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1、A Reference number ISO 11047:1998(E) INTERNATIONAL STANDARD ISO 11047 First edition 1998-05-01 Soil quality Determination of cadmium, chromium, cobalt, copper, lead, manganese, nickel and zinc in aqua regia extracts of soil Flame and electrothermal atomic absorption spectrometric methods Qualit du s
2、ol Dosage du cadmium, chrome, cobalt, cuivre, plomb, manganse, nickel et zinc dans les extraits de sol leau rgale Mthodes par spectromtrie dabsorption atomique avec flamme et atomisation lectrothermique Copyright International Organization for Standardization Provided by IHS under license with ISO L
3、icensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/19/2007 00:37:13 MDTNo reproduction or networking permitted without license from IHS -,-,- ISO 11047:1998(E) ISO 1998 All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized in any for
4、m or by any means, electronic or mechanical, including photocopying and microfilm, without permission in writing from the publisher. International Organization for Standardization Case postale 56 CH-1211 Genve 20 Switzerland Internetcentraliso.ch X.400c=ch; a=400net; p=iso; o=isocs; s=central Printe
5、d in Switzerland ii ContentsPage 1Scope 1 2Normative references .2 3Method A Determination of cadmium, chromium, cobalt, copper, lead, manganese, nickel and zinc by flame atomic absorption spectrometry2 3.1Principle 2 3.2Reagents.3 3.3Preparation of stock and standard solutions of individual element
6、s4 3.4Apparatus6 3.5Procedure .6 3.6Determination of test portion.9 3.7Calculation 9 3.8Precision .10 3.9Expression of results.10 3.10 Test report.10 4Method B Determination of cadmium, chromium, cobalt, copper, lead, manganese, nickel and zinc by electrothermal atomic absorption spectrometry 10 4.1
7、Principle 10 4.2Reagents.11 4.3Stock and standard solutions11 4.4Apparatus13 4.5Procedure .13 4.6Calibration and determination.15 4.7Plotting the graph15 4.8Calculation 15 4.9Expression of results.16 4.10 Precision .16 4.11 Test report.16 Annex A Results of interlaboratory tests17 Copyright Internat
8、ional Organization for Standardization Provided by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/19/2007 00:37:13 MDTNo reproduction or networking permitted without license from IHS -,-,- ISOISO 11047:1998(E) iii Foreword ISO (the International Organiza
9、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
10、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. D
11、raft 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. International Standard ISO 11047 was prepared by Technical Committee ISO/T
12、C 190, Soil quality, Subcommittee SC 3, Chemical methods and soil characteristics. Annex A of this International Standard is for information only. Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Re
13、sale, 04/19/2007 00:37:13 MDTNo reproduction or networking permitted without license from IHS -,-,- Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/19/2007 00:37:13 MDTNo reproduction or
14、 networking permitted without license from IHS -,-,- INTERNATIONAL STANDARD ISOISO 11047:1998(E) 1 Soil quality Determination of cadmium, chromium, cobalt, copper, lead, manganese, nickel and zinc in aqua regia extracts of soil Flame and electrothermal atomic absorption spectrometric methods WARNING
15、 The procedures in this International Standard should be carried out by competent, trained persons. Some of the techniques and reagents, including the use of equipment, are potentially very dangerous. Users of this International Standard who are not thoroughly familiar with the potential dangers and
16、 related safe practices should take professional advice BEFORE commencing any operation. 1 Scope This International Standard specifies two methods for the determination, by atomic absorption spectrometry, of one or more of cadmium, chromium, cobalt, copper, lead, manganese, nickel and zinc, in aqua
17、regia extracts of soil obtained in accordance with ISO 11466. The choice of method for any element depends on the amount of that element expected to be in a sample, and both methods might be needed to cover all the elements in one sample. The methods are applicable when the extractable element conte
18、nt is above or below the amount given in table 1 (as milligrams per kilogram, dry matter), as appropriate. The two methods are described separately as follows: Method A Determination of cadmium, chromium, cobalt, copper, lead, manganese, nickel and zinc by flame atomic absorption spectrometry. Metho
19、d B Determination of cadmium, chromium, cobalt, copper, lead, manganese, nickel and zinc by electrothermal atomic absorption spectrometry. Many of the procedures and reagents are common to both methods, and to the different elements within each method. Users are advised, however, to read the whole s
20、tandard carefully before embarking on any of the procedures. Table 1 Indicative limits of soil contents (mg/kg dry matter) for elements extractable in aqua regia in accordance with ISO 11446 ElementMethod A (flame AAS) Method B (electrothermal AAS) Cadmium 2 12 12 5 15 2 12 2 2 Copyright Internation
21、al Organization for Standardization Provided by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/19/2007 00:37:13 MDTNo reproduction or networking permitted without license from IHS -,-,- ISO 11047:1998(E) ISO 2 NOTE 1Indicative limits given in table 1 are
22、 appropriate to the equipment and techniques avaiable at the time of publication of this International Standard. Technical improvements may change this position in the future. NOTE 2This International Standard refers specifically to the use of atomic absorption spectrometry. Users of this Internatio
23、nal Standard are advised to operate their laboratories to accepted quality control procedures. Certified Reference Materials (CRM) should be used to establish the amounts of the relevant elements in in-house reference materials. The latter can be used for routine quality control of the procedures gi
24、ven in this International Standard. Results should be established with control charts, for each element, within the laboratory. No result should be accepted which falls outside an agreed limit. Quality control procedures based on a widely accepted statistical technique should be used to establish su
25、ch limit, to ensure that these are stable and that no long-term drift is occurring. Certified Reference Materials should be used regularly to maintain the integrity of the in-house reference materials and, thereby, the quality control system. 2 Normative references The following standards contain pr
26、ovisions which, through reference in this text, constitute provisions of this International Standard. At the time of publication, the editions indicated were valid. All standards are subject to revision, and parties to agreements based on this International Standard are encouraged to investigate the
27、 possibility of applying the most recent editions of 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 (trueness and precision) o
28、f measurement methods and results Part 1: General principles and definitions ISO 11465:1993, Soil quality Determination of dry matter and water content on a mass basis Gravimetric method ISO 11466: 1994, Soil quality Extraction of trace elements soluble in aqua regia 3 Method A Determination of cadm
29、ium, chromium, cobalt, copper, lead, manganese, nickel and zinc by flame atomic absorption spectrometry 3.1 Principle The method is based on the atomic absorption spectrometric measurement of the concentration of the element in an aqua regia extract of the sample, prepared in accordance with ISO 114
30、66, using the instrumental conditions given in table 2. Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/19/2007 00:37:13 MDTNo reproduction or networking permitted without license from I
31、HS -,-,- ISOISO 11047:1998(E) 3 Table 2 General analytical conditions for flame atomic absorption spectrometry ElementWavelength (nm) Flame typeLanthanum chloride Main Interferences Background correction Cadmium228,8Oxidizing air/ acetylene NoFeDeuterium Chromium357,9Reducing air/ acetylene or acety
32、lene/N2O Yes No Fe, Al Ca, Mg Halogen Cobalt240,7Oxidizing air/ acetylene NoDeuterium Copper324,8Oxidizing air/ acetylene NoDeuterium Lead217,0Oxidizing air/ acetylene NoDeuterium Manganese279,5Oxidizing air/ acetylene or acetylene/N2O Yes No Fe, SiDeuterium Nickel232,0Oxidizing air/ acetylene NoFeD
33、euterium Zinc213,9Oxidizing air/ acetylene NoDeuterium NOTE The wavelengths given are the most sensitive. Interferences are generally lower if the nitrous oxide flame is used for determination of chromium and manganese. Users should be aware that small changes in gas volume ratios can have significa
34、nt effects on the intensity of the analytical signal, and can also change the linearity of the instrument response. Also difference in acid strength, which will vary slightly from digest to digest, can have a measurable effect on some elements with some instruments especially if background correctio
35、n is not used. Users should, therefore, familiarize themselves with these aspects of their instruments performance. 3.2 Reagents All reagents shall be of recognized analytical grade. Use deionized water or water distilled from an all-glass apparatus, conforming to grade 2 of ISO 3696. The water used
36、 for blank determinations and for preparing reagents and standard solutions shall have a concentration of the element to be determined that is negligible compared with the lowest concentration of that element in the sample solutions. 3.2.1 Hydrochloric acid, 37 %; r 1,18 g/ml The same batch of hydro
37、chloric acid shall be used throughout the procedure. 3.2.2 Nitric acid, 65 %; r 1,42 g/ml The same batch of nitric acid shall be used throughout the procedure. 3.2.3 Nitric acid, diluted 1 + 3 (V/V) Add 250 ml of nitric acid (3.2.2) to 500 ml of water in a 1000 ml volumetric flask and fill to the ma
38、rk with water. Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/19/2007 00:37:13 MDTNo reproduction or networking permitted without license from IHS -,-,- ISO 11047:1998(E) ISO 4 3.2.4 Su
39、lfuric acid, 98 %; r 1,84 g/ml. The same batch of sulfuric acid shall be used throughout the procedure. 3.2.5 Sulfuric acid, diluted 1 + 9 (V/V). Add slowly with swirling or stirring (magnetic stirrer bar) 100 ml of sulfuric acid (3.2.4) to 700 ml of water in a 1000 ml volumetric flask, mix, cool an
40、d fill to the mark with water. 3.2.6 Lanthanum chloride solution, 37 g/l lanthanum. Dissolve 100 g of lanthanum(III) chloride, LaCl3.7H2O, in 700 ml water. Then quantitatively transfer it to a 1000 ml volumetric flask and fill to the mark with water. 3.2.7 Blank solution without lanthanum for calibr
41、ation Dilute 210 ml of hydrochloric acid (3.2.1) and 70 ml of nitric acid (3.2.2) with 500 ml water in a 1000 ml volumetric flask and fill to the mark with water. 3.2.8 Blank solution with lanthanum for calibration Dilute 210 ml of hydrochloric acid (3.2.1) and 70 ml of nitric acid (3.2.2) with 500
42、ml water in a 1000 ml volumetric flask. Add 100 ml lanthanum chloride solution (3.2.6) and fill to the mark with water. 3.2.9 Acetone 3.3 Preparation of stock and standard solutions of individual elements The stock solutions of all the elements shall be replaced after a maximum of one year, but the
43、standard solutions shall be renewed monthly as a minimum. If stock solutions are prepared directly from metals, care needs to be taken to ensure that the metal used is free of surface oxide layers. Stock solutions of metals are available commercially, and may be used, but their use should be control
44、led by appropriate laboratory procedures which meet accepted good laboratory practice. Records shall be kept of such control data. 3.3.1 Cadmium solutions WARNING Cadmium is highly toxic. Safety measures shall be taken to avoid ingestion. 3.3.1.1 Cadmium, stock solution corresponding to 1000 mg/l of
45、 cadmium. Weigh, to the nearest 0,0002 g, approximately 1,0000 g of cadmium metal (minimum purity 99,5 %) and dilute it in a covered 250 ml glass beaker with 40 ml of nitric acid (3.2.3). Then add 100 ml of water. Boil to expel nitrous fumes, cool, transfer to a 1000 ml volumetric flask and fill to
46、the mark with water. 3.3.1.2 Cadmium, standard solution corresponding to 20 mg/l of cadmium. Pipette 20,00 ml of the stock cadmium solution (3.3.1.1) into a 1000 ml volumetric flask. Add 20 ml of nitric acid (3.2.3) and fill to the mark with water. 3.3.2 Chromium solutions 3.3.2.1 Chromium, stock so
47、lution corresponding to 1000 mg/l of chromium. Dissolve 2,8290 g 0,0002 g of potassium dichromate, K2Cr2O7, dried at 130 C for 24 h, in a covered 400 ml glass beaker with 40 ml of water. Add 5 ml of sulfuric acid (3.2.4), cool, transfer to a 1000 ml volumetric flask and fill to the mark with water.
48、3.3.2.2 Chromium, standard solution corresponding to 20 mg/l of chromium. Pipette 20,00 ml of the stock chromium solution (3.3.2.1) into a 1000 ml volumetric flask. Add 20 ml of nitric acid (3.2.3) and fill to the mark with water. Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/19/2007 00:37:13 MDTNo reproduction or networking permitted without license from IHS -,