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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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GB/T 6730.72-2016English130 Add to Cart 0-9 seconds. Auto-delivery. Iron ores -- Determination of arsenic, chromium, cadmium, lead and mercury content -- Inductively coupled plasma-mass spectrometry method (ICP-MS) Valid
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.