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1、INTERNATIONAL STANDARD ISO 14869-2 First edition 2002-08-01 Reference number ISO 14869-2:2002(E) ISO 2002 Soil quality Dissolution for the determination of total element content Part 2: Dissolution by alkaline fusion Qualit du sol Mise en solution pour la dtermination des teneurs lmentaires totales
2、Partie 2: Mise en solution par fusion alcaline Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/25/2007 06:22:13 MDTNo reproduction or networking permitted without license from IHS -,-,-
3、ISO 14869-2:2002(E) ii ISO 2002 All rights reserved PDF disclaimer This PDF file may contain embedded typefaces. In accordance with Adobes licensing policy, this file may be printed or viewed but shall not be edited unless the typefaces which are embedded are licensed to and installed on the compute
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6、ntral Secretariat at the address given below. ISO 2002 All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized in any form or by any means, electronic or mechanical, including photocopying and microfilm, without permission in writing from either ISO
7、 at the address below or ISOs member body in the country of the requester. ISO copyright office Case postale 56 CH-1211 Geneva 20 Tel. + 41 22 749 01 11 Fax + 41 22 749 09 47 E-mail copyrightiso.ch Web www.iso.ch Printed in Switzerland Copyright International Organization for Standardization Provide
8、d by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/25/2007 06:22:13 MDTNo reproduction or networking permitted without license from IHS -,-,- ISO 14869-2:2002(E) ISO 2002 All rights reserved iii Foreword ISO (the International Organization for Standardi
9、zation) 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 has the right to b
10、e 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. International Standa
11、rds are drafted in accordance with the rules given in the ISO/IEC Directives, Part 3. 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 cas
12、ting a vote. Attention is drawn to the possibility that some of the elements of this part of ISO 14869 may be the subject of patent rights. ISO shall not be held responsible for identifying any or all such patent rights. International Standard ISO 14869-2 was prepared by Technical Committee ISO/TC 1
13、90, Soil quality, Subcommittee SC 3, Chemical methods and soil characteristics. ISO 14869 consists of the following parts, under the general title Soil quality Dissolution for the determination of total element content: Part 1: Dissolution with hydrofluoric and perchloric acids Part 2: Dissolution b
14、y alkaline fusion Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/25/2007 06:22:13 MDTNo reproduction or networking permitted without license from IHS -,-,- Copyright International Organ
15、ization for Standardization Provided by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/25/2007 06:22:13 MDTNo reproduction or networking permitted without license from IHS -,-,- INTERNATIONAL STANDARDISO 14869-2:2002(E) ISO 2002 All rights reserved 1 Soi
16、l quality Dissolution for the determination of total element content Part 2: Dissolution by alkaline fusion 1Scope This part of ISO 14869 specifies a method for the dissolution of total contents for the following elements in soils: Na, K, Mg, Ca, Ti, Mn, Fe, Al, Si. This list is not exhaustive, and
17、other elements are applicable for determination, provided they are not lost during the fusion process, where is the mass content of the element, expressed in milligrams per kilogram soil, is the detection limit, in milligrams per litre, for the element and analytical method considered, 3is a convent
18、ional factor, is the adjusted volume, in litres, of the final solution containing the dissolved sample, and is the mass of the test portion, in kilograms, the determination is not adversely affected by the high salt concentration in the resultant solution. The flux proposed in this method is suitabl
19、e for a wide range of materials, among which soil samples are relatively easy to deal with. 2Normative references The following normative documents contain provisions which, through reference in this text, constitute provisions of this part of ISO 14869. For dated references, subsequent amendments t
20、o, or revisions of, any of these publications do not apply. However, parties to agreements based on this part of ISO 14869 are encouraged to investigate the possibility of applying the most recent editions of the normative documents indicated below. For undated references, the latest edition of the
21、normative document referred to applies. Members of ISO and IEC maintain registers of currently valid International Standards. ISO 3696:1987, Water for analytical laboratory use Specification and test methods ISO 11464:1994, Soil quality Pretreatment of samples for physico-chemical analyses ISO 11465
22、:1993, Soil quality Determination of dry matter and water content on a mass basis Gravimetric method w (3d V/m) w d V m Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/25/2007 06:22:13 M
23、DTNo reproduction or networking permitted without license from IHS -,-,- ISO 14869-2:2002(E) 2 ISO 2002 All rights reserved 3Principle To avoid reduction of metallic oxides to metals, the dried and ground sample is first ignited at and afterwards fused with a mixture of dilithium tetraborate (one pa
24、rt) and lithium metaborate (four parts). While still liquid, the melt is poured quantitatively into dilute nitric acid. The suspension is then stirred until the solid phase dissolves completely. 4Reagents The reagents used shall meet the purity requirements of the subsequent analysis. 4.1Water, comp
25、lying with grade 2 of ISO 3696. 4.2Dilithium tetraborate, Li2B4O7, apparent density when packed = 1. 4.3Lithium metaborate, LiBO2, apparent density when packed = 0,8. 4.4Nitric acid, , . 4.5Nitric acid, . Dilute of nitric acid (4.4) with water (4.1) to make of solution. 5Apparatus 5.1Grinding mill,
26、capable of grinding dried soils without contamination by the elements of interest. 5.2Drying oven and dessicator, for the determination of dry matter in accordance with ISO 11465. 5.3Analytical balance, capable of weighing accurately to . 5.4Furnace, which can reach a temperature of within . 5.5Heat
27、ing device, capable of heating the proposed flux above its melting point. Several devices are allowed: inductively heated furnace; muffle furnace; air-propane Meker burner. 5.6Crucible, of about capacity, preferably made of platinum:gold (95:5) alloy or vitreous carbon. Molten borates wet some metal
28、s and their alloys. For this reason, the use of the above type of crucible is strongly recommended. Failure to do so can result in loss of melt, and the possibility of carry-over between subsequent dissolutions. 5.7Usual laboratory glassware, including beakers of capacity. 5.8Magnetic stirrer, with
29、polytetrafluoroethylene (PTFE)-coated follower. 6Procedure Mill a representative portion of the dried sample, prepared in accordance with ISO 11464, as fine as possible in order to obtain a subsample of approximately . Use a portion of that milled sample to determine the water content in accordance
30、with ISO 11465. 450 C c(HNO3)=15,2 mol/l =1,41 g/ml c(HNO3)=0,5 mol/l 32 ml1 l 0,000 1 g 450 C 25 C 1 h 30 ml 800 ml 20 g Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/25/2007 06:22:13
31、 MDTNo reproduction or networking permitted without license from IHS -,-,- ISO 14869-2:2002(E) ISO 2002 All rights reserved 3 Weigh precisely by means of the balance (5.3) about of the milled sample, and transfer to a crucible (5.6). Place the crucible in the furnace (5.4) and allow the temperature
32、to reach progressively during . Maintain this temperature for . Allow the crucible to cool to room temperature. Weigh of dilithium tetraborate (4.2) and of lithium metaborate (4.3), transfer to the crucible containing the ignited sample and mix thoroughly with a plastics spatula. Heat the mixture by
33、 means of the heating device (5.5) to between and until the boron salts melt and the sample dissolves completely. Depending on the type of heating device, dissolution is generally achieved within to . With unknown samples, it may be necessary to swirl the mixture at least once to verify that dissolu
34、tion is complete. WARNING Handle the hot crucible with tongs while wearing protective gloves and eye/face protection. Before the melt solidifies, carefully pour it quantitatively into a beaker (5.7) containing of dilute nitric acid (4.5). Stir the solution by means of a magnetic stirrer (5.8) until
35、the solid phase is dissolved; generally to is sufficient. Transfer this solution to a volumetric flask of capacity , or depending on the levels of concentration needed by the method of measurement for the elements of interest. Rinse the beaker with dilute acid (4.5), add these washings to the flask
36、and adjust the volume to the mark still using acid (4.5). If this solution is turbid, discard it and perform a new fusion with a smaller test portion. Using the same procedure without the sample, perform at least one blank test within each batch of fusions. Determinations should be undertaken within
37、 three days following the fusion. After a longer period of time, some compounds may hydrolyse or polymerize and precipitate, rendering the solution unusable. If Pt-alloy or vitreous carbon crucibles (5.6) are not available, melt adhesion is likely to occur. In this case, the crucible plus adhering m
38、elt should be placed in the beaker with nitric acid and the solid melt allowed to dissolve. This can take several hours. Care should be taken to ensure that the outside of the crucible is free of material containing elements of interest before it is immersed in the nitric acid, to avoid contaminatio
39、n of the sample solution. When the quantity of adhering melt is small enough, its dissolution can also be achieved by adding a few millilitres of nitric acid (4.5) to the crucible. In that case, slightly heating the solution on a hot plate may be necessary to assist dissolution. NOTE 1Experience has
40、 shown that dissolution of sample can be considerably prolonged if the material is not ground below . NOTE 2Very hot platinum alloy crucibles are best handled with platinum-tipped tongs to avoid problems of contamination from other metals. 7Test report Submit the test report either separately or in
41、conjunction with the test report of the subsequent analytical measurement. The test report shall contain the following information: a)a reference to this part of ISO 14869; b)complete identification of the sample; c)any details not specified in this part of ISO 14869, or which are optional, as well
42、as any factor which may have affected the results. 0,200 g 450 C 1 h 3 h 0,200 g0,002 g0,800 g0,005 g 1 000 C 1 100 C 10 min30 min 200 ml 15 min20 min 250 ml 500 ml1 000 ml 200 ml 250m Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=NASA Techn
43、ical Standards 1/9972545001 Not for Resale, 04/25/2007 06:22:13 MDTNo reproduction or networking permitted without license from IHS -,-,- ISO 14869-2:2002(E) ICS 13.080.10 Price based on 3 pages ISO 2002 All rights reserved Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/25/2007 06:22:13 MDTNo reproduction or networking permitted without license from IHS -,-,-