Ferromanganese,manganese-silicon alloy and manganese——Determination the content of manganese,silicon,iron and phosphorous——The X-ray fluorescence spectrometry method
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This standard is drafted in accordance with the rules given in GB/T 1.1-2009.
This standard was proposed by China Iron and Steel Industry Association.
This standard is under the jurisdiction of National Technical Committee on Pig Iron and Iron Alloy of Standardization Administration of China (SAC/TC 318).
Ferromanganese, manganese-silicon alloy and manganese metal—
Determination of the content of manganese, silicon, iron and phosphorous—
The X-ray fluorescence spectrometry method
Warning——Persons using this standard shall be familiar with normal laboratory practice. This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user to establish appropriate safety and health practices and to ensure compliance with any national regulatory conditions.
1 Scope
This standard specifies the determination of the content of manganese, silicon, iron and phosphorous in ferromanganese, manganese-silicon alloy and manganese metal by the X-ray fluorescence spectrometry method (casting glass sheet method).
This standard is applicable to the determination of the content of manganese, silicon, iron and phosphorous in ferromanganese, manganese-silicon alloy and manganese metal. See Table 1 for the determination range of each element.
Table 1 Element and its determination range
Analytical element Determination range (mass fraction)/%
Mn
Si
Fe
P 60.00–98.00
0.15–28.00
1.50–23.00
0.010–0.450
2 Normative references
The following documents are normatively referenced in this document and are indispensable for its application. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies.
GB/T 4010 Ferroallys sampling and preparation of samples for chemical analysis
GB/T 6379.1 Accuracy (trueness and precision) of measurement methods and results—Part 1: General principles and definitions
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 8170 Rules of rounding off for numerical values & expression and judgment of limiting values
GB/T 15000.3 Directives for the work of reference materials (3)—Reference materials—General and statistical principles for certification
GB/T 16597 Analytical methods of metallurgical products—General rule for X-ray fluorescence spectrometric methods
GB/T 28372 Ferroalloys—Sampling and preparation of samples—General rules
YB/T 082 Specification for certified reference materials for metallurgical products analysis
3 Principle
Subjected to pre-oxidized at low temperature, the samples are melted in platinum-gold crucible at high temperature, and cast into glass sheets. The X-ray fluorescence intensity of the elements to be measured in the glass sheet is measured. According to the calibration curve and X-ray fluorescence intensity of the elements to be measured, the mass fractions of manganese, silicon, iron and phosphorus in the samples are calculated.
4 Reagents and materials
Unless otherwise stated, only recognized analytical pure reagents and distilled water of Grade III and above specified in CB/T 6682 or water with equivalent purity shall be used.
4.1 Anhydrous lithium tetraborate, of analytical pure, in anhydrous state, otherwise heat it at 500°C for 4h before use.
4.2 Lithium tetraborate pre-oxidation crucible, selected according to the oxidation mode.
4.3 Lithium carbonate, of analytically pure, in anhydrous state, otherwise, heat it at 200°C for 2h before use.
4.4 Ammonium bromide, 300 g/L.
4.5 High-purity manganese dioxide (MnO2), with purity > 99.99%.
It is heated at 105°C for 2h, then cooled in a dryer.
Foreword i
1 Scope
2 Normative references
3 Principle
4 Reagents and materials
5 Instrument
6 Sampling and sample preparation
7 Preparation of casting glass sheet
8 Preparation of instruments
9 Analytical procedures
10 Calculation and representation of results
11 Precision
12 Test report
Annex A (Normative) Flow chart of acceptance procedures for test result