BS 6200-3 40 2-1997 Sampling and analysis of iron steel and other ferrous metals - Methods of analysis - Multi-element methods - Determination of nickel copper and cobalt contents .pdf

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1、BRITISH STANDARD BS 6200-3.40.2: 1997 ISO 13898-2: 1997 Sampling and analysis of iron, steel and other ferrous metals Part 3: Methods of analysis Section 3.40 Multi-element methods Subsection 3.40.2 Determination of nickel, copper and cobalt contents by inductively coupled plasma atomic emission spe

2、ctrometric method Determination of nickel content ICS 77.080.01BS 6200-3.40.2:1997 This British Standard, having been prepared under the directionof the Engineering SectorBoard, was published underthe authority of the Standards Board and comes intoeffect on 15 September 1997 BSI 09-1999 ISBN 0 580 2

3、8420 4 National foreword This British Standard reproduces verbatim ISO13898-2:1997 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 enquirer

4、s 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 repre

5、sented 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 Corresponde

6、nce 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 i

7、tself 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 5 and a back cover. This standard has been updated (see copyright date) and may have had amendments incorporated.

8、 This will be indicated in the amendment table on the inside front cover. Amendments issued since publication Amd. No. Date CommentsBS 6200-3.40.2:1997 BSI 09-1999 i Contents Page National foreword Inside front cover Foreword iii Text of ISO 13898-2 1ii blankBS 6200-3.40.2:1997 ii BSI 09-1999 Conten

9、ts Page 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 3 9 Test report 3 Annex A (informative) Additional information on the international cooperativetests 4 Annex B (informative) Graphical representation of

10、 precision data 5 Figure B.1 Logarithmic relationship between nickel content () and repeatability limit (r) or reproducibility limits (R and Rw) 5 Table 1 Nickel contents between 0,001 % (m/m) and 0,30 % (m/m) 2 Table 2 Example for nickel contents up to 0,010 % (m/m) 2 Table 3 Example for nickel con

11、tents between 0,010 % (m/m) and 0,060 % (m/m) 3 Table 4 3 Table A.1 4 Descriptors: Iron and steel products, unalloyed steels, unalloyed cast iron, chemical analysis, determination of content, nickel, spectrometric method, atomic emission spectrometric method. w NiBS 6200-3.40.2:1997 BSI 09-1999 iii

12、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 t

13、echnical 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

14、 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 Standard ISO13898-2 was

15、 prepared by Technical 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 spect

16、rometric method. 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 blankBS 6200-3.40.2:1997 BSI 09-19

17、99 1 1 Scope This part of ISO13898 specifies an inductively coupled plasma atomic emission spectrometric method for the determination of nickel content in unalloyed steel and unalloyed iron. The method is applicable to nickel contents between0,001% (m/m) and0,30% (m/m). 2 Normative references The fo

18、llowing standards 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

19、 investigate the possibility of applying the most recent editions of the standards indicated below. 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 5725-1:1994, Accuracy (true

20、ness and precision) of measurement methods and results Part1:General principles and definitions. ISO 5725-2:1994, Accuracy (trueness and precision) of measurement methods and results Part2:Determination of repeatability and reproducibility of a standard measurement method. ISO 5725-3:1994, Accuracy

21、(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 contents Inductively coupled plasma atomic emission spectrometric method Part1: Gener

22、al 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 in clause3 of ISO13898-1:1997. 4 Reagents During the analysis, unless otherwise stated, use only reagents o

23、f recognized analytical grade and only grade2 water as specified in ISO3696. In addition to the reagents given in clause4 of ISO13898-1:1997, the following are required. 4.1 Nickel standard solution 4.1.1 Stock solution, corresponding to1,0g of nickel per litre. Weigh, to the nearest0,1mg,1,000g of

24、nickel metal purity 99,9% (m/m) and transfer to a200ml beaker. Add50ml of nitric acid (4.3 of ISO13898-1:1997) cover with a watch-glass and heat to dissolve gently. Cool to ambient temperature, quantitatively transfer to a1000ml one-mark volumetric flask and dilute to the mark with water and mix. 1

25、ml of this stock solution contains1,0mg Ni. 4.1.2 Standard solution A, corresponding to0,100g of nickel per litre. Transfer20,0ml of the nickel 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. 1

26、ml of this standard solution contains0,10mg Ni. 4.1.3 Standard solution B, corresponding to0,020g of nickel per litre. Transfer 10,0ml of the nickel 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,

27、additional calibration series may be used. Prepare this standard solution immediately before use. 1 ml of this standard solution contains0,020mg Ni. 5 Apparatus The apparatus required is given in clause5 of ISO13898-1:1997. 6 Sampling Carry out sampling in accordance with ISO14284. 7 Procedure 7.1 T

28、est 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 Proceed as directed in7.3.1 of ISO13898-1:1997.BS 6200-3.40.2:1997 2 BSI 09-19

29、99 7.3.2 Preparation of the calibration solutions Transfer to 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 of ISO13898-1:1997), cover the beaker with a watch-glass and heat gently until the end of effervescence. Add10m

30、l of hydrochloric acid(4.2 of ISO13898-1:1997) 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. Using a pipette or burette, add to the volu

31、metric flasks the volume of nickel standard solutionA(4.1.2) indicated in Table 1. If the calibration graph is found to be non-linear, additional calibration series may be used (e.g. Table 2 and Table 3). If the internal standard technique is used, using a pipette, add2ml of the scandium internal st

32、andard solution (4.4 of ISO13898-1:1997) or10ml of the yttrium internal standard solution (4.5 of ISO13898-1:1997). 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 emi

33、tted intensities Proceed as directed in7.4.2 of ISO13898-1:1997. 7.4.3 Preparation of the calibration graph Proceed as directed in7.4.3 of ISO13898-1:1997. Table 1 Nickel contents between 0,001 % (m/m) and 0,30 % (m/m) Table 2 Example for nickel contents up to 0,010 % (m/m) Volume of nickel standard

34、solution A (4.1.2) Nickel concentration Corresponding nickel content in the test portion ml 4g/ml % (m/m) 0 a 5,0 10,0 15,0 20,0 30,0 0 2,50 5,00 7,50 10,00 15,00 0 0,050 0,100 0,150 0,200 0,300 a Zero member. Volume of nickel standardsolution B (4.1.3) Nickel concentration Corresponding nickel cont

35、ent 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 0,001 0 0,002 0 0,004 0 0,006 0 0,010 0 a Zero member.BS 6200-3.40.2:1997 BSI 09-1999 3 Table 3 Example for nickel contents between 0,010 % (m/m) and 0,060 % (m/m) Table 4 8 Expression of results 8.1 M

36、ethod 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 at11 levels of nickel, each laboratory making three determinations of nickel content at each level (see notes1 and2). The test samples used

37、 are listed inTable A.1. The results obtained were treated statistically in accordance with ISO5725-1, ISO5725-2 and ISO5725-3, using the data obtained from the samples containing11 levels of nickel within the application range. The data obtained showed a logarithmic relationship between nickel cont

38、ent and repeatability limit (r) and reproducibility limits (R and Rw) of the test results (see note3), as summarized inTable 4. The graphical representation of the data is given inAnnex B. NOTE 1Two of the three determinations were carried out under repeatability conditions as defined in ISO5725-1,

39、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 as in note1 using the same apparatus with a new calibration. NOTE 3From the r

40、esults 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, the within-laboratory reproducibility limit (Rw) was calculated using the procedure gi

41、ven in ISO5725-3. 9 Test report Proceed as directed in clause9 of ISO13898-1:1997. Volume of nickel standardsolution B (4.1.3) Nickel concentration Corresponding nickel content in the test portion ml 4g/ml % (m/m) 0 a 0,5 10,0 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

42、 a Zero member. Nickel content Repeatability limit Reproducibility limits % (m/m) r R Rw 0,001 0,002 0,005 0,010 0,020 0,050 0,000 39 0,000 46 0,000 56 0,000 66 0,000 77 0,000 95 0,000 76 0,000 95 0,001 3 0,001 6 0,002 0 0,002 8 0,000 55 0,000 67 0,000 87 0,001 0 0,001 3 0,001 6 0,050 0,100 0,200 0,

43、300 0,001 3 0,002 6 0,005 1 0,007 5 0,003 7 0,007 4 0,015 0,023 0,002 0 0,003 7 0,007 0 0,010BS 6200-3.40.2:1997 4 BSI 09-1999 Annex A (informative) Additional information on the international cooperative tests The repeatability and reproducibility data inTable 4 were derived from the results of int

44、ernational analytical trials carried out in1993 on nine steel samples and two iron samples in12 countries involving26 laboratories. The results of the trials were reported in document ISO/TC17/SC1 N1024, March1994. The graphical presentation of the precision data is given inAnnex B. The test samples

45、 used are listed inTable A.1. Table A.1 Sample Nickel content % (m/m) Precision data Certified Found Repeatability limit Reproducibility limits r R Rw JSS 003-3 (Unalloyed steel) 0,000 8 0,000 76 0,000 76 0,000 49 0,000 75 0,000 53 NR 1C (Unalloyed steel) 0,009 0 0,009 0 0,008 9 0,000 43 0,001 4 0,0

46、01 0 NR 21 (Unalloyed steel) 0,035 0,034 6 0,034 5 0,001 1 0,003 6 0,001 3 NBS 15h (Unalloyed steel) 0,017 0,017 8 0,017 8 0,000 69 0,002 3 0,001 1 NBS 16f (Unalloyed steel) 0,008 0,008 3 0,008 2 0,000 54 0,001 7 0,001 1 BAS 087-1 (Unalloyed steel) 0,118 0,119 0,119 0,002 9 0,010 8 0,004 3 BCS 452 (

47、Unalloyed steel) 0,19 0,191 0,191 0,004 0 0,014 6 0,005 6 IRSID 081-1 (Unalloyed steel) 0,042 0,042 2 0,042 2 0,000 90 0,002 4 0,002 1 IRSID 010-1 (Unalloyed steel) 0,259 0,264 0,264 0,008 9 0,017 5 0,010 7 EURO 488-1 (Pig iron) 0,065 1 0,065 5 0,065 4 0,001 2 0,004 3 0,002 3 EURO 487-1 (Pig iron) 0

48、,040 0,040 5 0,040 4 0,001 4 0,002 7 0,001 5 : general mean within a day : general mean between days WNi,1 WNi,2 WNi,1 WNi,2BS 6200-3.40.2:1997 BSI 09-1999 5 Annex B (informative) Graphical representation of precision data Nickel contents up to 0,03 %(m/m) Nickel contents between 0,03 %(m/m) and 0,3

49、 %(m/m) lgr = 0,224 6 lg 2,731 8 lgr = 0,994 1 lg 1,599 2 lgR = 0,331 3 lg 2,127 4 lgR = 0,988 8 lg 1,144 1 lgR W= 0,279 1 lg 2,419 0 lgR W= 0,920 8 lg 1,510 3 where is the average nickel content, expressed as a percentage by mass, obtained within a day; is the average nickel content, expressed as a percentage by mass, obtained between days. Figure B.1 Logarithmic relationship between nickel content () and repeatability limit (r) or reproducibility limits (R and Rw) w Ni,1 w Ni,1 w Ni,1 w Ni,1 w Ni,2 w Ni