SN/T 2697-2010 English PDF (SNT2697-2010)

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SN/T 2697-2010: Determination of sulfur, phosphorus, arsenic and chloride in coal for import and export. X-ray fluorescence spectrometric method
SN/T 2697-2010
SN
ENTRY-EXIT INSPECTION AND QUARANTINE INDUSTRY
STANDARD OF THE PEOPLE’S REPUBLIC OF CHINA
Determination of Sulfur, Phosphorus, Arsenic and Chloride
in Coal for Import and Export – X-Ray Fluorescence
Spectrometric Method
ISSUED ON: NOVEMBER 1, 2010
IMPLEMENTED ON: MAY 1, 2011
Issued by: General Administration of Quality Supervision, Inspection and
Quarantine of the People's Republic of China
Table of Contents
Foreword ... 3
1 Scope ... 4
2 Normative References ... 4
3 Method Summary ... 5
4 Reagents and Materials ... 5
5 Apparatus ... 5
6 Sampling and Sample Preparation ... 5
7 Preparation of Specimen ... 6
8 Analytical Procedures ... 6
9 Measurement ... 7
10 Calculation of Results... 7
11 Precision ... 7
Appendix A (Informative) Preparation of Standard Sample ... 8
Appendix B (Informative) Measurement Conditions of X-Ray Fluorescence
Spectrometer ... 10
Determination of Sulfur, Phosphorus, Arsenic and Chloride
in Coal for Import and Export – X-Ray Fluorescence
Spectrometric Method
1 Scope
This Standard specifies the X-ray fluorescence spectrometric method for determination of
sulfur, phosphorus, arsenic and chloride in coal.
This Standard is applicable to the determination of sulfur, phosphorus, arsenic and chlorine
content in imported and exported bitumite, anthracite and lignite. The measurement range of
each element is shown in Table 1.
Table 1 – Measurement Range of Each Element
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
Document.
GB/T 212 Proximate analysis of coal
GB/T 474 Preparation method of coal sample
GB/T 475 Method for manual sampling of commercial coal
GB/T 483 General rules for analytical and testing methods of coal
GB/T 6682 Water for analytical laboratory use - Specification and test methods
Element Measurement range (mass fraction)
GB/T 16597 Analytical methods of metallurgical products - General rule for X-ray
fluorescence spectrometric methods
3 Method Summary
Grind the coal sample to a certain fineness and press it into sheets; and measure the X-ray
fluorescence intensity of the element to be measured. Based on the quantitative relationship
between the X-ray fluorescence intensity of the element to be measured and the content of the
element to be measured, the regression equation and mathematical correction mode are selected
to calculate the content of the element to be measured.
4 Reagents and Materials
Unless otherwise specifies, all the used reagents are analytically pure, while water is Class-II
water specified in GB/T 6682.
4.1 Silicon dioxide, reference reagent; burn for 1h at 1000°C; and store in the dryer.
4.2 Sodium chloride, reference reagent; bake to constant weight at 500°C; and store in the dryer.
4.3 Boric acid, bake for 1h at 105°C; and store in the dryer.
4.4 Microcrystalline cellulose.
4.5 Gas, the gas ratio used by the flow counter is a mixture of 90% argon and 10% methane.
5 Apparatus
5.1 Wavelength dispersive X-ray fluorescence spectrometer, in compliance with the provisions
of GB/T 16597.
5.2 Analytical balance, sensitivity is 0.2mg.
5.3 Tablet press, the pressure is no less than 200kN.
5.4 Grinding facilities, agate, corundum or tungsten carbide mortar and pestle; automatic
grinding equipment can also be used.
6 Sampling and Sample Preparation
Sampling and sample preparation shall be carried out in accordance with the provisions of GB/T
475 and GB/T 474. The particle size shall be less than 0.2mm.
7 Preparation of Specimen
Place the air-dried coal sample (Clause 6) in the mortar (5.4) of the grinding facility and grind
it to a particle size less than 75μm.
8 Analytical Procedures
8.1 Determination of moisture content in the specimen
Test the moisture content of the specimen (Clause 7) according to the provisions of GB/T 212.
Weigh a certain amount of air-dried coal sample (Clause 6), place it in a 105°C oven; and dry
it in the air flow to constant weight. The moisture content shall be calculated according to the
mass loss of the specimen.
8.2 Preparation of specimen sheet
Accurately weigh 7g of the ground specimen (Clause 7) and 1g of microcrystalline cellulose in
the mortar (5.4) of the grinding facility, accurate to 0.2mg. After grinding until fully mixed,
weigh about 6g, accurate to 0.1g; rim with boric acid (4.3) as the base; and press with a tablet
press (5.3) under a pressure of 300kN for 40 s to form a specimen sheet. Use an ear cleaning
ball to blow away any particulate matter that may be present on the surface and place it in a
dryer. Avoid contact with the surface of the specimen to prevent contamination and damage to
the specimen sheet.
After preparing the specimen sheet, visually inspect whether the specimen is smooth and flat.
If the test piece has defects such as cracks or falling off, it shall be discarded and a new qualified
specimen sheet shall be prepared.
8.3 Preparation of standard sample sheet
The selected standard samples shall cover the content range of each element given in Table 1.
The serial standard samples are formed by using coal certified reference materials, coal certified
reference materials compounded with coal certified reference materials and mixed with silicon
dioxide (4.1), sodium chloride (4.2) and other methods, see Appendix A.
Prepare standard samples into standard sample sheets according to 8.2.
8.4 Drawing of standard curve
8.4.1 Measurement conditions
The measurement conditions for the characteristic spectral lines of each element were obtained
through optimization, see Appendix B.
8.4.2 Preparation and calibration of standard curve