SIST EN ISO 17947:2023
(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)
This document 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)
Diese Internationale Norm legt die Verfahren für die chemische Analyse von feinen Pulvern aus Siliciumnitrid, die als Ausgangsstoffe für Hochleistungskeramik verwendet werden, fest.
Diese Internationale Norm legt die Verfahren zur Bestimmung des Gesamtsiliciumgehalts, des Gesamtstickstoffgehalts, des Gehalts an Aluminium, Eisen, Calcium, Sauerstoff, Kohlenstoff, Fluor und Chlor in feinen Pulvern aus Siliciumnitrid fest.
Céramiques techniques - Méthodes pour l'analyse chimique de poudres fines de nitrure de silicium (ISO 17947:2014)
Ce document spécifie les méthodes d'analyse chimique des poudres fines de nitrure de silicium utilisées comme matière première pour les céramiques techniques.
Ce document décrit les méthodes de détermination des teneurs en silicium total, azote total, aluminium, fer, calcium, oxygène, carbone, fluor et chlore dans les poudres fines de nitrure de silicium.
Fina keramika (sodobna keramika, sodobna tehnična keramika) - Metode za kemijsko analizo finih praškov silicijevega nitrida (ISO 17947:2014)
Ta mednarodni standard določa metode za kemično analizo finih praškov silicijevega nitrida, ki se uporabljajo kot surovina za fino keramiko.
Ta mednarodni standard določa metode za določanje celotnega silicija, celotnega dušika, aluminija, železa, kalcija, kisika, ogljika, fluora in klora v finih praških silicijevega nitrida.
General Information
Standards Content (Sample)
SLOVENSKI STANDARD
01-maj-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 fines de nitrure
de silicium (ISO 17947:2014)
Ta slovenski standard je istoveten z: EN ISO 17947:2023
ICS:
81.060.30 Sodobna keramika Advanced ceramics
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
EN ISO 17947
EUROPEAN STANDARD
NORME EUROPÉENNE
March 2023
EUROPÄISCHE NORM
ICS 81.060.30
English Version
Fine ceramics (advanced ceramics, advanced technical
ceramics) - Methods for chemical analysis of fine silicon
nitride powders (ISO 17947:2014)
Céramiques techniques - Méthodes pour l'analyse Hochleistungskeramik - Verfahren zur chemischen
chimique de poudres fines de nitrure de silicium (ISO Analyse von feinen Pulvern aus Siliciumnitrid (ISO
17947:2014) 17947:2014)
This European Standard was approved by CEN on 10 March 2023.
CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this
European Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical references
concerning such national standards may be obtained on application to the CEN-CENELEC Management Centre or to any CEN
member.
This European Standard exists in three official versions (English, French, German). A version in any other language made by
translation under the responsibility of a CEN member into its own language and notified to the CEN-CENELEC Management
Centre has the same status as the official versions.
CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia,
Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway,
Poland, Portugal, Republic of North Macedonia, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Türkiye and
United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
CEN-CENELEC Management Centre: Rue de la Science 23, B-1040 Brussels
© 2023 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN ISO 17947:2023 E
worldwide for CEN national Members.
Contents Page
European foreword . 3
European foreword
The text of ISO 17947:2014 has been prepared by Technical Committee ISO/TC 206 "Fine ceramics” of
the International Organization for Standardization (ISO) and has been taken over as EN ISO 17947:2023
by Technical Committee CEN/TC 184 “Advanced technical ceramics” the secretariat of which is held by
DIN.
This European Standard shall be given the status of a national standard, either by publication of an
identical text or by endorsement, at the latest by September 2023, and conflicting national standards
shall be withdrawn at the latest by September 2023.
Attention is drawn to the possibility that some of the elements of this document may be the subject of
patent rights. CEN shall not be held responsible for identifying any or all such patent rights.
Any feedback and questions on this document should be directed to the users’ national standards body.
A complete listing of these bodies can be found on the CEN website.
According to the CEN-CENELEC Internal Regulations, the national standards organizations of the
following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria,
Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland,
Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Republic of
North Macedonia, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Türkiye and the
United Kingdom.
Endorsement notice
The text of ISO 17947:2014 has been approved by CEN as EN ISO 17947:2023 without any modification.
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
ISO 17947:2014(E)
© ISO 2014
All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized otherwise in any form
or by any means, electronic or mechanical, including photocopying, or posting on the internet or an intranet, without prior
written permission. Permission can be requested from either ISO at the address below or ISO’s member body in the country of
the requester.
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Published in Switzerland
ii © ISO 2014 – All rights reserved
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
ISO 17947:2014(E)
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
iv © ISO 2014 – All rights reserved
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 information
The committee responsible for this document is ISO/TC 206, Fine ceramics.
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
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 references
The 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 method
ISO 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
scheme
ISO 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 silicon
ISO 21068-3, Chemical analysis of silicon-carbide-containing raw materials and refractory products —
Part 3: Determination of nitrogen, oxygen and metallic and oxidic constituents
ISO 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 fluorides
ISO 26845, Chemical analysis of refractories — General requirements for wet chemical analysis, atomic
absorption spectrometry (AAS) and inductively coupled plasma atomic emission spectrometry (ICP-AES)
methods
EN 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
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 Weighing
Weigh 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 test
Blank 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
ISO 17947:2014(E)
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 method
7.2 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.
ISO 17947:2014(E)
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 silicon
Aspirate 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 curve
For 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
ISO 17947:2014(E)
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 Principle
A 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.
ISO 17947:2014(E)
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 the 0,1 mol/l sodium hydroxide solution, ml.
8.2.2.9 Boric acid.
8.2.2.10 Ammonium sulfate, more than 99,9 % (mass fraction) of purity.
8.2.3 Apparatus
Use ordinary laboratory apparatus for chemical analysis and the following.
8.2.3.1 Platinum crucible.
8.2.3.2 Pressure decomposition vessel, on the market.
An example is shown in Figure 1. Use the vessels for the exclusive use in this analysis only to avoid cross-
contamination by nitrogen. If the vessel which has ever contacted with nitric acid is used, the lower
values of nitrogen can be obtained.
6 © ISO 2014 – All rights reserved
ISO 17947:2014(E)
8.2.3.3 Air bath, capable of heating at 160 °C ± 5 °C.
8.2.3.4 Steam distillation apparatus, consisting of the components listed below.
An example of the apparatus is shown in Figure 2. Each component shall be made of hard glass coupled
by common ground joints and fixed by springs or clamps just as per ISO 21068-3, Figure 1.
Dimensions in millimetres
Key
1 centre screw
2 screw cap
3 top plate
4 PTFE cap
5 cylinder
6 PTFE bottle
7 bottom plate
Figure 1 — An example of sealed decomposition vessel
ȭ
ȭ60
45°
ISO 17947:2014(E)
Dimensions in millimetres
c
ȭ12
ȭ12
ȭ4
ȭ12
ȭ10
80 120
ȭ28
e
40 ȭ28
ȭ14
ȭ12
ȭ12
ȭ10
ȭ14
d
14 7
ȭ
b
ȭ10
f
a
Key
a flask (2,5 l) for generation of steam 3 Dumet wire
b trap (500 ml) 4 funnel with stopcock
c sphere and tube 5 rubber tube
d distillation flask (750 ml) 6 13 to15 coils
e Graham condenser 7 small holes
f receiver 8 electric heater
1 funnel 9 connection of rubber tube with pinchcock
2 ball joint 10 jack
Figure 2 — An example of steam distillation apparatus
8.2.3.5 Steam generation flask (2,5 l), equipped with a funnel with a cock, a throw-in heater (with
1 kW Nichrome wire), and a steam outlet tube.
8.2.3.6 Trap, the bottom of a bulb shall be connected to a rubber tube with a pinch cock for a drain.
The tip of steam leading-out tube shall have several small holes.
8.2.3.7 Bulb, equipped with a steam leading-in tube, a funnel with a cock, a splash-proof trap, etc.
The steam leading-in tube shall be cut in the middle enabling the exchange of the tip by connecting to a
rubber tube.
8 © ISO 2014 – All rights reserved
45°
ȭ60
ȭ12
30°
300 300
160 300 50
100 10 80
160 250 50
ISO 17947:2014(E)
8.2.3.8 Distillation flask (750 ml).
8.2.3.9 Coiled condenser.
8.2.3.10 Receiver, a tall beaker (300 ml) shall be used.
8.2.3.11 pH meter, readable to the smallest value of 0,1 equipped with a glass electrode.
8.2.4 Procedure
a) Acid pressure decomposition of sample. Weigh 0,15 g of the sample in a platinum crucible (20 ml)
and add 5 ml of sulfuric acid (1+1) and 5 ml of hydrofluoric acid. Position the crucible into a pressure
decomposition vessel and close according to the manufacturer’s instructions. Place the vessel
into an air bath and heat at 160 °C ± 5 °C for 16 h. Acid pressure decomposition under microwave
irradiation can be performed if available.
b) Preparation of sample solution. After cooling, disassemble the vessel. Transfer the solution into a
100 ml plastic beaker by washing the crucible with water. Add 5 g of boric acid and mix well.
c) Preparation of steam distillation apparatus. After transferring the solution into a distillation
flask, assemble a distillation apparatus and add exactly 50 ml of the 0,1 mol/l amidosulfuric acid
solution to the receiver. Fix the coiled condenser so that the tip is immersed in the solution. Pour
50 ml of the sodium hydroxide solution (500 g/l) through the funnel of the flask by washing the
funnel with water, make the solution volume about 150 ml and close the funnel cock.
d) Steam distillation. Perform the steam distillation with a steam flow of 4,5 ml to 5,0 ml per minute.
When the distillate reaches about 170 ml, lower the receiver to expose the tip of the condenser
above the liquid surface and continue distillation until the distillate reaches about 200 ml. Wash
the outside of the tip with a small amount of water. When using a new distillation apparatus or the
apparatus which has not been used for a long time, perform preliminary distillation for washing
inside of it for 2 h to 3 h.
e) Titration. Titrate the distillate with the 0,1 mol/l sodium hydroxide solution using the pH meter.
Take the end point as pH 5,5 and record the volume of the titrant.
8.2.5 Recovery measurement
Weigh 0,280 g of ammonium sulfate to the nearest 0,1 mg in a platinum crucible (20 ml), perform
operations of 8.2.4 and calculate the recovery according to Formula (4). The recovery shall be not less
than 99 %.
R = [{(50,00 × F) – (V × F )} × 0,0014007/(m × 0,2120)] × 100
(4)
where
R is the recovery, %;
F is the factor of the 0,1 mol/l amidosulfuric acid solution;
V is the titration volume of the 0,1 mol/l sodium hydroxide solution, ml;
F is the factor of the 0,1 mol/l sodium hydroxide solution;
m is the weighed amount of ammonium sulphate, g.
ISO 17947:2014(E)
8.2.6 Calculation
Calculate the content of total nitrogen in the sample according to Formula (5).
T.N = [{[(50,00 × F) – (V × F )] × [(0,0014007 × 100/R)]}/m] × 100
(5)
where
T.N is the content of total nitrogen in the sample, % (mass fraction);
F is the factor of the 0,1 mol/l amidosulfuric acid solution;
V is the titration volume of the 0,1 mol/l sodium hydroxide solution, ml;
F is the factor of the 0,1 mol/l sodium hydroxide solution;
R is the recovery (%) in 8.2.5;
m is the weighed amount of the sample, g.
8.3 Inert gas fusion-thermal conductivity method
8.3.1 Principle
A sample is fused together with a flux in a graphite crucible under inert gas flow to extract nitrogen
and other gases from the sample. The elemental nitrogen is determined using a thermal conductivity
detector after the removal of concomitants such as carbon monoxide, carbon dioxide, other gases, and
moisture.
8.3.2 Reagents
Reagents shall be as follows.
8.3.2.1 Helium, more than 99,99 % (volume fraction) of purity.
8.3.2.2 Flux, in shot or basket form made of tin or nickel.
Use a combination of metals which is different from a capsule.
8.3.3 Apparatus
8.3.3.1 Capsule, made of nickel or tin designated for each apparatus.
8.3.3.2 Graphite crucible, suitable for impulse furnace.
An example is shown in Figure 3 a) and Figure 3 b).
10 © ISO 2014 – All rights reserved
ISO 17947:2014(E)
Dimensions in millimetres
ȭ12.6
ȭ14
ȭ10.0
ȭ11.6
ȭ
ȭ6.7
a) b)
Figure 3 — An example of graphite crucible
8.3.4 Instrument
A commercial nitrogen analyser is available. It consists of the components listed below. The block
diagram is shown in Figure 4.
8.3.4.1 Inert gas refiner, consisting of a deoxidation tube (reduced copper) with an electric furnace, a
carbon dioxide absorption tube (sodium hydroxide shots for gas analysis), a dehydration tube (magnesium
perchlorate for drying), etc.
A denitrification tube (sponge titanium) is attached in some instruments.
8.3.4.2 Gas extractor, consisting of a sample feeder, an impulse furnace, etc.
The sample feeder can throw the sample-embedded capsule into the graphite crucible in the impulse
furnace under inert gas flow. The impulse furnace shall be capable of attaining about 3 000 °C. The upper
water-cooled copper electrode is fixed; whereas the lower electrode moves vertically. The graphite
crucible is sandwiched between both electrodes.
8.3.4.3 Combustion gas purifier, consisting of a dust collecting tube filled with glass wool, a carbon
dioxide absorption tube with sodium hydroxide shots for gas analysis, a dehydration tube with magnesium
perchlorate for drying, etc.
8.3.4.4 Gas detector, consisting of a thermal conductivity detector and an integration meter.
15.9
4.7 16.5
24.4
4 16
ISO 17947:2014(E)
12 34
67 4
Key
1 helium bomb
2 oxygen trap with electric heater
3 carbon dioxide trap
4 dehydration tube
5 impulse furnace
6 dust collector
7 oxidation tube with electric heater
8 thermal conductivity detector
Figure 4 — Block diagram of inert gas fusion–thermal conductivity method
8.3.5 Procedure
a) Amount of sample. Take 0,02 g to 0,04 g of the sample. If complete extraction of nitrogen can be
achieved, take up to 0,1 g of the sample.
b) Starting up of the instrument. Switch on the instrument and set the controls to the specified
values in accordance with the manufacturer’s instruction for operation. Wait until it becomes stable.
c) Preliminary heating. Set a new graphite crucible to the specified position of the impulse furnace.
Flow the inert gas, and then turn on the furnace. Heat the graphite crucible at the degassing
temperature for the specified period, and then heat it at the gas extraction temperature. Read the
integration meter (thereafter referred to as “integral value”). Repeat the steps of the degassing and
the gas extraction until a stable integral value is obtained.
d) Degassing of the graphite crucible. Put the specified amount of bath metal into a new graphite
crucible and place it at the specified position of the impulse furnace. Weigh the sample in a capsule
and enclose by using a jig. Place the capsule at the specified position of sample blower. Feed the inert
gas and energize the graphite crucible. Heat it at the degassing temperature for the specified period
and degas the graphite crucible and the bath metal.
e) Measuring. Throw the sample-embedded capsule into the graphite crucible. Energize the crucible,
and heat the sample at the gas extraction temperature for the specified period and read the integral
value.
8.3.6 Blank test
Run blank determinations according to the operations of 8.3.5 without taking a sample. Repeat these
operations three to five times and obtain an average value.
8.3.7 Calculation of calibration coefficient
Use the nitride whose nitrogen content is known and oxygen content is not greatly different from
the sample for calibration. Some of reference materials of silicon nitride powder can be available. If
12 © ISO 2014 – All rights reserved
ISO 17947:2014(E)
the nitride whose oxygen content is greatly different from that of the sample is used for calibration,
errors may arise. Perform the operations of 8.3.5 with usin
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