SN/T 3321.1-2012 PDF English
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Limestone and dolomite. Part 1: Determination of magnesium, silicon, aluminum, iron, manganese and phosphorus content. Inductively coupled plasma atomic emission spectrometry
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SN/T 3321.1-2012: PDF in English (SNT 3321.1-2012) SN/T 3321.1-2012
SN
ENTRY AND EXIT INSPECTION AND QUARANTINE INDUSTRY
STANDARD OF THE PEOPLE’S REPUBLIC OF CHINA
Limestone and dolomite - Part 1: Determination of
magnesium, silicon, aluminum, iron, manganese and
phosphorus content - Inductively coupled plasma
atomic emission spectrometry
ISSUED ON: DECEMBER 12, 2012
IMPLEMENTED ON: JULY 01, 2013
Issued by: General Administration of Quality Supervision, Inspection and
Quarantine of PRC
Table of 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
Limestone and dolomite - Part 1: Determination of
magnesium, silicon, aluminum, iron, manganese and
phosphorus content - Inductively coupled plasma
atomic emission spectrometry
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 (ρ = 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
......
Source: Above contents are excerpted from the PDF -- translated/reviewed by: www.chinesestandard.net / Wayne Zheng et al.
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