GB/T 13747.3-2020 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 13747.3-2020: Methods for chemical analysis of zirconium and zirconium alloys - Part 3: Determination of nickel content - Dimethyglyoxime spectrophotometry and inductively coupled plasma atomic emission spectrometry Status: Valid GB/T 13747.3: Historical versions
Basic dataStandard ID: GB/T 13747.3-2020 (GB/T13747.3-2020)Description (Translated English): Methods for chemical analysis of zirconium and zirconium alloys - Part 3: Determination of nickel content - Dimethyglyoxime spectrophotometry and inductively coupled plasma atomic emission spectrometry Sector / Industry: National Standard (Recommended) Classification of Chinese Standard: H14 Classification of International Standard: 77.120.99 Word Count Estimation: 10,196 Date of Issue: 2020-03-06 Date of Implementation: 2021-02-01 Older Standard (superseded by this standard): GB/T 13747.3-1992 Issuing agency(ies): State Administration for Market Regulation, China National Standardization Administration Summary: This standard specifies the method for the determination of nickel content in zirconium and zirconium alloys. This standard applies to the determination of nickel content in sponge zirconium, zirconium and zirconium alloys. Measurement range: Method 1 measurement range: 0.002% to 0.15%; Method 2 measurement range: 0.010% to 0.40%. When the measurement ranges overlap, the second method is the arbitration analysis method. GB/T 13747.3-2020: Methods for chemical analysis of zirconium and zirconium alloys - Part 3: Determination of nickel content - Dimethyglyoxime spectrophotometry and inductively coupled plasma atomic emission spectrometry---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 zirconium and zirconium alloys - Part 3.Determination of nickel content - Dimethyglyoxime spectrophotometry and inductively coupled plasma atomic emission spectrometry ICS 77.120.99 H14 National Standards of People's Republic of China Replace GB/T 13747.3-1992 Chemical analysis methods of zirconium and zirconium alloys Part 3.Determination of the amount of nickel Diacetyl oxime spectrophotometry and inductively coupled plasma 2020-03-06 released 2021-02-01 implementation State Administration for Market Regulation Issued by the National Standardization Management Committee ForewordGB/T 13747 "Methods for Chemical Analysis of Zirconium and Zirconium Alloys" is planned to be divided into 27 parts. ---Part 1.Determination of the amount of tin potassium iodate titration and phenylfluorone-polyethylene glycol octylphenyl ether spectrophotometry; ---Part 2.Determination of iron content 1,10-phenanthroline spectrophotometry and inductively coupled plasma atomic emission spectrometry; ---Part 3.Determination of nickel content diacetyl oxime spectrophotometry and inductively coupled plasma atomic emission spectrometry; ---Part 4.Determination of chromium content Diphenylcarbazide spectrophotometry and inductively coupled plasma atomic emission spectrometry; ---Part 5.Determination of aluminum content Chromazurol S-tetradecylpyridinium chloride spectrophotometric method; ---Part 6.Determination of copper content 2,9-dimethyl-1,10-phenanthroline spectrophotometry; ---Part 7.Determination of manganese content, potassium periodate spectrophotometry and inductively coupled plasma atomic emission spectrometry; ---Part 8.Determination of Drill Volume Nitroso R Salt Spectrophotometry; ---Part 9.Determination of magnesium content by flame atomic absorption spectrometry; ---Part 10.Determination of Tungsten Content Thiocyanate Spectrophotometric Method; ---Part 11.Determination of molybdenum content thiocyanate spectrophotometric method; ---Part 12.Determination of silicon content molybdenum blue spectrophotometry; ---Part 13.Determination of lead content by polarography; ---Part 14.Polarographic method for the determination of uranium content; ---Part 15.Determination of boron content Curcumin spectrophotometric method; ---Part 16.Determination of chlorine content, silver chloride turbidity method and ion selective electrode method; ---Part 17.Determination of cadmium content by polarography; ---Part 18.Determination of vanadium content Benzoyl phenyl hydroxylamine spectrophotometric method; ---Part 19.Determination of Titanium Content Diantipyrine methane spectrophotometry and inductively coupled plasma atomic emission spectrometry; ---Part 20.Determination of hafnium content inductively coupled plasma atomic emission spectrometry; ---Part 21.Determination of the amount of hydrogen inert gas melting infrared absorption method/thermal conductivity method; ---Part 22.Determination of oxygen and nitrogen content inert gas melting infrared absorption method/thermal conductivity method; ---Part 23.Determination of Nitrogen Content Distillation Separation-Nessler Reagent Spectrophotometry; ---Part 24.Determination of carbon content high frequency combustion infrared absorption method; ---Part 25.Determination of the amount of niobium 5-Br-PADAP spectrophotometry and inductively coupled plasma atomic emission spectrometry; ---Part 26.Determination of alloys and impurity elements inductively coupled plasma atomic emission spectrometry; --- Part 27.Determination of trace impurity elements inductively coupled plasma mass spectrometry. This part is Part 3 of GB/T 13747. This section was drafted in accordance with the rules given in GB/T 1.1-2009. This part replaces GB/T 13747.3-1992 "Methods for chemical analysis of zirconium and zirconium alloys for the determination of nickel content by dimethylglyoxime spectrophotometric method", and Compared with GB/T 13747.3-1992, the main technical changes except for editorial changes are as follows. --- Deleted "reference standard" (see Chapter 2 of the.1992 edition); --- Change the concentration of hydrofluoric acid from "(1 1)" to "(ρ=1.14g/mL)" (see 2.2.2,.1992 edition 4.1); ---Change the volume of dissolved acid of less than 2g sample from 5mL to 2.5mL (see Table 1,.1992 version 6.3.1); --- Add "Method Two Inductively Coupled Plasma Atomic Emission Spectrometry", the measurement range is 0.010% ~ 0.40% (see Chapter 3); ---Added test report clause (see Chapter 4); --- Change the allowable difference to the precision clause (see Chapter 8, Chapter 8 of the.1992 edition). 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. Xi'an Hantang Analysis and Testing Co., Ltd., Guangdong Industrial Analysis and Testing Center, Western Metal Materials Co., Ltd. Company, West New Zirconium Nuclear Material Technology Co., Ltd., Baoti Group Co., Ltd., Beikuang Testing Technology Co., Ltd., National Nuclear Zirconium and Hafnium Physical and Chemical Testing Co., Ltd., Shenzhen Zhongjin Lingnan Nonferrous Metal Co., Ltd., National Standard (Beijing) Inspection and Certification Co., Ltd. The main drafters of this section. Yang Pingping, Zhou Kai, Sun Baolian, Li Bo, Xiong Xiaoyan, Liu Biao, Zhao Huanjuan, Ren Jie, Li Fan, Hui Boning, Li Zhenqian, Feng Zhenhua, Qi Yujing, Wang Jie, Lin Ye, Guo Yanyao, Zhang Xu, Liu Liyuan. The previous versions of the standards replaced by this part are as follows. ---GB/T 13747.3-1992. Chemical analysis methods of zirconium and zirconium alloys Part 3.Determination of the amount of nickel Diacetyl oxime spectrophotometry and inductively coupled plasma Atomic emission spectrometry1 ScopeThis part of GB/T 13747 specifies the method for the determination of nickel content in zirconium and zirconium alloys. This section applies to the determination of nickel content in sponge zirconium, zirconium and zirconium alloys. Measuring range. Method 1 Measuring range. 0.002%~ 0.15%; Method 2 measurement range. 0.010%~0.40%. When the measurement ranges overlap, the second method is the arbitration analysis method. 2 Method-Dimethylglyoxime spectrophotometry 2.1 Principle The sample is dissolved in hydrofluoric acid, the excess hydrofluoric acid is complexed with a saturated solution of boric acid, the main zirconium is complexed with citric acid, and iodine is used as the oxidant. In the solution, nickel and dimethylglyoxime form a red complex, and its absorbance is measured at a wavelength of 540nm with a spectrophotometer. 2.2 Reagents Unless otherwise stated, only reagents and laboratory secondary water confirmed to be analytically pure are used in the analysis. 2.2.1 Nitric acid (1 1). 2.2.2 Hydrofluoric acid (ρ=1.13g/mL). 2.2.3 Saturated solution of boric acid. 2.2.4 Citric acid solution (200g/L). 2.2.5 Ammonia (1 1). 2.2.6 Iodine solution. Weigh 1.3g of iodine and 5g of potassium iodide in a 500mL beaker, dissolve and dilute to 500mL with water, and store in brown In the bottle. 2.2.7 Diacetyl oxime-ethanol solution (2g/L). Weigh 1.0 g of diacetyl oxime and dissolve it in 500 mL of ethanol. 2.2.8 Nickel standard storage solution. Weigh 1.0000g metallic nickel (wNi≥99.99%) into a 250mL beaker, add 10mL nitric acid (2.2.1), heat to dissolve, add 10mL sulfuric acid (1 1), heat until sulfuric acid fumes, and then transfer to a 1000mL volumetric flask, dilute with water Release to the mark and mix well. This solution 1mL contains 1mg nickel. 2.2.9 Nickel standard solution. Pipette 50.00mL nickel standard stock solution (2.2.8) into a 1000mL volumetric flask, dilute to the mark with water, and mix uniform. 1mL of this solution contains 50μg of nickel. 2.3 Apparatus Spectrophotometer. 2.4 Sample Process the sample into chips with a length not greater than 5mm. 2.5 Test procedure 2.5.1 Sample Weigh the sample (2.4) according to Table 1, accurate to 0.0001g. Table 1 Weighing amount and amount of dissolved acid 2.5.2 Parallel test Do two tests in parallel and take the average value. 2.5.3 Blank test Do a blank test with the sample. 2.5.4 Determination 2.5.4.1 Place the sample (2.5.1) in a 100mL polytetrafluoroethylene beaker, blow in a small amount of water, and add hydrofluoric acid (2.2.2) dropwise according to Table 1. After the sample is dissolved, add 0.5 mL of nitric acid (2.2.1) until the solution is clear, add 25 mL of boric acid saturated solution (2.2.3), and transfer to a 100 mL volume. In a measuring flask, dilute to the mark with water and mix well. 2.5.4.2 Pipette 20.00mL solution (2.5.4.1) into a 50mL volumetric flask. 2.5.4.3 Add 4 mL of citric acid solution (2.2.4) and 2.5 mL of iodine solution (2.2.6), mix well, let stand for 3 minutes, and add ammonia water (2.2.5) dropwise to dissolve The color of iodine in the solution disappeared and an excess of 5 mL was made. Cool to room temperature. 2.5.4.4 Add 2mL of diacetyl oxime-ethanol solution (2.2.7), dilute to the mark with water, mix well, and place for 15min. 2.5.4.5 Pipette part of the solution into a 3cm cuvette, use the blank solution with the sample as a reference, and place it at the wavelength of 540nm on the spectrophotometer Measure its absorbance. 2.5.4.6 Check the corresponding amount of nickel from the working curve, subtract the absorbance of the blank test solution. 2.5.5 Drawing of working curve 2.5.5.1 Pipette 0mL, 0.10mL, 0.50mL, 1.00mL, 1.50mL, 2.00mL nickel standard solution (2.2.9), put them in a group In a 50mL volumetric flask, dilute with water to about 20mL, and proceed as follows in 2.5.4.3 and 2.5.4.4. 2.5.5.2 Pipette part of the solution into a 3 cm cuvette, use the reagent blank solution as a reference, and measure it at a wavelength of 540 nm with a spectrophotometer. Absorbance, using nickel content as the abscissa and absorbance as the ordinate to draw the working curve. 2.6 Test data processing The nickel content is calculated as the mass fraction of nickel wNi, calculated according to formula (1). Where. m1---Check the amount of nickel from the working curve, in micrograms (μg); V0---Total volume of test solution, in milliliters (mL); m0---The mass of the sample, in grams (g); V1--- Divide the volume of the test solution in milliliters (mL). When the calculation result is less than 0.010%, one significant digit is reserved; when the calculation result is ≥0.010%, two significant digits are reserved. 2.7 Precision 2.7.1 Repeatability The measured values of two independent test results obtained under repeatability conditions are within the range of the average value given in Table 2. 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) adopts the line according to the data in Table 2 Obtained by sexual interpolation or extension method. 2.7.2 Reproducibility The measured values of two independent test results obtained under reproducibility conditions are within the range of the average value given in Table 3. The absolute difference does not exceed the reproducibility limit (R), and does not exceed 5% in the case of exceeding the reproducibility limit (R). Reproducibility limit (R) is adopted according to the data in Table 3 Obtained by linear interpolation or extension method. Table 3 Reproducibility limits (Method 1)3 Method two inductively coupled plasma atomic emission spectrometry3.1 Principle Dissolve the sample with hydrochloric acid and hydrofluoric acid, add nitric acid dropwise to oxidize. Determined by inductively coupled plasma atomic emission spectrometry, press work The curve method calculates the mass concentration of nickel and expresses the measurement result in mass fraction. 3.2 Reagents Unless otherwise stated, only reagents and laboratory secondary water confirmed to be analytically pure are used in the analysis. 3.2.1 Nitric acid (ρ=1.42g/mL). 3.2.2 Hydrochloric acid (1 1). 3.2.3 Hydrofluoric acid (11). 3.2.4 Metal zirconium (wZr≥99.95%, wNi< 0.0005%). 3.2.5 Nickel standard stock solution. Weigh 1.0000g metallic nickel (wNi≥99.99%) into a 250mL beaker, add 25mL nitric acid (3.2.1), cover with a watch glass, dissolve at low temperature, cool, transfer to a 1000mL volumetric flask, dilute to the mark with water, and mix. This solution 1mL contains 1mg nickel. 3.2.6 Nickel standard solution. pipette 10.00mL nickel standard stock solution (3.2.5) into a 100mL volumetric flask, add 1mL nitric acid (3.2.1), dilute to the mark with water, and mix well. This solution 1mL contains 100μg nickel. 3.2.7 Argon gas (volume fraction ≥99.99%). 3.3 Apparatus Inductively coupled plasma atomic emission spectrometer, with hydrofluoric acid resistant sampling system. 3.4 Sample Process the sample into chips with a length not greater than 5mm. 3.5 Test procedure 3.5.1 Sample Weigh 0.50g sample (3.4), accurate to 0.0001g. 3.5.2 Parallel test Do two tests in parallel and take the average value. 3.5.3 Blank test Weigh the metal zirconium (3.2.4) equivalent to the sample, and do a blank test with the sample. 3.5.4 Preparation of test solution 3.5.4.1 Place the sample (3.5.1) in a.200mL polytetrafluoroethylene beaker, add 10mL hydrochloric acid (3.2.2), add 2mL hydrofluoric acid (3.2.3), heat at low temperature until the sample is completely dissolved, add 0.5mL nitric acid (3.2.1) to oxidize, and cool to room temperature. 3.5.4.2 Transfer to a 100mL plastic volumetric flask, dilute to the mark with water, and mix. 3.5.5 Preparation of working curve solution Weigh 0.500g of metallic zirconium (3.2.4) into a set of.200mL PTFE beakers, dissolve them according to 3.5.4, and divide them after cooling. Don't move into a group of 100mL plastic volumetric flasks, add 0mL, 0.50mL, 1.00mL, 5.00mL, 10.00mL, 20.00mL respectively Nickel standard solution (3.2.6), dilute to the mark with water, and mix. 3.5.6 Determination 3.5.6.1 Recommended analysis line wavelength. 231.60nm. 3.5.6.2 On the inductively coupled plasma atomic emission spectrometer, measure the working curve solution (3.5.5) at the selected analysis wavelength, and then When the curve linearity k≥0.999, the test solution (3.5.4) is measured, the background of the element spectrum line is checked and corrected at the appropriate position, and the The computer automatically gives the mass concentration of nickel. 3.6 Test data processing The nickel content is calculated as the mass fraction wNi of nickel and calculated according to formula (2). The calculation result retains two significant digits. 3.7 Precision 3.7.1 Repeatability The measured values of two independent test results obtained under repeatability conditions are within the average range given in Table 4, and the test results are absolutely poor. The value does not exceed the repeatability limit (r), and it does not exceed 5% if it exceeds the repeatability limit (r). Repeatability limit (r) uses linear interpolation according to the data in Table 4 Method or extension method. 3.7.2 Reproducibility The measured values of two independent test results obtained under reproducibility conditions are within the range of the average value given in Table 5, and the test results are absolutely poor. The value does not exceed the reproducibility limit (R) and does not exceed 5% when the reproducibility limit (R) is exceeded. The reproducibility limit (R) is linear within the data in Table 5. Obtained by interpolation or extension method.4 Test reportThe test report should include the following. ---Test object; ---This part number; ---Method used; ---result; --- Anomalies observed; ---Test date. ......Tips & Frequently Asked Questions:Question 1: How long will the true-PDF of GB/T 13747.3-2020_English be delivered?Answer: Upon your order, we will start to translate GB/T 13747.3-2020_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 13747.3-2020_English with my colleagues?Answer: Yes. The purchased PDF of GB/T 13747.3-2020_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. 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