content; ---Part 3.Determination of copper content; ---Part 4.Determination of iron content; ---Part 5.Determination of silicon content; ---Part 6.Determination of cadmium content; ---Part 7.Determination of manganese content; ---Part 8.Determination of zinc content; ---Part 9.Determination of lithium content by flame atomic absorption spectrometry; ---Part 10.Determination of tin content; ---Part 11.Determination of lead content; ---Part 12.Determination of titanium content; ---Part 13.Determination of vanadium content; ---Part 14.Determination of nickel content; ---Part 15.Determination of boron content; ---Part 16.Determination of magnesium content; ---Part 17.Determination of strontium content; ---Part 18.Determination of chromium content; ---Part 19.Determination of Zirconium Content; ---Part 20.Determination of Gallium Content Butyl Rhodamine B Spectrophotometry; ---Part 21.Determination of calcium content; ---Part 22.Determination of beryllium content; ---Part 23.Determination of antimony content; ---Part 24.Determination of total rare earth content; ---Part 25.Determination of element content by inductively coupled plasma atomic emission spectrometry; ---Part 26.Determination of carbon content by infrared absorption method; ---Part 27.Determination of cerium, lanthanum and scandium content by inductively coupled plasma atomic emission spectrometry; ---Part 28.Determination of cobalt content by flame atomic absorption spectrometry; ---Part 29.Determination of molybdenum content thiocyanate spectrophotometric method; ---Part 30.Determination of hydrogen content by heating extraction thermal conductivity method; ---Part 31.Determination of phosphorus content molybdenum blue spectrophotometric method; ---Part 32.Determination of Bismuth Content; ---Part 33.Determination of potassium content by flame atomic absorption spectrometry; ---Part 34.Determination of sodium content by flame atomic absorption spectrometry; ---Part 35.Determination of Tungsten Content Thiocyanate Spectrophotometric Method; ---Part 36.Determination of silver content by flame atomic absorption spectrometry; --- Part 37.Determination of Niobium Content. This part is part 23 of GB/T 20975. This section was drafted in accordance with the rules given in GB/T 1.1-2009. This part replaces GB/T 20975.23-2008 "Methods for chemical analysis of aluminum and aluminum alloys Part 23.Determination of antimony content. Iodination Compared with GB/T 20975.23-2008, Potassium Spectrophotometry, except for editorial changes, the main technical changes are as follows. --- Added standard use safety warnings; --- Modify the "scope", increase the determination of the antimony content of the aluminum antimony master alloy, and expand the measurement range (see Chapter 1,.2008 edition Chapter 1); --- Added "Normative Reference Documents" (see Chapter 2); --- Added "Terms and Definitions" (see Chapter 3); ---Modified the precision of "potassium iodide spectrophotometry" (see Chapter 4.7,.2008 edition); --- Added "cerium sulfate titration method" (see Chapter 5); --- Deleted "quality control and assurance" (see Chapter 9 of the.2008 edition); --- Added "Test Report" (see Chapter 6). This part was proposed by China Nonferrous Metals Industry Association. This part is under the jurisdiction of the National Nonferrous Metals Standardization Technical Committee (SAC/TC243). Drafting organizations of this section. Northeast Light Alloy Co., Ltd., Guangdong Industrial Analysis and Testing Center, Non-ferrous Metal Technology and Economic Research Institute, Changsha Research Institute of Mining and Metallurgy Co., Ltd., Xi'an Hantang Analysis and Testing Co., Ltd., Hebei Sitong New Metal Materials Co., Ltd., Gui Prefectural and Provincial Institute of Analysis and Testing, Shandongnanshan Aluminum Co., Ltd., Beikuang Testing Technology Co., Ltd., Shandong Yankuang Light Alloy Co., Ltd. The main drafters of this section. Zhou Bing, Zhang Tianjiao, Xi Huan, Xiong Xiaoyan, Gao Xinyu, Cheng Zhenjin, Yang Xin, Li Wei, Shuai Ruicheng, Wang Qiang, Kuai Lijun, Xu Sheng, Wei Yanqin, Xiong Fangxiang, Zhang Hongxia, Li Wenzhi, Bai Xiaoxia, Zhang Huiling. The previous versions of the standards replaced by this part are as follows. ---GB/T 6987.23-1986, GB/T 6987.23-2001; ---GB/T 20975.23-2008. Chemical analysis methods of aluminum and aluminum alloys Part 23.Determination of Antimony Content Warning---Personnel using this section should have practical experience in formal laboratory work. This section does not point out all possible safety issues question. 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 20975 specifies the potassium iodide spectrophotometric method and the cerium sulfate titration method to determine the antimony content in aluminum and aluminum alloys. This section applies to the arbitration determination of antimony content in aluminum and aluminum alloys. Potassium iodide spectrophotometric determination range. 0.0040%~0.25%; Determination range of cerium sulfate titration method. 4.00%~16.50%.2 Normative referencesThe following documents are indispensable for the application of this document. For dated reference documents, only the dated version applies to this article Pieces. For undated references, the latest version (including all amendments) applies to this document. GB/T 8005.2 Terminology of Aluminum and Aluminum Alloy Part 2.Chemical Analysis GB/T 8170-2008 Numerical rounding rules and the expression and determination of limit values3 Terms and definitionsThe terms and definitions defined in GB/T 8005.2 apply to this document.4 Potassium iodide spectrophotometry4.1 Method summary The sample is dissolved in sodium hydroxide, in a sulfuric acid medium, the copper is masked with thiourea, the iron is masked with ascorbic acid, and the color is developed by potassium iodide. The absorbance was measured at a wavelength of 330.0nm to determine the antimony content. 4.2 Reagents Unless otherwise stated, only used reagents and laboratory secondary water confirmed to be analytically pure in the analysis. 4.2.1 Pure aluminum (wAl≥99.99%, wSb≤0.0010%). 4.2.2 Sulfuric acid (ρ=1.84g/mL). 4.2.3 Sulfuric acid (12.6, about 5mol/L). 4.2.4 Sulfuric acid (about 2.5mol/L). Dilute sulfuric acid (4.2.3) 1 times. 4.2.5 Potassium iodide solution (550g/L). 4.2.6 Sodium hydroxide solution (200g/L). 4.2.7 Ascorbic acid solution (150g/L, ready when used). 4.2.8 Thiourea solution (100g/L). 4.2.9 Iron solution (0.5mg/mL). Weigh 1.08g ferric ammonium sulfate [Fe(NH4)(SO4)2·12H2O], dissolve it in 100mL water, add 25mL sulfuric acid (4.2.4), transferred to a 250mL volumetric flask, dilute to the mark with water, and mix. 4.2.10 Antimony standard storage solution. use a certified standard solution to prepare. Or weigh 0.1000g antimony powder (wSb≥99.99%) in In a 100mL beaker, add 5mL sulfuric acid (4.2.2), heat to dissolve, after the dissolution is complete, wash with sulfuric acid (4.2.3) into a 1000mL volumetric flask In, dilute to the mark with sulfuric acid (4.2.3) and mix well. 1mL of this solution contains 0.1mg of antimony. 4.2.11 Antimony standard solution. Pipette 50.00mL antimony standard stock solution (4.2.10) into a 250mL volumetric flask, add 25mL water, Sulfuric acid (4.2.4) is diluted to the mark and mixed (the sulfuric acid concentration of the solution is about 2.5mol/L). This solution 1mL contains 0.02mg antimony. 4.3 Apparatus Spectrophotometer (with UV part), quartz absorption cell. 4.4 Sample Process the sample into chips with a thickness of not more than 1mm. 4.5 Analysis steps 4.5.1 Sample Weigh the sample (4.4) with a mass (m0) of 1.00g, accurate to 0.0001g. 4.5.2 Parallel test Do two tests in parallel and take the average value. 4.5.3 Blank test Weigh 1.00g pure aluminum (4.2.1), add iron solution (4.2.9) corresponding to the content of the sample, and do a blank test with the sample (4.5.1). 4.5.4 Determination 4.5.4.1 Place the sample (4.5.1) in a 250mL beaker, add 20mL of sodium hydroxide solution (4.2.6), and cover with a watch glass. Be violent After the reaction stops, slowly heat until the sample is completely dissolved. 4.5.4.2 Remove the beaker and let it cool slightly. Carefully add 63mL sulfuric acid (4.2.3), heat to dissolve the salts and evaporate to a volume of about 70mL, remove, Slightly colder. 4.5.4.3 Use medium-speed quantitative filter paper to filter the sample solution in a 100mL volumetric flask (V0), wash the beaker and filter paper with hot water, and cool. To Dilute to the mark with water and mix well. 4.5.4.4 When the mass fraction of antimony is 0.0040%~0.060%, the pipetting volume (V1) is 25.00mL sample solution (4.5.4.3). In a 50mL volumetric flask; when the mass fraction of antimony is >0.060%~0.25%, the pipetting volume (V1) is 5.00mL sample solution (4.5.4.3). In a 50mL volumetric flask, add 22.0mL sulfuric acid (4.2.4). 4.5.4.5 Add 5mL thiourea solution (4.2.8) and 5mL ascorbic acid solution to a 50mL volumetric flask containing sample solution (4.5.4.4) (4.2.7), 10mL potassium iodide solution (4.2.5), dilute to the mark with water, and mix. Leave it for 10 minutes. 4.5.4.6 Put part of the sample solution (4.5.4.5) in a quartz absorption cell, take the blank test (4.5.3) as a reference, and set it at the wavelength of the spectrophotometer. The absorbance was measured at 330.0nm. Find the corresponding antimony mass (m1) from the working curve. 4.5.5 Drawing of working curve 4.5.5.1 Pipette 0mL, 0.50mL, 1.00mL, 3.00mL, 5.00mL, 8.00mL antimony standard solution (4.2.11) into a group In a 50mL volumetric flask, add 28.0mL, 27.5mL, 27.0mL, 25.0mL, 23.0mL, 20.0mL sulfuric acid (4.2.4) sequentially. plus Add 5mL thiourea solution (4.2.8), 5mL ascorbic acid solution (4.2.7), 10mL potassium iodide solution (4.2.5), dilute to the mark with water, mix uniform. Leave it for 10 minutes. 4.5.5.2 Put the standard solution (4.5.5.1) in the quartz absorption cell, and use the reagent blank (without antimony standard solution) as the reference, Measure the absorbance at a wavelength of 330.0nm with a meter (4.3). Using antimony mass as the abscissa and absorbance as the ordinate, the working curve is drawn. 4.6 Test data processing The antimony content is calculated as the antimony mass fraction wSb, calculated according to formula (1). The calculation result retains two significant digits. Numerical rounding is implemented in 3.2 and 3.3 of GB/T 8170-2008. 4.7 Precision 4.7.1 Repeatability The measured values of two independent test results obtained under repeatability conditions, within the average range given below, these two test results The absolute difference does not exceed the repeatability limit r, and the case of exceeding the repeatability limit r does not exceed 5%. The repeatability limit r is within the linear range according to the data in Table 1. Obtained by interpolation or extension method. 4.7.2 Reproducibility The measured values of two independent test results obtained under reproducibility conditions, within the average range given below, these two test results The absolute difference does not exceed the reproducibility limit R, and the case of exceeding the reproducibility limit R does not exceed 5%. Reproducibility limit R is linear according to the data in Table 2 Obtained by interpolation or extension.5 Cerium sulfate titration method5.1 Method summary The sample is dissolved in sulfuric acid. In the acid solution, the antimony (Ⅲ) is oxidized to antimony (Ⅴ) by cerium sulfate. Excessive cerium sulfate discolors the methyl orange. Determine the end point of the titration to determine the antimony content. 5.2 Reagents Unless otherwise stated, only reagents and laboratory tertiary water confirmed to be analytically pure are used in the analysis. 5.2.1 Hydrochloric acid (ρ=1.19g/mL). 5.2.2 Sulfuric acid (1 1). 5.2.3 Standard titration solution of cerium sulfate (c≈0.016mol/L). ---Preparation. Weigh 16g cerium sulfate [Ce(SO4)2·4H2O] in a 1000mL beaker, add.200mL sulfuric acid (5.2.2), 600mL of water, heated to dissolve, cooled to room temperature. Transfer to a 2500mL volumetric flask, dilute to the mark with water, and mix. ---Calibration. Weigh 3 parts (m2) of 0.0400g pure antimony (wSb≥99.99%) in a 500mL conical flask and add 20mL concentrated sulfuric acid (ρ=1.84g/L), heat to dissolve until it is clear, continue to heat until white smoke is just emitted, remove and cool. Blow with water Wash the bottle mouth, add 80mL water, heat and boil for 5min, remove, add 20mL hydrochloric acid (5.2.1), add 2 drops to 3 drops of methyl Orange solution (5.2.4), immediately titrate with cerium sulfate standard titration solution until the solution turns from red to light yellow, which is the end point. Parallel mark Determine the volume range of the cerium sulfate standard titration solution (5.2.3) consumed should not be more than 0.15mL, whichever is the average value (V4). Along with the calibration blank test, record the volume (V3) of the cerium sulfate standard titration solution (5.2.3) consumed. ---Calculation. Calculate the concentration c of the standard titration solution of cerium sulfate according to formula (2). 60.88---The molar mass of antimony (1/2Sb), in grams per mole (g/mol). The calculation result retains four significant figures. The rounding of values shall be implemented in 3.2 and 3.3 of GB/T 8170-2008. 5.2.4 Methyl orange solution (1g/L). 5.3 Specimen Process the sample into chips with a thickness of not more than 1mm. 5.4 Analysis steps 5.4.1 Sample Weigh the sample (5.3) with a mass (m3) of 0.20g to the nearest 0.0001g. 5.4.2 Parallel test Do two tests in parallel and take the average value. 5.4.3 Blank test Do a blank test with the sample (5.4.1) and record the volume (V5) of the cerium sulfate standard titration solution (5.2.3) consumed. 5.4.4 Determination Place the sample (5.4.1) in a 500mL Erlenmeyer flask, add 40mL sulfuric acid (5.2.2), heat until the sample is completely dissolved, remove and cool. Rinse the bottle mouth with water, add about 80mL of water, heat and boil for 5min, remove, add 20mL of hydrochloric acid (5.2.1), add 2 drops to 3 drops of methyl orange Solution (5.2.4), immediately titrate with cerium sulfate standard titration solution (5.2.3) until the solution changes from red to light yellow, which is the end point, and record the consumption of sulfur The volume (V6) of cerium acid standard titration solution (5.2.3). 5.5 Test data processing The antimony content is calculated as the antimony mass fraction wSb, calculated according to formula (3). m3 --- the mass of the sample, in grams (g). The calculation result is expressed to two digits after the decimal point. The rounding of values shall be implemented in 3.2 and 3.3 of GB/T 8170-2008. 5.6 Precision 5.6.1 Repeatability The measured values of two independent test results obtained under repeatability conditions, within the average range given below, these two test results The absolute difference does not exceed the repeatability limit r, and the case of exceeding the repeatability limit r does not exceed 5%. Repeatability limit r is linear within the data in Table 3 Obtained by interpolation or extension method. 5.6.2 Reproducibility The measured values of two independent test results obtained under reproducibility conditions, within the average range given below, these two test results The absolute difference of is not greater than the reproducibility limit R, and the case of exceeding the reproducibility limit R does not exceed 5%. Reproducibility limit R is linear according to the data in Table 4 Obtained by interpolation or extension.6 Test reportThe test report should include the following. a) The number, name and method used in this section; b) All necessary information about identification of samples, laboratory, analysis date, report date, etc.; c) Express the test results in an appropriate form; d) Abnormal phenomena during the test; e) Signatures of review and approval personnel. ......Tips & Frequently Asked Questions:Question 1: How long will the true-PDF of GB/T 20975.23-2020_English be delivered?Answer: Upon your order, we will start to translate GB/T 20975.23-2020_English as soon as possible, and keep you informed of the progress. The lead time is typically 1 ~ 3 working days. The lengthier the document the longer the lead time.Question 2: Can I share the purchased PDF of GB/T 20975.23-2020_English with my colleagues?Answer: Yes. 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