1、BRITISH STANDARD BS 6200-3.40.4: 1997 ISO13898-4: 1997 Sampling and analysis of iron, steel and other ferrous metals Part3: Methods of analysis Section3.40 Multi-element methods Subsection3.40.4 Determination of nickel, copper and cobalt contents by inductively coupled plasma atomic emission spectro
2、metric method Determination of cobalt content ICS77.080.01BS 6200-3.40.4:1997 This British Standard, having been prepared under the directionof the Engineering SectorBoard, was published underthe authority of the Standards Board and comes into effect on 15 September1997 BSI 09-1999 ISBN0 580 28418 2
3、 National foreword This British Standard reproduces verbatim ISO13898-4:1997 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 responsiblity to: aid enquirers to u
4、nderstand 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 represented
5、 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 Correspondence In
6、dex”, 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 itself
7、confer immunity from legal obligations. Summary of pages This document comprises a front cover, an inside front cover, pages i and ii, theISO title page, pages ii to iv, pages 1 to 4 and a back cover. This standard has been updated (see copyright date) and may have had amendments incorporated. This
8、will be indicated in the amendment table on the inside front cover. Amendments issued since publication Amd. No. Date CommentsBS 6200-3.40.4:1997 BSI 09-1999 i Contents Page National foreword Inside front cover Foreword iii Text of ISO 13898-4 1ii blankBS 6200-3.40.4:1997 ii BSI 09-1999 Contents Pag
9、e Foreword 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 2 Annex A (informative) Additional information on the international cooperativetests 3 Annex B (informative) Graphical representation of preci
10、sion data 4 Figure B.1 Logarithmic relationship between cobalt content () and repeatability limit (r) or reproducibility limits (R and R W ) 4 Table 1 Cobalt contents between0,001% (m/m) and0,10% (m/m) 2 Table 2 Example for cobalt contents up to0,010% (m/m) 2 Table 3 2 Table A.1 3 w CoBS 6200-3.40.4
11、:1997 BSI 09-1999 iii 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
12、 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 Commissio
13、n (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 least75% of the member bodies casting a vote. International S
14、tandard ISO13898-3 was prepared by Technical Committee ISO/TC17, Steel, Subcommittee SC1, Methods of determination of chemical composition. ISO13898 consists of the following parts, under the general title Steel and iron Determination of nickel, copper and cobalt contents Inductively coupled plasma
15、atomic emission spectrometric method. Part1: General requirements and sample dissolution; Part2: Determination of nickel content; Part3: Determination of copper content; Part4: Determination of cobalt content. Annex A andAnnex B of this part of ISO13898 are for information only. Descriptors: Iron an
16、d steel products, unalloyed steels, unalloyed cast iron, chemical analysis, determination of content, cobalt, spectrometric method, atomic emission spectrometric method.iv blankBS 6200-3.40.4:1997 BSI 09-1999 1 1 Scope This part of ISO13898 specifies an inductively coupled plasma atomic emission spe
17、ctrometric method for the determination of cobalt content in unalloyed steel and unalloyed iron. The method is applicable to cobalt contents between0,001% (m/m) and0,10% (m/m). 2 Normative references The following standards contain provisions which, through reference in this text, constitute provisi
18、ons 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 the possibility of applying the most recent editions of the standards indicated b
19、elow. Members of IEC and ISO 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 precision) of measurement methods and results Part2:Determination of repeatability an
20、d reproducibility of a standard measurement method. ISO 5725-3:1994, Accuracy (trueness and precision) of measurement methods and results Part3:Intermediate measures of the precision of a standard measurement method. ISO 13898-1:1997, Steel and iron Determination of nickel, cobalt and copper content
21、s Inductively coupled plasma atomic emission spectrometric method Part1: General requirements and sample dissolution. ISO 14284:1996, Steel and iron Sampling and preparation of samples for the determination of chemical composition. 3 Principle The principle is described inclause3 of ISO13898-1:1997.
22、 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 inclause4 of ISO13898-1:1997, the following are required. 4.1 Cobalt, standard solution. 4.1.1 Stock solution, c
23、orresponding to1,0g of cobalt per litre. Weigh, to the nearest0,1mg,1,000g of cobalt metal purity99,99% (m/m) and transfer to a200ml beaker. Add50ml of nitric acid(4.3 of ISOISO13898-1: 1) ), cover with a watch-glass and heat to dissolve gently. Cool to ambient temperature, transfer into a1000ml one
24、-mark volumetric flask quantitatively and dilute to the mark with water and mix. 1ml of this stock solution contains1,0mg Co. 4.1.2 Standard solution, corresponding to0,020g of cobalt per litre. Transfer10,0 ml of the cobalt stock solution (4.1.1) to a500ml one-mark volumetric flask, dilute to the m
25、ark 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 contains0,020mg Co. 5 Apparatus The apparatus required is given inclause5 ofISO13898-1: 1) .
26、6 Sampling Carry out sampling in accordance with ISO14284. 7 Procedure 7.1 Test portion Weigh, to the nearest1mg, about1,00g of the test sample. 7.2 Blank test (corresponding to the zero member) Proceed as directed in7.2 of ISO13898-1:1997. 7.3 Determination 7.3.1 Preparation of the test solution Pr
27、oceed as directed in7.3.1 of ISO13898-1:1997. 7.3.2 Preparation of the calibration solutions Introduce into a series of six200ml beakers1,00g 0,001g of the pure iron (4.1 of ISO13898-1:1997). Add to each beaker10ml of nitric acid (4.3 ofISO13898-1:1997), cover the beaker with a watch-glass and heat
28、gently until the end of effervescence. Add10ml of hydrochloric acid(4.2 ofISO13898-1:1997) and continue the heating until complete dissolution occurs. Cool to ambient temperature and transfer the solution to six200ml one-mark volumetric flasks, rinsing the beakers with the minimum quantity of water.
29、BS 6200-3.40.4:1997 2 BSI 09-1999 Using a pipette or burette, add to the volumetric flasks the volume of cobalt standard solution(4.1.2) indicatedinTable 1. If the calibration graph is found to be non-linear, an additional calibration series may be used (e.g.Table 2). If the internal standard techni
30、que is used, using a pipette, add2ml of the scandium internal standard solution(4.4 ofISOISO13898-1:1997) or10ml of the yttrium internal standard solution (4.5 of ISO13898-1:1997). Dilute to the mark with water and mix. Table 1 Cobalt contents between0,001% (m/m) and0,10% (m/m) Table 2 Example for c
31、obalt contents up to0,010% (m/m) 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 ofISO13898-1:1997. 7.4.3 Preparation of the calibration graph Proceed as dire
32、cted in7.4.3 ofISO13898-1:1997. 8 Expression of results 8.1 Method of calculation Proceed as directed in8.1 of ISO13898-1:1997. 8.2 Precision A planned trial of this method was carried out by26 laboratories in12 countries at eight levels of cobalt, each laboratory making three determinations of coba
33、lt content at each level (seenotes). The test samples used are listed inTable A.1. The results obtained were treated statistically in accordance withISO5725-1, ISO5725-2 and ISO5725-3, using the data obtained from the samples containing eight levels of cobalt within the application range. The data o
34、btained showed a logarithmic relationship between cobalt content and repeatability limit (r) and reproducibility limits (R and Rw) of the test results (seenotes), as summarized inTable 3. (seenotes). The graphical representation of the data is given inAnnex B. Table 3 NOTE 1Two of the three determin
35、ations were carried out under repeatability conditions as defined inISO5725-1, 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 same operator
36、 as innote1 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 inISO5725-2. From the first result obtained on day1 and the result obtained on day2, the within
37、-laboratory reproducibility limit (Rw) was calculated using the procedure given inISO5725-3. 9 Test report Proceed as directed inclause9 of ISO13898-1:1997. Volume of cobalt standard solution (4.1.2) Cobalt concentration Corresponding cobalt content in the test portion ml 4 g/ml % (m/m) 0 a 5,0 10,0
38、 20,0 30,0 50,0 0 0,50 1,00 2,00 3,00 5,00 0 0,010 0,020 0,040 0,060 0,100 a Zero member. Volume of cobalt standard solution(4.1.2) Cobalt concentration Corresponding cobalt content in the test portion ml 4g/ml % (m/m) 0 a 0,5 1,0 2,0 3,0 5,0 0 0,050 0,100 0,200 0,300 0,500 0 0,0010 0,0020 0,0040 0,
39、0060 0,0100 a Zero member. Cobalt content Repeatability limit Reproducibility limits % (m/m) r R Rw 0,001 0,002 0,005 0,010 0,020 0,050 0,100 0,00018 0,00025 0,00037 0,00050 0,00068 0,00102 0,0014 0,00051 0,00070 0,00105 0,0014 0,0019 0,0029 0,0040 0,00030 0,00040 0,00057 0,00075 0,00098 0,0014 0,00
40、18BS 6200-3.40.4:1997 BSI 09-1999 3 Annex A (informative) Additional information on the international cooperative tests The repeatability and reproducibility data inTable 3 were derived from the results of international analytical trials carried out in1993 on seven steel samples and one iron sample
41、in12 countries involving26 laboratories. The results of the trials were reported in documentISO/TC17/SC1N1024, March1994. The graphical presentation of the precision data is giveninAnnex B. The test samples used are listed inTable A.1. Table A.1 Sample Cobalt content %(m/m) Precision data Certified
42、Found Repeatability limit Reproducibility limits r R R W JSS003-3 (unalloyed steel) 0,0010 0,00097 0,00098 0,00024 0,00048 0,00039 NR1C (unalloyedsteel) 0,0046 0,0047 0,0047 0,00026 0,00084 0,00038 NR21 (unalloyedsteel) 0,008 0,0080 0,0080 0,00043 0,0017 0,00060 NBS16f (unalloyed steel) 0,003 0,0036
43、 0,0036 0,00034 0,00087 0,00049 BAS087-1 (unalloyed steel) 0,015 0,0149 0,0148 0,00042 0,0013 0,00093 BCS456-1 (unalloyed steel) 0,052 0,054 0,054 0,0015 0,003 6 0,0023 IRSID081-1 (unalloyed steel) 0,017 0,0175 0,0174 0,00064 0,0017 0,00101 EURO487-1 (pigiron) 0,0088 0,0085 0,0085 0,00066 0,0094 0,0
44、0060 : general mean within a day : general mean between days w Co,1 w Co,2 w Co,1 w Co,2BS 6200-3.40.4:1997 4 BSI 09-1999 Annex B (informative) Graphical representation of precision data lg r = 0,439 5 lg 2,4211 lg R = 0,445 9 lg 1,9538 lg R W= 0,392 8 lg 2,3409 where is the average cobalt content,
45、expressed as a percentage by mass, obtained within a day; is the average cobalt content, expressed as a percentage by mass, obtained between days. Figure B.1 Logarithmic relationship between cobalt content () and repeatability limit (r) or reproducibility limits (R and R w ) w Co,1 w Co,1 w Co,2 w C
46、o,1 w Co,2 w Co5 blankBS 6200-3.40.4: 1997 ISO13898-4: 1997 BSI 389 Chiswick High Road London W4 4AL BSIBritishStandardsInstitution BSI is the independent national body responsible for preparing BritishStandards. It presents the UK view on standards in Europe and at the international level. It is in
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