1、BRITISH STANDARDBS ISO 22962:2008Titanium and titanium alloys Determination of iron Inductively coupled plasma atomic emission spectrometryICS 77.120.50g49g50g3g38g50g51g60g44g49g42g3g58g44g55g43g50g56g55g3g37g54g44g3g51g40g53g48g44g54g54g44g50g49g3g40g59g38g40g51g55g3g36g54g3g51g40g53g48g44g55g55g4
2、0g39g3g37g60g3g38g50g51g60g53g44g42g43g55g3g47g36g58BS ISO 22962:2008This British Standard was published under the authority of the Standards Policy and Strategy Committee on 30 May 2008 BSI 2008ISBN 978 0 580 57635 5National forewordThis British Standard is the UK implementation of ISO 22962:2008.T
3、he UK participation in its preparation was entrusted to Technical Committee NFE/35, Light metals and their alloys.A list of organizations represented on this committee can be obtained on request to its secretary.This publication does not purport to include all the necessary provisions of a contract.
4、 Users are responsible for its correct application.Compliance with a British Standard cannot confer immunity from legal obligations.Amendments/corrigenda issued since publicationDate CommentsReference numberISO 22962:2008(E)INTERNATIONAL STANDARD ISO22962First edition2008-01-15Titanium and titanium
5、alloys Determination of iron Inductively coupled plasma atomic emission spectrometry Titane et alliages de titane Dosage du fer Spectromtrie dmission atomique par plasma couplage inductif BS ISO 22962:2008ii iiiContents Page Foreword iv 1 Scope . 1 2 Normative references . 1 3 Principle. 1 4 Reagent
6、s 1 5 Apparatus 3 6 Sample . 3 7 Procedure 3 8 Expression of result . 7 9 Precision 8 Bibliography . 9 BS ISO 22962:2008iv Foreword ISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). The work of preparing International
7、 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 represented on that committee. International organizations, governmental and non-governmental, in liaison with ISO, a
8、lso take part in the work. ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization. International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 2. The main task of technical commit
9、tees is to prepare International Standards. 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 least 75 % of the member bodies casting a vote. Attention is drawn to the pos
10、sibility 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 rights. ISO 22962 was prepared by Technical Committee ISO/TC 79, Light metals and their alloys, Subcommittee SC 11, Titanium. BS ISO 22962
11、:20081Titanium and titanium alloys Determination of iron Inductively coupled plasma atomic emission spectrometry 1 Scope This International Standard specifies an inductively coupled plasma atomic emission spectrometric method for the determination of the mass fraction of iron in titanium and titaniu
12、m alloys. The method is applicable to titanium and titanium alloys with a mass fraction of iron in the range from 0,01 % to 3,0 %. 2 Normative references The following referenced documents are indispensable for the application of this document. For dated references, only the edition cited applies. F
13、or undated references, the latest edition of the referenced document (including any amendments) applies. ISO 384:1978, Laboratory glassware Principles of design and construction of volumetric glassware ISO 648:1), Laboratory glassware Single volume pipettes ISO 1042:1998, Laboratory glassware One-ma
14、rk volumetric flasks ISO 3696:1987, Water for analytical laboratory use Specifications and test methods ISO 4787:1984, Laboratory glassware Volumetric glassware Methods for use and testing of capacity 3 Principle Dissolve the test portion in nitric acid and hydrofluoric acid, or sulfuric acid and hy
15、drofluoric acid. Determine the iron concentration in the test portion using an inductively coupled plasma (ICP)-atomic emission spectrometer. 4 Reagents 4.1 General During the analysis, use only reagents of recognized analytical grade and water that complies with grade 2 of ISO 3696. 1) To be publis
16、hed. (Revision of ISO 648:1977) BS ISO 22962:20082 4.2 Hydrochloric acid (1+1) Add slowly 500 ml of hydrochloric acid (201,16 g/ml to 1,19 g/ml) to 500 ml of water (4.1). 4.3 Nitric acid (20 1,42 g/ml) 4.4 Nitric acid (1+1) Add slowly 500 ml of nitric acid (20 1,42 g/ml) to 500 ml of water. 4.5 Hydr
17、ofluoric acid (1+1) Add, carefully and slowly, 100 ml of hydrofluoric acid (20 1,14 g/ml) to 100 ml of water. 4.6 Sulfuric acid (1+1) Add slowly 500 ml of sulfuric acid (20 1,84 g/ml) to 500 ml of water, while stirring and cooling. 4.7 Sulfuric acid (1+3) Add slowly 100 ml of sulfuric acid (20 1,84
18、g/ml) to 300 ml of water, while stirring and cooling. 4.8 Titanium Minimum purity 99 % (mass fraction), the mass fraction of iron is as low as possible and already known. If the mass fraction of iron is unknown, it should be determined by the mass fraction of iron in ISO 22960. 4.9 Cobalt solution (
19、1 mg Co/ml) Weigh 1,00 g of cobalt metal minimum purity 99,5 % (mass fraction) into a 300 ml beaker, heat and decompose with 40 ml of nitric acid (4.4). After cooling, transfer to a 1 000 ml volumetric flask, make up to the mark with water and mix. 4.10 Yttrium solution (1 mg Y/ml) Weigh 1,27 g of y
20、ttrium oxide(III) minimum purity 99,5 % (mass fraction) into a 300 ml beaker, heat and decompose with 20 ml of hydrochloric acid (4.2). After cooling, transfer to a 1 000 ml volumetric flask, make up to the mark with water and mix. 4.11 Lanthanum solution (1 mg La/ml) Weigh 1,17 g of lanthanum oxide
21、(III) minimum purity 99,5 % (mass fraction) into a 300 ml beaker, heat and decompose with 20 ml of hydrochloric acid (4.2). After cooling, transfer to a 1 000 ml volumetric flask, make up to the mark with water and mix. 4.12 Iron standard solution (0,500 mg Fe/ml) Weigh, to the nearest 0,1 mg, 0,500
22、 g of iron metal minimum purity 99,9 % (mass fraction), into a 300 ml beaker, heat and decompose with 30 ml of hydrochloric acid (4.2). Add 5 ml of nitric acid (4.4) to oxidize iron and heat until nitrogen oxides evaporate. After cooling, transfer to a 1 000 ml volumetric flask, make up to the mark
23、with water and mix. BS ISO 22962:200835 Apparatus 5.1 General Use normal laboratory apparatus. 5.2 Volumetric glassware, of class A complying with ISO 384, ISO 648 and ISO 1042. Use in accordance with ISO 4787. 5.3 Polyethylene beaker and watch glass. 5.4 Polytetrafluoroethylene (PTFE) beaker and PT
24、FE watch glass. 5.5 Analytical balance, sensitive to 0,1 mg. 5.6 ICP-atomic emission spectrometer capable of simultaneously measuring the iron emission line 238,20 nm, or 259,94 nm and the emission line of the internal standard cobalt (228,62 nm), yttrium (371,03 nm), lanthanum (398,85 nm), titanium
25、 (255,60 nm) or titanium (333,21 nm). A hydrofluoric-acid-resistant nebulizer is recommended for the decomposition method with nitric acid and hydrofluoric acid (7.3.2). 6 Sample 6.1 Sampling The sampling procedure for titanium and titanium alloys shall be agreed upon until a corresponding standard
26、method has been published. 6.2 Test portion Extract a test portion of 0,50 g from the test sample and weigh to the nearest 0,1 mg. 7 Procedure 7.1 Number of determinations Carry out the determination at least in duplicate, as far as possible under repeatability conditions, on each sample. 7.2 Blank
27、test Carry out a blank test in parallel with the analysis, using the same quantities of all reagents but omitting the test portion. 7.3 Preparation of calibration solution 7.3.1 General Prepare the calibration solutions in accordance with 7.3.2, 7.3.3 or 7.3.4. BS ISO 22962:20084 7.3.2 In the case o
28、f decomposition with nitric acid and hydrofluoric acid (This method is used for the procedure described in 7.4.2) Weigh four samples of titanium (4.8), each of 0,50 g, and transfer to polyethylene beakers (200 ml). Add 50 ml of nitric acid (4.4) and 10 ml of hydrofluoric acid (4.5), cover with a pol
29、yethylene watch glass and heat gently on a water bath to decompose the titanium sample. Continue heating until nitrogen oxides evaporate. Cool to room temperature. Remove a watch glass, add, from a burette or pipette, 0 ml, 10 ml, 20 ml and 30 ml of iron standard solution (4.12). Transfer the soluti
30、on into a 100 ml volumetric flask. Add 5,0 ml of internal standard solution cobalt (4.9), make up to the mark with water and mix. Immediately, transfer the solution into a dry polyethylene or PTFE bottle with a stopper and reserve. 7.3.3 In the case of decomposition with sulfuric acid and hydrofluor
31、ic acid (This method is used for the procedure described in 7.4.3) Weigh four samples of titanium (4.8), each of 0,50 g, and transfer to PTFE beakers (200 ml). Add 20 ml of sulfuric acid (4.6) and 4 ml of hydrofluoric acid (4.5), cover with a PTFE watch glass and heat gently to decompose the titaniu
32、m. If the decomposition is incomplete, add a small quantity of hydrofluoric acid (4.5) and heat again. Add 4 ml of nitric acid (4.4), and heat for a few minutes. Remove the watch glass, continue heating until white fumes appear for about 5 min. Then cool to room temperature, and rinse the inside of
33、the beaker with a small quantity of water. Heat again until strong white fumes appear for 2 to 3 min. The volume of sulfuric acid remaining in the beaker will influence the intensity of emission. Therefore, it is recommended that care be taken to keep a constant volume of the remaining sulfuric acid
34、. However, that influence will be cancelled by using an internal standard method. Cool to room temperature. Add 20 ml of hydrochloric acid (4.2) and a small quantity of water to dissolve the salt. Add, from a burette or pipette, 0 ml, 10 ml, 20 ml, and 30 ml of iron standard solution (4.12). Transfe
35、r the solution into a 100 ml volumetric flask. Add 5,0 ml of internal standard solution cobalt (4.9), yttrium (4.10) or lanthanum (4.11), make up to the mark with water and mix. 7.3.4 In the case of decomposition with sulfuric acid (This method is used for the procedure in 7.4.4) Weigh four samples
36、of titanium (4.8), each of 0,50 g, and transfer to conical beakers (100 ml). Add 40 ml of sulfuric acid (4.7), cover with a watch glass and heat gently to decompose all of the titanium (maintaining the volume with distilled water). After dissolution of the titanium, add nitric acid (4.3) drop by dro
37、p for titanium oxidation, and heat the solution until white fumes appear. Cool to room temperature. Remove a watch glass, add, from a burette or pipette, 0 ml, 10 ml, 20 ml and 30 ml of iron standard solution (4.12). Transfer the solution into a 100 ml volumetric flask with water. Make up to the mar
38、k with water and mix. BS ISO 22962:200857.4 Preparation of a test solution for presentation to the ICP-atomic emission spectrometer 7.4.1 General Prepare the test solutions for presentation to the ICP-atomic emission spectrometer in accordance with 7.4.2, 7.4.3 or 7.4.4. 7.4.2 Decomposition with nit
39、ric acid and hydrofluoric acid NOTE This method is applicable for the determination of iron in titanium (including commercially available pure titanium) and titanium alloys. Transfer the test portion to a polyethylene beaker (200 ml). Add 50 ml of nitric acid (4.4) and 10 ml of hydrofluoric acid (4.
40、5), cover with a polyethylene watch glass and heat gently on a water bath to decompose the test portion. Continue heating until nitrogen oxides evaporate. Cool to room temperature. Remove the watch glass and transfer the solution into a 100 ml volumetric flask. Add 5,0 ml of internal standard soluti
41、on cobalt (4.9), make up to the mark with water and mix. Immediately, transfer the solution into a dry polyethylene or PTFE bottle with a stopper and reserve. 7.4.3 Decomposition with sulfuric acid and hydrofluoric acid NOTE This method is applicable for the determination of iron in titanium (includ
42、ing commercially available pure titanium) and titanium alloys. Transfer the test portion to a PTFE beaker (200 ml). Add 20 ml of sulfuric acid (4.6) and 4 ml of hydrofluoric acid (4.5), cover with a PTFE watch glass and heat gently to decompose the test portion. If decomposition is incomplete, add a
43、 small quantity of hydrofluoric acid (4.5) and heat again. Add 4 ml of nitric acid (4.4) and heat for a few minutes. Remove the watch glass, continue heating until white fumes appear for 5 min. After cooling to room temperature, rinse the inside of the beaker with a small quantity of water. Heat aga
44、in until strong white fumes appear for 2 to 3 min. The volume of the sulfuric acid remaining in the beaker will influence the intensity of emission . Therefore, it is recommended that care be taken to keep a constant volume of the remaining sulfuric acid. However, that influence will be cancelled by
45、 using an internal standard method. Cool to room temperature. Add 20 ml of hydrochloric acid (4.2) and a small quantity of water to dissolve the salt. After cooling to room temperature, transfer the solution into a 100 ml volumetric flask. Add 5,0 ml of internal standard solution cobalt (4.9), yttri
46、um (4.10) or lanthanum (4.11), make up to the mark with water and mix. 7.4.4 Decomposition with sulfuric acid (using titanium as the internal standard) NOTE This method uses titanium as the internal standard, and is applicable to the determination of iron in commercially available pure titanium only
47、. Transfer the test portion to conical beakers (100 ml). BS ISO 22962:20086 Add 40 ml of sulfuric acid (4.7), cover with a watch glass and heat gently to decompose the titanium (maintaining the volume with distilled water). After dissolution of the titanium, add nitric acid (4.3) drop by drop for ti
48、tanium oxidation. Heat the solution until white fumes appear. After cooling to room temperature, transfer the solution into a 100 ml volumetric flask with water. Make up to the mark with water and mix. 7.5 Determination of iron concentration 7.5.1 General The instrument shall be set up in accordance
49、 with the manufacturers instruction. Chose appropriate background correction positions and ignite the plasma torch for at least 30 min before use, to allow stabilization. Measure the emission intensity using the ICP-atomic emission spectrometer using the internal standard method. When using devices for a computer system preparation of a working curve, standardization (drift correction, normalization, recalibration) and measurement of iron concentration shall be in accordance with the operating manual for the devices computer system sof
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