GB/T 3286.11-2022 PDF English
US$280.00 · In stock · Download in 9 secondsGB/T 3286.11-2022: Methods for chemical analysis of limestone and dolomite - Part 11: Determination of calcium oxide, magnesium oxide, silicon dioxide, aluminium oxide and iron oxide content - Wavelength dispersive X-ray fluorescence spectrometry (Fused cast bead method) Delivery: 9 seconds. True-PDF full-copy in English & invoice will be downloaded + auto-delivered via email. See step-by-step procedureStatus: Valid GB/T 3286.11: Evolution and historical versions
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| GB/T 3286.11-2022 | English | 280 |
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Methods for chemical analysis of limestone and dolomite - Part 11: Determination of calcium oxide, magnesium oxide, silicon dioxide, aluminium oxide and iron oxide content - Wavelength dispersive X-ray fluorescence spectrometry (Fused cast bead method)
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| GB/T 3286.11-1993 | English | 239 |
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Methods for chemical analysis of limestone and delo-mite The flame atomic absorption spectrometric methodfor the determination of magnesium and iron content
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GB/T 3286.11-2022: Methods for chemical analysis of limestone and dolomite - Part 11: Determination of calcium oxide, magnesium oxide, silicon dioxide, aluminium oxide and iron oxide content - Wavelength dispersive X-ray fluorescence spectrometry (Fused cast bead method)
---This is an excerpt. Full copy of true-PDF in English version (including equations, symbols, images, flow-chart, tables, and figures etc.), auto-downloaded/delivered in 9 seconds, can be purchased online: https://www.ChineseStandard.net/PDF.aspx/GBT3286.11-2022
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 73.080
CCS D 52
GB/T 3286.11-2022
Methods for chemical analysis of limestone and dolomite -
Part 11.Determination of calcium oxide, magnesium oxide,
silicon dioxide, aluminium oxide and iron oxide content -
Wavelength dispersive X-ray fluorescence spectrometry
(Fused cast bead method)
Issued on. MARCH 09, 2022
Implemented on. OCTOBER 01, 2022
Issued by. State Administration for Market Regulation;
Standardization Administration of the People’s Republic of China.
Table of Contents
Foreword... 3
Introduction... 5
1 Scope... 6
2 Normative references... 6
3 Terms and definitions... 7
4 Principle... 7
5 Reagents and materials... 7
6 Instruments and equipment... 8
7 Sampling and sample preparation... 8
8 Preparation of fused cast bead... 9
9 Preparation of instruments... 10
10 Analysis steps... 10
11 Calculation and expression of results... 13
12 Precision... 13
13 Test report... 14
Annex A (informative) Recommended X-ray spectrometer measurement conditions 15
Annex B (normative) Procedure for acceptance of sample analysis results... 16
Annex C (informative) Raw data of precision tests... 17
Bibl
1 Scope
This document specifies the determination of calcium oxide, magnesium oxide, silicon
dioxide, aluminium oxide and iron oxide content in limestone and dolomite by
wavelength dispersive X-ray fluorescence spectrometry.
This document applies to the determination of calcium oxide, magnesium oxide, silicon
dioxide, aluminium oxide and iron oxide content in limestone and dolomite. The
determination range is shown in Table 1.
2 Normative references
The following referenced documents are indispensable for the application of this
document. For dated references, only the edition cited applies. For undated references,
the latest edition of the referenced document (including any amendments) applies.
GB/T 2007.2 General rules for the sampling and sample preparation of minerals in
bulk - Sample preparation by manual 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 judgement
of limiting values
GB/T 15000.3 Directives for the work of reference materials - Part 3.Reference
materials - Characterization and assessment of homogeneity and stability
GB/T 16597 Analytical methods of metallurgical products - General rule for X-ray
fluorescence spectrometric methods
JJG 810 Wavelength dispersive X-ray fluorescence spectrometers
YB/T 082 Specification for certified reference materials for metallurgical product
analysis
3 Terms and definitions
There are no terms or definitions to be defined in this document.
4 Principle
The sample is ignited at high temperature and melted with borate to prepare fused cast
beads. The sample on the surface layer is irradiated by primary X-rays to produce
characteristic X-ray fluorescence. After spectroscopy by the crystal, the detector
measures the X-ray fluorescence intensity at the 2θ angle corresponding to the selected
characteristic wavelength.
5 Reagents and materials
Unless otherwise stated, only approved analytical reagents are used in the analysis, and
the water for test shall be distilled water of Grade 3 or above specified in GB/T 6682 or
water with a purity equivalent to it.
5.1 Ammonium iodide. solid, analytical reagent.
5.2 Lithium borate mixed flux (lithium tetraborate. lithium metaborate = 67.33). solid;
it shall be in an anhydrous dry state, otherwise it needs to be burned at 500 ℃ ± 10 ℃
for 4 hours, cooled to room temperature, and then placed in a desiccator for later use.
5.4 Argon methane gas (90 % Ar - 10 % CH4). selected according to the instrument.
6 Instruments and equipment
6.1 Melting furnace
The temperature field of the melting furnace shall be uniform. It shall be able to
maintain a temperature of at least 1100 ℃ ± 10 ℃. It can choose an electric melting
furnace, a gas melting furnace or a high-frequency induction melting furnace.
6.3 Crucible and mold
The crucible and mold (or the crucible that is also used as a mold) are made of non-
wetting platinum-gold alloy (95 % Pt - 5 % Au). The crucible shall have a certain
thickness to prevent deformation after heating. The bottom of the mold shall be kept
flat. For directly formed crucibles, there shall be a flat bottom.
6.4 Balance
The minimum division is 0.1 mg.
6.5 High-temperature furnace
The maximum working temperature for a long time shall reach a temperature of 1100 ℃.
6.6 Oven
It is able to control the temperature at 105 ℃ ± 5 ℃.
7 Sampling and sample preparation
7.1 Sampling and sample preparation shall be carried out according to the provisions of
GB/T 2007.2.All samples shall pass through the 0.125 mm sieve.
7.2 Limestone and dolomite samples shall be dried in an oven at 105 ℃ ± 5 ℃ for 2
hours before analysis, and then placed in a desiccator to cool to room temperature. The
retention time of the dried sample shall not exceed 8 hours, otherwise it shall be dried
again.
8 Preparation of fused cast bead
8.1 Ignition treatment of the sample
Weigh 1.50 g ± 0.01 g of the sample that has been dried and cooled to room temperature
(see Clause 7) and place it in a square porcelain dish. Place the dish into a high-
temperature furnace (see 6.5) and ignite at 1050 ℃ ± 50 ℃ until constant weight.
8.2 Calculation of loss on ignition
Take out the sample from the high-temperature furnace, place it in a desiccator, cool it
to room temperature, weigh it, and calculate the loss on ignition of the sample according
to formula (1).
8.3 Preparation of the fused bead of the sample
Accurately weigh 0.7000 g ± 0.0005 g of the sample that has been ignited and dried and
cooled to room temperature (see 8.2), place it in a glass stirring dish, add 7.0000 g ±
0.0005 g of borate mixed flux (see 5.2) powder, and mix well. Completely transfer it to
a platinum-gold crucible (see 6.3).
8.4 Fused cast bead
Transfer the crucible shown in 8.3 to the melting furnace (see 6.1), pre-melt at 1050 ℃
± 20 ℃ for 2 minutes, melt for 13 minutes, take it out, and directly shape or mold it
into a measurable glass piece.
9 Preparation of instruments
9.1 Working environment of instruments
The working environment of the instrument shall comply with the provisions of GB/T
16597.
10 Analysis steps
10.1 Measurement conditions
Select appropriate measurement conditions based on the type of instrument used,
element to be analyzed, coexisting elements, and their content variation ranges.
10.2 Plotting and confirmation of calibration curve
10.2.1 Plotting of calibration curve
Under selected working conditions, use an X-ray fluorescence spectrometer to measure
the fused cast beads of a series of reference materials/standard samples. The lowest
number of points on the working curve shall be no less than 8 points, and each sample
bead shall be measured at least twice.
10.3 Analysis of the unknown sample
10.3.1 Standardization of instruments
Regularly perform standardization confirmation on the instrument, usually using a fixed
sample to check whether there is a significant change in the X-ray intensity of the
element corresponding to the component to be measured (see Annex A). If there is a
significant change, it indicates that the instrument has drifted.
......
Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al.
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