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GB/T 15076.1-2017 PDF English

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GB/T 15076.1-2017: Methods for chemical analysis of tantalum and niobium -- Part 1: Determination of tantalum content in niobium -- Inductively coupled plasma atomic emission spectrometry
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GB/T 15076.1: Evolution and historical versions

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GB/T 15076.1-2017English105 Add to Cart 0-9 seconds. Auto-delivery Methods for chemical analysis of tantalum and niobium -- Part 1: Determination of tantalum content in niobium -- Inductively coupled plasma atomic emission spectrometry Valid
GB/T 15076.1-1994English239 Add to Cart 3 days Methods for chemical analysis of tantalum and niobium. Determihation of tantalum content in niobium Obsolete

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GB/T 15076.1-2017: Methods for chemical analysis of tantalum and niobium -- Part 1: Determination of tantalum content in niobium -- Inductively coupled plasma atomic emission spectrometry


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GB NATIONAL STANDARD OF THE PEOPLE’S REPUBLIC OF CHINA ICS 77.120.99 H 14 Replacing GB/T 15076.1-1994 Methods for Chemical Analysis of Tantalum and Niobium - Part 1: Determination of Tantalum Content in Niobium - Inductively Coupled Plasma Atomic Emission Spectrometry ISSUED ON: OCTOBER 14, 2017 IMPLEMENTED ON: MAY 1, 2018 Issued by: General Administration of Quality Supervision, Inspection and Quarantine of the People’s Republic of China; Standardization Administration of the People’s Republic of China.

Table of Contents

Foreword ... 3 1 Scope ... 5 2 Method Summary ... 5 3 Reagents and Materials ... 5 4 Instruments ... 6 5 Specimens ... 6 6 Analytical Procedures ... 6 7 Calculation of Analytical Results ... 7 8 Precision ... 8 9 Test Report ... 9

Foreword

GB/T 15076 Methods for Chemical Analysis of Tantalum and Niobium is divided into 16 parts: ---Part 1: Determination of Tantalum Content in Niobium - Inductively Coupled Plasma Atomic Emission Spectrometry; ---Part 2: Determination of Niobium Content in Tantalum - Inductively Coupled Plasma Atomic Emission Spectrometry and Stratography Gravimetry; ---Part 3: Determination of Copper Content - Flame Atomic Absorption Spectrometry; ---Part 4: Determination of Iron Content - 1,10-Phenanthroline Spectrophotometry; ---Part 5: Determination of Molybdenum and Tungsten Contents - Inductively Coupled Plasma Atomic Emission Spectrometry; ---Part 6: Determination of Silicon Content - Inductively Coupled Plasma Atomic Emission Spectrometry; ---Part 7: Determination of Phospherus Content in Niobium - 4-Formyloxy-pentyl Keton- [2] Extraction Separation Phosphomolybdate Blue Spectrophotometry and Inductively Coupled Plasma Atomic Emission Spectrometry; ---Part 8: Determination of Carbon and Sulphur Contents; ---Part 9: Determination of Iron, Chromium, Nickel, Manganese, Titanium, Aluminum, Copper, Tin, Lead and Zirconium Contents in Tantalum; ---Part 10: Determination of Iron, Nickel, Chromium, Titanium, Zirconium, Aluminum and Manganese Contents in Niobium - Direct Current Arc Atomic Emission Spectrometry; ---Part 11: Determination of Arsenic, Antimony, Lead, Tin and Bismuth Contents in Niobium - Direct Current Arc Atomic Emission Spectrometry; ---Part 12: Determination of Phosphorus Content in Tantalum; ---Part 13: Determination of Nitrogen Content - Inert Gas Fusion Thermal Conductivity Method; ---Part 14: Determination of Oxygen Content; ---Part 15: Determination of Hydrogen Content; ---Part 16: Determination of Sodium and Potassium Contents. This is Part 1 of GB/T 15076. Methods for Chemical Analysis of Tantalum and Niobium - Part 1: Determination of Tantalum Content in Niobium - Inductively Coupled Plasma Atomic Emission Spectrometry

1 Scope

This Part of GB/T 15076 stipulates the determination method for tantalum content in niobium. This Part is applicable to the determination of tantalum content in niobium, niobium hydroxide and niobium oxide. The determination range is 0.0050% ~ 3.00%.

2 Method Summary

Use nitric acid and hydrofluoric acid to dissolve the test portion. In a dilute acid medium, use argon plasma as the ionization source, and directly conduct the determination through inductively coupled plasma atomic emission spectrometry.

3 Reagents and Materials

Unless otherwise stated, the reagents used in this Part are all guaranteed reagents that comply with national standards or industry standards, and the water used is Grade-2 water. 3.1 Hydrofluoric acid ( = 1.14 g/mL). 3.2 Nitric acid ( = 1.42 g/mL). 3.3 Niobium matrix: wNb  99.99%, wTa  0.0001%. 3.4 Tantalum standard storage solution: accurately weigh-take 1.0000 g of pure tantalum (wTa > 99.99%) in a 250 mL polyethylene beaker, use a polyethylene lid to cover it, and add 10 mL of hydrofluoric acid (3.1). Dropwise add 10 mL of nitric acid (3.2) and dissolve it on 80 C water bath. After complete dissolution, transfer it to a 1,000 mL volumetric flask, use water to dilute it to the scale and mix it well. 1 mL of this solution contains 1 mg of tantalum. Store it in a polyethylene volumetric flask. 3.5 Tantalum standard solution: transfer-take 10.00 mL of tantalum standard storage solution (3.4) into a 100 mL volumetric flask, add 2 mL of hydrofluoric acid (3.1), use water to dilute to the scale, and mix it well. 1 mL of this solution contains 100 g of tantalum. Store it in a polyethylene volumetric flask. 3.6 Argon: volume fraction is not less than 99.99%. 6.4.2 In accordance with Table 1, add hydrofluoric acid (3.1). After the violent reaction stops, dropwise add 4 mL of nitric acid (3.2), heat at a low temperature, until the test portion is completely dissolved, then remove and cool it to room temperature. When the oxide is not easily dissolved to clarity by this method, a hot-pressure digestion device can be used to dissolve the sample. Transfer the solution into a 100 mL polyethylene volumetric flask, use water to dilute to the scale, and mix it well. 6.5 Drawing of Working Curve 6.5.1 0.0050%  wTa < 0.050% In accordance with Table 1, weigh-take 6 portions of the niobium matrix (3.3) equivalent to the test portion, and respectively place them in six 100 mL polytetrafluoroethylene beakers. Respectively add 0 mL, 0.25 mL, 0.50 mL, 1.00 mL, 2.00 mL and 3.00 mL of the tantalum standard solution (3.5), and follow 6.4.2 for the following steps. 6.5.2 0.050% < wTa  0.50% In accordance with Table 1, weigh-take 6 portions of the niobium matrix (3.3) equivalent to the test portion, and respectively place them in six 100 mL polytetrafluoroethylene beakers. Respectively add 0 mL, 1.00 mL, 2.00 mL, 5.00 mL, 10.00 mL and 15.00 mL of the tantalum standard solution (3.5), and follow 6.4.2 for the following steps. 6.5.3 0.50% < wTa  3.00% In accordance with Table 1, weigh-take 6 portions of the niobium matrix (3.3) equivalent to the test portion, and respectively place them in six 100 mL polytetrafluoroethylene beakers. Respectively add 0 mL, 0.25 mL, 0.50 mL, 1.00 mL, 2.00 mL and 3.00 mL of the tantalum standard storage solution (3.4), and follow 6.4.2 for the following steps. 6.6 Determination After the instrument is optimized, in accordance with the recommended analysis line, from low to high, measure the emission intensity of tantalum in the standard series that draws the working curve. Take the mass concentration of tantalum as the x-coordinate and the emission intensity of the analysis line as the y-coordinate, and have a computer automatically draw the working curve. When the correlation coefficient of the working curve reaches above 0.999, measure the emission intensity of tantalum in the test portion blank (6.3) solution and the test portion solution (6.4.2), and the computer automatically calculates the mass concentration of tantalum from the working curve.

7 Calculation of Analytical Results

The tantalum content is calculated based on the mass fraction of tantalum wTa and in accordance with Formula (1): ......
Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al.


      

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