1、 Reference number ISO 16918-1:2009(E) ISO 2009INTERNATIONAL STANDARD ISO 16918-1 First edition 2009-01-15 Steel and iron Determination of nine elements by the inductively coupled plasma mass spectrometric method Part 1: Determination of tin, antimony, cerium, lead and bismuth Acier et fer Dosage de
2、neuf lments par spectromtrie de masse avec plasma induit par haute frquence Partie 1: Dosage de ltain, de lantimoine, du crium, du plomb et du bismuth ISO 16918-1:2009(E) PDF disclaimer This PDF file may contain embedded typefaces. In accordance with Adobes licensing policy, this file may be printed
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7、 Fax + 41 22 749 09 47 E-mail copyrightiso.org Web www.iso.org Published in Switzerland ii ISO 2009 All rights reservedISO 16918-1:2009(E) ISO 2009 All rights reserved iiiContents Page Foreword iv 1 Scope1 2 Normative references1 3 Principle1 4 Reagents.2 5 Apparatus.4 6 Measurement specifications 5
8、 6.1 Minimum precision (RSD).5 6.2 Limit of detection (LOD) and limit of quantification (LOQ) .5 7 Sampling.6 8 Washing6 9 Procedure.6 9.1 Test portion6 9.2 Blank test solution blank sample solution.6 9.3 Preparation of the test solution .6 10 Standard solutions 8 10.1 Multi-element standard solutio
9、ns of the elements Sn, Sb, Pb and Bi .8 10.2 Standard solutions of the element Ce.9 11 Preparation of internal standard solutions (“internal standards”) Y, Rh and Lu.9 11.1 Preparation in polystyrene test tubes .9 11.2 Preparation in volumetric flasks10 12 Calibration blank solution and calibration
10、solutions 10 12.1 Preparation in volumetric flasks10 12.2 Preparation in polystyrene test tubes .11 13 Conditioning of the ICP-MS instrument 14 14 ICP-MS measurements14 15 Plotting of calibration graphs.14 16 Expression of results15 16.1 Method of calculation15 16.2 Precision.15 17 Test report17 Ann
11、ex A (informative) Additional information on the international co-operative tests.18 Annex B (informative) Interferences in the determination of elements Sn, Sb, Ce, Pb and Bi using ICP- MS .28 Bibliography29 ISO 16918-1:2009(E) iv ISO 2009 All rights reservedForeword ISO (the International Organiza
12、tion 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 committee has been established
13、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 electrotechnical standardization. In
14、ternational Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 2. The main task of technical committees is to prepare International Standards. Draft International Standards adopted by the technical committees are circulated to the member bodies for voting. Publi
15、cation as an International Standard requires approval by at least 75 % of the member bodies casting a vote. 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 r
16、ights. ISO 16918-1 was prepared by Technical Committee ISO/TC 17, Steel, Subcommittee SC 1, Methods of determination of chemical composition. ISO 16918 consists of the following parts, under the general title Steel and iron Determination of nine elements by the inductively coupled plasma mass spectr
17、ometric method: Part 1: Determination of tin, antimony, cerium, lead and bismuth Part 2: Determination of boron, silver, indium and thallium INTERNATIONAL STANDARD ISO 16918-1:2009(E) ISO 2009 All rights reserved 1Steel and iron Determination of nine elements by the inductively coupled plasma mass s
18、pectrometric method Part 1: Determination of tin, antimony, cerium, lead and bismuth 1 Scope This part of ISO 16918 specifies a method for analysing steel and iron for the trace element determinations of Sn, Sb, Ce, Pb and Bi using inductively coupled plasma mass spectrometry (ICP-MS). The method is
19、 applicable for trace elements in the mass fraction ranges (g/g) as follows: Sn: 5 g/g to 200 g/g; Sb: 1 g/g to 200 g/g; Ce: 10 g/g to 1 000 g/g; Pb: 0,5 g/g to 100 g/g; Bi: from 0,3 g/g to 30 g/g. Interferences in the determination of trace elements using ICP-MS are listed in Annex B. 2 Normative r
20、eferences The following referenced documents are indispensable for the application of this document. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies. ISO 648, Laboratory glassware Single-vo
21、lume pipettes ISO 1042, Laboratory glassware One-mark volumetric flasks ISO 14284, Steel and iron Sampling and preparation of samples for the determination of chemical composition 3 Principle A test portion is dissolved in an acid-mixture of hydrochloric acid, nitric acid and hydrofluoric acid using
22、 either a microwave-assisted system or a traditional hot plate. Diluted wet-digested samples are introduced into an inductively coupled plasma mass spectrometer (ICP-MS), via a peristaltic pump. Simultaneous measurements of the intensities of elements with atomic mass units of concern (mass spectra)
23、 are carried out using ICP-MS techniques. Calibration blank and calibration solutions are matrix-matched with the major elements of steel, and mineral acids are used for wet-digestion. Internal standards are used throughout in order to compensate for any instrument drift. ISO 16918-1:2009(E) 2 ISO 2
24、009 All rights reserved4 Reagents During the analysis, unless other stated, use only reagents of high purity quality containing less than 0,000 1 % mass fraction of each element or equivalent purity. The % given below refers to % mass fraction. 4.1 Hydrochloric acid, 30 % HCl, 1,15 g/ml or 38 %, 1,1
25、9 g/ml. 4.2 Nitric acid, 70 % HNO 3 , 1,42 g/ml. 4.3 Hydrofluoric acid, 49 % HF, 1,16 g/ml. 4.4 Nitric acid, 65 % HNO 3 , 1,40 g/ml. 4.5 Ultra-pure water, produced by a water purification system giving a resistivity of 18 M /cm or higher. 4.6 Washing solution for ICP-MS. In a 500 ml plastic bottle (
26、e.g. polyethylene) pour about 400 ml of ultra-pure water (4.5), then add 15 ml hydrochloric acid (4.1), 5 ml nitric acid (4.2) and 2,5 ml hydrofluoric acid (4.3) and make it up to volume with ultra-pure water (4.5). The quality of the acids can be checked prior to use by a mass spectrum scan with th
27、e ICPMS instrument. It is recommended to use a solution of 300 l HCl (4.1) + 100 l HNO 3(4.2) + 50 l HF (4.3) with about 3 ml ultra- pure water (4.5) and make it up to a volume of 10 ml. If peaks of elements of concern are present, a new flask of acid shall be used and a new check of the same elemen
28、ts shall be carried out. 4.7 10 % nitric acid solution, HNO 3diluted 1+9. In a 100 ml volumetric flask pour about 70 ml of ultra-pure water (4.5), then add 10 ml concentrated HNO 3(4.2), and dilute to volume with ultra-pure water (4.5). 4.8 NaOH solution, 7,5 mol/l, 1,33 g/ml. 4.9 NaOH solution, 0,2
29、 mol/l. Dispense 2,7 ml of 7,5 mol/l NaOH (4.8) into a 100 ml volumetric flask, and dilute to volume with ultra-pure water (4.5). The solution shall be stored in a polyethylene bottle or similar. 4.10 Aqua regia (HCl+HNO 3= 3+1). Prepare aqua regia in a 30 ml beaker (or similar) by dispensing 9 ml H
30、Cl (4.1) and 3 ml HNO 3(4.2) into the beaker. 4.11 Diluted aqua regia solution, diluted 4+10. Dispense 100 ml ultra-pure water (4.5) into a 150 ml flask. Then add 40 ml aqua regia (4.10) and mix. Do not make the solution up to volume. 4.12 50 % nitric acid solution, HNO 3diluted 1+1. In a 100 ml vol
31、umetric flask, pour about 30 ml of ultra-pure water (4.5), then add 50 ml concentrated HNO 3(4.2) and dilute to volume with ultra-pure water (4.5). 4.13 Perchloric acid, 70 % HClO 4 , 1,68 g/ml. ISO 16918-1:2009(E) ISO 2009 All rights reserved 34.14 50 % hydrochloric acid solution, HCl diluted 1+1.
32、In a 100 ml volumetric flask, pour about 30 ml of ultra-pure water (4.5), then add 50 ml concentrated HCl (4.1) and dilute to volume with ultra-pure water (4.5). 4.15 Iron, high purity quality containing less than 0,000 1 % mass fraction of each element. 4.16 Standard stock solutions, corresponding
33、to 1 000 mg element per litre. 4.16.1 Tin standard stock solution Dissolve 100,0 mg of high purity tin metal (99,9 % mass fraction, minimum) in 3 ml HCl (4.1) and 1 ml HNO 3(4.2) in a 250 ml beaker. Heat gently to complete dissolution, cool, transfer into a 100 ml volumetric flask, make the solution
34、 up to volume with ultra-pure water (4.5) and mix well. Store the tin standard stock solution in a polyethylene bottle. 4.16.2 Antimony standard stock solution Dissolve 100,0 mg of high purity antimony metal (99,9 % mass fraction, minimum) in 3 ml HCl (4.1) and 1 ml HNO 3(4.2) in a 250 ml beaker. He
35、at gently to complete dissolution, cool, transfer into a 100 ml volumetric flask, make the solution up to volume with ultra-pure water (4.5) and mix well. Store the antimony standard stock solution in a polyethylene bottle. 4.16.3 Cerium standard stock solution Dissolve 288,5 mg of pure cerium(IV) s
36、ulfate, Ce(SO 4 ) 24H 2 O, in 50 ml of a solution of diluted aqua regia (4.11) in a 100 ml volumetric flask. After complete dissolution, make the solution up to volume with diluted aqua regia (4.11) and mix well. Store the cerium standard stock solution in a polyethylene bottle. 4.16.4 Lead standard
37、 stock solution Dissolve 100,0 mg of high purity lead metal (99,9 % mass fraction, minimum) in 20 ml of 50 % HNO 3(4.12) in a 250 ml beaker. Heat gently to complete dissolution, cool, transfer into a 100 ml volumetric flask, make the solution up to volume with ultra-pure water (4.5) and mix well. St
38、ore the lead standard stock solution in a polyethylene bottle. 4.16.5 Bismuth standard stock solution Dissolve 100,0 mg of high purity bismuth metal (99,9 % mass fraction, minimum) in 3 ml HCl (4.1) and 1 ml HNO 3(4.2) in a 250 ml beaker. Heat gently to complete dissolution, cool, transfer into a 10
39、0 ml volumetric flask, make the solution up to volume with ultra-pure water (4.5) and mix well. Store the bismuth standard stock solution in a polyethylene bottle. 4.16.6 Rhodium standard stock solution Dissolve 203,6 mg of pure rhodium(III) chloride, RhCl 3 , in 6 ml aqua regia (4.10), freshly prep
40、ared, in a 100 ml volumetric flask. After complete dissolution, make the solution up to volume with ultra-pure water (4.5) and mix well. Store the rhodium standard stock solution in a polyethylene bottle. ISO 16918-1:2009(E) 4 ISO 2009 All rights reserved4.16.7 Yttrium standard stock solution Dissol
41、ve 127,0 mg of pure yttrium trioxide, Y 2 O 3 , in 6 ml aqua regia (4.10), freshly prepared, in a 100 volumetric flask. After complete dissolution, make the solution up to volume with ultra-pure water (4.5) and mix well. Store the yttrium standard stock solution in a polyethylene bottle. 4.16.8 Lute
42、tium standard stock solution Dissolve 113,7 mg of pure lutetium trioxide, Lu 2 O 3 , in 6 ml aqua regia (4.10), freshly prepared, in a 100 ml volumetric flask. After complete dissolution, make the solution up to volume with ultra-pure water (4.5) and mix well. Store the lutetium standard stock solut
43、ion in a polyethylene bottle. 4.16.9 Titanium standard stock solution Dissolve 100,0 mg of pure titanium metal (99,9 % mass fraction, minimum) in 30 ml of 50 % HCl (4.14) and 0,2 ml of HF (4.3) in a 250 ml beaker. Heat gently to complete dissolution, cool, transfer into a 100 ml volumetric flask, ma
44、ke the solution up to volume with ultra-pure water (4.5) and mix well. Store the titanium standard stock solution in a polyethylene bottle. 4.17 Iron matrix solution, 10 000 mg of Fe per litre Weigh 0,5 g of the high purity iron (4.15) to the nearest 0,01 mg and transfer it to a 250 ml beaker. Add 2
45、0 ml ultra-pure water, and then 0,1 ml HCl (4.1) and finally 5 ml HNO 3(4.2). Heat gently to dissolve the iron chips. After complete dissolution, cool, transfer into a 50 ml volumetric flask, make the solution up to volume with ultra-pure water (4.5) and mix well. Store the iron matrix solution in a
46、 polyethylene bottle. 4.18 Mass calibration solution, 100 g/l of each of the elements Ti, Y, Rh, Sb, Ce, Pb and Bi Dispense about 50 ml ultra-pure water (4.5) into a 1 000 ml volumetric flask, and then add 100 l of each of the standard stock solutions of Ti (4.16.9), Y (4.16.7), Rh (4.16.6), Sb (4.1
47、6.2), Ce (4.16.3), Pb (4.16.4) and Bi (4.16.5). Make the solution up to volume with ultra-pure water (4.5) and mix well. 5 Apparatus 5.1 Laboratory glassware and plastic ware, including volumetric flasks, watch-glasses, beakers, polyethylene bottles, polyethylene pipette tips, polystyrene tubes. All
48、 volumetric glassware shall be Class A in accordance with ISO 648 and ISO 1042. 5.2 Micro-pipettes The following micro-pipettes are used: 5 l to 40 l, 50 l to 200 l, 100 l to 1 000 l and 1 ml to 5 ml. 5.3 Microwave-assisted digestion system, consisting of a laboratory microwave oven and a carousel o
49、r holder for polytetrafluoroethylene (PTFE) pressure vessels. A time-step programme can be used, and during the wet-digestion procedure both pressure and temperature are registered and can be followed on a monitor. ISO 16918-1:2009(E) ISO 2009 All rights reserved 55.4 ICP-MS instruments 5.4.1 Magnetic sector ICP-MS (high resolution ICP-MS) 5.4.2 Quadropole ICP-MS (low resolution ICP-MS) 5.4.3 Time-of-flight ICP-MS (ICP-TOF-MS) For optimum running of the ICP-MS instruments, the manu
