Fine ceramics (advanced ceramics, advanced technical ceramics) — Methods for chemical analysis of aluminium nitride powders

This document specifies methods for the chemical analysis of fine aluminium nitride powders used as the raw material for fine ceramics. This document stipulates the determination methods of the aluminium, total nitrogen, boron, calcium, copper, iron, magnesium, manganese, molybdenum, nickel, potassium, silicon, sodium, titanium, tungsten, vanadium, zinc, zirconium, carbon, chlorine, fluorine, and oxygen contents in aluminium nitride powders. The aluminium content is determined by using either an acid pressure decomposition-CyDTA-zinc back titration method or an acid digestion-inductively coupled plasma-optical emission spectrometry (ICP-OES) method. The total nitrogen content is determined by using an acid pressure decomposition-distillation separation-acidimetric titration method, a direct decomposition-distillation separation-acidimetric titration method, or an inert gas fusion-thermal conductivity method. The boron, calcium, copper, iron, magnesium, manganese, molybdenum, nickel, potassium, silicon, sodium, titanium, tungsten, vanadium and zinc contents are determined by using an acid digestion-ICP-OES method or an acid pressure decomposition-ICP-OES method. The sodium and potassium contents are determined via an acid pressure decomposition-flame emission method or an acid pressure decomposition-atomic absorption spectrometry method. The oxygen content is determined by using an inert gas fusion-IR absorption spectrometry method, while that of carbon is determined via a combustion-IR absorption spectrometry method or a combustion-conductometry method. The chlorine and fluorine contents are determined by using a pyrohydrolysation method followed by ion chromatography or spectrophotometry.

Céramiques techniques — Méthodes d’analyse chimique des poudres de nitrure d'aluminium

General Information

Status
Published
Publication Date
30-Jan-2019
Current Stage
6060 - International Standard published
Start Date
31-Jan-2019
Completion Date
31-Jan-2019
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ISO 21814:2019 - Fine ceramics (advanced ceramics, advanced technical ceramics) -- Methods for chemical analysis of aluminium nitride powders
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INTERNATIONAL ISO
STANDARD 21814
First edition
2019-02
Fine ceramics (advanced ceramics,
advanced technical ceramics) —
Methods for chemical analysis of
aluminium nitride powders
Céramiques techniques — Méthodes d’analyse chimique des poudres
de nitrure d'aluminium
Reference number
ISO 21814:2019(E)
ISO 2019
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ISO 21814:2019(E)
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© ISO 2019

All rights reserved. Unless otherwise specified, or required in the context of its implementation, no part of this publication may

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Published in Switzerland
ii © ISO 2019 – All rights reserved
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ISO 21814:2019(E)
Contents Page

Foreword ........................................................................................................................................................................................................................................vi

1 Scope ................................................................................................................................................................................................................................. 1

2 Normative references ...................................................................................................................................................................................... 1

3 Terms and definitions ..................................................................................................................................................................................... 2

4 Analytes and ranges .......................................................................................................................................................................................... 2

5 Preparation of the test sample ............................................................................................................................................................... 2

5.1 General ........................................................................................................................................................................................................... 2

5.2 Sampling ....................................................................................................................................................................................................... 3

5.3 Drying ............................................................................................................................................................................................................. 3

5.4 Weighing ....................................................................................................................................................................................................... 3

6 Reporting the analytical values ............................................................................................................................................................. 3

6.1 Number of analyses............................................................................................................................................................................. 3

6.2 Blank test ..................................................................................................................................................................................................... 3

6.3 Evaluation of the analytical values......................................................................................................................................... 3

6.4 Expression of the analytical values ....................................................................................................................................... 3

7 Determination of the aluminium content .................................................................................................................................. 4

7.1 Classification of the determination methods ................................................................................................................ 4

7.2 Acid decomposition-ICP-OES method ................................................................................................................................. 4

7.2.1 Principle .................................................................................................................................................................................. 4

7.2.2 Reagents .................................................................................................................................................................................. 4

7.2.3 Apparatus and instruments.................................................................................................................................... 4

7.2.4 Procedure ............................................................................................................................................................................... 5

7.2.5 Blank test ................................................................................................................................................................................ 5

7.2.6 Drawing of the calibration curve ....................................................................................................................... 5

7.2.7 Calculation ............................................................................................................................................................................. 5

7.3 Acid pressure decomposition-CyDTA-zinc back titration method ............................................................. 5

7.3.1 Principle .................................................................................................................................................................................. 5

7.3.2 Reagents .................................................................................................................................................................................. 6

7.3.3 Apparatus and instruments.................................................................................................................................... 6

7.3.4 Procedure ............................................................................................................................................................................... 8

7.3.5 Blank test ................................................................................................................................................................................ 8

7.3.6 Calculation ............................................................................................................................................................................. 8

8 Determination of the total nitrogen content ........................................................................................................................... 8

8.1 Classification of the determination methods ................................................................................................................ 8

8.2 Acid pressure decomposition-distillation separation-acidimetric titration method ................. 9

8.2.1 Principle .................................................................................................................................................................................. 9

8.2.2 Reagents .................................................................................................................................................................................. 9

8.2.3 Apparatus ............................................................................................................................................................................10

8.2.4 Procedure ............................................................................................................................................................................12

8.2.5 Recovery measurement ..........................................................................................................................................12

8.2.6 Calculation ..........................................................................................................................................................................13

8.3 Direct decomposition-distillation separation-acidimetric titration method .................................13

8.3.1 Principle ...............................................................................................................................................................................13

8.3.2 Reagents ...............................................................................................................................................................................13

8.3.3 Apparatus ............................................................................................................................................................................13

8.3.4 Procedure ............................................................................................................................................................................13

8.3.5 Recovery measurement ..........................................................................................................................................13

8.3.6 Calculation ..........................................................................................................................................................................13

8.4 Inert gas fusion-thermal conductivity method ........................................................................................................13

8.4.1 Principle ...............................................................................................................................................................................13

8.4.2 Reagents ...............................................................................................................................................................................14

8.4.3 Apparatus ............................................................................................................................................................................14

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ISO 21814:2019(E)

8.4.4 Instrument .........................................................................................................................................................................14

8.4.5 Procedure ............................................................................................................................................................................15

8.4.6 Blank test .............................................................................................................................................................................16

8.4.7 Calculation of the calibration coefficient .................................................................................................16

8.4.8 Calculation ..........................................................................................................................................................................17

9 Determination of the sodium and potassium contents .............................................................................................17

9.1 Classification of the determination methods .............................................................................................................17

9.2 Acid pressure decomposition-flame emission method ....................................................................................17

9.2.1 Principle ...............................................................................................................................................................................17

9.2.2 Reagents ...............................................................................................................................................................................17

9.2.3 Instruments .......................................................................................................................................................................18

9.2.4 Procedure ............................................................................................................................................................................18

9.2.5 Blank test .............................................................................................................................................................................18

9.2.6 Drawing of the calibration curve ....................................................................................................................18

9.2.7 Calculation ..........................................................................................................................................................................18

9.3 Acid pressure decomposition-atomic absorption spectrometry method .........................................19

9.3.1 Principle ...............................................................................................................................................................................19

9.3.2 Reagents ...............................................................................................................................................................................19

9.3.3 Instruments .......................................................................................................................................................................19

9.3.4 Procedure ............................................................................................................................................................................19

9.3.5 Blank test .............................................................................................................................................................................19

9.3.6 Drawing of the calibration curve ....................................................................................................................19

9.3.7 Calculation ..........................................................................................................................................................................19

10 Determination of the trace element contents .....................................................................................................................19

10.1 Classification of the determination methods .............................................................................................................19

10.2 Acid decomposition-ICP-OES method ..............................................................................................................................20

10.2.1 Principle ...............................................................................................................................................................................20

10.2.2 Reagents ...............................................................................................................................................................................20

10.2.3 Apparatus and instruments.................................................................................................................................20

10.2.4 Procedure ............................................................................................................................................................................21

10.2.5 Blank test .............................................................................................................................................................................21

10.2.6 Drawing of the calibration curve ....................................................................................................................21

10.2.7 Calculation ..........................................................................................................................................................................21

10.3 Acid pressure decomposition-ICP-OES method ......................................................................................................22

10.3.1 General...................................................................................................................................................................................22

10.3.2 Reagents ...............................................................................................................................................................................22

10.3.3 Apparatus and instruments.................................................................................................................................22

10.3.4 Procedure ............................................................................................................................................................................22

10.3.5 Blank test .............................................................................................................................................................................22

10.3.6 Drawing of the calibration curve ....................................................................................................................22

10.3.7 Calculation ..........................................................................................................................................................................22

11 Determination of the oxygen content ..........................................................................................................................................22

11.1 Principle .....................................................................................................................................................................................................22

11.2 Reagents.....................................................................................................................................................................................................22

11.3 Apparatus .................................................................................................................................................................................................23

11.4 Instruments ............................................................................................................................................................................................23

11.5 Procedure .................................................................................................................................................................................................23

11.6 Blank test ..................................................................................................................................................................................................23

11.7 Calculation of the calibration coefficient .......................................................................................................................23

11.8 Calculation ...............................................................................................................................................................................................23

12 Determination of the carbon content ..........................................................................................................................................24

12.1 Classification of the determination methods .............................................................................................................24

12.2 Combustion (resistance furnace)-IR absorption spectrometry ................................................................24

12.2.1 Principle ...............................................................................................................................................................................24

12.2.2 Reagents ...............................................................................................................................................................................24

12.2.3 Apparatus ............................................................................................................................................................................24

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ISO 21814:2019(E)

12.2.4 Instrument .........................................................................................................................................................................24

12.2.5 Procedure ............................................................................................................................................................................25

12.2.6 Blank test .............................................................................................................................................................................26

12.2.7 Calculation of the calibration coefficient .................................................................................................26

12.2.8 Calculation ..........................................................................................................................................................................27

12.3 Combustion (radio frequency heating furnace)-thermal conductometry ........................................27

12.3.1 Principle ...............................................................................................................................................................................27

12.3.2 Reagents ...............................................................................................................................................................................27

12.3.3 Apparatus ............................................................................................................................................................................27

12.3.4 Instrument .........................................................................................................................................................................27

12.3.5 Procedure ............................................................................................................................................................................28

12.3.6 Blank test .............................................................................................................................................................................29

12.3.7 Calculation of the calibration coefficient .................................................................................................29

12.3.8 Calculation ..........................................................................................................................................................................29

12.4 Combustion (radio frequency heating furnace)-IR absorption spectrometry .............................29

12.4.1 Principle ...............................................................................................................................................................................29

12.4.2 Reagents ...............................................................................................................................................................................29

12.4.3 Apparatus ............................................................................................................................................................................29

12.4.4 Instrument .........................................................................................................................................................................29

12.4.5 Procedure ............................................................................................................................................................................30

12.4.6 Blank test .............................................................................................................................................................................31

12.4.7 Calculation of the calibration coefficient .................................................................................................31

12.4.8 Calculation ..........................................................................................................................................................................31

13 Determination of the fluorine and chlorine contents .................................................................................................31

13.1 Principle .....................................................................................................................................................................................................31

13.2 Reagents.....................................................................................................................................................................................................31

13.3 Apparatus and instruments ......................................................................................................................................................32

13.4 Procedure .................................................................................................................................................................................................33

13.4.1 Extraction of fluorine and chlorine from the sample ....................................................................33

13.4.2 Determination of the fluorine and chlorine contents ...................................................................33

13.5 Blank test ..................................................................................................................................................................................................33

13.6 Drawing of the calibration curve ..........................................................................................................................................34

13.7 Calculation ...............................................................................................................................................................................................34

14 Test report ................................................................................................................................................................................................................34

Annex A (informative) Analytical results obtained from the round robin test .....................................................35

Bibliography .............................................................................................................................................................................................................................36

© ISO 2019 – All rights reserved v
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ISO 21814:2019(E)
Foreword

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