BS ISO 22036-2009 Soil quality - Determination of trace elements in extracts of soil by inductively coupled plasma-atomic emission spectrometry (ICP-AES)《土质 使用感应耦合等离子体-原子发射光谱法(ICP-.pdf

1、BS ISO22036:2008ICS 13.080.10NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBRITISH STANDARDSoil quality Determination of traceelements in extractsof soil by inductivelycoupled plasma -atomic emissionspectrometry (ICP -AES)This British Standardwas published under theauthority

2、of the StandardsPolicy and StrategyCommittee on 31 March2009 BSI 2009ISBN 978 0 580 55668 5Amendments/corrigenda issued since publicationDate CommentsBS ISO 22036:2008National forewordThis British Standard is the UK implementation of ISO 22036:2008.The UK participation in its preparation was entrust

3、ed to TechnicalCommittee EH/4, Soil quality.A list of organizations represented on this committee can be obtained onrequest to its secretary.This publication does not purport to include all the necessary provisionsof a contract. Users are responsible for its correct application.Compliance with a Bri

4、tish Standard cannot confer immunityfrom legal obligations.BS ISO 22036:2008Reference numberISO 22036:2008(E)ISO 2008INTERNATIONAL STANDARD ISO22036First edition2008-12-15Soil quality Determination of trace elements in extracts of soil by inductively coupled plasma - atomic emission spectrometry (IC

5、P-AES) Qualit du sol Dosage des lments traces dans des extraits de sol par spectromtrie dmission atomique avec plasma induit par haute frquence (ICP-AES) BS ISO 22036:2008ISO 22036:2008(E) PDF disclaimer This PDF file may contain embedded typefaces. In accordance with Adobes licensing policy, this f

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8、hat the file is suitable for use by ISO member bodies. In the unlikely event that a problem relating to it is found, please inform the Central Secretariat at the address given below. COPYRIGHT PROTECTED DOCUMENT ISO 2008 All rights reserved. Unless otherwise specified, no part of this publication ma

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10、 + 41 22 749 01 11 Fax + 41 22 749 09 47 E-mail copyrightiso.org Web www.iso.org Published in Switzerland ii ISO 2008 All rights reservedBS ISO 22036:2008ISO 22036:2008(E) ISO 2008 All rights reserved iiiContents Page Foreword iv 1 Scope1 2 Normative references1 3 Terms and definitions .2 4 Principl

11、e3 5 Interferences 6 5.1 General .6 5.2 Spectral interferences.6 5.3 Non-spectral interferences.7 6 Reagents.8 7 Instrumentation .9 8 Procedure.10 8.1 Cleaning of glassware.10 8.2 Instrument performance parameters.10 8.3 Instrument optimization11 8.4 Alignment of the spectrometer 11 8.5 Calibration

12、methods12 8.6 Solutions to be prepared 12 8.7 Measurement procedure.13 9 Calculation of results 14 10 Precision.14 11 Expression of results14 12 Test report15 Annex A (informative) Repeatability and precision results 16 Annex B (informative) Interferences .19 Bibliography30 BS ISO 22036:2008ISO 2203

13、6:2008(E) iv ISO 2008 All rights reservedForeword 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 b

14、ody 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, also take part in the work. ISO collaborates closely with the International Electro

15、technical 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 committees is to prepare International Standards. Draft International Standards adopted

16、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 possibility that some of the elements of this document may be the subject of patent r

17、ights. ISO shall not be held responsible for identifying any or all such patent rights. ISO 22036 was prepared by Technical Committee ISO/TC 190, Soil quality, Subcommittee SC 3, Chemical methods and soil characteristics. BS ISO 22036:2008INTERNATIONAL STANDARD ISO 22036:2008(E) ISO 2008 All rights

18、reserved 1Soil quality Determination of trace elements in extracts of soil by inductively coupled plasma - atomic emission spectrometry (ICP-AES) WARNING The procedures in this International Standard should be carried out by competent, trained persons. Some of the techniques and reagents, including

19、the use of equipment, are potentially very dangerous. Users of this International Standard who are not thoroughly familiar with the potential dangers and related safe practices should take professional advice before commencing any operation. 1 Scope This International Standard describes the determin

20、ation of trace elements in digests or extraction solutions from soil by inductively coupled plasma - atomic emission spectrometry (ICP-AES) for 34 elements (see Table 1). This multi-element determination method is applicable to soil extracts obtained with aqua regia in accordance with ISO 11466, wit

21、h DTPA in accordance with ISO 14870 or other weak extractants, or soil extracts for the determination of total element contents using the acid digestion method of ISO 14869-1 or the fusion method of ISO 14869-2. The choice of calibration method depends on the extractant and can be adapted to the ext

22、ractant concentration. 2 Normative references 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

23、 Guide 32, Calibration in analytical chemistry and use of certified reference materials ISO 3696, Water for analytical laboratory use Specification and test methods ISO 5725-1, Accuracy (trueness and precision) of measurement methods and results Part 1: General principles and definitions ISO 5725-2,

24、 Accuracy (trueness and precision) of measurement methods and results Part 2: Basic method for the determination of repeatability and reproducibility of a standard measurement method ISO 11465, Soil quality Determination of dry matter and water content on a mass basis Gravimetric method ISO 11466, S

25、oil quality Extraction of trace elements soluble in aqua regia ISO 14869-1, Soil quality Dissolution for the determination of total element content Part 1: Dissolution with hydrofluoric and perchloric acids ISO 14869-2, Soil quality Dissolution for the determination of total element content Part 2:

26、Dissolution by alkaline fusion ISO 14870, Soil quality Extraction of trace elements by buffered DTPA solution BS ISO 22036:2008ISO 22036:2008(E) 2 ISO 2008 All rights reserved3 Terms and definitions For the purposes of this document, the terms and definitions given in ISO 5725-1, ISO 5725-2, ISO Gui

27、de 32 and the following apply. 3.1 analyte element to be determined 3.2 blank calibration solution solution prepared in the same way as the calibration solution but leaving out the analytes 3.3 blank test solution solution prepared in the same way as the test sample solution but omitting the test po

28、rtion 3.4 calibration solution solution used to calibrate the instrument, prepared from stock solutions by adding acids, buffer, reference element and salts as needed 3.5 instrument detection limit lowest concentration that can be detected with a defined statistical probability using a clean instrum

29、ent and a clean solution NOTE The clean solution is usually dilute nitric acid. 3.6 laboratory sample sample sent to the laboratory for analysis 3.7 linearity straight-line relationship between the mean result of measurement and the quantity (concentration) of the analyte 3.8 method detection limit

30、lowest concentration that can be detected using a specific analytical method with a defined statistical probability for defined maximum matrix element concentrations 3.9 pure chemical chemical with the highest available purity and known stoichiometry NOTE The content of analyte and contaminants shou

31、ld be known with an established degree of certainty. 3.10 stock solution solution with accurately known analyte concentration(s), prepared from pure chemicals (3.9) NOTE Stock solutions are reference materials within the meaning of ISO Guide 30. 3.11 test sample portion taken from the laboratory sam

32、ple after homogenizing, grinding, dividing, etc. BS ISO 22036:2008ISO 22036:2008(E) ISO 2008 All rights reserved 33.12 test sample solution solution prepared after extraction or dissolution of the test sample according to appropriate specifications NOTE The test sample solution is intended for use f

33、or measurement. 4 Principle Inductively coupled plasma - atomic emission spectrometry (ICP-AES) can be used to determine trace elements in solution. The solution is dispersed by a suitable nebulizer and the resulting aerosol is transported into the plasma torch. In a radio-frequency inductively coup

34、led plasma the solvent is evaporated, the dried salts are then vaporized, dissociated, atomized and ionized. The atoms or ions are excited thermally and the number of photons emitted during transition to a lower energy level are measured with optical emission spectrometry. The spectra are dispersed

35、by a grating spectrometer, and the intensities of the emission lines are monitored by photosensitive devices. The identification of the element takes place by means of the wavelength of the radiation (energy of photons), while the concentration of the element is proportional to the intensity of the

36、radiation (number of photons). The ICP-AES method can be used to perform multi-element determinations using sequential or simultaneous optical systems and axial or radial viewing of the plasma. Table 1 shows examples of recommended wavelengths, and detection limits for one particular instrument. Dat

37、a given are valid for water acidified with nitric acid with an optimized instrument. Using other instruments can lead to different detection limits. Adoption of other wavelengths is possible. Table 1 Recommended wavelengths and estimated detection limits for selected elements and wavelengths obtaine

38、d using ICP-AES Varian, Vista-MPX megapixel (CD detector features) 9Element wavelengths and analytical lines Axial viewing Radial viewing Element Wavelength nm Lines I = atom II = ion Detection limitg/l aDetection limitmg/kg bDetection limit g/l aDetection limitmg/kg bAluminium 396,068 308,215 309,2

39、71 396,152 167,078 I I I l 1 2,6 0,1 0,3 0,10 0,26 0,01 0,03 4 4 1 0,4 0,4 0,1 Antimony 206,833 217,581 231,146 I I l 0,5 1,8 2 0,5 0,18 0,2 16 5 1,6 0,5 Arsenic 188,979 193,696 197,198 189,042 188,979 I l l 2 1 5 1,5 0,2 0,1 0,5 0,15 12 11 5 1,2 1,1 0,5 Barium 233,527 455,403 493,409 II II II 0,06

40、0,01 0,04 0,006 0,001 0,004 0,7 0,15 0,15 0,07 0,02 0,02 Beryllium 313,107 313,402 234,861 II II II 0,03 0,01 0,01 0,003 0,001 0,001 0,15 0,15 0,05 0,02 0,02 0,005 Bismuth 223,061 306,771 315,887 I l 1,8 17 0,18 1,7 6 0,6 Boron 208,959 249,678 249,772 I I l 0,7 1,1 0,5 0,07 0,11 0,05 1,2 1,5 1 0,12

41、0,15 0,1 BS ISO 22036:2008ISO 22036:2008(E) 4 ISO 2008 All rights reservedTable 1 (continued) Element wavelengths and analytical lines Axial viewing Radial viewing Element Wavelength nm Lines I = atom II = ion Detection limitg/l aDetection limitmg/kg bDetection limit g/l aDetection limitmg/kg bCadmi

42、um 214,438 226,502 228,802 II II II 0,1 0,11 0,20 0,01 0,011 0,02 0,5 0,6 0,5 0,05 0,06 0,05 Calcium 396,847 317,933 393,366 II II II 0,5 0,3 0,5 0,05 0,03 0,05 0,3 6,5 0,03 0,7 Chromium 267,716 205,552 206,149 283,563 284,325 II II II II II 0,1 0,3 0,2 0,01 0,03 0,02 1 0,1 Cobalt 238,892 228,616 23

43、0,786 II II II 0,4 0,4 0,04 0,04 1,2 1 0,1 0,1 Copper 327,396 224,700 324,754 I II I 0,3 0,6 0,03 0,06 1,5 0,1 Iron 238,204 239,562 259,940 II II II 0,3 0,5 0,03 0,05 0,9 0,7 0,09 0,07 Lead 220,353 216,999 224,688 261,418 283,306 II I I I I 0,4 1,8 0,04 0,18 8 0,8 Lithium 670,783 460,286 I I 1,7 67

44、0,17 6,7 1 0,1 Magnesium 279,553 279,079 285,213 279,806 II II I II 0,02 1 0,06 1,5 0,002 0,1 0,006 0,15 0,1 4 0,25 10 0,01 0,4 0,025 1 Manganese 257,610 260,569 279,482 293,306 403,076 259,372 II II II II I ll 0,10 0,4 0,8 0,05 0,01 0,04 0,08 0,005 0,13 1 0,01 0,1 Mercury 194,227 253,652 184,890 II

45、 I I 1,2 1 0,12 0,1 2,5 2 0,25 0,20 Molybdenum 202,030 204,598 II II 0,2 0,6 0,02 0,06 2 3 0,2 0,3 Nickel 231,604 221,647 216,555 232,003 II II I ll 0,4 0,3 0,15 0,04 0,03 0,015 2,1 1,4 0,2 0,14 Phosphorus 177,428 178,222 213,618 214,914 I I I l 1,5 7 1,3 1 0,15 0,7 0,13 0,1 25 5,3 11 2,5 0,53 1,1 B

46、S ISO 22036:2008ISO 22036:2008(E) ISO 2008 All rights reserved 5Table 1 (continued) Element wavelengths and analytical lines Axial viewing Radial viewing Element Wavelength nm Lines I = atom II = ion Detection limitg/l aDetection limitmg/kg bDetection limit g/l aDetection limitmg/kg bPotassium 766,4

47、91 769,896 I I 0,2 23 0,02 2,3 4 12 0,4 1,2 Rubidium 780,03 I 1 0,1 5 0,5 Selenium 196,026 203,985 I I 0,8 2,8 0,08 0,28 16 1,6 Silicon 251,611 212,412 288,158 I I I 0,9 1,3 1 0,09 0,13 0,1 2,2 5 0,22 0,5 Silver 328,068 338,289 I I 0,4 1 0,04 0,1 1 2 0,1 0,2 Sodium 589,592 588,995 330,237 I I I 0,6

48、12 69 0,06 1,2 6,9 1,5 15 0,2 0,15 Strontium 407,771 421,552 460,733 II II I 0,01 0,01 0,3 0,001 0,001 0,03 0,1 0,1 0,01 0,01 Sulfur 181,962 182,036 I 4 0,4 13 1,3 Thallium 190,800 190,864 II II 2 0,2 13 0,1 Tin 189,933 235,484 283,998 II I l 6 23 11 0,6 2,3 8 20 0,8 2,0 Titanium 336,121 334,941 337

49、,280 II II II 0,15 0,2 0,2 0,015 0,02 0,02 1 0,25 1 0,1 0,25 0,1 Vanadium 292,402 309,310 311,837 290,882 310,230 II II II ll ll 0,3 0,08 0,1 0,03 0,008 0,01 2 0,2 Zinc 213,856 202,548 206,200 I II ll 0,05 0,03 0,15 0,005 0,003 0,015 0,8 0,7 2 0,08 0,07 0,02 aTypical 3-sigma detection limits using 30 s integration time. bThe detection limit (LOD), as a mass fraction of the soil sample in mg/kg dry matter, is given assuming that a test sample of 1 g is extracted and diluted to 100 ml. The LOD shown in Tabl