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YS/T 575.23-2021Methods for chemical analysis of bauxite - Part 22: Determination of element content - X-ray fluorescence spectrometry (English PDF)

铝土矿石化学分析方法 第23部分:元素含量的测定 X射线荧光光谱法

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Issued by

Ministry of Industry and Information Technology

Level / Type

National · Recommended

Issue date

March 5, 2021

Implementation date

July 1, 2021

Scope

YS/T 575.23-2021 is the English-translated version of 铝土矿石化学分析方法 第23部分:元素含量的测定 X射线荧光光谱法.

YS/T 575.23-2021 — 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.

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Document preview — YS/T 575.23-2021

National Standard of the People's Republic of China

ICS
71.040.40

Issued by: Ministry of Industry and Information Technology

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

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);

h) ADD the detection method of "high sulfur content sample" (see 8.2.2);

i) MODIFY the test data processing (see Chapter 9; Chapter 7 of the 2009 edition);

j) ADD the "test report" (see Chapter 11).

Please note that some contents of this document may involve patents. The issuing

agency of this document does not assume the responsibility for identifying patents.

This document was proposed by AND shall be under the jurisdiction of the National

Technical Committee for Standardization of Nonferrous Metals (SAC/TC 243).

Drafting organizations of this document. Chinalco Zhengzhou Nonferrous Metals

Research Institute Co., Ltd., Kunming Metallurgical Research Institute Co., Ltd.,

Chinalco Mining Co., Ltd., Shandong Nanshan Aluminum Co., Ltd., Guangdong

Academy of Sciences Industrial Analysis and Testing Center, Shimadzu Enterprise

Management (China) Co., Ltd.

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

Composition Determination range % Composition

Determination range

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.

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

5.2 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).

5.4 Monitoring sample

The monitoring sample shall be a stable glass piece containing all calibration elements;

its concentration shall make the statistical error of its counting rate less than or equal to

the statistical error of the counting rate of the calibration elements.

6 Instruments and equipment

6.1 Platinum-gold alloy crucible (95%Pt + 5%Au).

6.4 Wavelength dispersive X-ray fluorescence spectrometer. End window rhodium

target X-ray tube.

6.5 Oven. Controllable temperature 105 °C ± 5 °C.

6.6 High temperature muffle furnace. Temperature not less than 800 °C; controllable

temperature, temperature control accuracy ± 25 °C.

7 Samples

7.1 Burning sample. The sample is burned according to the requirements of YS/T

575.19 and placed in a dryer for use.

7.2 Drying sample. The sample particle size shall be less than 150 µm; it is pre-dried in

an oven (6.5) at 105 °C ± 25 °C for 2 h, placed in a dryer, cooled to room temperature

before use.

8 Test steps

8.1 Parallel test

Two tests are performed in parallel; the average value is taken.

8.2 Samples

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

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.

8.4 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
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.

9 Test data processing

According to the fluorescence X-ray intensity of the unknown sample, calculate the

mass concentration of each substance from the calibration curve.

10 Precision

10.1 Repeatability limit

The absolute difference between the two independent test results, as obtained under

repeatability conditions, shall not exceed the repeatability limit (r) within the range of

the average values given below; the case of exceeding the repeatability limit (r) shall

not exceed 5%. The repeatability limit (r) is obtained by linear interpolation or

extension method, according to the data in Table 2.

11 Test report

This Chapter specifies the contents of the test report. At least the following aspects shall

Composition Content %

YS/T 575.23-2021

YS

NONFERROUS MEAL INDUSTRY STANDARD

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);

h) ADD the detection method of "high sulfur content sample" (see 8.2.2);

i) MODIFY the test data processing (see Chapter 9; Chapter 7 of the 2009 edition);

j) ADD the "test report" (see Chapter 11).

Please note that some contents of this document may involve patents. The issuing

agency of this document does not assume the responsibility for identifying patents.

This document was proposed by AND shall be under the jurisdiction of the National

Technical Committee for Standardization of Nonferrous Metals (SAC/TC 243).

Drafting organizations of this document. Chinalco Zhengzhou Nonferrous Metals

Research Institute Co., Ltd., Kunming Metallurgical Research Institute Co., Ltd.,

Chinalco Mining Co., Ltd., Shandong Nanshan Aluminum Co., Ltd., Guangdong

Academy of Sciences Industrial Analysis and Testing Center, Shimadzu Enterprise

Management (China) Co., Ltd.

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

Composition Determination range % Composition

Determination range

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.

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

5.2 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).

5.4 Monitoring sample

The monitoring sample shall be a stable glass piece containing all calibration elements;

its concentration shall make the statistical error of its counting rate less than or equal to

the statistical error of the counting rate of the calibration elements.

6 Instruments and equipment

6.1 Platinum-gold alloy crucible (95%Pt + 5%Au).

6.4 Wavelength dispersive X-ray fluorescence spectrometer. End window rhodium

target X-ray tube.

6.5 Oven. Controllable temperature 105 °C ± 5 °C.

6.6 High temperature muffle furnace. Temperature not less than 800 °C; controllable

temperature, temperature control accuracy ± 25 °C.

7 Samples

7.1 Burning sample. The sample is burned according to the requirements of YS/T

575.19 and placed in a dryer for use.

7.2 Drying sample. The sample particle size shall be less than 150 µm; it is pre-dried in

an oven (6.5) at 105 °C ± 25 °C for 2 h, placed in a dryer, cooled to room temperature

before use.

8 Test steps

8.1 Parallel test

Two tests are performed in parallel; the average value is taken.

8.2 Samples

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

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.

8.4 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
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.

9 Test data processing

According to the fluorescence X-ray intensity of the unknown sample, calculate the

mass concentration of each substance from the calibration curve.

10 Precision

10.1 Repeatability limit

The absolute difference between the two independent test results, as obtained under

repeatability conditions, shall not exceed the repeatability limit (r) within the range of

the average values given below; the case of exceeding the repeatability limit (r) shall

not exceed 5%. The repeatability limit (r) is obtained by linear interpolation or

extension method, according to the data in Table 2.

11 Test report

This Chapter specifies the contents of the test report. At least the following aspects shall

Composition Content %

......

......
This preview omits tables, figures, formulas and parts of the technical clauses. The complete document — 14 pages — is available in the English PDF.

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