GB/T 8647.11-2019 PDF English
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Methods for chemical analysis of nickel -- Part 11: Determination of magnesium, aluminum, manganese, cobalt, copper, zinc, cadmium, tin, antimony, lead, bismuth contents -- Inductively coupled plasma mass spectrometry
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GB/T 8647.11-2019: Methods for chemical analysis of nickel -- Part 11: Determination of magnesium, aluminum, manganese, cobalt, copper, zinc, cadmium, tin, antimony, lead, bismuth contents -- Inductively coupled plasma mass spectrometry
---This is an excerpt. Full copy of true-PDF in English version (including equations, symbols, images, flow-chart, tables, and figures etc.), auto-downloaded/delivered in 9 seconds, can be purchased online: https://www.ChineseStandard.net/PDF.aspx/GBT8647.11-2019
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 77.120.40
H 13
GB/T 8647.11-2019
Methods for chemical analysis of nickel - Part 11.
Determination of magnesium, aluminum, manganese, cobalt,
copper, zinc, cadmium, tin, antimony, lead, bismuth contents
- Inductively coupled plasma mass spectrometry
Issued on: DECEMBER 31, 2019
Implemented on: NOVEMBER 01, 2020
Issued by. State Administration for Market Regulation;
Standardization Administration of the People’s Republic of China.
Table of Contents
Foreword... 3
1 Scope... 5
2 Method summary... 5
3 Reagents or materials... 5
4 Instrumentation... 6
5 Sample... 6
6 Test procedure... 7
7 Test data processing... 8
8 Precision... 8
9 Test report... 9
Foreword
GB/T 8647 “Methods for chemical analysis of nickel” is divided into 11 parts.
- Part 1.Determination of iron content - Sulfosalicylic acid spectrophotometric
method;
- Part 2.Determination of aluminium content - Electrothermal atomic absorption
spectrometric method;
- Part 3.Determination of silicon content - Molybdenum blue spectrophotometric
method;
- Part 4.Determination of phosphorous content - Molybdenum blue
spectrophotometric method;
- Part 5.Determination of magnesium content - Flame atomic absorption
spectrometric method;
- Part 6.Determination of cadmium, cobalt, copper, manganese, lead and zinc
contents - Flame atomic absorption spectrometric method;
- Part 7.Determination of arsenic, antimony, bismuth, tin and lead contents -
Electrothermal atomic absorption spectrometric method;
- Part 8.Determination of sulphur content - Infra-red absorption method after high
frequency induction furnace combustion;
- Part 9.Determination of carbon content - Infra-red absorption method after high
frequency induction furnace combustion;
- Part 10.Determination of arsenic, cadmium, lead, zinc, antimony, bismuth, tin,
cobalt, copper, manganese, magnesium, silicon, aluminium, iron contents - Atomic
emission spectrometric method;
- Part 11.Determination of magnesium, aluminum, manganese, cobalt, copper, zinc,
cadmium, tin, antimony, lead, bismuth contents - Inductively coupled plasma mass
spectrometry.
This Part is Part 11 of GB/T 8647.
This Part was drafted in accordance with the rules given in GB/T 1.1-2009.
This Part was proposed by China Nonferrous Metals Industry Association.
This Part shall be under the jurisdiction of the National Technical Committee on
Nonferrous Metals of Standardization Administration of China (SAC/TC 243).
Methods for chemical analysis of nickel - Part 11.
Determination of magnesium, aluminum, manganese, cobalt,
copper, zinc, cadmium, tin, antimony, lead, bismuth contents
- Inductively coupled plasma mass spectrometry
1 Scope
This Part of GB/T 8647 specifies the methods for the determination of magnesium,
aluminum, manganese, cobalt, copper, zinc, cadmium, tin, antimony, lead, and bismuth
contents in nickel.
This Part applies to the determination of magnesium, aluminum, manganese, cobalt,
copper, zinc, cadmium, tin, antimony, lead, and bismuth contents in nickel. The
determination range is 0.00010 % ~ 0.0050 %.
2 Method summary
Dissolve the sample in nitric acid, on an inductively coupled plasma mass spectrometer,
using the working curve method and the method of online addition of an internal
standard mixed solution of scandium, rhodium, and rhenium, determine the contents of
magnesium, aluminum, manganese, cobalt, copper, zinc, cadmium, tin, antimony, lead,
and bismuth in the test solution.
3 Reagents or materials
Unless otherwise specified, the water used in the analysis is grade 1 water or water of
equivalent purity. All test instruments are thoroughly rinsed with hot nitric acid and then
rinsed with water.
3.1 Nitric acid (ρ = 1.42 g/mL), MOS grade.
3.2 Nitric acid (1 + 1).
3.3 Standard stock solution. Use valid, certified single-element standard stock solutions
of magnesium, aluminum, manganese, cobalt, copper, zinc, cadmium, tin, antimony,
lead, bismuth, scandium, rhodium, and rhenium, with a mass concentration of 1000
μg/mL.
3.4 Mixed standard solution A. Respectively transfer 1.00 mL of each standard stock
solution (3.3) of magnesium, aluminum, manganese, cobalt, copper, zinc, cadmium, tin,
antimony, lead, and bismuth into a 100 mL volumetric flask containing 10 mL of nitric
acid (3.2), dilute to the mark with water, and mix thoroughly. 1 mL of this solution
contains 10 μg of magnesium, aluminum, manganese, cobalt, copper, zinc, cadmium,
tin, antimony, lead, and bismuth respectively.
3.5 Mixed standard solution B. Respectively transfer 1.00 mL of each mixed standard
solution A (3.4) into a 100 mL volumetric flask containing 10 mL of nitric acid (3.2),
dilute to the mark with water, and mix thoroughly. 1 mL of this solution contains 100
ng of magnesium, aluminum, manganese, cobalt, copper, zinc, cadmium, tin, antimony,
lead, and bismuth respectively.
3.6 Internal standard mixed standard solution. Use the standard stock solution of
scandium, rhodium, and rhenium (3.3) with a mass concentration of 1000 μg/mL, dilute
sequentially before use, so that 1 mL of the diluted solution contains 10 ng of scandium,
rhodium, and rhenium respectively. The medium is nitric acid (2 + 98).
3.7 Argon (wAr ≥ 99.99 %).
4 Instrumentation
4.1 Inductively coupled plasma mass spectrometer, with an instrument mass resolution
of not less than 0.8 amu ± 0.1 amu.
4.2 The recommended mass numbers for isotope determination of magnesium,
aluminum, manganese, cobalt, copper, zinc, cadmium, tin, antimony, lead, bismuth,
scandium, rhenium, and rhodium are shown in Table 1.
5 Sample
The sample shall be in the form of crumbs or powder.
6 Test procedure
6.1 Test material
Weigh 1.00 g of the sample, to the nearest 0.0001 g.
6.2 Parallel test
Perform two tests in parallel.
6.3 Blank test
Perform a blank test along with the test material.
6.4 Determination
6.4.1 Place the test material (6.1) in a 100 mL polytetrafluoroethylene or quartz beaker,
add 20.0 mL of nitric acid (3.2), and heat at low temperature until the test material is
completely dissolved. Remove the beaker, cool down and transfer to a 100 mL plastic
volumetric flask, dilute to the mark with water, and mix thoroughly.
6.4.2 Take 10.00 mL of the test solution (6.4.1) into a 100 mL plastic volumetric flask,
add 2.0 mL of nitric acid (3.1), dilute to the mark with water, and mix thoroughly.
6.4.3 Under the selected instrument operating conditions, according to the isotope mass
numbers recommended in Table 1, using the working curve method and the method of
online addition of the internal standard mixed standard solution (3.6), determine the test
solution (6.4.2) and the blank test solution (6.3) simultaneously with the series standard
solutions. The instrument automatically calculates the mass concentration of each
determined element in the test solution based on the working curve.
6.5 Plotting of working curve
6.5.1 Respectively transfer 0 mL, 1.00 mL, 5.00 mL, 10.00 mL, and 20.00 mL of mixed
standard solution B (3.5) and 0.50 mL of mixed standard solution A (3.4) to a set of 100
mL plastic volumetric flasks, add 2.0 mL of nitric acid (3.1), dilute to the mark with
water, and mix thoroughly.
6.5.2 On an inductively coupled plasma mass spectrometer, under the selected
instrument operating conditions, according to the isotope mass numbers recommended
in Table 1, using the method of online addition of the internal standard mixed standard
solution (3.6), determine the series standard solutions (6.5.1). The instrument
automatically plots the working curve. The correlation coefficient of the working curve
for each element shall be above 0.999, otherwise the determination shall be repeated,
or the series standard solutions shall be re-prepared for determination.
...... Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al.
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