YS/T 575.23-2021 PDF in English
YS/T 575.23-2021 (YS/T575.23-2021, YST 575.23-2021, YST575.23-2021)
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| YS/T 575.23-2021 | English | 280 |
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Methods for chemical analysis of bauxite - Part 22: Determination of element content - X-ray fluorescence spectrometry
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| YS/T 575.23-2009 | English | 150 |
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Method for chemical analysis of aluminum ores. Part 23: Determination of element contents X-ray fluorescence spectrometric mehtod
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Standards related to (historical): YS/T 575.23-2021
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YS/T 575.23-2021: PDF in English (YST 575.23-2021) YS/T 575.23-2021
YS
NONFERROUS MEAL INDUSTRY STANDARD
OF THE PEOPLE’S REPUBLIC OF CHINA
ICS 71.040.40
CCS H 30
Replacing YS/T 575.23-2009
Methods for chemical analysis of bauxite - Part 23:
Determination of element contents - X-ray fluorescence
spectrometry method
ISSUED ON: MARCH 05, 2021
IMPLEMENTED ON: JULY 01, 2021
Issued by: Ministry of Industry and Information Technology
Table of Contents
Foreword ... 3
Introduction ... 6
1 Scope ... 7
2 Normative references ... 7
3 Terms and definitions ... 8
4 Principle ... 8
5 Reagents or materials ... 8
6 Instruments and equipment ... 9
7 Samples ... 9
8 Test steps ... 9
9 Test data processing ... 12
10 Precision ... 12
11 Test report ... 14
Appendix A (Informative) Operating parameters of X-ray fluorescence spectrometer
... 16
Foreword
This document was drafted in accordance with the provisions of GB/T 1.1-2020
"Directives for standardization - Part 1: Rules for the structure and drafting of
standardizing documents".
This document is Part 23 of YS/T 575 "Methods for chemical analysis of bauxite". YS/T
575 has published the following parts:
- Part 1: Determination of aluminium oxide content EDTA titrimetric method;
- Part 2: Determination of silicon dioxide content - Gravimetric-molybdenum blue
photometric method;
- Part 3: Determination of silicon dioxide content molybdenum blue photometric
method;
- Part 4: Determination of iron oxide content - Dichromate titrimetric method;
- Part 5: Determination of iron oxide content - Orthophenanthroline photometric
method;
- Part 6: Determination of titanium dioxide content - Diantipyrylmethane
photometric method;
- Part 7: Determination of calcium oxide content - Flame atomic absorption
spectrophotometric method;
- Part 8: Determination of magnesium oxide content - Flame atomic absorption
spectrophotometric method;
- Part 9: Determination of potassium oxide and sodium oxide content - Flame atomic
absorption spectrophotometric method;
- Part 10: Determination of manganese oxide content - Flame atomic absorption
spectrophotometric method;
- Part 11: Determination of chromium oxide content - Flame atomic absorption
spectrophotometric method;
- Part 12: Determination of vanadium pentoxide content - N-benzoy-N-
phenylhydroxylamine photometric method;
- Part 13: Determination of zinc content flame - Atomic absorption
spectrophotometric method;
- Part 14: Determination the total content of rare earth oxide - Tribromo-arsenazo
photometric method;
- Part 15: Determination of gallium oxide content - Rhodamine B-extraction
photometric method;
- Part 16: Determination of phosphorus pentoxide content - Molybdenum blue
spectrophotometric method;
- Part 17: Determination of sulfur content - Direct combustion-iodometric method;
- Part 18: Determination of total carbon content - Non-aqueous titrimetric method
after combustion;
- Part 19: Determination of the loss on ignition Gravimetric method;
- Part 20: Preparation of pre-dried sample;
- Part 21: Determination of organic carbon content titrimetric method;
- Part 22: Determination of hydroscopic moisture on gravimetric method;
- Part 23: Determination of element contents - X-ray fluorescence spectrometric
method;
- Part 24: Determination of carbon content and sulfur content - Infrared absorption
method;
- Part 25: Determination of sulfur content - Coulometric titration method.
This document replaces YS/T 575.23-2009 "Methods for chemical analysis of bauxite
- Part 23: Determination of element contents - X-ray fluorescence spectrometry
method". Compared with YS/T 575.23-2009, in addition to structural adjustments and
editorial changes, the main technical changes are as follows:
a) MODIFY the measurement range of "Al2O3" content (see Chapter 1; Chapter 1 of
the 2009 edition);
b) MODIFY the measurement range of "S" content (see Chapter 1; Chapter 1 of the
2009 edition);
c) DELETE the "correction factor" of flux (see 3.1.2 of the 2009 edition);
d) ADD the pre-oxidant "lithium nitrate" (see 5.2.2);
e) MODIFY the "sample" (see Chapter 7; Chapter 5 of the 2009 edition);
f) MODIFY the "test material" (see 8.2; Chapter 6.2 of the 2009 edition);
g) ADD the "high temperature muffle furnace" (see 6.6);
Methods for chemical analysis of bauxite - Part 23:
Determination of element contents - X-ray fluorescence
spectrometry method
Warning - People using this document shall have practical experience in formal
laboratory work. This document does not point out all possible safety issues. The
user is responsible for taking appropriate safety and health measures and ensuring
that the conditions specified in relevant national regulations are met.
1 Scope
This document specifies the determination method of aluminum oxide, silicon dioxide,
total iron (expressed as Fe2O3), titanium dioxide, potassium oxide, sodium oxide,
calcium oxide, magnesium oxide, phosphorus pentoxide, manganese oxide, sulfur,
vanadium, gallium, zinc in bauxite.
This document is applicable to the determination of aluminum oxide, silicon dioxide,
total iron (expressed as Fe2O3), titanium dioxide, potassium oxide, sodium oxide,
calcium oxide, magnesium oxide, phosphorus pentoxide, manganese oxide, sulfur,
vanadium, gallium, zinc in bauxite. The determination range is as shown in Table 1.
2 Normative references
The contents of the following documents constitute the essential provisions of this
document through normative references in the text. Among them, for dated references,
only the version corresponding to that date applies to this document; for undated
references, the latest version (including all amendments) applies to this document.
GB/T 8170 Rules of rounding off for numerical values and expression and
judgement of limiting values
YS/T 575.19 Methods for chemical analysis of bauxite - Part 19: Determination of
loss on ignition - Gravimetric method
3 Terms and definitions
There are no terms and definitions that need to be defined in this document.
4 Principle
The sample is melted with anhydrous lithium tetraborate and lithium metaborate mixed
flux. Ammonium nitrate solution or lithium nitrate is added as a pre-oxidant; a small
amount of saturated lithium bromide or ammonium iodide solution is added as a
demolding agent. It is melted in an automatic melting machine and cast into a glass
sample. The fluorescence X-ray intensity of each element in the sample is measured by
an X-ray fluorescence spectrometer; a calibration curve is established. The calibration
equation is used to correct the absorption enhancement effect between elements; the
content of each element in the sample is calculated from the calibration curve.
5 Reagents or materials
Unless otherwise specified, only reagents confirmed as analytically pure and distilled
or deionized water or water of relatively pure quality are used in the analysis.
5.1 Flux
5.1.1 Anhydrous lithium tetraborate and lithium metaborate mixed flux, which has a
mass ratio of 12:22; after burning at 700 °C for 2 h, place in a desiccator for use.
5.1.2 Anhydrous lithium tetraborate and lithium metaborate mixed flux, which has a
mass ratio of 67:33; after burning at 700 °C for 2 h, place in a desiccator for use.
5.2 Pre-oxidant
5.2.1 Ammonium nitrate solution (500 g/L).
5.2.2 Lithium nitrate.
5.3 Release agent
Lithium bromide saturated solution or ammonium iodide solution (300 g/L).
8.2.1 Burning-based samples
According to the mass ratio of sample (7.1) to flux (5.1.1) of 1:8 ~ 1:10 (the
recommended sample weight is 0.5 g ~ 0.7 g), accurately weigh the flux (5.1.1) and
sample (7.1) in a platinum-gold alloy crucible (6.1), to an accuracy of 0.1 mg; stir
evenly; add 1 drop of release agent (5.3).
8.2.2 Dry-base test material
a) Conventional sample: According to the mass ratio of sample (7.2) to flux (5.1.1)
of 1:8 ~ 1:10 (the recommended sample weight is 0.5 g ~ 0.7 g), accurately weigh
the sample (7.2) and flux (5.1.1) into a platinum-gold alloy crucible (6.1); stir
evenly; add 2 mL of ammonium nitrate solution (5.2.1); add 5 drops of release
agent (5.3); place in a 700 °C high-temperature muffle furnace (6.6) for pre-
oxidation for 5 min.
b) Samples with high sulfur content: According to the mass ratio of sample (7.2),
flux (5.1.2) and pre-oxidant (5.2.2) of 1:10:1.5 (the recommended sample weight
is 0.5 g ~ 0.7 g), accurately weigh each substance into a platinum-gold alloy
crucible (6.1); stir evenly; add 5 drops of release agent (5.3); place in a 600 °C ±
25 °C high temperature muffle furnace (6.6) for pre-oxidation for 15 min.
Note: When using the dry-based sample measurement method, attention shall be paid to the
difference in loss-on-ignition of different types of bauxite. If the fluorescence instrument
software has a loss-on-ignition correction function, the sample can be prepared directly
according to the above method, meanwhile the sample loss-on-ignition can be input into the
software for correction. If the instrument's loss-on-ignition correction function is not used,
the difference in loss-on-ignition of different types of bauxite must be considered,
meanwhile the bauxite samples must be classified to establish the working curve and
measurement.
8.3 Preparation of measurement samples
8.3.1 Melting
Put the sample (8.2) into the melting machine, to melt it at 1070 °C ~ 1150 °C for 10
min ~ 15 min. During the melting process, rotate the crucible to allow the small molten
beads and samples adhering to the crucible wall to enter the melt. The melting machine
automatically shakes the crucible, at regular intervals to drive out bubbles and mix the
melt.
8.3.2 Casting
Pour the melt (8.3.1) in the crucible into the mold (6.2), which was heated to 800 °C.
Remove the mold from the flame. After cooling, peel off the formed glass sample from
the mold. If the sample is directly formed after melting in the crucible, the crucible shall
be shaken before cooling to drive out bubbles. The formed glass sample shall be
uniform and transparent, with a smooth surface, no bubbles, no crystallization.
8.3.3 Sample storage
A label shall be attached to the non-measurement surface of the glass sample and stored
in a desiccator to prevent moisture absorption and contamination. When measuring,
only the edge of the sample shall be held, to avoid contamination of the measurement
surface.
8.4 Determination
8.4.1 Measurement conditions
The measurement conditions depend on the equipment. Please refer to Appendix A to
set the working parameters.
8.4.2 Calibration
8.4.2.1 Selection of calibration samples: National standard substances can be selected
as calibration samples. Each element shall have a standard series, which have a
sufficient content range and a certain gradient. If the above standard samples cannot
meet the requirements, appropriate artificially prepared calibration samples shall be
added. For high sulfur content samples, artificially prepared calibration samples can be
obtained by adding national pyrite standard substances.
8.4.2.2 Calibration curve establishment: Prepare the selected calibration samples into
calibration samples according to steps 8.2 ~ 8.3. Measure the fluorescence intensity of
each element in the calibration sample, according to the selected measurement
conditions. Draw the calibration curve, where the y-axis represents the net intensity of
fluorescence X-rays and the x-axis represents the mass concentration. Select the
theoretical α coefficient or the basic parameter method, to calibrate the absorption
enhancement effect between elements, according to the calibration curve.
8.4.2.3 Calibration of interference spectral line: For elements with spectral line overlap
interference, spectral line overlap interference calibration is required.
8.4.2.4 Instrument drift calibration: Use the monitoring sample (5.4) to perform
instrument drift calibration. The first measurement of fluorescence intensity of the
monitoring sample (5.4) shall be the same as the start-up measurement of the calibration
sample, to ensure the effectiveness of drift calibration.
8.4.3 Measurement of unknown samples
Prepare national standard materials and unknown samples into standard material
samples and unknown samples, respectively, according to 8.2 ~ 8.3. Start the
quantitative analysis program, to measure the standard material samples. If the analysis
results of the elements in the standard material samples meet the repeatability
......
Source: Above contents are excerpted from the PDF -- translated/reviewed by: www.chinesestandard.net / Wayne Zheng et al.
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