GB/T 20975.22-2020 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 20975.22-2020: Methods for chemical analysis of aluminium and aluminium alloys - Part 22: Determination of beryllium content Status: Valid GB/T 20975.22: Historical versions
Basic dataStandard ID: GB/T 20975.22-2020 (GB/T20975.22-2020)Description (Translated English): Methods for chemical analysis of aluminium and aluminium alloys - Part 22: Determination of beryllium content Sector / Industry: National Standard (Recommended) Classification of Chinese Standard: H12 Classification of International Standard: 77.120.10 Word Count Estimation: 10,138 Date of Issue: 2020-06-02 Date of Implementation: 2021-04-01 Older Standard (superseded by this standard): GB/T 20975.22-2008 Quoted Standard: GB/T 8005.2; GB/T 8170-2008 Issuing agency(ies): State Administration for Market Regulation, China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 spectrophotometric method for the determination of beryllium content in aluminum and aluminum alloys. This standard applies to the arbitration determination of beryllium content in aluminum and aluminum alloys. The measuring range of the Elektrocyanine R spectrophotometry (I): 0.0001%��0.45%; the measuring range of the Elektrocyanine R spectrophotometry (II): 2.00%��6.50%. GB/T 20975.22-2020: Methods for chemical analysis of aluminium and aluminium alloys - Part 22: Determination of beryllium 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 22.Determination of beryllium content ICS 77.120.10 H12 National Standards of People's Republic of China Replace GB/T 20975.22-2008 Chemical analysis methods of aluminum and aluminum alloys Part 22.determination of beryllium 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 22 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 20975.22-2008 "Methods for chemical analysis of aluminum and aluminum alloys Part 22.Determination of beryllium content Compared with GB/T 20975.22-2008, the main technical changes except for the editorial changes are as follows. --- Added standard use safety warnings; --- Added "Normative Reference Documents" (see Chapter 2); --- Added "Definitions and Terms" (see Chapter 3); ---Modified "Electronic Cyanuran R spectrophotometry (Ⅰ)" weighing sample (see Table 1,.2008 edition of Table 1); ---Modified "Electronic Cyanuran R spectrophotometry (Ⅰ)" working curve segmentation (see 4.5.5,.2008 edition of 6.5); ---Modified the precision of "Electronic Cyanuran R Spectrophotometry (Ⅰ)" (see Chapter 4.7, Chapter 8 of the.2008 edition); ---Added "Electronic Cyanuran R Spectrophotometry (Ⅱ)" (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., Guizhou Institute of Analysis and Testing, Non-ferrous Metal Technology and Economic Research Institute, Shanxi Dongyan Mining Light Alloy Co., Ltd., Changsha Research Institute of Mining and Metallurgy Co., Ltd., China Aluminum Material Application Research Institute Co., Ltd. Suzhou Branch, China Aluminum Ruimin Co., Ltd. The main drafters of this section. Zhou Bing, Zhao Yongjun, Xi Huan, Zhao Shizhuo, Wang Xue, Wang Peng, Wang Yue, Yang Binghong, Han Xiao, Yang Hongbo, Shi Yu, Ma Yue, Lan Zheng, Wang Guojun, Ji Yanli, Li Chao, He Wenxiu, Liu Shuangqing. The previous versions of the standards replaced by this part are as follows. ---GB/T 6987.22-1987, GB/T 6987.22-2001; ---GB/T 20975.22-2008. Chemical analysis methods of aluminum and aluminum alloys Part 22.determination of beryllium 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 stipulates the spectrophotometric method for the determination of beryllium in aluminum and aluminum alloys by the Elektrocyanine Blue R spectrophotometric method. This section applies to the arbitration determination of beryllium content in aluminum and aluminum alloys. The spectrophotometric method with chrome cyanide blue R (Ⅰ) Measuring range. 0.0001%~0.45%; Elysium cyanide blue R spectrophotometry (Ⅱ) measuring range. 2.00%~6.50%.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 Yilai chrome cyan blue R spectrophotometry (Ⅰ) 4.1 Method summary The sample is dissolved in hydrochloric acid and nitric acid, and disodium edetate and sodium tartrate are used as masking agents, and the pH value is 9.5 ammonia-ammonium nitrate buffer In the solution, beryllium forms a ternary complex with chrome cyanide R (SCR) and cetyltrimethylammonium bromide (CTMAB), which is measured in a spectrophotometer. The absorbance at 560.0nm is measured to determine the content of beryllium. 4.2 Reagents Unless otherwise stated, only reagents and laboratory secondary water confirmed to be analytically pure are used in the analysis. 4.2.1 Sulfuric acid (ρ=1.84g/mL). 4.2.2 Nitric acid (ρ=1.42g/mL). 4.2.3 Hydrofluoric acid (ρ=1.14g/mL). 4.2.4 Ammonia (ρ=0.90g/mL). 4.2.5 Hydrochloric acid (1 1). 4.2.6 Disodium ethylenediaminetetraacetic acid (Na2EDTA) solution (100g/L), need to be filtered. 4.2.7 Sodium tartrate solution (1mol/L), need to be filtered. 4.2.8 Solochrome cyanine R (Solochrome cyanine R, SCR) solution (2g/L). weigh 0.500g SCR in a 250mL beaker, Add 2mL nitric acid (4.2.2), stir well with a glass rod, then add about 150mL water to dissolve it completely, and transfer it into a 250mL volumetric flask. For turbidity, filter, dilute to the mark with water, and mix well. 4.2.9 Cetyltrimethylammonium bromide (CTMAB) solution (4g/L). Weigh 1.000g CTMAB in a 250mL beaker and add About 150mL of water, 10mL of ethanol, stir, warm to make it completely dissolved, transfer to a 250mL volumetric flask, dilute to the mark with water, and mix. (If crystals appear during use, it can be warmed to clear). 4.2.10 Ammonia-ammonium nitrate buffer solution. Weigh 51.8g of ammonium nitrate and dissolve in about 400mL of water, add 65mL of ammonia (4.2.4), shake uniform. Adjust to pH 9.5 with ammonia (4.2.4) or nitric acid (1 1) (measured by pH meter), transfer it into a 500mL volumetric flask, and dilute with water to Scale and mix well. 4.2.11 Aluminum solution (20mg/mL). Weigh 20.00g pure aluminum (wAl≥99.99%) in a.2000mL beaker, cover with a watch glass, and divide Add 600mL of hydrochloric acid (4.2.5), slowly heat until completely dissolved, remove, cool, transfer to a 1000mL volumetric flask, dilute with water Release to the mark and mix well. 4.2.12 Beryllium standard storage solution. use a certified standard solution to prepare. This solution 1mL contains 0.1mg beryllium. 4.2.13 Beryllium standard solution A. Pipette 25.00mL beryllium standard stock solution (4.2.12) into a 500mL volumetric flask, add 167mL salt Acid (4.2.5), dilute to the mark with water, mix well (prepared when used). 1mL of this solution contains 5μg of beryllium. 4.2.14 Beryllium standard solution B. Pipette 20.00mL beryllium standard solution A (4.2.13) into a 100mL volumetric flask, add 33mL hydrochloric acid (4.2.5), dilute to the mark with water, and mix well (prepared when used). This solution 1mL contains 1μg beryllium. 4.2.15 Beryllium standard solution C. Pipette 20.00mL beryllium standard solution A (4.2.13) into a 500mL volumetric flask, add 83mL hydrochloric acid (4.2.5), dilute to the mark with water, and mix well (prepared when used). This solution 1mL contains 0.2μg beryllium. 4.2.16 p-nitrophenol solution (2g/L). 4.3 Apparatus 4.3.1 Spectrophotometer. 4.3.2 pH meter or ion meter. 4.4 Sample Process the sample into chips with a thickness of not more than 1mm. 4.5 Analysis steps 4.5.1 Sample According to Table 1, weigh the sample (4.4) of the corresponding mass (m1) to the nearest 0.0001g. 4.5.2 Parallel test Do two tests in parallel and take the average value. 4.5.3 Blank test Pipette 5.0mL aluminum solution (4.2.11) in a 50mL volumetric flask, and operate according to 4.5.4.4 and 4.5.4.5 below. 4.5.4 Determination 4.5.4.1 Place the sample (4.5.1) in a 250mL beaker, add 10mL of water, and slowly add 30mL of hydrochloric acid in batches (4.2.5), cover with a watch glass, after the violent reaction stops, add 2mL of nitric acid (4.2.2), heat until the sample is completely dissolved, and remove. According to Table 1, Filter with medium-speed quantitative filter paper in the corresponding volumetric flask (V1), wash the beaker with hot water and precipitate 7 to 8 times, and cool. When the sample is silicon When the amount fraction is ≥1.00%, place the precipitate and filter paper in a platinum crucible after filtration, burn it at 700℃ for 30min, take it out, cool it, and add 2mL sulfuric acid (4.2.1), 5mL hydrofluoric acid (4.2.3), dropwise add nitric acid (4.2.2) to make the solution clear, heat to volatilize the silicon, remove, cool, and add dropwise A small amount of hydrochloric acid (4.2.5) to dissolve the residue (if turbidity needs to be filtered), the solution is combined in the above sample solution. 4.5.4.2 Dilute the sample solution (4.5.4.1) to the mark with water and mix well. Transfer the corresponding volume (V2) to a 50mL volumetric flask according to Table 1. In, and add aluminum solution (4.2.11). 4.5.4.3 Add 1.5mL sodium tartrate solution (4.2.7) and shake well. Add 15.00mL Na2EDTA solution (4.2.6), add immediately Add 1 drop of p-nitrophenol solution (4.2.16), and adjust the solution from colorless to light yellow with ammonia (4.2.4) under constant shaking, then add 2.00mL ammonia (4.2.4); add 5.00mL ammonia-ammonium nitrate buffer solution (4.2.10), shake well; add 4.00mL CTMAB solution (4.2.9), shake slowly, and place for about 5 minutes. It should not be placed after adding Na2EDTA solution, and the subsequent steps should be carried out continuously. 4.5.4.4 According to Table 1, add SCR solution (4.2.8), dilute to the mark with water, and mix. 4.5.4.5 Move part of the sample solution (4.5.4.4) into the quartz absorption cell, take the blank test (4.5.3) as the reference, and set it at the wavelength of the spectrophotometer. Measure the absorbance at 560.0nm, and find out the corresponding mass of beryllium (m2) from the working curve. 4.5.5 Drawing of working curve 4.5.5.1 According to the mass fraction of beryllium, the preparation of the working curve series standard solution is divided into the following two types. a) When the mass fraction of beryllium is 0.0001%~0.0050%. add 5.0mL aluminum solution to a set of 50mL volumetric flasks (4.2.11), sequentially add 0mL, 0.50mL, 2.50mL, 5.00mL, 7.50mL, 10.00mL beryllium standard solution C (4.2.15). Add 1.5mL sodium tartrate solution (4.2.7), shake well. Add 15.00mL Na2EDTA solution (4.2.6), immediately add 1 drop of p-nitrophenol solution (4.2.16), and adjust the solution with ammonia (4.2.4) under constant shaking. The color changes to light yellow, then add 2.00mL ammonia (4.2.4); add 5.00mL ammonia-ammonium nitrate buffer solution (4.2.10), shake Evenly; add 4.00mL CTMAB solution (4.2.9), shake slowly, and place for about 5min. Add 2.00mL SCR solution (4.2.8), dilute to the mark with water, and mix well. It should not be placed after adding Na2EDTA solution, and the subsequent steps should be continuous get on. b) When the mass fraction of beryllium is >0.0050%~0.40%. add 5.0mL aluminum solution to a set of 50mL volumetric flasks (4.2.11), respectively add 0mL, 0.50mL, 2.50mL, 5.00mL, 7.50mL, 10.00mL beryllium standard solution B (4.2.14). Add 1.5mL sodium tartrate solution (4.2.7), shake well. Add 15.00mL Na2EDTA solution (4.2.6), immediately add 1 drop of p-nitrophenol solution (4.2.16), and adjust the solution with ammonia (4.2.4) under constant shaking. The color changes to light yellow, then add 2.00mL ammonia (4.2.4); add 5.00mL ammonia-ammonium nitrate buffer solution (4.2.10), shake Evenly; add 4.00mL CTMAB solution (4.2.9), shake slowly, and place for about 5min. Add 3.00mL SCR solution (4.2.8), dilute to the mark with water, and mix well. It should not be placed after adding Na2EDTA solution, and the subsequent steps should be continuous get on. 4.5.5.2 Transfer part of the series of standard solutions (4.5.5.1) into the quartz absorption cell, and use the reagent blank solution (without beryllium standard solution) as the reference In comparison, the absorbance was measured at a wavelength of 560.0nm with a spectrophotometer, the mass of beryllium was used as the abscissa and the absorbance was the ordinate, and the working curve was drawn. 4.6 Processing of test data The content of beryllium is calculated by the mass fraction of beryllium wBe, calculated according to formula (1). When the mass fraction of beryllium is less than 0.0010%, the calculation result retains a significant number; when the mass fraction of beryllium is ≥0.0010%, the calculation result is retained Two significant digits. The rounding of values shall be 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 2. Obtained by interpolation or extension. 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 3 Obtained by interpolation or extension. 5 Spectrophotometry with chrome cyanide blue R (Ⅱ) 5.1 Method summary The sample is dissolved in hydrochloric acid, and disodium edetate and sodium tartrate are used as masking agents, and the pH value is 9.5 ammonia-ammonium nitrate buffer solution Among them, beryllium forms a ternary complex with chrome cyanide R (SCR) and cetyltrimethylammonium bromide (CTMAB), which is at the wavelength of the spectrophotometer. The absorbance is measured at 560.0nm to determine the content of beryllium. 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 Nitric acid (ρ=1.42g/mL). 5.2.2 Ammonia (ρ=0.90g/mL). 5.2.3 Hydrochloric acid (1 1). 5.2.4 Sodium tartrate solution (200g/L), need to be filtered. 5.2.5 Disodium ethylenediaminetetraacetic acid (Na2EDTA) solution (100g/L), need to be filtered. 5.2.6 Cetyltrimethylammonium bromide (CTMAB) solution (4g/L). Weigh 1.000g of CTMAB into a 250mL beaker and add About 150mL water, 10mL ethanol, stir and warm to dissolve them completely, transfer them into a 250mL volumetric flask, dilute to the mark with water, and mix (make If crystals appear during use, it can be warmed to clear). 5.2.7 Solochrome cyanine R (Solochrome cyanine R, SCR) solution (2g/L). weigh 0.500g SCR into a 250mL beaker, Add 2 mL of nitric acid (5.2.1), stir with a glass rod, then add about 150 mL of water to dissolve it completely, and transfer it to a 250 mL volumetric flask. For turbidity, filter, dilute to the mark with water, and mix well. 5.2.8 Ammonia-ammonium nitrate buffer solution. Weigh 51.8g of ammonium nitrate and dissolve in about 400mL of water, add 65mL of ammonia (5.2.2), and mix. Use ammonia (5.2.2) or nitric acid (1 1) to adjust the pH to 9.5 (measured by a pH meter), transfer it into a 500mL volumetric flask, and dilute with water to Degree, mix well. 5.2.9 Beryllium standard storage solution. use a certified standard solution to prepare. This solution 1mL contains 0.1mg beryllium. 5.2.10 Beryllium standard solution D. Pipette 10.00mL beryllium standard stock solution (5.2.9) into a 500mL volumetric flask, add 167mL hydrochloric acid (5.2.3), dilute to the mark with water, mix well (prepared when used). This solution 1mL contains 2μg beryllium. 5.2.11 p-nitrophenol solution (2g/L). 5.3 Apparatus 5.3.1 Spectrophotometer. 5.3.2 pH meter. 5.4 Sample Process the sample into chips with a thickness of not more than 1mm. 5.5 Analysis steps 5.5.1 Sample Weigh a sample (5.4) with a mass (m3) of 0.250g, accurate to 0.0001g. 5.5.2 Parallel test Do two tests in parallel and take the average value. 5.5.3 Blank test Do a blank test with the sample (5.5.1). 5.5.4 Determination 5.5.4.1 Place the sample (5.5.1) in a 250mL beaker, add 20mL of hydrochloric acid (5.2.3) in batches, cover with a watch glass, and wait After the strong reaction stops, heat to dissolve the sample completely, cool it, and transfer it to a 250mL volumetric flask (V3) (if insoluble matter needs to be filtered), dilute with water To the mark, mix well. 5.5.4.2 The pipetting volume (V4) is 5.00mL sample solution (5.5.4.1) in a 250mL volumetric flask (V5), and 20mL hydrochloric acid is added (5.2.3), dilute to the mark with water, and mix well. 5.5.4.3 Pipette the volume (V6) 5.00mL sample solution (5.5.4.2) into a 50mL volumetric flask. 5.5.4.4 Add 1.0mL sodium tartrate so......Tips & Frequently Asked Questions:Question 1: How long will the true-PDF of GB/T 20975.22-2020_English be delivered?Answer: Upon your order, we will start to translate GB/T 20975.22-2020_English as soon as possible, and keep you informed of the progress. 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