GB/T 3286.11-2022 PDF English
Search result: GB/T 3286.11-2022_English: PDF (GB/T3286.11-2022)
| Standard ID | Contents [version] | USD | STEP2 | [PDF] delivered in | Name of Chinese Standard | Status |
| GB/T 3286.11-2022 | English | 280 |
Add to Cart
|
0-9 seconds. Auto-delivery.
|
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)
| Valid |
| GB/T 3286.11-1993 | English | 239 |
Add to Cart
|
2 days
|
Methods for chemical analysis of limestone and delo-mite The flame atomic absorption spectrometric methodfor the determination of magnesium and iron content
| Obsolete |
BUY with any currencies (Euro, JPY, GBP, KRW etc.): GB/T 3286.11-2022 Related standards: GB/T 3286.11-2022
PDF Preview: GB/T 3286.11-2022
GB/T 3286.11-2022: PDF in English (GBT 3286.11-2022) GB/T 3286.11-2022
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
Bibliography... 22
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)
WARNING - Personnel using this document shall have practical experience in
regular laboratory work. This document does not identify all possible security
issues. Users are responsible for taking appropriate safety and health measures
and ensuring compliance with the conditions specified in relevant national
regulations.
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. After calculation of calibration curve and correction of
coexisting elements, calculate the mass fractions of calcium oxide, magnesium oxide,
silicon dioxide, aluminium oxide and iron oxide in the sample.
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.
5.3 Reference material/standard sample. used for plotting calibration curves and quality
control. The selected reference material/standard sample shall comply with the
provisions of GB/T 15000.3 or YB/T 082, and the content of each component to be
analyzed shall cover the analysis range and have an appropriate gradient.
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.
6.2 X-ray fluorescence spectrometer
It shall comply with the provisions and requirements of JJG 810 and GB/T 16597.For
instruments that need to use argon methane gas, the cylinder shall be close to the
instrument. When the pressure of the cylinder is lower than 1 MPa, it shall be replaced
in time and stabilized for more than 2 hours.
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.
into a measurable glass piece. The total amount of the sample and flux can be selected
according to the type of casting mold used, and they shall always be consistent.
The fused bead of the sample shall be a uniform glass. The analysis surface of the fused
bead of the sample shall be sufficiently flat, and there shall be no inclusions such as
bubbles and unmelted small particles inside.
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.
9.2 Working conditions of instruments
The working conditions of the X-ray spectrometer shall be optimized according to the
needs of the instrument before measurement.
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.
a) The counting time for the element to be analyzed depends on the content of the
element being measured and the analytical precision to be achieved, which is
generally 5 s ~ 60 s.
b) The counting rate generally does not exceed the maximum linear counting rate of
the counter used.
c) The selection of light tube voltage and current shall consider the minimum
excitation voltage of the spectral line for determination and the rated power of the
light tube.
d) See Annex A for the recommended element analysis lines, spectroscopic crystals,
2θ angles, light tube voltages and currents, and possible interfering elements.
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
S - the standard deviation of the determined value of the component to be analyzed
in the reference material/standard sample, expressed in %;
N - the number of laboratories of the determined value of the reference
material/standard sample.
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.
When the instrument drifts, perform drift correction on the instrument by measuring the
X-ray intensity of the reference material/standard sample. It can use either single-point
correction or two-point correction.
During single-point correction, a reference material/standard sample is used to perform
drift correction on the X-ray intensity, which is generally expressed by formula (4).
Among them, by substituting the X-ray intensity corresponding to the curve of the
standard sample into Ic and substituting the currently measured X-ray intensity of the
standard sample into Ix, the correction coefficient α value can be obtained.
Two-point correction uses two standard samples set at both ends of the correction curve
for drift correction, which is generally expressed by formula (5). Among them, by
substituting the X-ray intensity corresponding to the curve of the standard sample into
Ic and substituting the currently measured X-ray intensity of the standard sample into
Ix, the correction coefficient α and β values can be obtained. The correction interval can
be determined based on the stability of the instrument.
where.
Ic - the corrected X-ray intensity of the unknown sample, in kilo-counts per second
(kcps);
Ix - the measured X-ray intensity of the unknown sample, in kilo-counts per second
(kcps);
α, β - the correction coefficients.
NOTE. The instrument generally has a drift correction function. If the instrument has a drift
correction function, just use its own drift correction function.
10.3.2 Confirmation of standardization
After drift correction, analyze the reference material/standard sample, and confirm that
the analysis value shall comply with the provisions of 10.2.2 or be within the
laboratory’s accreditation range.
10.3.3 Measurement of the unknown sample
According to the working conditions selected in 10.1 and the procedure in Annex B,
use an X-ray fluorescence spectrometer to measure the X-ray fluorescence intensity of
the element corresponding to the component to be analyzed (see Annex A) in the
unknown sample.
11 Calculation and expression of results
According to GB/T 8170, using the X-ray fluorescence intensity measurement value of
the unknown sample, calculate the ignition base content of the component to be
analyzed from the calibration curve.
Calculate the dry basis content of the component to be analyzed according to formula
(6).
where.
C0 - the dry basis content of the component to be analyzed of the unknown sample,
expressed in %;
C1 - the ignition base content of the component to be analyzed of the unknown
sample, expressed in %;
L - the loss on ignition of the sample, expressed in %.
When the difference between the two analytical values of the unknown sample does not
exceed the repeatability limit (r) listed in Table 2, the average value of the two is taken
as the final analysis result. If the r value is exceeded, the procedure in Annex B shall be
followed.
12 Precision
The precision data in this document are the test results of 8 laboratories jointly
analyzing 8 samples of different levels in 2020.The precision determined according to
the statistical methods of GB/T 6379.1 and GB/T 6379.2 is shown in Table 2.The raw
data of the precision tests are shown in Annex C.
......
Source: Above contents are excerpted from the PDF -- translated/reviewed by: www.chinesestandard.net / Wayne Zheng et al.
|