GB/T 15076.6-2020 English PDFUS$119.00 · In stock
Delivery: <= 3 days. True-PDF full-copy in English will be manually translated and delivered via email. GB/T 15076.6-2020: Methods for chemical analysis of tantalum and niobium - Part 6: Determination of silicon content - Inductively coupled plasma atomic emission spectrometry Status: Valid GB/T 15076.6: Historical versions
Basic dataStandard ID: GB/T 15076.6-2020 (GB/T15076.6-2020)Description (Translated English): Methods for chemical analysis of tantalum and niobium - Part 6: Determination of silicon content - 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: 6,618 Date of Issue: 2020-03-06 Date of Implementation: 2021-02-01 Issuing agency(ies): State Administration for Market Regulation, China National Standardization Administration GB/T 15076.6-2020: Methods for chemical analysis of tantalum and niobium - Part 6: Determination of silicon content - 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 tantalum and niobium - Part 6.Determination of silicon content - Inductively coupled plasma atomic emission spectrometry ICS 77.120.99 H14 National Standards of People's Republic of China Replace GB/T 15076.6-1994 Tantalum-niobium chemical analysis method Part 6.determination of silicon content Inductively coupled 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 15076 "Methods for Chemical Analysis of Tantalum and Niobium" is divided into 16 parts. ---Part 1.Determination of tantalum content in niobium by inductively coupled plasma atomic emission spectrometry; ---Part 2.Determination of the amount of niobium in tantalum inductively coupled plasma atomic emission spectrometry and chromatography gravimetric method; ---Part 3.Determination of copper content by flame atomic absorption spectrometry; ---Part 4.Determination of iron content 1,10-phenanthroline spectrophotometry; ---Part 5.Determination of the amount of molybdenum and tungsten by inductively coupled plasma atomic emission spectrometry; ---Part 6.Determination of silicon content by inductively coupled plasma atomic emission spectrometry; ---Part 7.Determination of phosphorus content in niobium 4-methyl-pentanone-[2] extraction separation phosphomolybdenum blue spectrophotometry and inductively coupled plasma Bulk atomic emission spectroscopy; ---Part 8.Determination of carbon and sulfur content by high-frequency combustion infrared absorption method; ---Part 9.Determination of the amount of iron, chromium, nickel, manganese, titanium, aluminum, copper, tin, lead and zirconium in tantalum by DC arc atomic emission spectrometry; ---Part 10.Determination of the content of iron, nickel, chromium, titanium, zirconium, aluminum and manganese in niobium by DC arc atomic emission spectrometry; ---Part 11.Determination of arsenic, antimony, lead, tin and bismuth in niobium by DC arc atomic emission spectrometry; ---Part 12.Determination of Phosphorus in Tantalum by Ethyl Acetate Extraction and Separation of Phosphomolybdenum Blue Spectrophotometry; ---Part 13.Determination of nitrogen content inert gas fusion thermal conductivity method; ---Part 14.Determination of oxygen content inert gas melting infrared absorption method; ---Part 15.Determination of hydrogen content inert gas fusion thermal conductivity method; ---Part 16.Determination of sodium and potassium content by flame atomic absorption spectrometry. This part is Part 6 of GB/T 15076. This section was drafted in accordance with the rules given in GB/T 1.1-2009. This part replaces GB/T 15076.6-1994 "Methods for chemical analysis of tantalum and niobium-Determination of silicon content in tantalum". This part is consistent with GB/T 15076.6- Compared with.1994, the main technical changes except for editorial changes are as follows. ---The measurement method was changed from "spectrophotometry" to "inductively coupled plasma atomic emission spectrometry"; ---Expanded the measurement range, the measurement range was changed from "0.0005%~0.070%" to "0.0005%~0.50%" (see Chapter 1, Chapter 1 and Chapter 9 of the.1994 edition); ---The reference standard is deleted (see Chapter 2 of the.1994 edition); ---Add sample clause (see Chapter 5); --- Added precision clause (see Chapter 8); ---Added the test report clause (see Chapter 9). 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. Ningxia Dongfang Tantalum Co., Ltd., Guangdong Guangsheng Rare Metal Photoelectric New Material Co., Ltd., Northwest Rare Metal Materials Research Institute Ningxia Co., Ltd., Jiujiang Nonferrous Metal Smelting Co., Ltd., Xi'an Hantang Analysis and Testing Co., Ltd. The main drafters of this section. Zhang Junfeng, Huang Shuang, Xu Ninghui, Zhang Zhong, Wang Qiao, Xie Lu, Jia Menglin, Liu Gang, Zhang Jinju. The previous versions of the standards replaced by this part are as follows. ---GB/T 15076.6-1994. Tantalum-niobium chemical analysis method Part 6.determination of silicon content Inductively coupled plasma atomic emission spectrometry1 ScopeThis part of GB/T 15076 specifies the determination of silicon content in tantalum and niobium by inductively coupled plasma atomic emission spectrometry. This section applies to the determination of silicon content in tantalum, niobium and their hydroxides, oxides, carbides and potassium fluorotantalate. Measuring range. 0.0005%~0.50%.2 PrincipleThe sample is dissolved in nitric acid and hydrofluoric acid, in a dilute acid medium, using argon plasma as the ionization source, and direct inductively coupled plasma Atomic emission spectrometry.3 Reagents or materialsUnless otherwise stated, only reagents confirmed to be MOS grade and laboratory grade 2 water are used in the analysis. 3.1 Nitric acid (ρ=1.42g/mL). 3.2 Hydrofluoric acid (ρ=1.14g/mL). 3.3 Metal tantalum (wTa≥99.99%, wSi≤0.0001%). 3.4 Niobium metal (wNb≥99.99%, wSi≤0.0001%). 3.5 Silicon standard storage solution. Weigh 2.1394g silica (wSiO2≥99.99%) into a platinum crucible, add 10g sodium carbonate-potassium carbonate Mix the flux, mix well, melt on the blowtorch until it is clear, then burn for 10 minutes. After cooling, immerse with hot water, heat until the solution is clear, and move after cooling Put it into a 1000mL volumetric flask, dilute to the mark with water, and mix well. 1mL of this solution contains 1mg of silicon. Store in a polyethylene bottle. 3.6 Silicon standard solution. Pipette 10.00mL silicon standard stock solution (3.5) in a 100mL volumetric flask, dilute to the mark with water, and mix. 1mL of this solution contains 100μg of silicon. Store in a polyethylene bottle. 3.7 Argon (volume fraction not less than 99.99%).4 Equipment4.1 Inductively coupled plasma atomic emission spectrometer, equipped with hydrofluoric acid resistant sampling system, resolution < 0.006nm (200nm). 4.2 The recommended silicon analysis line is 251.612nm.5 samples5.1 The particle size of tantalum powder is less than 700μm; the particle size of niobium powder is less than 180μm; the particle size of tantalum-niobium carbide is less than 150μm. 5.2 Tantalum powder should be dried in vacuum at 80℃~150℃ for 4h in advance, cooled to room temperature, and vacuum packaged in a composite aluminum foil bag; Substances, oxides and potassium fluorotantalate should be pre-baked at 105°C~110°C for 2h, and placed in a desiccator to cool to room temperature for later use. 5.3 From the top 10cm of the niobium ingot to any part of the middle, use a planer to remove the skin and sample the shavings. The size of the shavings should be uniform, and And the particles should be as small as possible.6 Test procedure6.1 Sample Weigh the sample according to Table 1, accurate to 0.0001g. 6.2 Parallel test Do two tests in parallel and take the average value. 6.3 Blank test Weigh the metal tantalum (3.3) or metal niobium (3.4) equivalent to the sample, and do a blank test with the sample. 6.4 Preparation of analysis test solution 6.4.1 Place the tantalum-niobium sample (6.1) in a 100mL polyethylene/PTFE beaker and moisten it with a little water. 6.4.2 Slowly add 2mL of nitric acid (3.1), and 4mL of hydrofluoric acid (3.2) dropwise. After the violent reaction stops, place in a water bath not higher than 60℃ Heat to complete dissolution, remove and cool, add 2mL nitric acid (3.1). Transfer the solution into a 100mL polyethylene volumetric flask and dilute with water to Scale and mix well. When the oxide is not easy to dissolve to clarification by this method, a hot-pressure digestion device can be used to dissolve the sample. 6.5 Drawing of working curve 6.5.1 Working curve I According to Table 1, weigh 6 parts of metal tantalum (3.3) or metal niobium (3.4) equivalent to the sample, and place them in 6 100mL polyethylene plastic bottles. Add 0mL, 0.050mL, 0.20mL, 0.50mL, 2.00mL, 5.00mL silicon standard solution (3.6) respectively, the following steps are according to 6.4.2 operating. 6.5.2 Working curve Ⅱ According to Table 1, weigh 6 parts of metal tantalum (3.3) or metal niobium (3.4) equivalent to the sample, and place them in 6 100mL polyethylene plastic bottles. Add 0mL, 0.50mL, 1.00mL, 2.00mL, 5.00mL, 10.00mL silicon standard solution (3.6) respectively, the following steps follow 6.4.2 operating. 6.6 Determination After the instrument is optimized, according to the recommended analysis line, measure the emitted light intensity of the measured element in the standard series of the working curve drawn from low to high. Taking the mass concentration as the abscissa and the intensity of the emitted light from the analysis line as the ordinate, the computer automatically draws the working curve. When the linear relationship of the working curve When it reaches above 0.999, measure the emitted light intensity of the measured element in the sample blank solution (6.3) and sample solution (6.4.2), and the computer will automatically Calculate the mass concentration of the measured element from the working curve.7 Test data processingThe silicon content is calculated as the mass fraction of silicon wSi, calculated according to formula (1). When wSi< 0.010%, the result obtained is kept to four decimal places; when wSi≥0.010%, the result obtained keeps three significant digits.8 Precision8.1 Repeatability The measured values of two independent test results obtained under repeatability conditions are within the average range given in Table 2.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) adopts the line according to the data in Table 2 Obtained by sexual interpolation or extension method. 8.2 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.9 Test reportThe test report should include the following. ---Test object; ---This part number; ---result; --- Anomalies observed; ---Test date. ......Tips & Frequently Asked Questions:Question 1: How long will the true-PDF of GB/T 15076.6-2020_English be delivered?Answer: Upon your order, we will start to translate GB/T 15076.6-2020_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 15076.6-2020_English with my colleagues?Answer: Yes. The purchased PDF of GB/T 15076.6-2020_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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