Steel - Determination of boron content - Curcumin spectrophotometric method after distillation (ISO 13900:1997)

Method for determination of boron content between 0,00005 % and 0,001 % in steel.

Stahl - Bestimmung des Borgehaltes - Curcumin-Verfahren - Fotometrische Bestimmung nach Destillation (ISO 13900:1997)

Aciers - Dosage du bore - Méthode spectrophotométrique à la curcumine après distillation (ISO 13900:1997)

Jeklo - Določevanje bora - Kurkuminska spektrofotometrijska metoda po destilaciji (ISO 13900:1997)

General Information

Status
Published
Publication Date
16-Jul-2002
Current Stage
9093 - Decision to confirm - Review Enquiry
Due Date
03-Jun-2009
Completion Date
03-Jun-2009

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SLOVENSKI STANDARD
SIST EN ISO 13900:2003
01-april-2003

-HNOR'RORþHYDQMHERUD.XUNXPLQVNDVSHNWURIRWRPHWULMVNDPHWRGDSRGHVWLODFLML

,62

Steel - Determination of boron content - Curcumin spectrophotometric method after

distillation (ISO 13900:1997)

Stahl - Bestimmung des Borgehaltes - Curcumin-Verfahren - Fotometrische Bestimmung

nach Destillation (ISO 13900:1997)
Aciers - Dosage du bore - Méthode spectrophotométrique a la curcumine apres
distillation (ISO 13900:1997)
Ta slovenski standard je istoveten z: EN ISO 13900:2002
ICS:
77.040.30 Kemijska analiza kovin Chemical analysis of metals
77.080.20 Jekla Steels
SIST EN ISO 13900:2003 en

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

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SIST EN ISO 13900:2003
---------------------- Page: 2 ----------------------
SIST EN ISO 13900:2003
EUROPEAN STANDARD
EN ISO 13900
NORME EUROPÉENNE
EUROPÄISCHE NORM
July 2002
ICS 77.080.20
English version
Steel - Determination of boron content - Curcumin
spectrophotometric method after distillation (ISO 13900:1997)

Aciers - Dosage du bore - Méthode spectrophotométrique à Stahl - Bestimmung des Borgehaltes - Curcumin-Verfahren

la curcumine après distillation (ISO 13900:1997) - Fotometrische Bestimmung nach Destillation (ISO

13900:1997)
This European Standard was approved by CEN on 26 May 2002.

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 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 Management Centre has the same status as the official

versions.

CEN members are the national standards bodies of Austria, Belgium, Czech Republic, Denmark, Finland, France, Germany, Greece,

Iceland, Ireland, Italy, Luxembourg, Malta, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and United Kingdom.

EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
Management Centre: rue de Stassart, 36 B-1050 Brussels

© 2002 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN ISO 13900:2002 E

worldwide for CEN national Members.
---------------------- Page: 3 ----------------------
SIST EN ISO 13900:2003
EN ISO 13900:2002 (E)
Foreword

The text of the International Standard from Technical Committee ISO/TC 17 "Steel" of the

International Organization for Standardization (ISO) has been taken over as a European

Standard by Technical Committee ECISS/TC 20 "Methods of chemical analysis of ferrous

products", the secretariat of which is held by SIS.

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 January 2003, and conflicting national

standards shall be withdrawn at the latest by January 2003.

According to the CEN/CENELEC Internal Regulations, the national standards organizations of

the following countries are bound to implement this European Standard: Austria, Belgium,

Czech Republic, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy,

Luxembourg, Malta, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and the

United Kingdom.
Endorsement notice

The text of the International Standard ISO 13900:1997 has been approved by CEN as a

European Standard without any modifications.

NOTE Normative references to International Standards are listed in annex ZA (normative).

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SIST EN ISO 13900:2003
EN ISO 13900:2002 (E)
Annex ZA
(normative)
Normative references to international publications
with their relevant European publications

This European Standard incorporates by dated or undated reference, provisions from other

publications. These normative references are cited at the appropriate places in the text and the

publications are listed hereafter. For dated references, subsequent amendments to or revisions

of any of these publications apply to this European Standard only when incorporated in it by

amendment or revision. For undated references the latest edition of the publication referred to

applies (including amendments).

NOTE Where an International Publication has been modified by common modifications,

indicated by (mod.), the relevant EN/HD applies.
Publication Year Title EN Year
ISO 1042 1998 Laboratory glassware - One-mark volumetric EN ISO 1042 1999
flasks
ISO 3696 1987 Water for analytical laboratory use - EN ISO 3696 1995
Specification and test methods
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SIST EN ISO 13900:2003
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SIST EN ISO 13900:2003
INTERNATIONAL IS0
STANDARD
13900
First edition
1997-08- 15
Steel
- Determination of boron content -
Curcumin spectrophotometric method after
distillation
Aciers M&hode spectrophotomktrique i la curcumine
- Dosage du bore -
apr& distillation
Reference number
IS0 13900: 1997(E)
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SIST EN ISO 13900:2003
IS0 13900: 1997(E)
Foreword

IS0 (the International Organization for Standardization) is a worldwide federation of national standards bodies (IS0

member bodies). The work of preparing International Standards is normally carried out through IS0 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. IS0 collaborates closely with the International Electrotechnical

Commission (IEC) on all matters of electrotechnical standardization.

Draft International Standards adopted by the technical committees are circulated to the member bodies for voting.

Publication as an International Standard requires approval by at least 75 % of the member bodies casting a vote.

International Standard IS0 13900 was prepared by Technical Committee ISOFC 17, Steel, Subcommittee SC 1,

Methods of determination of chemical composition.
Annexes A to C of this International Standard are for information only.
0 IS0 1997

All rights reserved. Unless otherwise specified, no part of this publication may be reproduced

or utilized in any form or by any means, electronic or mechanical, including photocopying and

microfilm, without permission in writing from the publisher.
International Organization for Standardization
Case postale 56 l CH-1211 Geneve 20 l Switzerland
Internet central @ isoch
x.400 c=ch; a=400net; p=iso; o=isocs; s=central
Printed in Switzerland
---------------------- Page: 8 ----------------------
SIST EN ISO 13900:2003
INTERNATIONAL STANDARD o IS0 ISO13900:1997( E)
Steel - Determination of boron content - Curcumin
spectrophotometric method after distillation
1 scope

This International Standard specifies a method for the determination of the boron content in steel using a curcumin

spectrophotometric method after distillation.

The method is applicable to a boron content of between 0,000 05 % (m/m) and 0,001 0 % (m/m).

2 Normative references

The following standards contain provisions which, through reference in this text, constitute provisions of this

International Standard. At the time of publication, the editions indicated were valid. All standards are subject to

revision, and parties to agreements based on this International Standard are encouraged to investigate the

possibility of applying the most recent editions of the standards indicated below. Members of IEC and IS0 maintain

registers of currently valid International Standards.

IS0 385-l :I 984, Laboratory glassware - Burettes - Part 1: General requirements.

IS0 648: 1977, Laboratory glassware - One-mark pipettes.
IS0 1042: ----I), Laboratory glassware - One-mark volumetric flasks.

IS0 3696:1987, Water for analytical laboratory use - Specification and test methods.

IS0 5725-l :I 994, Accuracy (trueness and precision) of measurement methods and results - Par? I: General

principles and definitions.

IS0 5725-2:1994, Accuracy (trueness and precision) of measurement methods and results - Part 2: Basic method

for the determination of repeatability and reproducibility of a standard measurement method.

IS0 5725-3:1994, Accuracy (trueness and precision) of measurement methods and results - Pat? 3: Intermediate

measures of the precision of a standard measurement method.

IS0 14284 :I 996, Steel and iron - Sampling and preparation of samples for the determination of chemical

composition.
3 Principle
Dissolution of a test portion in hydrochloric and nitric acids.
1) To be published. (Revision of IS0 1042:1983)
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SIST EN ISO 13900:2003
0 IS0
IS0 13900: 1997(E)

Decomposition of boron compounds (nitrides etc.) with orthophosphoric and sulfuric acids at a temperature of

290 OC.

Distillation of the solution after the addition of methanol and collection of methylborate in a receiver containing

sodium hydroxide solution.
Formation of a coloured complex between orthoboric acid and curcumin in a
Evaporation of the solution to dryness.
methanol medium.
Spectrophotometric measurement at a wavelength of about 550 nm.
4 Reagents

During the analysis, unless otherwise stated, use only reagents of recognized analytical grade and only grade 2

water as specified in IS0 3696.
4.1 Pure iron, free from boron or with a known residual amount of boron.
4.2 Hydrochloric acid, p about 1,19 g/ml.
4.3 Nitric acid, p about 1,40 g/ml.
4.4 Sulfuric acid, p about 1,84 g/ml.
4.5 Orthophosphoric acid, p about 1,71 g/ml, boron content less than 0,02 pg/ml.
4.6 Acetic acid, free from aldehyde, p about 1,05 g/ml.

In order to test the acetic acid for the presence of aldehyde, pour 20 ml of acetic acid (p about I,05 g/ml) and 1 ml

of potassium permanganate solution (1 g/l) into a 50 ml beaker. In the absence of aldehyde, the initial violet colour

of potassium permanganate will persist ; otherwise the solution will become an easily identifiable brown colour after

15 min.
4.7 Acid mixture A
Add one volume of hydrochloric acid (4.2) to two volumes of acetic acid (4.6).
4.8 Acid mixture B

While cooling under water and swirling, add in small portions a volume of sulfuric acid (4.4) to an equal volume of

acetic acid (4.6).
4.9 Sodium hydroxide, 8 g/l solution.
4.10 Methanol, minimum assay 99,6 % (VW).
4.11 Boron, standard solution.
4.11 .l Stock solution, corresponding to 0,lO g of boron per litre.

Weigh, to the nearest 0,000 1 g, 0,286 0 g of orthoboric acid (H,BO,). Place in a 250 ml beaker and dissolve in

about 200 ml of water. Transfer the solution quantitatively to a 500 ml one-mark volumetric flask. Dilute to the

mark with water and mix. Store in a polypropylene bottle (5.2).
1 ml of this stock solution contains 0,lO mg of boron.
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SIST EN ISO 13900:2003
0 IS0
IS0 13900: 1997(E)
4.11.2 Standard solution, corresponding to 0,001 g of boron per litre.

Transfer I,0 ml of the stock solution (4.11J) to a 100 ml one-mark volumetric flask. Dilute to the mark with water

and mix. Store in a polypropylene bottle (5.2).
Prepare this solution immediately before use.
1 ml of this standard solution contains 1 pg of boron.
4.12 Curcumin, acetic acid solution, 1,25 g/l.

Weigh 0,125 g of curcumin, [CH,O(OH)C,H,CH=CHCO],CH,, in a polypropylene or quartz vessel, add 60 ml of

acetic acid (4.6) and mix. Heat in a water bath at 40 OC and stir using a magnetic stirrer. After dissolution, cool and

transfer to a 100 ml polypropylene volumetric flask. Dilute to the mark with acetic acid and mix.

4.13 Carrier gas, nitrogen, argon or dry air.
5 Apparatus

Glassware, polypropylene or quartz equipment rinsed with acetic acid (4.6) then with water and finally dried. All

volumetric glassware shall be grade A, in accordance with IS0 3851, IS0 648 or IS0 1042, as appropriate.

Ordinary laboratory apparatus and the following shall be used.
5.1 Volumetric flask, of capacity 100 ml.
100 ml and 500 ml.
5.2 Polypropylene bottles, of capacitie
...

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