1、BRITISH STANDARD BS 6200-3.40.1: 1997 ISO 13898-1: 1997 Sampling and analysis of iron, steel and other ferrous metals Part 3: Methods of analysis Section 3.40 Multi-element methods Subsection 3.40.1 Determination of nickel, copper and cobalt contents by inductively coupled plasma atomic emission spe
2、ctrometric method General requirements and sample dissolution ICS 77.080.01BS6200-3.40.1:1997 This British Standard, having been prepared under the directionof the Engineering SectorBoard, was published underthe authority of the Standards Board and comesintoeffect on 15 September 1997 BSI 09-1999 IS
3、BN 0 580 28421 2 National foreword This British Standard reproduces verbatim ISO13898-1:1997 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: a
4、id enquirers 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 organiza
5、tions represented 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
6、Correspondence 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 do
7、es not of itself 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 8 and a back cover. This standard has been updated (see copyright date) and may have had amendments in
8、corporated. This will be indicated in the amendment table on the inside front cover. Amendments issued since publication Amd. No. Date CommentsBS6200-3.40.1:1997 BSI 09-1999 i Contents Page National foreword Inside front cover Foreword iii Text of ISO 13898-1 1ii blankBS6200-3.40.1:1997 ii BSI 09-19
9、99 Contents Page Foreword iii Introduction 1 1 Scope 1 2 Normative references 1 3 Principle 1 4 Reagents 2 5 Apparatus 2 6 Sampling 3 7 Procedure 3 8 Expression of results 4 9 Test report 5 Annex A (normative) Procedures for the determination of instrumental criteria 6 Annex B (informative) Test sam
10、ples used in the interlaboratory test 8 Annex C (informative) Bibliography 8 Table 1 Application ranges of the elements to be determined 1 Table 2 Examples of analytical lines of the elements to be determined 2 Table 3 Background equivalent concentration and detection limit 3 Descriptors: Iron and s
11、teel products, unalloyed steels, unalloyed cast iron, chemical analysis, determination of content, nickel, copper, cobalt, spectrometric method, atomic emission spectrometric method, generalities.BS6200-3.40.1:1997 BSI 09-1999 iii Foreword ISO (the International Organization for Standardization) is
12、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 committee has been established has the right to be represent
13、ed 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 electrotechnical standardization. Draft International Standards a
14、dopted 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 ISO13898-1 was prepared by Technical Committee ISO/TC17, Steel, Subcommittee SC1, M
15、ethods 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 method. Part 1: General requirements and sample dissolution;
16、 Part 2: Determination of nickel content; Part 3: Determination of copper content; Part 4: Determination of cobalt content. Annex A forms an integral part of this part of ISO13898.Annex B andAnnex C are for information only.iv blankBS6200-3.40.1:1997 BSI 09-1999 1 Introduction This part of ISO13898
17、is to be used in conjunction with subsequent parts which specify methods for the determination of individual elements in steel and iron by inductively coupled plasma atomic emission spectrometric method (ICP-AES). Although the analytical methods are specified as independent standards, more than one
18、element in a single test solution can be determined. ISO 13898 is optimized to give the highest accuracy for each individual element, which implies that the multi-element capability of the ICP technique is not utilized. 1 Scope 1.1 This part of ISO13898 specifies a method for determination of nickel
19、, copper and cobalt contents in unalloyed steel and unalloyed iron within the ranges specified inTable 1 by means of inductively coupled plasma atomic emission spectrometric method. Table 1 Application ranges of the elements tobedetermined 1.2 This part of ISO13898 specifies the general requirements
20、 for analyses by ICP-AES, preparation and dissolution of the test portion and method of calculation and the procedures used for the evaluation of the precision data of the individual methods specified in the subsequent parts. 1.3 The International Standard specifies two alternative methods of evalua
21、ting concentrations in test solutions. One is with, the other is without the use of an internal standard. 2 Normative references The following standards contain provisions which, through reference in this text, constitute provisions of this part of ISO13898. At the time of publication, the editions
22、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 below. Members of IEC and ISO maintain registers of currently valid Inte
23、rnational Standards. ISO 385-1:1984, Laboratory glassware Burettes Part 1: General requirements. ISO 648:1977, Laboratory glassware One-mark pipettes. ISO 1042:1983, Laboratory glassware One-mark volumetric flasks. ISO 3696:1987, Water for analytical laboratory use Specification and test methods. IS
24、O 13898-2:1997, Steel and iron Determination of nickel, cobalt and copper contents Inductively coupled plasma atomic emission spectrometric method Part 2: Determination of nickel content. ISO 13898-3:1997, Steel and iron Determination of nickel, cobalt and copper contents Inductively coupled plasma
25、atomic emission spectrometric method Part 3: Determination of copper content. ISO 13898-4:1997, Steel and iron Determination of nickel, cobalt and copper contents Inductively coupled plasma atomic emission spectrometric method Part 4: Determination of cobalt content. ISO 14284:1996, Steel and iron S
26、ampling and preparation of samples for the determination of chemical composition. 3 Principle Dissolution of a test portion in a mixture of hydrochloric and nitric acids and dilution of the solution to known volume. If necessary, addition of scandium or yttrium as internal standard. Nebulization of
27、the solution into an inductively coupled plasma atomic emission spectrometer and measurement of the intensity of the emitted light from each element, or with emitted light from scandium or yttrium, simultaneously. Examples of the analytical lines are given inTable 2. Element Application range % (m/m
28、) Nickel Copper Cobalt 0,001 to 0,30 0,001 to 0,40 0,001 to 0,10BS6200-3.40.1:1997 2 BSI 09-1999 Table 2 Examples of analytical lines oftheelements to be determined 4 Reagents During the analysis, unless otherwise stated, use only reagents of recognized analytical grade and only grade 2 water as spe
29、cified in ISO3696. 4.1 Pure iron, containing less than0,0001%(m/m) of each element. 4.2 Hydrochloric acid, approximately1,19g/ml, diluted1 + 1. 4.3 Nitric acid, approximately1,40g/ml, diluted1 + 1. 4.4 Scandium internal standard solution, corresponding to1g of scandium per litre. Weigh, to the neare
30、st1mg,1,534g of scandium oxide purity 99,98%(m/m). Transfer to a500ml beaker and dissolve in40ml of nitric acid (4.3). Transfer to a1000ml one-mark volumetric flask, dilute to the mark with water and mix. 1 ml of this internal standard solution contains1mg Sc. 4.5 Yttrium internal standard solution,
31、 corresponding to1g of yttrium per litre. Weigh, to the nearest1mg,1,270g of yttrium oxide purity 99,98%(m/m). Transfer to a500ml beaker and dissolve in50ml of hydrochloric acid(4.2). Transfer into a1000ml one-mark volumetric flask, dilute to the mark with water and mix. 1 ml of this internal standa
32、rd solution contains1mg Y. 4.6 Standard solutions of each element to be determined Prepare separately for each element as specified in the appropriate part of ISO13898. 5 Apparatus All volumetric glassware shall be class A, in accordance with ISO385-1, ISO648 or ISO1042 as appropriate. Ordinary labo
33、ratory equipment and 5.1 Atomic emission spectrometer, equipped with inductively coupled plasma (ICP-AES). The ICP-AES used will be satisfactory if after optimization according to7.4.1 it meets the performance criteria given in5.1.1 to5.1.3. The spectrometer can be either the simultaneous or the seq
34、uential type. If a sequential spectrometer can be equipped with an extra arrangement for simultaneous measurement of the internal standard line (scandium or yttrium), it can be used with the internal standard technique. If the sequential spectrometer is not equipped with this arrangement, an interna
35、l standard cannot be used and an alternative technique without internal standard can be applied. 5.1.1 Short term stability SeeA.1.3. The standard deviation of ten measurements of the absolute intensity or ratioed intensity of the emitted light of the most concentrated calibration solution is calcul
36、ated for each element to be determined. The relative standard deviation shall not exceed(0,4%) of the mean absolute or ratioed intensities. Element Analytical lines nm Nickel Copper Cobalt Scandium Yttrium 231,60 324,75 or 327,40 228,62 361,38 or 424,68 (internal standard) 371,03 (internal standard)
37、BS6200-3.40.1:1997 BSI 09-1999 3 5.1.2 Background equivalent concentration and detection limit SeeA.1.1 andA.1.2. The background equivalent concentration (BEC) and detection limit (DL) is calculated for the analytical line in a solution containing only the analyte element. The value shall be below t
38、he values indicated inTable 3. 5.1.3 Graph linearity SeeA.2. The linearity of the calibration graph is checked by calculating the correlation coefficient. This coefficient shall be more than0,999. Table 3 Background equivalent concentration and detection limit 6 Sampling Carry out sampling in accord
39、ance with ISO14284. 7 Procedure 7.1 Test portion Weigh, to the nearest1mg,1,000g of the test sample. 7.2 Blank test (corresponding to the zero member) In parallel with the determination of the content and following the same procedure, carry out a blank test using the same quantities of all the reage
40、nts including the pure iron (4.1). 7.3 Determination 7.3.1 Preparation of the test solution Place the test portion (7.1) in a200ml beaker. Add10ml of nitric acid (4.3), cover the beaker with a watch-glass and heat gently until the effervescence ceases. Add10ml of hydrochloric acid(4.2) and continue
41、the heating until complete dissolution occurs. Cool to ambient temperature and transfer the solution quantitatively to a200ml one-mark volumetric flask. If the internal standard technique is used, using a pipette, add2ml of the scandium internal standard solution (4.4) or10ml of yttrium internal sta
42、ndard solution (4.5). Dilute to the mark with water and mix. 7.3.2 Preparation of the calibration solutions Proceed as directed in the relevant part of ISO13898. 7.4 Spectrometric measurements 7.4.1 Optimization of the instrument Start the ICP-AES and let it run for at least one hour before taking a
43、ny measurements. Adjust all instrumental parameters, each gas flow-rate (outer, intermediate or central), torch position, entrance slits, exit slits, photomultiplier tube voltage, wavelength of the analytical line specified in Table 2, pre-spraying time and integrating time according to the instrume
44、nt manufacturers recommended operating practices and guidelines (seeAnnex A) while aspirating the highest concentration of calibration solution. Prepare the software to measure the intensity, mean value and relative standard deviation of the analytical line. Analytical line BEC DL nm mg/l mg/l Ni 23
45、1,60 Cu 324,75 Co 228,62 1,5 0,8 0,8 0,04 0,02 0,04BS6200-3.40.1:1997 4 BSI 09-1999 Set an appropriate observation time and high voltage on the attenuators and measure the high standard to give optimum intensity reading according to the manufacturers recommendation. If an internal standard is used p
46、repare the software to use the scandium line (361,38nm) or the yttrium line (371,03nm) as an internal standard and to calculate the ratio between the intensity of each element and scandium or yttrium intensity. The intensity of the internal standard shall be measured simultaneously with the analyte
47、intensity. Check the instrument performance requirements given in5.1.1 to5.1.3. 7.4.2 Measurements of the emitted intensities If the absolute intensities are to be measured, the temperatures of all solutions shall be within1 C of each other. Filter all solutions through a medium texture filter paper
48、. Discharge the first2ml to3ml. Measure the absolute intensity or intensity ratio of the analytical line beginning with the lowest calibration solution (zero member). Continue with two or three unknown test solutions, then the next lowest calibration solution, two or more unknown solutions and so on
49、. In this way all unknown test solutions are measured with the same time period as the calibration solutions, minimising any possible drift between calibration and unknown test solutions. For each solution make five integrations and check that the short term stability is the same as specified in5.1.1 and calculate the mean intensity or the mean ratioed intensity for each solution. Subtract the mean absolute intensity or the mean ratioed intensity (I 0 ) of the zero member from the mean absolute intensit
