1、BRITISH STANDARD BS 6200-3.40.3: 1997 ISO 13898-3: 1997 Sampling and analysis of iron, steel and other ferrous metals Part 3: Methods of analysis Section 3.40 Multi-element methods Subsection 3.40.3 Determination of nickel, copper and cobalt contents by inductively coupled plasma atomic emission spe
2、ctrometric method Determination of copper content ICS 77.080.01BS6200-3.40.3:1997 This British Standard, having been prepared under the directionof the Engineering SectorBoard, was published underthe authority of the Standards Board and comes intoeffect on 15September1997 BSI 03-2000 ISBN 0 580 2841
3、9 0 National foreword This British Standard reproduces verbatim ISO13898-3:1997 and implements it as the UK national standard. The UK participation in its preparation was entrusted to Technical Committee ISE/18, Sampling and analysis of iron and steel, which has the responsibility to: aid enquirers
4、to understand the text; present to the responsible international/European committee any enquiries on the interpretation, or proposals for change, and keep the UK interests informed; monitor related international and European developments and promulgate them in the UK. A list of organizations represe
5、nted on this committee can be obtained on request to its secretary. Cross-references The British Standards which implement international or European publications referred to in this document may be found in the BSI Standards Catalogue under the section entitled “International Standards Correspondenc
6、e Index”, or by using the “Find” facility of the BSI Standards Electronic Catalogue. A British Standard does not purport to include all the necessary provisions of a contract. Users of British Standards are responsible for their correct application. Compliance with a British Standard does not of its
7、elf confer immunity from legal obligations. Summary of pages This document comprises a front cover, an inside front cover, pagesi andii, theISO title page, pagesii toiv, pages1 to5 and a back cover. This standard has been updated (see copyright date) and may have had amendments incorporated. This wi
8、ll be indicated in the amendment table on the inside front cover. Amendments issued since publication Amd. No. Date CommentsBS6200-3.40.3:1997 BSI 03-2000 i Contents Page National foreword Inside front cover Foreword iii Text of ISO 13898-3 1ii blankBS6200-3.40.3:1997 ii BSI 03-2000 Contents Page Fo
9、reword iii 1 Scope 1 2 Normative references 1 3 Principle 1 4 Reagents 1 5 Apparatus 1 6 Sampling 1 7 Procedure 1 8 Expression of results 2 9 Test report 3 Annex A (informative) Additional information on the international cooperative tests 4 Annex B (informative) Graphical representation of precisio
10、n data 5 Figure B.1 Logarithmic relationship betweencopper content ( Cu ) and repeatabilitylimit (r) or reproducibility limits (R and R W ) 5 Table 1 Copper contents between 0,001% (m/m) and 0,40% (m/m) 2 Table 2 Example for copper contents up to 0,008% (m/m) 2 Table 3 Example for copper contents be
11、tween 0,008% (m/m) and 0,080% (m/m) 2 Table 4 3 Table A.1 4 Descriptors: Iron and steel products, unalloyed steels, unalloyed cast iron, chemical analysis, determination of content, copper, spectrometric method, atomic emission spectrometric method. wBS6200-3.40.3:1997 BSI 03-2000 iii Foreword ISO (
12、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 commi
13、ttee 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 electrotec
14、hnical 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 least75% of the member bodies casting a vote. International Standard ISO13898-3 was prepared by T
15、echnical Committee ISO/TC17, Steel, Subcommittee SC1, Methods of determination of chemical composition. ISO 13898 consists of the following parts, under the general title Steel and iron Determination of nickel, copper and cobalt contents Inductively coupled plasma atomic emission spectrometric metho
16、d. Part 1: General requirements and sample dissolution; Part 2: Determination of nickel content; Part 3: Determination of copper content; Part 4: Determination of cobalt content. Annex A and Annex B of this part of ISO13898 are for information only.iv blankBS6200-3.40.3:1997 BSI 03-2000 1 1 Scope Th
17、is part of ISO13898 specifies an inductively coupled plasma atomic emission spectrometric method for the determination of copper content in unalloyed steel and unalloyed iron. The method is applicable to copper contents between0,001% (m/m) and 0,40% (m/m). 2 Normative references The following standa
18、rds contain provisions which, through reference in this text, constitute provisions of this part of ISO13898. At the time of publication, the editions indicated were valid. All standards are subject to revision, and parties to agreements based on this part of ISO13898 are encouraged to investigate t
19、he possibility of applying the most recent editions of the standards indicated below. Members of IECandISO maintain registers of currently valid International Standards. ISO 3696:1987, Water for analytical laboratory use Specification and test methods. ISO 5725-2:1994, Accuracy (trueness and precisi
20、on) of measurement methods and results Part 2: Determination of repeatability and reproducibility of a standard measurement method. ISO 5725-3:1994, Accuracy (trueness and precision) of measurement methods and results Part 3: Intermediate measures of the precision of a standard measurement method. I
21、SO 13898-1:1997, Steel and iron Determination of nickel, cobalt and copper contents Inductively coupled plasma atomic emission spectrometric method Part 1: General requirements and sample dissolution. ISO 14284:1996, Steel and iron Sampling and preparation of samples for the determination of chemica
22、l composition. 3 Principle The principle is described in clause 3 of ISO13898-1:1997. 4 Reagents During the analysis, unless otherwise stated, use only reagents of recognized analytical grade and only grade2 water as specified in ISO3696. In addition to the reagents given in clause 4 of ISO13898-1:1
23、997, the following are required. 4.1 Copper, standard solution. 4.1.1 Stock solution, corresponding to0,80g of copper per litre. Weigh, to the nearest0,1mg, 0,800g of copper metal purity99,99% (m/m) and transfer to a200ml beaker. Add50ml of nitric acid (4.3 of ISO13898-1:1997) cover with a watch-gla
24、ss and heat to dissolve gently. Cool to ambient temperature, transfer into a 1000ml one-mark volumetric flask quantitatively and dilute to the mark with water and mix. 1ml of this stock solution contains0,80mg Cu. 4.1.2 Standard solution A, corresponding to0,08g of copper per litre. Transfer20,0ml o
25、f the copper stock solution (4.1.1) to a200ml one-mark volumetric flask, dilute to the mark with water and mix. Prepare this standard solution immediately before use. 1ml of this standard solution contains0,08mgCu. 4.1.3 Standard solution B, corresponding to0,016g of copper per litre. Transfer10,0ml
26、 of the copper stock solution (4.1.1) to a500ml one-mark volumetric flask, dilute to the mark with water and mix. If the calibration graph is found to be non-linear, an additional calibration series may be used. Prepare this standard solution immediately before use. 1ml of this standard solution con
27、tains0,016mg Cu. 5 Apparatus The apparatus required is given in clause 5 of ISO13898-1:1997. 6 Sampling Carry out sampling in accordance with ISO14284. 7 Procedure 7.1 Test portion Weigh, to the nearest1 mg, approximately1,00g of the test sample. 7.2 Blank test (corresponding to the zero member) Pro
28、ceed as directed in7.2 of ISO13898-1:1997. 7.3 Determination 7.3.1 Preparation of the test solution Proceed as directed in 7.3.1 of ISO 13898-1:1997.BS6200-3.40.3:1997 2 BSI 03-2000 7.3.2 Preparation of the calibration solutions Introduce into a series of six200 ml beakers1,00g 0,001g of the pure ir
29、on (4.1 of ISO13898-1:1997). Add to each beaker 10ml of nitric acid (4.3 of ISO13898-1:1997), cover the beaker with a watch-glass and heat gently until the end of effervescence. Add 10ml of hydrochloric acid(4.2 of ISO13898-1:1997) and continue the heating until complete dissolution occurs. Cool to
30、ambient temperature and transfer the solution to six 200ml one-mark volumetric flasks, rinsing the beakers with the minimum quantity of water. Using a pipette or burette, add to the volumetric flasks the volume of copper standard solution A(4.1.2) indicated inTable 1. If the calibration graph is fou
31、nd to be non-linear, additional calibration series may be used (e.g.Table 2 andTable 3). If the internal standard technique is used, using a pipette, add2ml of the scandium internal standard solution (4.4 of ISO13898-1:1997) or 10ml of the yttrium internal standard solution (4.5 of ISO13898-1:1997).
32、 Dilute to the mark with water and mix. 7.4 Spectrometric measurements 7.4.1 Optimization of the instrument Proceed as directed in7.4.1 of ISO13898-1:1997. 7.4.2 Measurements of the emitted intensities Proceed as directed in7.4.2 of ISO13898-1:1997. 7.4.3 Preparation of the calibration graph Proceed
33、 as directed in7.4.3 of ISO13898-1:1997. Table 1 Copper contents between 0,001% (m/m) and 0,40% (m/m) Table 2 Example for copper contents up to 0,008% (m/m) Table 3 Example for copper contents between 0,008% (m/m) and 0,080% (m/m) 8 Expression of results 8.1 Method of calculation Proceed as directed
34、 in 8.1 of ISO13898-1:1997. 8.2 Precision A planned trial of this method was carried out by26 laboratories in12 countries at10 levels of copper, each laboratory making three determinations (see notes) of copper content at each level. The test samples used are listed inTable A.1. The results obtained
35、 were treated statistically in accordance with ISO5725-1, ISO5725-2 and ISO5725-3, using the data obtained from the samples containing10 levels of copper within the application range. Volume of copper standard solution A Copper concentration Corresponding copper content in the test portion ml 4g/ml
36、% (m/m) 0 a 10,0 15,0 20,0 30,0 50,0 0 4,00 6,00 8,00 12,00 20,00 0 0,080 0,120 0,160 0,240 0,400 a Zero member. Volume of copper standard solution B Copper concentration Corresponding copper content in the test portion ml 4g/ml % (m/m) 0 a 0 0 0,5 0,040 0,000 8 1,0 0,080 0,001 6 2,0 0,160 0,003 2 3
37、,0 0,240 0,004 8 5,0 0,400 0,008 0 a Zero member. Volume of copper standard solution B Copper concentration Corresponding copper content in the test portion ml 4g/ml % (m/m) 0 a 0 0 5,0 0,40 0,008 10,0 0,80 0,016 20,0 1,60 0,032 30,0 2,40 0,048 50,0 4,00 0,080 a Zero member.BS6200-3.40.3:1997 BSI 03
38、-2000 3 The data obtained showed a logarithmic relationship between copper content and repeatability limit (r) and reproducibility limits (R and R w ) of the test results (see notes), as summarized inTable 4. The graphical representation of the data is given inAnnex B. Table 4 NOTE 1Two of the three
39、 determinations were carried out under repeatability conditions as defined in ISO5725-1, i.e.one operator, same apparatus, identical operating conditions, same calibration, and a minimum period of time. NOTE 2The third determination was carried out at a different time (on a different day) by the sam
40、e operator as in note1 using the same apparatus with a new calibration. NOTE 3From the results obtained on day1 the repeatability limit (r) and reproducibility limit (R) were calculated using the procedure specified in ISO5725-2. From the first result obtained on day1 and the result obtained on day2
41、, the within-laboratory reproducibility limit (R w ) was calculated using the procedure given in ISO5725-3. 9 Test report Proceed as directed in clause 9 of ISO13898-1:1997. Copper content Repeatability limit Reproducibility limits % (m/m) r R R W 0,001 0,000 16 0,000 23 0,000 24 0,002 0,000 23 0,00
42、0 37 0,000 35 0,005 0,000 37 0,000 70 0,000 58 0,010 0,000 54 0,001 1 0,000 84 0,020 0,000 77 0,001 8 0,001 2 0,050 0,001 3 0,003 4 0,002 0 0,100 0,001 8 0,005 4 0,002 9 0,200 0,002 6 0,008 4 0,004 2 0,400 0,003 8 0,014 0,006 1BS6200-3.40.3:1997 4 BSI 03-2000 Annex A (informative) Additional informa
43、tion on the international cooperative tests The repeatability and reproducibility data inTable 4 were derived from the results of international analytical trials carried out in1993 on nine steel samples and one iron sample in12 countries involving26 laboratories. The results of the trials were repor
44、ted in document ISO/TC17/SC1N1024, March1994. The graphical presentation of the precision data is given inAnnex B. The test samples used are listed inTable A.1. Table A.1 Sample Copper content % (m/m) Precision data Certified Found Repeatability limit Reproducibility limits Cu,1 Cu,2 r R R W JSS 003
45、-3 (unalloyed steel) 0,001 4 0,001 41 0,001 39 0,000 17 0,000 43 0,000 33 NR 1C (Unalloyed steel) 0,001 4 0,001 45 0,001 42 0,000 30 0,000 36 0,000 59 NR 21 (Unalloyed steel) 0,045 0,042 6 0,042 6 0,001 2 0,002 3 0,001 4 NBS 15h (Unalloyed steel) 0,013 0,012 6 0,012 6 0,000 37 0,000 82 0,000 55 NBS
46、16f (Unalloyed steel) 0,006 0,005 1 0,005 1 0,000 57 0,000 87 0,000 84 BAS 087-1 (Unalloyed steel) 0,171 0,172 0,172 0,003 6 0,008 0 0,007 1 BCS 452 (Unalloyed steel) 0,22 0,217 0,217 0,003 3 0,016 0 0,006 3 IRSID 081-1 (Unalloyed steel) 0,026 0,025 4 0,025 5 0,000 91 0,001 6 0,000 73 IRSID 010-1 (U
47、nalloyed steel) 0,279 0,281 0,281 0,003 2 0,013 0 0,000 70 EURO 487-1 (Pig iron) 0,021 6 0,022 1 0,022 1 0,000 80 0,001 7 0,000 83 Cu,1 : general mean within a day Cu,2 : general mean between days w w w wBS6200-3.40.3:1997 BSI 03-2000 5 Annex B (informative) Graphical representation of precision dat
48、a Figure B.1 Logarithmic relationship between copper content ( Cu ) and repeatability limit (r) or reproducibility limits (R and R W ) wBS 6200-3.40.3: 1997 ISO 13898-3: 1997 BSI 389 Chiswick High Road London W4 4AL BSIBritishStandardsInstitution BSI is the independent national body responsible for
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