GB/T 20975.14-2020 English PDFUS$259.00 · In stock
Delivery: <= 3 days. True-PDF full-copy in English will be manually translated and delivered via email. GB/T 20975.14-2020: Methods for chemical analysis of aluminium and aluminium alloys - Part 14: Determination of nickel content Status: Valid GB/T 20975.14: Historical versions
Basic dataStandard ID: GB/T 20975.14-2020 (GB/T20975.14-2020)Description (Translated English): Methods for chemical analysis of aluminium and aluminium alloys - Part 14: Determination of nickel content Sector / Industry: National Standard (Recommended) Classification of Chinese Standard: H12 Classification of International Standard: 77.120.10 Word Count Estimation: 14,129 Date of Issue: 2020-06-02 Date of Implementation: 2021-04-01 Older Standard (superseded by this standard): GB/T 20975.14-2008 Quoted Standard: GB/T 8005.2; GB/T 8170-2008 Issuing agency(ies): State Administration for Market Regulation, China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 determination of nickel content in aluminum and aluminum alloys by dimethylglyoxime spectrophotometry, flame atomic absorption spectrometry, Na2EDTA titration, and dimethylglyoxime gravimetric method. This standard applies to the arbitration determination of nickel content in aluminum and aluminum alloys. Measurement range of diacetyl oxime spectrophotometry: 0.001 0%��0.010%; flame atomic absorption spectrometry measurement range: 0.005 0%��3.00%; Na2EDTA titration method measurement range: 5.00%��25.00%; Measurement range of diacetyl oxime gravimetric method: 5.00%��30.00%. GB/T 20975.14-2020: Methods for chemical analysis of aluminium and aluminium alloys - Part 14: Determination of nickel 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 14.Determination of nickel content ICS 77.120.10 H12 National Standards of People's Republic of China Replace GB/T 20975.14-2008 Chemical analysis methods of aluminum and aluminum alloys Part 14.Determination of Nickel 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 14 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 20975.14-2008 "Methods for Chemical Analysis of Aluminum and Aluminum Alloy Part 14.Determination of Nickel Content", and Compared with GB/T 20975.14-2008, the main technical changes except for editorial changes are as follows. --- Added standard use safety warnings; --- Added "Normative Reference Documents" (see Chapter 2); --- Added "Terms and Definitions" (see Chapter 3); ---Modified the precision of the diacetyl oxime spectrophotometric method (see Chapter 4.8, Chapter 8 of the.2008 edition); ---Modified the precision of the flame atomic absorption method (see Chapter 5.7, Chapter 17 of the.2008 edition); ---Added "Na2EDTA Titration" (see Chapter 6); ---Added the "diacetyl oxime weight method" (see Chapter 7); ---Added requirements for reagents and water used in analysis (see 4.2, 5.2, 6.2, 7.2); --- Added "Test Report" (see Chapter 8). 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. Guizhou Institute of Analysis and Testing, Northeast Light Alloy Co., Ltd., Non-ferrous Metal Technology and Economic Research Institute, China Aluminum Zhengzhou Nonferrous Metal Research Institute Co., Ltd., Changsha Research Institute of Mining and Metallurgy Co., Ltd., Xi'an Hantang Analysis and Testing Co., Ltd., Kunming Metallurgical Jinan Research Institute, Hebei Sitong New Metal Materials Co., Ltd., Southwest Aluminum (Group) Co., Ltd., Shandongnanshan Aluminum Co., Ltd. Co., Ltd., China Aluminum Materials Application Research Institute Co., Ltd. The main drafters of this section. Li Jiahua, Xi Huan, Wang Xue, Li Zhiyun, Cui Shuang, Zhou Yuanjing, Wu Yuqiang, Li Zhihui, Tan Haiyan, Zhou Bing, Zhang Huilin, Kuang Yuyun, Zeng Hao, Chen Xiaoqian, Li Tuo, Zhang Jine, Yu Xing, Zhang Yingying, Xing Yinjuan, Sun Jianlei, Lou Yue, Liu Weili. The previous versions of the standards replaced by this part are as follows. ---GB/T 6987.14-1986, GB/T 6987.14-2001; ---GB/T 6987.15-1986, GB/T 6987.15-2001; ---GB/T 20975.14-2008. Chemical analysis methods of aluminum and aluminum alloys Part 14.Determination of Nickel 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 diacetyl oxime spectrophotometry, flame atomic absorption spectrometry, Na2EDTA titration, diacetyl Determination of nickel content in aluminum and aluminum alloy by ketoxime gravimetric method. This section applies to the arbitration determination of nickel content in aluminum and aluminum alloys. Determination range of diacetyl oxime spectrophotometry. 0.0010%~ 0.010%; flame atomic absorption spectrometry measurement range. 0.0050%~3.00%; Na2EDTA titration measurement range. 5.00%~ 25.00%; determination range of diacetyl oxime gravimetric method. 5.00%~30.00%. Note. When the mass fraction of nickel is >0.0050%~0.010%, flame atomic absorption spectrometry is used as the arbitration method; the mass fraction of nickel is 5.00%~25.00% When using Na2EDTA titration method as the arbitration method.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 Diacetyl oxime spectrophotometry4.1 Method summary The sample was dissolved with hydrochloric acid. In sodium hydroxide solution, iron is used as carrier to co-precipitate with nickel, filtered, and the precipitate is dissolved in mixed acid. In a Under constant acidity, add tartaric acid, hydroxylamine hydrochloride and sodium thiosulfate to complex interference elements. The complexation of nickel and diacetyl oxime extracted with chloroform And then back-extracted with dilute hydrochloric acid to make nickel into the water phase. Oxidize with bromine water and add dimethylglyoxime to the ammonia solution to make nickel develop. The absorbance at 445.0nm wavelength of the photometer is measured to determine the nickel content. 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 Nitric acid (ρ=1.42g/mL). 4.2.2 Hydrochloric acid (ρ=1.19g/mL). 4.2.3 Hydrofluoric acid (ρ=1.14g/mL). 4.2.4 Ammonia (ρ=0.90g/mL). 4.2.5 Hydrogen peroxide (ρ=1.10g/mL). 4.2.6 Bromine water (saturated solution). 4.2.7 Ammonia (1 27). 4.2.8 Hydrochloric acid (1 1). 4.2.9 Hydrochloric acid-nitric acid mixed acid. Pipette.200mL nitric acid (4.2.1) and 50mL hydrochloric acid (4.2.8), and mix. 4.2.10 Sulfuric acid (1 1). 4.2.11 Hydrochloric acid (1 5). 4.2.12 Hydrochloric acid (1 23). 4.2.13 Sodium hydroxide solution (250g/L), stored in plastic bottles. 4.2.14 Sodium hydroxide solution (2g/L). 4.2.15 Tartaric acid solution (300g/L). 4.2.16 Ferric chloride solution (1mg/mL). Weigh 0.48g iron trichloride (FeCl3·6H2O) or 0.3g iron trioxide (FeCl3) to dissolve In 5mL hydrochloric acid (4.2.8), dilute to 100mL with water, and mix. 4.2.17 Hydroxylamine hydrochloride solution (100g/L), ready when used. 4.2.18 Sodium thiosulfate solution (500g/L). 4.2.19 Diacetyl oxime ethanol solution (10g/L). 4.2.20 Trichloromethane. 4.2.21 Nickel standard storage solution A. Weigh 1.0000g nickel (wNi≥99.99%), place it in a 250mL beaker, add 10mL water and 10mL nitric acid (4.2.1), heat until the nickel is completely dissolved, add 10mL hydrochloric acid (4.2.2), heat to evaporate to dryness (can not be scorched), then add 10mL hydrochloric acid (4.2.2), continue to heat and evaporate to dryness. Add 20mL hydrochloric acid (4.2.2) and heat to dissolve the salts, then transfer to 1000mL volume. In a measuring flask, let cool. Dilute to the mark with water and mix well. This solution 1mL contains 1mg nickel. 4.2.22 Nickel standard solution A. Pipette 10.0mL nickel standard stock solution A (4.2.21) into a 1000mL volumetric flask and dilute with water to Mix well, this solution 1mL contains 0.01mg nickel. 4.3 Apparatus 4.3.1 Spectrophotometer. 4.3.2 Acidity 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 Weigh a sample (4.4) with a mass (m) 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 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 400mL beaker, slowly add 25mL of hydrochloric acid (4.2.8), and cover with a watch glass. Wait for violent reaction to stop After stopping, heat until the sample is completely dissolved. If the sample is difficult to dissolve, you can add an appropriate amount of hydrogen peroxide (4.2.5) to completely dissolve the sample and heat it to decompose Excessive hydrogen peroxide. Dilute with water to about 80mL, filter with slow quantitative filter paper, wash with hot water, and collect the filtrate and washing liquid in 400mL beaker. 4.5.4.2 Move the filter paper and residue into a platinum crucible, dry it and ash completely (do not burn the filter paper) and cool. Add 1mL~2mL sulfuric acid (4.2.10), 5mL hydrofluoric acid (4.2.3), and then dropwise add nitric acid (4.2.1) until the solution is clear, heat and evaporate until the sulfuric acid fumes are removed. Burn (≤700℃) 10min, cool, add a few milliliters of hot water and 1mL~2mL hydrochloric acid (4.2.8), slightly heat to dissolve the salts, incorporate this solution The main filtrate (4.5.4.1) is diluted with water to about 150mL. 4.5.4.3 Add 0.5mL ferric chloride solution (4.2.16) (if the mass fraction of iron in the sample is greater than 0.2%, it is not necessary to add ferric chloride solution Solution) and 45mL sodium hydroxide solution (4.2.14), the test solution is heated to 70 ℃ ~ 90 ℃ and kept for 20 minutes, then boil for 2 minutes ~ 3 minutes. 4.5.4.4 Filter with a fritted glass funnel (ϕ4.5μm~ϕ9μm) and wash immediately with hot sodium hydroxide solution (4.2.14). will Mix 10 mL of hot hydrochloric acid-nitric acid mixed acid (4.2.9) with 10 mL of hot water, use it to dissolve the precipitate on the funnel in the original beaker, and then use the hot Wash with water. Heat to dissolve the salts completely, and cool down. Transfer the test solution to a.200mL volumetric flask (V1), dilute to the mark with water, and mix. Pipette volume (V2) of 50mL test solution (4.5.4.4) into a 150mL beaker. 4.5.4.5 Add 10mL tartaric acid solution (4.2.15), 5mL hydroxylamine hydrochloride solution (4.2.17), add sodium hydroxide to dissolve under constant stirring The solution (4.2.13) is adjusted to pH 4.5~5.0.Add 10mL sodium thiosulfate solution (4.2.18), and use sodium hydroxide solution under stirring [(4.2.13) and (4.2.14)] adjusted to pH 6.5.Transfer the test solution into a 250mL separatory funnel and wash with as little water as possible. 4.5.4.6 Add 5mL of diacetyl oxime ethanol solution (4.2.19) and mix well. Add 10mL chloroform (4.2.20), shake for 2min, 置layered. Transfer the organic phase to the second 100mL separatory funnel, wash with 1mL~2mL chloroform (4.2.20) (without shaking) water Put the phases into a separatory funnel containing the organic phase. Add 5mL of trichloromethane (4.2.20) to the water phase, shake for 30s, and stand still for layering. The organic phase was also transferred to the second separatory funnel. Use 5mL chloroform (4.2.20) to extract once, and combine the organic phases. Discard the water phase. 4.5.4.7 In the second separatory funnel containing the organic phase, add 20mL ammonia (4.2.7), shake for 30s, and let stand for layering. Organic phase Transfer to the third 100mL separatory funnel. Wash with 1mL~2mL chloroform (4.2.20). The organic phase is combined in the third split In the funnel, the water phase is stored in the second separatory funnel. 4.5.4.8 In the third separatory funnel containing the organic phase, add 20mL ammonia (4.2.7), shake for 30s, and let stand for layering. Organic phase Transfer to the fourth 100mL separatory funnel. Wash with 1mL~2mL chloroform (4.2.20). The organic phase is combined in the fourth split In the funnel, move the water phase into the second separatory funnel and wash with 5mL chloroform (4.2.20), shaking for 30s. Stand still and layer, release there The machine phase is in the fourth separatory funnel. Then wash with 1mL~2mL trichloromethane (4.2.20). Combine the organic phases and discard the aqueous phase. 4.5.4.9 In the fourth separatory funnel containing the organic phase, add 20 mL of hydrochloric acid (4.2.12), shake for 30 seconds, and stand for separation. Will be organic The phase shifted into the fifth 100 mL separatory funnel. Wash with 1mL~2mL chloroform (4.2.20). The organic phase is combined and the water phase is stored in The fourth separatory funnel. The organic phase was treated twice with 10 mL of hydrochloric acid (4.2.12) each time, and separated after each treatment. Organic phase Transfer to the sixth and seventh separatory funnels respectively. Wash with 1mL~2mL chloroform (4.2.20) respectively, and collect all water phases in The fourth separatory funnel. After the third treatment, the organic phase was discarded. 4.5.4.10 In the fourth separatory funnel containing the water phase, add 5mL chloroform (4.2.20), shake for 30s, and stand for stratification. Discard The organic phase. Then add 5mL chloroform (4.2.20), shake for 30s, and stand to separate layers. Carefully release the organic phase and discard it. 4.5.4.11 Move the water phase into a 100mL volumetric flask, wash carefully with water, add 10mL hydrochloric acid (4.2.11), and dilute with water to about 80mL. Heat to 35 ℃ ~ 40 ℃, in constant shaking, dropwise add bromine water (4.2.6) until orange-yellow appears, then excess 2mL, and cool. Slowly add ammonia (4.2.4) while shaking until the color disappears and an excess of 1 mL, cool. Add 1mL of diacetyl oxime ethanol solution (4.2.19), Dilute to the mark with water and mix well. The absorbance was measured after being placed for 30 minutes and completed within 60 minutes. 4.5.4.12 Move a part of the test solution (4.5.4.11) into the absorption cell, and use the blank test solution (4.5.3) made with the sample as a reference. The absorbance was measured at a wavelength of 445.0nm with a photometer. Find the corresponding nickel mass (m1) from the working curve. 4.6 Drawing of working curve 4.6.1 Pipette 0mL, 0.50mL, 1.00mL, 2.00mL, 5.00mL, 10.00mL nickel standard solution A (4.2.22) into a set of dry In a dry 150mL beaker, dilute with water to about 40mL. The following shall be carried out according to 4.5.4.5~4.5.4.11. 4.6.2 Move part of the solution (4.6.1) into the absorption cell, take the reagent blank solution as a reference, and measure at the wavelength of the spectrophotometer at 445.0nm The absorbance, the nickel mass as the abscissa and the absorbance as the ordinate, draw the working curve. 4.7 Test data processing The nickel content is calculated as the nickel mass fraction wNi, calculated according to formula (1). wNi= m1V1×10-3 mV2 × 100% (1) Where. m1---The quality of nickel found on the working curve, in milligrams (mg); V1---The total volume of the test solution, in milliliters (mL); m ---the mass of the sample, in grams (g); V2--Divide the volume of the test solution in milliliters (mL). The calculation result retains two significant digits. The rounding of values shall be implemented in 3.2 and 3.3 of GB/T 8170-2008. 4.8 Precision 4.8.1 Repeatability The measured values of two independent test results obtained under repeatability conditions are within the average range given in Table 1.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. Table 1 wNi/% 0.0010 0.0050 0.0099 r/% 0.0002 0.0008 0.0010 4.8.2 Reproducibility The measured values of two independent test results obtained under reproducibility conditions are within the average range given in Table 2.These two test results The absolute difference does not exceed the reproducibility limit R, and the reproducibility limit R does not exceed 5%. The reproducibility limit R is linear according to the data in Table 2. Obtained by interpolation or extension. Table 2 wNi/% 0.0010 0.0050 0.0099 R/% 0.0002 0.0009 0.00125 Flame atomic absorption spectrometry5.1 Method summary The sample is dissolved with hydrochloric acid and hydrogen peroxide, and the nickel is measured with an air-acetylene lean flame at the wavelength of 232.0nm in the atomic absorption spectrometer. The absorbance is used to determine the nickel content. 5.2 Reagents Unless otherwise stated, only reagents and laboratory secondary water confirmed to be analytically pure are used in the analysis. 5.2.1 Pure aluminum (wAl≥99.99%, wNi≤0.0003%). 5.2.2 Nitric acid (ρ=1.42g/mL). 5.2.3 Hydrofluoric acid (ρ=1.14g/mL). 5.2.4 Hydrogen peroxide (ρ=1.10g/mL). 5.2.5 Hydrochloric acid (1 1). 5.2.6 Sulfuric acid (1 1). 5.2.7 Aluminum matrix solution (20mg/mL). Weigh 20.00g of pure aluminum (5.2.1) and place it in a 1000mL beaker. 600mL hydrochloric acid (5.2.5), covered with a watch glass. After the violent reaction stops, slowly heat to complete dissolution, and then add a few drops of hydrogen peroxide (5.2.4), boil for a few minutes, decompose excess hydrogen peroxide, and cool. Transfer the solution into a 1000mL volumetric flask, dilute to the mark with water, Mix well. 5.2.8 Nickel standard storage solution B. Weigh 1.0000g nickel (wNi≥99.99%), plac......Tips & Frequently Asked Questions:Question 1: How long will the true-PDF of GB/T 20975.14-2020_English be delivered?Answer: Upon your order, we will start to translate GB/T 20975.14-2020_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 20975.14-2020_English with my colleagues?Answer: Yes. The purchased PDF of GB/T 20975.14-2020_English will be deemed to be sold to your employer/organization who actually pays for it, including your colleagues and your employer's intranet.Question 3: Does the price include tax/VAT?Answer: Yes. Our tax invoice, downloaded/delivered in 9 seconds, includes all tax/VAT and complies with 100+ countries' tax regulations (tax exempted in 100+ countries) -- See Avoidance of Double Taxation Agreements (DTAs): List of DTAs signed between Singapore and 100+ countriesQuestion 4: Do you accept my currency other than USD?Answer: Yes. If you need your currency to be printed on the invoice, please write an email to Sales@ChineseStandard.net. In 2 working-hours, we will create a special link for you to pay in any currencies. Otherwise, follow the normal steps: Add to Cart -- Checkout -- Select your currency to pay.Question 5: Should I purchase the latest version GB/T 20975.14-2020?Answer: Yes. Unless special scenarios such as technical constraints or academic study, you should always prioritize to purchase the latest version GB/T 20975.14-2020 even if the enforcement date is in future. Complying with the latest version means that, by default, it also complies with all the earlier versions, technically. |
