prEN ISO 17947
(Main)Fine ceramics (advanced ceramics, advanced technical ceramics) - Methods for chemical analysis of fine silicon nitride powders (ISO 17947:2014)
Fine ceramics (advanced ceramics, advanced technical ceramics) - Methods for chemical analysis of fine silicon nitride powders (ISO 17947:2014)
ISO 17947:2014 specifies the methods for the chemical analysis of fine silicon nitride powders used as the raw material for fine ceramics. It stipulates the determination methods of total silicon, total nitrogen, aluminium, iron, calcium, oxygen, carbon, fluorine, and chlorine in fine silicon nitride powders.
Hochleistungskeramik - Verfahren zur chemischen Analyse von feinen Pulvern aus Siliciumnitrid (ISO 17947:2014)
Céramiques techniques - Méthodes pour l'analyse chimique de poudres de nitrure de silicium (ISO 17947:2014)
Fina keramika (sodobna keramika, sodobna tehnična keramika) - Metode za kemijsko analizo finih praškov silicijevega nitrida (ISO 17947:2014)
General Information
Standards Content (Sample)
SLOVENSKI STANDARD
oSIST prEN ISO 17947:2023
01-januar-2023
Fina keramika (sodobna keramika, sodobna tehnična keramika) - Metode za
kemijsko analizo finih praškov silicijevega nitrida (ISO 17947:2014)
Fine ceramics (advanced ceramics, advanced technical ceramics) - Methods for
chemical analysis of fine silicon nitride powders (ISO 17947:2014)
Hochleistungskeramik - Verfahren zur chemischen Analyse von feinen Pulvern aus
Siliciumnitrid (ISO 17947:2014)
Céramiques techniques - Méthodes pour l'analyse chimique de poudres de nitrure de
silicium (ISO 17947:2014)Ta slovenski standard je istoveten z: prEN ISO 17947
ICS:
81.060.30 Sodobna keramika Advanced ceramics
oSIST prEN ISO 17947:2023 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
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oSIST prEN ISO 17947:2023
INTERNATIONAL ISO
STANDARD 17947
First edition
2014-09-01
Fine ceramics (advanced ceramics,
advanced technical ceramics) —
Methods for chemical analysis of fine
silicon nitride powders
Céramiques techniques — Méthodes pour l’analyse chimique de
poudres de nitrure de silicium
Reference number
ISO 17947:2014(E)
ISO 2014
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oSIST prEN ISO 17947:2023
ISO 17947:2014(E)
COPYRIGHT PROTECTED DOCUMENT
© ISO 2014
All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized otherwise in any form
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Published in Switzerland
ii © ISO 2014 – All rights reserved
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oSIST prEN ISO 17947:2023
ISO 17947:2014(E)
Contents Page
Foreword ..........................................................................................................................................................................................................................................v
Introduction ................................................................................................................................................................................................................................vi
1 Scope ................................................................................................................................................................................................................................. 1
2 Normative references ...................................................................................................................................................................................... 1
3 Analytes and ranges .......................................................................................................................................................................................... 2
4 Preparation of test sample ......................................................................................................................................................................... 2
4.1 Sampling ....................................................................................................................................................................................................... 2
4.2 Drying ............................................................................................................................................................................................................. 2
4.3 Weighing ....................................................................................................................................................................................................... 2
5 Apparatus and reagents ................................................................................................................................................................................ 2
6 Blank test ...................................................................................................................................................................................................................... 2
7 Determination of total silicon ................................................................................................................................................................. 3
7.1 Classification of determination methods ......................................................................................................................... 3
7.2 Fusion-dehydration/insolubilization separation-gravimetry and ICP-OES ....................................... 3
7.3 XRF using fused cast-bead method ....................................................................................................................................... 5
8 Determination of total nitrogen ........................................................................................................................................................... 5
8.1 Classification of determination methods ......................................................................................................................... 5
8.2 Acid pressure decomposition-distillation separation-acidimetric titration method ................. 5
8.3 Inert gas fusion-thermal conductivity method ........................................................................................................10
8.4 Fusion-ammonia separation-acidimetric titration method ..........................................................................13
9 Determination of aluminium, iron, and calcium ..............................................................................................................13
9.1 Principle .....................................................................................................................................................................................................13
9.2 Reagents.....................................................................................................................................................................................................13
9.3 Apparatus and instrument .........................................................................................................................................................14
9.4 Procedure .................................................................................................................................................................................................14
9.5 Blank test ..................................................................................................................................................................................................15
9.6 Drawing calibration curve ..........................................................................................................................................................15
9.7 Calculation ...............................................................................................................................................................................................15
10 Determination of oxygen ..........................................................................................................................................................................16
10.1 Principle .....................................................................................................................................................................................................16
10.2 Reagents.....................................................................................................................................................................................................16
10.3 Apparatus .................................................................................................................................................................................................16
10.4 Instrument ...............................................................................................................................................................................................16
10.5 Procedure .................................................................................................................................................................................................16
10.6 Blank test ..................................................................................................................................................................................................16
10.7 Calculation of calibration coefficient ................................................................................................................................16
10.8 Calculation ...............................................................................................................................................................................................17
11 Determination of carbon ...........................................................................................................................................................................17
11.1 Classification of determination methods ......................................................................................................................17
11.2 Combustion (RF furnace)-IR absorption spectrometry ...................................................................................17
11.3 Combustion (resistance furnace)-coulometry .........................................................................................................20
11.4 Combustion (resistance furnace)-gravimetry ..........................................................................................................20
11.5 Combustion (resistance furnace)-conductometry ................................................................................................20
12 Determination of fluorine and chlorine ....................................................................................................................................20
12.1 Principle .....................................................................................................................................................................................................20
12.2 Reagents.....................................................................................................................................................................................................20
12.3 Apparatus and instruments ......................................................................................................................................................21
12.4 Procedure .................................................................................................................................................................................................21
12.5 Blank test ..................................................................................................................................................................................................22
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12.6 Drawing calibration curve ..........................................................................................................................................................22
12.7 Calculation ...............................................................................................................................................................................................22
13 Reporting analytical values ....................................................................................................................................................................23
13.1 Number of analyses..........................................................................................................................................................................23
13.2 Evaluation of analytical values ...............................................................................................................................................23
13.3 Expression of analytical values ..............................................................................................................................................23
14 Test report ................................................................................................................................................................................................................24
Annex A (informative) List of commercial certified reference materials ...................................................................25
Annex B (informative) Analytical results obtained from a round robin test ...........................................................26
Annex C (informative) Spectral lines for ICP-OES .................................................................................................................................31
Bibliography .............................................................................................................................................................................................................................32
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ISO 17947:2014(E)
Foreword
ISO (the International Organization for Standardization) is a worldwide federation of national standards
bodies (ISO member bodies). The work of preparing International Standards is normally carried out
through ISO technical committees. Each member body interested in a subject for which a technical
committee has been established has the right to be represented on that committee. International
organizations, governmental and non-governmental, in liaison with ISO, also take part in the work.
ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of
electrotechnical standardization.The procedures used to develop this document and those intended for its further maintenance are
described in the ISO/IEC Directives, Part 1. In particular the different approval criteria needed for the
different types of ISO documents should be noted. This document was drafted in accordance with the
editorial rules of the ISO/IEC Directives, Part 2 (see www.iso.org/directives).Attention is drawn to the possibility that some of the elements of this document may be the subject of
patent rights. ISO shall not be held responsible for identifying any or all such patent rights. Details of
any patent rights identified during the development of the document will be in the Introduction and/or
on the ISO list of patent declarations received (see www.iso.org/patents).Any trade name used in this document is information given for the convenience of users and does not
constitute an endorsement.For an explanation on the meaning of ISO specific terms and expressions related to conformity
assessment, as well as information about ISO’s adherence to the WTO principles in the Technical Barriers
to Trade (TBT) see the following URL: Foreword - Supplementary informationThe committee responsible for this document is ISO/TC 206, Fine ceramics.
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ISO 17947:2014(E)
Introduction
This International Standard has been developed from Japanese Industrial Standard JIS R 1603:2007
with reference to CEN ENV 14226:2002 and ASTM C1494-01:2007, and is applicable to the chemical
analysis of silicon nitride raw powders for fine ceramics use. This International Standard covers both
major and minor constituents such as total silicon, total nitrogen, and some of trace metallic and non-
metallic elements.vi © ISO 2014 – All rights reserved
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oSIST prEN ISO 17947:2023
INTERNATIONAL STANDARD ISO 17947:2014(E)
Fine ceramics (advanced ceramics, advanced technical
ceramics) — Methods for chemical analysis of fine silicon
nitride powders
1 Scope
This International Standard specifies the methods for the chemical analysis of fine silicon nitride
powders used as the raw material for fine ceramics.This International Standard stipulates the determination methods of total silicon, total nitrogen,
aluminium, iron, calcium, oxygen, carbon, fluorine, and chlorine in fine silicon nitride powders.
2 Normative referencesThe following documents, in whole or in part, are normatively referenced in this document and are
indispensable for its application. For dated references, only the edition cited applies. For undated
references, the latest edition of the referenced document (including any amendments) applies.
ISO 2828, Aluminium oxide primarily used for the production of aluminium — Determination of fluorine
content — Alizarin complexone and lanthanum chloride spectrophotometric methodISO 3696, Water for analytical laboratory use — Specification and test methods
ISO 6353-1, Reagents for chemical analysis — Part 1: General test methods
ISO 6353-2, Reagents for chemical analysis — Part 2: Specifications — First series
ISO 6353-3, Reagents for chemical analysis — Part 3: Specifications — Second series
ISO 8656-1, Refractory products — Sampling of raw materials and unshaped products — Part 1: Sampling
schemeISO 21068-2, Chemical analysis of silicon-carbide-containing raw materials and refractory products —
Part 2: Determination of loss on ignition, total carbon, free carbon and silicon carbide, total and free silica
and total and free siliconISO 21068-3, Chemical analysis of silicon-carbide-containing raw materials and refractory products —
Part 3: Determination of nitrogen, oxygen and metallic and oxidic constituentsISO 21438-2, Workplace atmospheres — Determination of inorganic acids by ion chromatography — Part 2:
Volatile acids, except hydrofluoric acid (hydrochloric acid, hydrobromic acid and nitric acid)
ISO 21438-3, Workplace atmospheres — Determination of inorganic acids by ion chromatography — Part 3:
Hydrofluoric acid and particulate fluoridesISO 26845, Chemical analysis of refractories — General requirements for wet chemical analysis, atomic
absorption spectrometry (AAS) and inductively coupled plasma atomic emission spectrometry (ICP-AES)
methodsEN 12698-1, Chemical analysis of nitride bonded silicon carbide refractories - Part 1: Chemical methods
EN 12698-2, Chemical analysis of nitride bonded silicon carbide refractories - Part 2: XRD methods
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ISO 17947:2014(E)
3 Analytes and ranges
Analytes and ranges specified in this International Standard shall be as follows.
a) Total silicon (T. Si), range of 30 % to 70 % (mass fraction)b) Total nitrogen (T. N), range of 30 % to 45 % (mass fraction)
c) Aluminium (Al), range of 0,001 % to 0,6 % (mass fraction)
d) Iron (Fe), range of 0,001 % to 0,6 % (mass fraction)
e) Calcium (Ca), range of 0,001 % to 0,03 % (mass fraction)
f) Oxygen (O), range of 0,05 % to 5 % (mass fraction)
g) Carbon (C), range of 0,01 % to 6 % (mass fraction)
h) Fluorine (F), range of 0,001 % to 0,2 % (mass fraction)
i) Chlorine (Cl), range of 0,001 % to 0,2 % (mass fraction)
4 Preparation of test sample
The method of preparing samples shall be in accordance with ISO 8656-1 unless otherwise mutually
agreed upon between the analyser and the customer.4.1 Sampling
Take the sample in accordance with ISO 8656-1.
4.2 Drying
Take about 10 g of the sample into a flat-type weighing bottle (60 mm × 30 mm) and spread it uniformly
over the bottom of the bottle. Place the bottle in an air bath at 110 °C ± 5 °C for 2 h without a lid, and then
cool in a desiccator (desiccant: magnesium perchlorate for drying) with a lid for 1 h.
4.3 WeighingWeigh the sample of the required quantity to the nearest 0,1 mg using a balance.
5 Apparatus and reagents
Unless otherwise specified in each determination, use ordinary laboratory apparatus for chemical
analysis listed in ISO 26845, Clause 4, as necessary. Reagents should conform to the requirements of
ISO 6353-1, ISO 6353-2, and ISO 6353-3, as appropriate. Unless otherwise specified in each determination,
use corresponding reagents of analytical grade listed in ISO 26845, Clause 5, as necessary.
6 Blank testBlank test shall be carried out by using identical quantities of reagents, conditions, and procedures
throughout each determination to correct the analytical values obtained.2 © ISO 2014 – All rights reserved
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7 Determination of total silicon
7.1 Classification of determination methods
Total silicon shall be determined by either of the following methods. If analytical results with four
figures are required, use the method A. If analytical results with two or three figures are required, the
method B can be used.— Method A: Fusion–dehydration/insolubilization separation–gravimetry and ICP-OES
— Method B: XRF using fused cast-bead method7.2 Fusion-dehydration/insolubilization separation-gravimetry and ICP-OES
7.2.1 Principle
A sample is fused with alkaline carbonate and the melt is treated with an acid to separate into two
parts of silicon, insoluble silicon and soluble silicon, by filtration. Insoluble silicon is determined
using gravimetry as silicon dioxide converted after ignition, whereas soluble silicon in the filtrate is
determined using ICP-OES. The sum of them represents the total silicon.7.2.2 Reagents
Reagents of analytical grade shall be used. Reagent solutions shall be preserved in plastic bottles.
7.2.2.1 Water, of grade 1 or superior specified in ISO 3696.7.2.2.2 Sodium carbonate, anhydrous, specified in ISO 6353-3 or that of higher grade.
7.2.2.3 Hydrochloric acid (1+1), (1+4), (1+50), prepared by diluting hydrochloric acid with water,
respectively.7.2.2.4 Sulfuric acid (1+1), (1+4), prepared by diluting sulfuric acid with water, respectively.
7.2.2.5 Cellulose powder.7.2.2.6 Polyethylene oxide solution [0,05 % (m/V)], prepared by dissolving polyethylene oxide with
water.7.2.2.7 Hydrofluoric acid, concentration of 48 %.
7.2.3 Apparatus and instruments
Use ordinary laboratory apparatus and instruments for chemical analysis in accordance with ISO 26845,
Clause 4.7.2.3.1 Platinum dish.
7.2.3.2 Platinum crucible.
7.2.3.3 Burner, capable of heating at 1 100 °C.
7.2.3.4 Muffle furnace, capable of being operated at 1 100 °C.
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7.2.3.5 Balance, readable to 0,1 mg.
7.2.3.6 Inductively coupled plasma optical emission spectrometer (ICP-OES).
7.2.4 Procedure
The procedure shall be as follows. The procedure described in ISO 21068-2, Clause 8 can be alternatively
used.7.2.4.1 Fusion of sample
Weigh 0,30 g of the sample and 2,0 g of sodium carbonate, anhydrous into a platinum dish and mix well.
Start to heat carefully and increase the temperature gradually to 1 000 °C to completely fuse the sample
using a burner or in a muffle furnace.7.2.4.2 Separation of silicon
Add 20 ml of hydrochloric acid (1+1) to dissolve the melt on a hot plate. Silicon dioxide will appear to
be jellified and precipitated at this stage. There are two methods to separate the precipitated silicon
dioxide.a) Dehydrate carefully the precipitate to dryness in order to prevent it from spattering and add 5 ml
of hydrochloric acid and 20 ml of water to dissolve any salt mixed with the precipitate. Filtrate the
precipitate with a filter paper and wash with hot hydrochloric acid (1+50) several times and then
with hot water sufficiently until it contains no salt. Receive the filtrate and washings together in a
volumetric flask and make constant volume. Preserve this precipitate for gravimetry of insoluble
silicon and the solution for the ICP-OES determination of soluble silicon, respectively.
b) After eduction of jellified silicon dioxide, add 0,05 g of cellulose powder and 10 ml of polyethylene
oxide solution to agglomerate silicon dioxide for easy filtration. Filtrate and wash in the same
procedure, and then preserve this precipitate for gravimetry of insoluble silicon and the solution
for the ICP-OES determination of soluble silicon, respectively.7.2.4.3 Gravimetry for insoluble silicon
Transfer the precipitate embedded in the filter paper together into a platinum crucible and ignite at
1 100 °C after charring and ashing the paper. Weigh the crucible. Moisten the precipitate in the crucible
with a few drops of water and sulfuric acid (1+1) and add 10 ml of hydrofluoric acid. Then evaporate to
dryness on a hot plate to remove all of silicon dioxide, ignite it at 1 100 °C and weigh the crucible again.
The loss of mass after hydrofluoric acid treatment shall be the amount of insoluble silicon dioxide.
7.2.4.4 ICP-OES for soluble siliconAspirate an aliquot of the preserved solution into an Ar plasma of ICP-OES to determine soluble silicon
in the sample.7.2.5 Blank test
Run blank determinations according to the operations of 7.2.4.1 to 7.2.4.4 without taking a sample.
7.2.6 Drawing calibration curveFor ICP-OES, prepare calibration solutions to span the range of concentration of silicon in the test
solution. Each calibration solution shall have a similar matrix to the test solution.
With those calibration solutions, draw calibration curves for soluble silicon to establish the relation
between the emission intensity and the amount of silicon.4 © ISO 2014 – All rights reserved
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7.2.7 Calculation
With the amount of insoluble silicon in 7.2.4.3, soluble silicon in 7.2.4.4 and the blank test in 7.2.5,
calculate the content of total silicon according to Formula (1).T.Si = [{(m – m ) + (A – A )} / m ] × 0,4674 × 100
1 0 1 0
(1)
where
T.Si is the content of total silicon in the sample, % (mass fraction);
m is the amount of insoluble silicon dioxide in the sample, g;
m is the amount of insoluble silicon dioxide in the blank test, g;
A is the amount of soluble silicon dioxide in the sample, g;
A is the amount of insoluble silicon dioxide in the blank test, g;
m is the weighed amount of the sample, g.
7.3 XRF using fused cast-bead method
The procedure shall be in accordance with EN 12698-2.
8 Determination of total nitrogen
8.1 Classification of determination methods
Total nitrogen shall be determined by either of the following methods. If analytical results with four
figures are required, use the method A or C. If two figures are required, the method B can be used.
— Method A: Acid pressure decomposition–distillation separation–acidimetric titration method
— Method B: Inert gas fusion–thermal conductivity method— Method C: Fusion–ammonia separation–acidimetric titration method
8.2 Acid pressure decomposition-distillation separation-acidimetric titration method
8.2.1 PrincipleA sample is decomposed in a pressure decomposition vessel with a mixture of hydrofluoric acid and
sulfuric acid to convert nitrogen into ammonia. Add boric acid and transfer the solution into a distillation
flask. Add sodium hydroxide and perform steam distillation. React the distilled ammonia with a known
amount of amidosulfuric acid and back-titrate the excess of amidosulfuric acid with a standardized
sodium hydroxide solution.8.2.2 Reagents
Reagents of analytical grade shall be used. Reagent solutions shall be preserved in plastic bottles.
8.2.2.1 Water, of grade 1 or superior specified in ISO 3696.8.2.2.2 Hydrofluoric acid.
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8.2.2.3 Sulfuric acid.
8.2.2.4 Sodium hydroxide, more than 97,0 % (mass fraction) of purity.
8.2.2.5 Sodium hydroxide solution (500 g/l), prepared by dissolving sodium hydroxide in water.
8.2.2.6 Amidosulfuric acid, more than 99,0 % (mass fraction) of purity.8.2.2.7 0,1mol/l amidosulfuric acid solution, prepared by weighing 10,0 g of amidosulfuric acid and
dissolving in water to make 1 000 ml. Calculate the factor of this solution according to Formula (2).
F = m × P/(9,7095 × 100)(2)
where
F is the factor of the 0,1 mol/l amidosulfuric acid solution;
m is the weighed amount of amidosulfuric acid, g;
P is the purity of amidosulfuric acid, % (mass fraction).
8.2.2.8 0,1 mol/l sodium hydroxide solution, prepared by dissolving sodium hydroxide in water in
accordance with ISO 21068-3, 5.2.2.8. Take exactly 50 ml of the 0,1 mol/l amidosulfuric acid solution in
a beaker (200 ml) and dilute with water to about 100 ml. Titrate this solution with the 0,1 mol/l sodium
hydroxide solution using a pH meter. Take the end point as pH 5,5 and determine the volume of the titrant
consumed. Calculate the factor of this solution according to Formula (3).F = F × 50,00/V (3)
where
F is the factor of the 0,1 mol/l sodium hydroxide solution;
F is the factor of the 0,1 mol/l amidosulfuric acid solution;
V is the titration volume of th
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