GB/T 6730.72-2016 PDF in English
GB/T 6730.72-2016 (GB/T6730.72-2016, GBT 6730.72-2016, GBT6730.72-2016)
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Iron ores -- Determination of arsenic, chromium, cadmium, lead and mercury content -- Inductively coupled plasma-mass spectrometry method (ICP-MS)
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Standards related to (historical): GB/T 6730.72-2016
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GB/T 6730.72-2016: PDF in English (GBT 6730.72-2016) GB/T 6730.72-2016
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 73.060.10
D 31
Iron ores - Determination of arsenic, chromium, cadmium,
lead and mercury content - Inductively coupled plasma-mass
spectrometry method (ICP-MS)
(ICP-MS)
ISSUED ON: FEBRUARY 24, 2016
IMPLEMENTED ON: NOVEMBER 01, 2016
Issued by: General Administration of Quality Supervision, Inspection and
Quarantine of PRC;
National Standardization Administration.
Table of Contents
Foreword ... 3
1 Scope ... 4
2 Normative references ... 4
3 Principles ... 5
4 Reagents ... 5
5 Instruments ... 5
6 Sampling and specimen preparation ... 6
7 Analytical procedures ... 6
8 Result calculation ... 8
9 Test report ... 10
Appendix A (Informative) Instrument working conditions and test samples ... 11
Appendix B (Informative) Flow chart for acceptance of specimen analysis value ... 12
Iron ores - Determination of arsenic, chromium, cadmium,
lead and mercury content - Inductively coupled plasma-mass
spectrometry method (ICP-MS)
Warning: Personnel using this Part shall have practical experience in regular
laboratory work. This Part does not address all possible safety issues. Users are
responsible for taking appropriate safety and health measures and ensuring
compliance with the conditions stipulated in relevant national regulations.
1 Scope
This Part of GB/T 6730 specifies the method for the determination of arsenic, chromium,
cadmium, lead, mercury in iron ore, by inductively coupled plasma mass spectrometry
(ICP-MS).
This Part applies to natural iron ore, iron concentrate, sinter and pellets. The
measurement range is as shown in Table 1.
2 Normative references
The following documents are essential to the application of this document. For the dated
documents, only the versions with the dates indicated are applicable to this document;
for the undated documents, only the latest version (including all the amendments) is
applicable to this standard.
GB/T 602 Chemical reagent - Preparations of standard solutions for impurity
GB/T 6379.2 Accuracy (trueness and precision) of measurement methods and
results - Part 2: Basic method for the determination of repeatability and
reproducibility of a standard measurement method
GB/T 6682 Water for analytical laboratory use - Specification and test methods
GB/T 6730.1 Iron ores - Preparation of predried test samples for chemical analysis
GB/T 10322.1 Iron ores - Sampling and sample preparation procedures
GB/T 12806 Laboratory glassware - One-mark volumetric flasks
GB/T 12807 Laboratory glassware - Graduated pipettes
3 Principles
The sample is digested by high-temperature sealed microwave acid. The treated
solution is diluted with dilute nitric acid to constant volume. The 45Sc, 72Ge, 115In, 209Bi
are used as internal standards, to directly carry out ICP-MS measurement.
4 Reagents
Unless otherwise specified, the reagents for analysis shall be of superior purity or
purified to the superior purity level; the water shall comply with the grade 2 water
specified in GB/T 6682.
4.1 Hydrochloric acid, ρ = 1.19 g/mL.
4.2 Hydrofluoric acid, ρ = 1.13 g/mL.
4.3 Nitric acid, ρ = 1.40 g/mL.
4.4 Nitric acid, 2 + 98.
4.5 Standard stock solutions of chromium, arsenic, cadmium, mercury, lead: All are
1000 μg/mL (nitric acid medium, medium volume concentration is about 5%), OR
prepared using certified reference materials within the validity period.
4.6 The 45Sc, 72Ge, 115In, 209Bi standard solution: 1.0 μg/mL (nitric acid medium,
medium volume concentration is about 5%).
4.7 High-purity argon gas, which has a purity not less than 99.999%.
5 Instruments
5.1 General equipment and appliances
Unless otherwise specified, routine laboratory equipment such as volumetric flasks and
pipetting devices shall comply with Level A, which is specified in GB/T 12806 and
GB/T 12807.
5.2 Inductively coupled plasma mass spectrometer
For the instrument parameters and usage conditions, refer to the requirements in
Appendix A. It is equipped with a hydrofluoric acid-resistant sampling system.
5.3 High temperature and pressure microwave digestion furnace
Equipped with polytetrafluoroethylene (PTFE) high temperature resistant pressure
sealed digestion tank (volume not more than 60 mL), its working conditions refer to the
requirements in Appendix A. OR it may use other digestion equipment with the same
function.
6 Sampling and specimen preparation
6.1 Laboratory specimens
Specimens shall be taken and prepared in accordance with GB/T 10322.1. Generally,
the specimen particle size shall be less than 100 μm. If the content of combined water
or easy oxides in the specimen is high, the particle size shall be less than 160 μm.
6.2 Preparation of pre-dried specimens
Thoroughly mix the laboratory specimens. Take specimens using the reduction method.
Dry the specimen at 105 °C ± 2 °C, in accordance with GB/T 6730.1.
7 Analytical procedures
7.1 Sample amount
Weigh 0.1 g ± 0.05 g of pre-dried specimen (see 6.2), accurate to 0.0001 g.
7.2 Number of measurements
Referring to the procedures in Appendix B, measure the same pre-dried specimen at
least twice independently and take the average value.
Note: "Independent" means that the results of the second and subsequent measurements are not
affected by the results of the previous measurements. In this analytical method, this condition
means repeated measurements by the same operator at different times or by different operators,
including the use of appropriate recalibration.
7.3 Blank test and verification test
7.3.1 Blank test: Perform a blank test along with sample analysis.
7.3.2 Verification test: Analyze the same type of standard sample, along with the sample
Note 2: Such standard samples shall not be used, unless it is confirmed that there is no deviation
from the standard value.
The acceptability of the analytical results for each specimen depends on the
acceptability of the analytical results of the corresponding CRM or RM. If the CRM or
RM results fail the accuracy test, the relevant specimen results are unacceptable and the
specimen shall be re-dissolved and measured.
9 Test report
The test report shall include the following information:
a) Name and address of the testing laboratory;
b) Test report release date;
c) The number of this Part;
d) Necessary detailed description of the specimen itself;
e) Analytical results;
f) The number corresponding to the analytical result;
g) Any abnormal characteristics during the measurement process and any operations
not specified in this Part that may affect the analysis results of the specimen or
standard sample.
......
Source: Above contents are excerpted from the PDF -- translated/reviewed by: www.chinesestandard.net / Wayne Zheng et al.
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