SN/T 3321.1-2012Limestone and dolomite - Part 1: Determination of magnesium, silicon, aluminum, iron, manganese and phosphorus content - Inductively coupled plasma atomic emission spectrometry (English PDF)
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Issued by
General Administration of Quality Supervision, Inspection and Quarantine of PRC
Level / Type
National · Recommended
Issue date
December 12, 2012
Implementation date
July 1, 2013
Scope
SN/T 3321.1-2012 (Limestone and dolomite - Part 1: Determination of magnesium, silicon, aluminum, iron, manganese and phosphorus content - Inductively coupled plasma atomic emission spectrometry) is available as an English-translated PDF.
SN/T 3321.1-2012 is the Chinese standard "Limestone and dolomite - Part 1: Determination of magnesium, silicon, aluminum, iron, manganese and phosphorus content - Inductively coupled plasma atomic emission spectrometry".
Its scope clause reads: This Part of SN/T 3321 specifies a method for the determination of magnesium, silicon, aluminum, iron, manganese, phosphorus content in limestone and dolomite, by inductively coupled plasma atomic emission spectrometry (ICP- AES).
This Part applies to the determination of magnesium, silicon, aluminum, iron, manganese, phosphorus content in limestone and dolomite. The measurement range of each element is as shown in Table 1.
Its clauses include method summary; reagents and materials; instruments and equipment; preparation of specimen; analytical procedures. It was issued by the General Administration of Quality Supervision, Inspection and Quarantine of PRC on 2012-12-12 and took effect on 2013-07-01.
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Document preview — SN/T 3321.1-2012
National Standard of the People's Republic of China
Issued by: General Administration of Quality Supervision, Inspection and Quarantine of PRC
Contents
- Foreword...3
- 1 Scope...4
- 2 Normative references...4
- 3 Method summary...5
- 4 Reagents and materials...5
- 5 Instruments and equipment...5
- 6 Preparation of specimen...6
- 7 Analytical procedures...6
- 8 Result calculation...8
- 9 Result representation...8
- 10 Precision...8
- Appendix A (Informative) Reference wavelength of element...10
- Appendix B (Informative) Reference working conditions of instrument...11
- Appendix C (Informative) Preparation of calibration curve series solutions...12
1 Scope
This Part of SN/T 3321 specifies a method for the determination of magnesium, silicon, aluminum, iron, manganese, phosphorus content in limestone and dolomite, by inductively coupled plasma atomic emission spectrometry (ICP-
AES).
This Part applies to the determination of magnesium, silicon, aluminum, iron, manganese, phosphorus content in limestone and dolomite. The measurement range of each element 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 2007.2 General rules for the sampling and sample preparation of minerals in bulk - Manual method of sample preparation
GB/T 6682 Water for analytical laboratory use - Specification and test methods
3 Method summary
The specimen is melted by lithium metaborate, leached by diluted nitric acid;
the test solution is measured by inductively coupled plasma atomic emission spectrometer; the content of each element is determined according to the calibration curve.
4 Reagents and materials
Unless otherwise specified, only use excellent grade pure reagents; the experimental water shall meet the requirements of grade-2 water, which are specified in GB/T 6682.
4.1 Lithium metaborate (purity > 99.99%).
4.2 Nitric acid (rho = 1.42 g/mL).
4.3 Nitric acid solution (1 + 9).
4.4 Nitric acid solution (5 + 95).
4.5 Single-element standard solution (1000 µg/mL): Standard solutions of
magnesium, silicon, aluminum, iron, manganese, phosphorus shall be prepared, according to the method of GB/T 602; OR it may directly purchase certified standard solutions.
4.6 Manganese standard stock solution (100 µg/mL): Accurately pipette 10 mL
of manganese standard solution (4.5) into a 100 mL volumetric flask. Use nitric acid solution (4.4) to dilute it to the mark. Mix well. 1 mL of this solution contains
100 µg of manganese.
4.7 Phosphorus standard stock solution (100 µg/mL): Accurately pipette 10 mL
of phosphorus standard solution (4.5) into a 100 mL volumetric flask. Use nitric acid solution (4.4) to dilute it to the mark. Mix well. 1 mL of this solution contains
100 µg of phosphorus.
5 Instruments and equipment
5.1 Inductively coupled plasma atomic emission spectrometer: The instrument
shall be able to provide a stable plasma moment flame. The analysis wavelength parameters of each element are as shown in Appendix A. See
Appendix B for the working conditions of the instrument.
5.2 Analytical balance: The accuracy is 0.1 mg.
5.3 Platinum crucible.
5.4 High temperature furnace: The use temperature is 1000 °C.
5.5 Electrothermal magnetic stirrer.
5.6 Stirring magnet, 10 mm long, coated with Teflon.
6 Preparation of specimen
6.1 Prepare the specimen, according to GB/T 2007.2.
6.2 The specimen shall be processed to a particle size of less than 0.125 mm.
6.3 Limestone and dolomite specimens shall be dried at 105 °C ~ 110 °C, for 2 h before analysis; then cooled to room temperature in a desiccator.
7 Analytical procedures
7.1 Amount of sample
Weigh 0.1 g of sample, accurate to 0.1 mg.
Carry out parallel determinations on two sets of samples.
7.2 Blank test
Except that the sample to be tested is not added, the blank test is carried out according to step 7.3.
7.3 Sample decomposition and preparation of test solution
7.3.1 Place the sample (7.1) in a platinum crucible (5.3). Add 0.6 g of lithium metaborate (4.1). Mix well. Add a platinum cover. Place the platinum crucible in a high-temperature furnace. Gradually increase the furnace temperature to
1000 °C. Melt it for 10 min. Take it out. Cool it.
7.3.2 Use water to rinse the outer wall of the platinum crucible. Put the magnetic stirrer (5.6) into the platinum crucible. Place the platinum crucible and the platinum cover in a 300 mL beaker. Add 50 mL of nitric acid solution (4.3). Cover a watch glass. Heat it while stirring on a magnetic stirrer-electric hot plate, until
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This preview omits tables, figures, formulas and parts of the technical clauses. The complete document — 12 pages — is available in the English PDF.
Referenced standards
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