GB/T 15076.1-2017 English PDF (GBT15076.1-2017)

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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
GB/T 15076.1-2017
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):