YS/T 896-2013 English PDF (YST896-2013)

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YS/T 896-2013: Methods for chemical analysis of high purity niobium. Determination of trace impurity element content. Inductively coupled plasma mass spectrometry
YS/T 896-2013
YS
NONFERROUS METAL INDUSTRY STANDARD
OF THE PEOPLE’S REPUBLIC OF CHINA
ICS 77.120.99
H 63
Methods for Chemical Analysis of High Purity Niobium -
Determination of Trace Impurity Element Content -
Inductively Coupled Plasma Mass Spectrometry
ISSUED ON: OCTOBER 17, 2013
IMPLEMENTED ON: MARCH 1, 2014
Issued by: Ministry of Industry and Information Technology of the People’s
Republic of China
Table of Contents
Foreword ... 3
1 Scope ... 4
2 Method Summary ... 4
3 Reagents ... 4
4 Instruments ... 5
5 Specimens ... 6
6 Analytical Procedures ... 6
7 Calculation of Analytical Results ... 7
8 Allowable Difference ... 7
9 Test Report ... 7
Methods for Chemical Analysis of High Purity Niobium -
Determination of Trace Impurity Element Content -
Inductively Coupled Plasma Mass Spectrometry
1 Scope
This Standard stipulates the method for the determination of lithium, beryllium, boron,
magnesium, titanium, vanadium, manganese, iron, cobalt, nickel, copper, zinc, gallium, arsenic,
strontium, zirconium, tantalum, molybdenum, cadmium, tin, antimony, hafnium, tungsten, lead
and bismuth in high purity niobium.
This Standard is applicable to the determination of trace impurity element content in high purity
niobium. The determination range is 0.0001% ~ 0.010%.
2 Method Summary
Use nitric acid and hydrofluoric acid to dissolve the test portion, use rhodium internal standard
for calibration, and conduct direct determination through an inductively coupled plasma mass
spectrometer. In accordance with the working curve method, calculate the mass concentration
of each element, and express the determination result as mass fractions.
3 Reagents
Unless otherwise stated, the reagents used in the analysis are guaranteed reagents; the water
used is Grade-1 water.
3.1 Hydrofluoric acid ( = 1.16 g/mL).
3.2 Nitric acid ( = 1.42 g/mL).
3.3 Nitric acid (1 + 1).
3.4 Lithium, beryllium, boron, magnesium, titanium, vanadium, manganese, iron, cobalt, nickel,
copper, zinc, gallium, arsenic, strontium, zirconium, tantalum, molybdenum, cadmium, tin,
antimony, hafnium, tungsten, lead, bismuth and rhodium single-element standard storage
solution (national standard sample / national reference substance), the mass concentration is
1,000 g/mL.
3.5 Mixed standard solution A: respectively transfer-take 10.00 mL of each element of standard
storage solution (except rhodium) (3.4) in 1,000 mL plastic volumetric flasks, add 2 mL of
hydrofluoric acid (3.1) and 20 mL of nitric acid (3.3); use water to dilute to the scale and mix
5 Specimens
The specimens are processed into chips with a side length not exceeding 2 mm.
6 Analytical Procedures
6.1 Test Portion
Weigh-take 0.10 g of specimen, accurate to 0.0001 g.
6.2 Number of Determinations
Independently carry out two determinations and take the average value.
6.3 Blank Test
Carry out a blank test along with the test portion.
6.4 Preparation of Solutions
6.4.1 Preparation of test portion solution
Place the test portion (6.1) in a 50 mL plastic beaker, add a small amount of water, 2 mL of
nitric acid (3.2) and 2 mL of hydrofluoric acid (3.1), heat to completely dissolve the test portion,
and cool it. Transfer to a 100 mL plastic volumetric flask, add 1.00 mL of rhodium internal
standard solution (3.7), use water to dilute to the scale, and mix it well.
6.4.2 Preparation of standard series solutions
Transfer-take 0 mL, 0.20 mL, 0.50 mL, 1.00 mL, 2.00 mL, 5.00 mL and 10.00 mL of the mixed
standard solution B (3.6) in a series of 100 mL plastic volumetric flasks. Respectively add 1.00
mL of the rhodium internal standard solution (3.7), use water to dilute to the scale and mix it
well.
6.5 Measurement
6.5.1 On the inductively coupled plasma mass spectrometer, after the instrument stably operates,
under the selected instrument operating conditions, in accordance with the recommended
isotope mass numbers shown in Table 1, use the prepared standard series solutions (6.4.2) to
standardize or calibrate the working curve. The correlation coefficient of the working curve of
each element shall be above 0.999, otherwise, it is necessary to re-standardize or re-prepare
standard series solutions for standardization.
6.5.2 Determine the analytical test solution (6.4.1) and blank test solution. The instrument
automatically processes data in accordance with the working curve, calculates and outputs the
mass concentration of each element.