1、BSI Standards PublicationBS ISO 6101-3:2014Rubber Determinationof metal content by atomicabsorption spectrometryPart 3: Determination of copper contentBS ISO 6101-3:2014 BRITISH STANDARDNational forewordThis British Standard is the UK implementation of ISO 6101-3:2014. Itsupersedes BS 7164-28.1:1997
2、 which is withdrawn.The UK participation in its preparation was entrusted to TechnicalCommittee PRI/23, Test methods for rubber and non-blackcompounding ingredients.A list of organizations represented on this committee can beobtained on request to its secretary.This publication does not purport to i
3、nclude all the necessaryprovisions of a contract. Users are responsible for its correctapplication. The British Standards Institution 2014. Published by BSI StandardsLimited 2014ISBN 978 0 580 82376 3ICS 83.060Compliance with a British Standard cannot confer immunity fromlegal obligations.This Briti
4、sh Standard was published under the authority of theStandards Policy and Strategy Committee on 31 July 2014.Amendments issued since publicationDate Text affectedBS ISO 6101-3:2014 ISO 2014Rubber Determination of metal content by atomic absorption spectrometry Part 3: Determination of copper contentC
5、aoutchouc Dtermination de la teneur en mtal par spectromtrie dabsorption atomique Partie 3: Dosage du cuivreINTERNATIONAL STANDARDISO6101-3Third edition2014-08-01Reference numberISO 6101-3:2014(E)BS ISO 6101-3:2014ISO 6101-3:2014(E)ii ISO 2014 All rights reservedCOPYRIGHT PROTECTED DOCUMENT ISO 2014
6、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
7、 from either ISO at the address below or ISOs member body in the country of the requester.ISO copyright officeCase postale 56 CH-1211 Geneva 20Tel. + 41 22 749 01 11Fax + 41 22 749 09 47E-mail copyrightiso.orgWeb www.iso.orgPublished in SwitzerlandBS ISO 6101-3:2014ISO 6101-3:2014(E) ISO 2014 All ri
8、ghts reserved iiiContents PageForeword iv1 Scope . 12 Normative references 13 Principle 14 Reagents 25 Apparatus . 26 Sampling 37 Procedure. 37.1 Test portion 37.2 Preparation of test solution . 47.3 Preparation of the calibration graph 47.4 Determination . 57.5 Blank determination 57.6 Number of de
9、terminations . 68 Expression of results 69 Precision . 710 Test report . 7Annex A (informative) Method of standard additions 8Annex B (informative) Precision 10Bibliography .11BS ISO 6101-3:2014ISO 6101-3:2014(E)ForewordISO (the International Organization for Standardization) is a worldwide federati
10、on 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
11、. 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 tho
12、se 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 (
13、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 do
14、cument 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 a
15、nd expressions related to conformity assessment, as well as information about ISOs 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 45, Rubber and rubber products,
16、 Subcommittee SC 2, Testing and analysis.This third edition cancels and replaces the second edition (ISO 6101-3:1997), which has been technically revised.ISO 6101 consists of the following parts, under the general title Rubber Determination of metal content by atomic absorption spectrometry: Part 1:
17、 Determination of zinc content Part 2: Determination of lead content Part 3 Determination of copper content Part 4: Determination of manganese content Part 5: Determination of iron content Part 6: Determination of magnesium contentiv ISO 2014 All rights reservedBS ISO 6101-3:2014INTERNATIONAL STANDA
18、RD ISO 6101-3:2014(E)Rubber Determination of metal content by atomic absorption spectrometry Part 3: Determination of copper contentWARNING Persons using this part of ISO 6101 should be familiar with normal laboratory practice. This part of ISO 6101 does not purport to address all of the safety prob
19、lems, if any, associated with its use. It is the responsibility of the user to establish appropriate safety and health practices and to ensure compliance with any national regulatory conditions.1 ScopeThis part of ISO 6101 specifies an atomic absorption spectrometric method for the determination of
20、the copper content of rubbers.The method is applicable to raw rubber and rubber products having copper contents above 1 ppm. Copper contents below this limit can be determined, provided that suitable adjustments are made to the mass of the test portion and/or to the concentrations of the solutions u
21、sed. The use of the standard additions method can lower the bottom limit of detection.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 u
22、ndated references, the latest edition of the referenced document (including any amendments) applies.ISO 123, Rubber latex SamplingISO 124, Latex, rubber Determination of total solids contentISO 247, Rubber Determination of ashISO 648, Laboratory glassware Single-volume pipettesISO 1042, Laboratory g
23、lassware One-mark volumetric flasksISO 1772, Laboratory crucibles in porcelain and silicaISO 1795, Rubber, raw natural and raw synthetic Sampling and further preparative proceduresISO 4793, Laboratory sintered (fritted) filters Porosity grading, classification and designation3 PrincipleA test portio
24、n is ashed at 550 C 25 C in accordance with ISO 247, method A. The ash is dissolved in hydrochloric acid or nitric acid. The solution is aspirated into an atomic absorption spectrometer and the absorption is measured at a wavelength of 324,7 nm, using a copper hollow-cathode lamp as the copper emiss
25、ion source. Any silicates are volatilized by sulfuric and hydrofluoric acid.NOTE ISO 6955:1982 defines the spectrometric terms used in this part of ISO 6101. ISO 2014 All rights reserved 1BS ISO 6101-3:2014ISO 6101-3:2014(E)4 ReagentsDuring the analysis, unless otherwise stated, use only reagents of
26、 recognized analytical grade and only distilled water or water of equivalent purity.4.1 Hydrochloric acid, 20= 1,18 Mg/m3, 37 % (m/m).4.2 Hydrochloric acid, diluted 1 + 2.Dilute 1 volume of concentrated hydrochloric acid (4.1) with 2 volumes of water.4.3 Sulfuric acid, 20= 1,84 Mg/m3, 95 % (m/m) to
27、97 % (m/m).4.4 Sulfuric acid, diluted 1 + 3.Add carefully 1 volume of concentrated sulfuric acid (4.3) to 3 volumes of water.4.5 Hydrofluoric acid, 20= 1,13 Mg/m3, 38 % (m/m) to 40 % (m/m).4.6 Hydrogen peroxide, 30 % (m/m) solution.4.7 Concentrated nitric acid, 20= 1,41 Mg/m3.4.8 Dilute nitric acid,
28、 1,6 % (by mass), prepared by carefully pipetting 11,5 cm3of concentrated nitric acid (4.7) into a 1 000 cm3one-mark volumetric flask, making up to the mark with water and mixing thoroughly.4.9 Standard copper stock solution, containing 1 g of Cu per 1 000 cm3.Either use a commercially available sta
29、ndard copper solution, or prepare as follows:Weigh, to the nearest 0,1 mg, 1 g of electrolytic copper (purity 99,9 %) and dissolve in 50 cm3of concentrated hydrochloric acid (4.1). Add 15 cm3of hydrogen peroxide solution (4.6). After dissolution, decompose the excess hydrogen peroxide by boiling. Al
30、low to cool and transfer quantitatively to a 1 000 cm3one-mark volumetric flask (see 5.5). Dilute to the mark and mix thoroughly.1 cm3of this standard stock solution contains 1 000 g of Cu.4.10 Standard copper solution, containing 10 mg of Cu per 1 000 cm3.Carefully pipette 10 cm3of the standard cop
31、per stock solution (4.9) into a 1 000 cm3one-mark volumetric flask (see 5.5) and dilute to the mark with 1 + 2 hydrochloric acid (4.2) or dilute nitric acid (4.8), and mix thoroughly. Prepare this solution on the day of use.1 cm3of this standard stock solution contains 10 g of Cu.5 ApparatusOrdinary
32、 laboratory apparatus, plus the following.5.1 Atomic absorption spectrometer, fitted with a burner fed with acetylene and air, compressed to at least 60 kPa and 300 kPa, respectively, and also fitted with a copper hollow-cathode lamp as the copper emission source.The instrument shall be operated in
33、accordance with the manufacturers instructions for optimum performance.2 ISO 2014 All rights reservedBS ISO 6101-3:2014ISO 6101-3:2014(E)Alternatively, an electrothermal atomization device (graphite furnace) may be used. It shall be operated by a competent person in accordance with the manufacturers
34、 instructions for optimum performance.5.2 Balance, accurate to 0,1 mg.5.3 Muffle furnace, capable of being maintained at a temperature of 550 C 25 C.5.4 Glass filter crucible, filter pore size 16 m to 40 m (porosity grade P40 according to ISO 4793).5.5 One-mark volumetric flasks, glass-stoppered, of
35、 capacities 50 cm3, 100 cm3, 200 cm3, 500 cm3and 1 000 cm3, complying with the requirements of ISO 1042, class A.5.6 Volumetric pipettes, of capacities 5 cm3, 10 cm3, 20 cm3, and 50 cm3, complying with the requirements of ISO 648, class A.5.7 Graduated pipette, of capacity 1cm3, complying with the r
36、equirements of ISO 835, class A.5.8 Electric hotplate, or heated sand bath.5.9 Steam bath.5.10 Platinum or borosilicate-glass rod, for use as a stirrer.5.11 Crucible, of platinum, and of capacity 50 cm3to 150 cm3depending on the test portion size.5.12 Crucible, of silica, porcelain, or borosilicate
37、glass, of capacity 50 cm3to 150 cm3depending on the test portion size, complying with the requirements of ISO 1772.5.13 Ashless filter paper.6 SamplingCarry out sampling as follows: raw rubber: in accordance with ISO 1795; latex: in accordance with ISO 123; products: to be representative of the whol
38、e batch.7 Procedure7.1 Test portionWeigh, to the nearest 0,1 mg, approximately 1 g to 5 g of rubber product and 5 g to 10 g of raw rubber, milled or finely cut, into an appropriate crucible. Wrap the test portion in an ashless filter paper and place into an appropriate crucible (5.11 or 5.12). The s
39、ize of the test portion shall be judged by prior knowledge of the approximate amount of copper present.For natural rubber latex concentrate, take a portion of thoroughly mixed latex containing about 10 g of total solids, make into a thin film by pouring the portion onto a glass plate, dry to constan
40、t mass as specified in ISO 124 and cut into small pieces.For raw, natural rubber, take the test portion from a test sample prepared in accordance with ISO 1795. ISO 2014 All rights reserved 3BS ISO 6101-3:2014ISO 6101-3:2014(E)7.2 Preparation of test solution7.2.1 Destruction of organic matterAsh th
41、e test portion in accordance with method A of ISO 247, in the muffle furnace (5.3), maintained at 550 C 25 C. If the ash is black, caused by small amounts of carbon black, stir carefully with the platinum or borosilicate-glass rod (5.10) and continue heating.7.2.2 Dissolution of inorganic residue us
42、ing hydrochloric acidAfter ashing, allow the crucible and its contents to cool to ambient temperature. Add 20 cm3of concentrated hydrochloric acid (4.1). Heat the mixture on the steam bath (5.9) for at least 10 min. Do not let the reaction mixture boil. Allow to cool to ambient temperature and trans
43、fer the solution quantitatively, with the aid of water, to a 50 cm3one-mark volumetric flask (5.5). If the ash is not totally dissolved, proceed as follows. Transfer the solution and the undissolved ash quantitatively, with the aid of water, to a platinum crucible (5.11). Add a few drops of concentr
44、ated sulfuric acid (4.3) and 5 cm3of hydrofluoric acid (4.5). Heat on the electric hotplate or heated sand bath (5.8) in a fume cupboard and evaporate to dryness, while stirring with a platinum rod (5.10). Repeat this digestion with the same quantities of sulfuric and hydrofluoric acids two more tim
45、es. Allow to cool to ambient temperature, add 20 cm3of concentrated hydrochloric acid (4.1), heat for 10 min and transfer quantitatively, with the aid of water, to a 50 cm3one-mark volumetric flask (5.5). Dilute to the mark with water and mix thoroughly. Insoluble matter can settle and, if so, shall
46、 be filtered off using a filter crucible (5.4) just before making spectrometric measurements in accordance with 7.3.Test solutions should contain approximately 12 % hydrochloric acid. If evaporation, etc., has reduced or increased this concentration, adjust accordingly with concentrated hydrochloric
47、 acid (4.1) or water.7.2.3 Dissolution of inorganic residue using nitric acid Alternative methodAdd 10 cm3of dilute nitric acid (4.8) to the cooled residue. Cover with a watch glass and heat on a steam bath (5.9) for at least 30 min. Allow to cool to ambient temperature. Filter the contents of the c
48、rucible into a 50 cm3one-mark volumetric flask, rinsing the crucible, and making up to the mark with dilute nitric acid (4.8).7.3 Preparation of the calibration graph7.3.1 Preparation of calibration solutions7.3.1.1 Into a series of five 100 cm3one-mark volumetric flasks (see 5.5), introduce, using
49、pipettes (see 5.6) the volumes of standard copper solution (4.10) indicated in Table 1. Dilute to the mark with 1 + 2 hydrochloric acid solution (4.2) or dilute nitric acid (4.8) and mix thoroughly.Table 1 Standard calibration solutionsVolume of standard copper solution cm3Mass of copper contained in 1 cm3g50 520 210 14 ISO 2014 All rights reservedBS ISO 6101-3:2014ISO 6101-3:2014(E)Volume of standard copper solution cm3Mass of copper contained in 1 cm3g5 0,50 07.3.1.2 Prepare the set o
