GB/T 13747.4-2020 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 13747.4-2020: Methods for chemical analysis of zirconium and zirconium alloys - Part 4: Determination of chromium content - Diphenylcarbazide spectrophotometry and inductively coupled plasma atomic emission spectrometry Status: Valid GB/T 13747.4: Historical versions
Basic dataStandard ID: GB/T 13747.4-2020 (GB/T13747.4-2020)Description (Translated English): Methods for chemical analysis of zirconium and zirconium alloys - Part 4: Determination of chromium content - Diphenylcarbazide 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77.120.99 Word Count Estimation: 10,159 Date of Issue: 2020-03-06 Date of Implementation: 2021-02-01 Older Standard (superseded by this standard): GB/T 13747.4-1992 Issuing agency(ies): State Administration for Market Regulation, China National Standardization Administration Summary: This standard specifies the method for the determination of chromium content in zirconium and zirconium alloys. This standard applies to the determination of chromium content in sponge zirconium, zirconium and zirconium alloys. Measurement range: 0.002 0% ~ 0.20%. The second method is the arbitration analysis method. GB/T 13747.4-2020: Methods for chemical analysis of zirconium and zirconium alloys - Part 4: Determination of chromium content - Diphenylcarbazide 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 4.Determination of chromium content - Diphenylcarbazide spectrophotometry and inductively coupled plasma atomic emission spectrometry ICS 77.120.99 H14 National Standards of People's Republic of China Replace GB/T 13747.4-1992 Chemical analysis methods of zirconium and zirconium alloys Part 4.Determination of the amount of chromium Diphenylcarbazide spectrophotometry and inductive coupling Plasma atomic emission spectrometry 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 4 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 13747.4-1992 "Methods for chemical analysis of zirconium and zirconium alloys for the determination of chromium content by diphenylcarbazide spectrophotometric method." Compared with GB/T 13747.4-1992, the main technical changes in this part are as follows except for editorial changes. --- Deleted "reference standard" (see Chapter 2 of the.1992 edition); --- Parallel test has been added (see 2.5.2); ---When the chromium content is 0.0020%~0.020%, add 1 mL of sulfuric acid (1 4) after taking the sample (see 2.5.4.2, 6.3.2 of the.1992 edition); ---Method 1 working curve increase 0.50μg/mL (see 2.5.5.1,.1992 version 6.4.1); ---Add inductively coupled plasma atomic emission spectrometry (see Chapter 3); --- Increased precision (see 2.7 and 3.7); ---Added the test report (see Chapter 4). 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., Western Metal Materials Co., Ltd., Western New Zirconium Nuclear Material Technology Co., Ltd., Shenzhen Zhongjin Lingnan Nonferrous Metals Co., Ltd., Guangdong Industrial Analysis and Testing Center. The main drafters of this section. Liu Leilei, Zhou Kai, Zhang Danli, Yang Xin, Liu Houyong, Liang Wei, Li Weimin, Hui Boning, Zuo Hongyi, Lin Shaoyang, Zhou Zhiping, Xie Hui, Wang Fang, Wang Jin. The previous versions of the standards replaced by this part are as follows. ---GB/T 13747.4-1992. Chemical analysis methods of zirconium and zirconium alloys Part 4.Determination of the amount of chromium Diphenylcarbazide spectrophotometry and inductive coupling Plasma atomic emission spectrometry1 ScopeThis part of GB/T 13747 specifies the method for determining the chromium content in zirconium and zirconium alloys. This section applies to the determination of chromium content in sponge zirconium, zirconium and zirconium alloys. Measuring range. 0.0020%~0.20%. Method two is arbitration Analytical method. 2 Method-Diphenylcarbazide spectrophotometry 2.1 Principle The sample was dissolved with sulfuric acid and ammonium sulfate. Use potassium permanganate to oxidize chromium. In the presence of urea, excess potassium permanganate is separated with sodium nitrite. It generates a red-purple complex with diphenylcarbazide and measures its absorbance at a wavelength of 540nm in a spectrophotometer. 2.2 Reagents Unless otherwise specified, only reagents and laboratory secondary water confirmed to be analytically pure are used in the analysis. 2.2.1 Ammonium sulfate. 2.2.2 Sulfuric acid (ρ=1.84g/mL). 2.2.3 Sulfuric acid (1 4). 2.2.4 Potassium permanganate solution (30g/L). 2.2.5 Urea solution (100g/L). 2.2.6 Sodium nitrite solution (10g/L). 2.2.7 Diphenylcarbazide ethanol solution. Weigh 0.50g of diphenylcarbazide, dissolve it in 100mL ethanol, and store it in a brown bottle (within one week) effective). 2.2.8 Chromium standard storage solution. Weigh 0.2829g of potassium dichromate (reference reagent) that has been dried at 105°C for 2 hours, dissolve it in water, and transfer it into In a 1000mL volumetric flask, dilute to the mark with water and mix well. This solution 1mL contains 100μg chromium. 2.2.9 Chromium standard solution. Pipette 10.00mL chromium standard stock solution (2.2.8) into a 100mL volumetric flask, dilute to the mark with water, and mix uniform. This solution 1mL contains 10μg chromium. 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. 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 150mL beaker, add 6g of ammonium sulfate (2.2.1) and 10mL of sulfuric acid (2.2.2), cover with a watch glass, Heat to complete decomposition, cool to room temperature, add about 30mL of water to dissolve the salts, transfer to a 100mL volumetric flask, dilute to the mark with water, Mix well. 2.5.4.2 When the chromium content is 0.0020%~0.020%, pipette 10.00mL test solution into a 150mL beaker, add 1.0mL sulfuric acid (2.2.3) and 39mL water; when the chromium content is greater than 0.020%~0.20%, pipette 5.00mL test solution into a 150mL beaker, add 2.0mL Sulfuric acid (2.2.3) and 43mL water. 2.5.4.3 Add potassium permanganate solution (2.2.4) dropwise until the solution turns into a stable red and excess 2 to 3 drops, then slowly boil for a few minutes to make the chromium oxide Completely. After cooling to room temperature, add 20 mL of urea solution (2.2.5), shake well, add dropwise sodium nitrite solution (2.2.6) to make potassium permanganate The magenta disappears, shake until the bubbles stop, transfer to a 100mL volumetric flask, cool to room temperature with running water, add 5mL diphenylcarbazide ethanol Solution (2.2.7), dilute to the mark with water, mix well, and place for 5 min. 2.5.4.4 Pipette part of the solution into a 1cm cuvette, use the blank solution with the sample as a reference, and use the spectrophotometer with a wavelength of 540nm At the place, measure its absorbance. Find the corresponding chromium content from the working curve. 2.5.5 Drawing of working curve 2.5.5.1 Pipette 0mL, 0.50mL, 1.00mL, 3.00mL, 5.00mL, 7.00mL, 10.00mL chromium standard solution (2.2.9), Do not place it in a set of 150mL beakers, add 4.0mL sulfuric acid (2.2.3), and dilute with water to about 50mL volume. Follow 2.5.4.3 get on. 2.5.5.2 Pipette part of the solution into a 1cm cuvette, use the reagent blank solution as a reference, and measure at the wavelength of 540nm on the spectrophotometer. Its absorbance. Use chromium content as the abscissa and absorbance as the ordinate to draw a working curve. 2.6 Test data processing The chromium content is calculated as the mass fraction wCr of chromium, calculated according to formula (1). 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 value of the independent test result obtained under the reproducibility condition is within the range of the average value given in Table 3. The difference does not exceed the reproducibility limit (R), and 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.3 Method two inductively coupled plasma atomic emission spectrometry3.1 Principle Dissolve the sample with hydrochloric acid and hydrofluoric acid. Add nitric acid dropwise for oxidation. Use inductively coupled plasma atomic emission spectrometry to determine Calculate the mass concentration of chromium by curve method, and express the measurement result by mass fraction. 3.2 Reagents Unless otherwise specified, only reagents and laboratory secondary water confirmed to be analytically pure are used in the analysis. 3.2.5 Chromium standard storage solution. weigh 2.8293g of potassium dichromate (reference reagent) that has been dried at 105°C for 2 hours, dissolve it in water, and transfer it into In a 1000mL volumetric flask, dilute to the mark with water and mix well. This solution 1mL contains 1.0mg chromium. 3.2.6 Chromium standard solution. Pipette 10.00mL chromium standard stock solution (3.2.5) into a 100mL volumetric flask, dilute to the mark with water, and mix uniform. This solution 1mL contains 100μg chromium. 3.2.7 Argon gas (volume fraction ≥99.99%). 3.3 Apparatus Inductively coupled plasma atomic emission spectrometer with hydrofluoric acid resistant atomizer 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), 2mL hydrofluoric acid (3.2.3), heating at low temperature until the sample is completely dissolved, add 0.5mL nitric acid (3.2.1). 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 6 parts of 0.500g metal zirconium (3.2.4) into a set of.200mL PTFE beakers, dissolve them according to 3.5.4, and cool Then transfer to a set of 100mL plastic volumetric flasks, add 0mL, 0.50mL, 1.00mL, 5.00mL, 10.00mL, 25.00mL in sequence Chromium standard solution (3.2.6), dilute to the mark with water, and mix. 3.5.6 Measurement 3.5.6.1 Recommended analysis line. 267.71nm. 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 chromium. 3.6 Test data processing The chromium content is calculated as the mass fraction of chromium wCr, calculated according to formula (2). 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 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) adopts the line according to the data in Table 4 Obtained by sexual interpolation 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. 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 5 Obtained by linear interpolation or extension method.4 Test reportThe test report should include the following. ---Test object; ---This standard number; ---Method used; ---result; --- Anomalies observed; ---Test date. ......Tips & Frequently Asked Questions:Question 1: How long will the true-PDF of GB/T 13747.4-2020_English be delivered?Answer: Upon your order, we will start to translate GB/T 13747.4-2020_English as soon as possible, and keep you informed of the progress. 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