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1、INTERNATIONAL STANDARD ISO 15178 First edition 2000-11-01 Reference number ISO 15178:2000(E) ISO 2000 Soil quality Determination of total sulfur by dry combustion Qualit du sol Dosage du soufre total par combustion sche Copyright International Organization for Standardization Provided by IHS under l
2、icense with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/24/2007 21:42:25 MDTNo reproduction or networking permitted without license from IHS -,-,- ISO 15178:2000(E) ii ISO 2000 All rights reserved PDF disclaimer This PDF file may contain embedded typefaces. In accordance wi
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6、on may be reproduced or utilized in any form or by any means, elec- tronic or mechanical, including photocopying and microfilm, without permission in writing from either ISO at the address below or ISOs mem- ber body in the country of the requester. ISO copyright office Case postale 56 CH-1211 Genev
7、a 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 Provided by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/24/2007 21:42:25 MDTNo repr
8、oduction or networking permitted without license from IHS -,-,- ISO 15178:2000(E) ISO 2000 All rights reserved iii Foreword ISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). The work of preparing International Standar
9、ds is normally carried out through ISO technical com- mittees. 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 liai- son with ISO, also
10、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 3. Draft International Standards adopted
11、 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 International Standard may be the subj
12、ect of patent rights. ISO shall not be held responsible for identifying any or all such patent rights. International Standard ISO 15178 was prepared by Technical Committee ISO/TC 190,Soil quality, Subcommittee SC 3,Chemical methods and soil characteristics. Annex A of this International Standard is
13、for information only. Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/24/2007 21:42:25 MDTNo reproduction or networking permitted without license from IHS -,-,- Copyright International O
14、rganization for Standardization Provided by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/24/2007 21:42:25 MDTNo reproduction or networking permitted without license from IHS -,-,- INTERNATIONAL STANDARDISO 15178:2000(E) ISO 2000 All rights reserved 1 S
15、oil quality Determination of total sulfur by dry combustion WARNING This International Standard may involve hazardous materials, operations and equipment. This International Standard does not purport to address all of the safety problems associated with its use. It is the responsibility of the user
16、of this International Standard to consult and establish appropriate health and safety practices and determine the applicability of regulatory limitations prior to use. 1Scope This International Standard describes a procedure using dry combustion for the determination of total sulfur in soil samples.
17、 It is applicable to all types of air-dried soil samples. NOTEHigh-temperature combustion methods might not determine total sulfur, only combustible sulfur. The difference between total and combustible sulfur is usually negligible in soils. 2Normative references The following normative documents con
18、tain provisions which, through reference in this text, constitute provisions of this International Standard. For dated references, subsequent amendments to, or revisions of, any of these publica- tions do not apply. However, parties to agreements based on this International Standard are encouraged t
19、o investi- gate the possibility of applying the most recent editions of the normative documents indicated below. For undated references, the latest edition of the normative document referred to applies. Members of ISO and IEC maintain registers of currently valid International Standards. ISO 11464,S
20、oil quality Pretreatment of samples for physico-chemical analyses. ISO 11465,Soil quality Determination of dry matter and water content on a mass basis Gravimetric method. 3Principle The sulfur content of a soil sample, pretreated in accordance with ISO 11464, is determined by heating the sample to
21、a temperature of at leastin a stream of oxygen-containing gas. Organically and inorganically bound sul- fur is converted to SO2. This reaction may in some cases need a higher temperature or the addition of catalysts, modifiers or accelerators. At temperatures, SO3may be formed in the presence of exc
22、ess oxygen. This SO3has to be reduced to SO2using an appropriate reagent, e. g. copper. The SO2arising from the combustion is measured by infrared spectrometry, thermal conductivity or other suitable detection technique. Gases resulting from the combustion which may interfere with the detection stag
23、e have to be removed from the stream of gas prior to de- tection. This method is for use with commercially available sulfur analysers equipped to carry out the preceding operations automatically. These instruments shall be calibrated using chemical compounds or standard reference materials of known
24、sulfur content based on the range of sulfur in each sample analysed. NOTEComplete decomposition of sulfur-containing compounds may not occur at lower temperatures, especially in the presence of free alkaline or alkaline earth carbonates or sulfates. In such cases, temperaturesor the use of matrix mo
25、difiers such as WO3or V2O5may be necessary. The efficiency of the quantitative recovery of sulfur from such soils can be tested using substances such as calcium sulfate. 1 150 C 1 350 C Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=NASA Tech
26、nical Standards 1/9972545001 Not for Resale, 04/24/2007 21:42:25 MDTNo reproduction or networking permitted without license from IHS -,-,- ISO 15178:2000(E) 2 ISO 2000 All rights reserved 4Reagents All reagents used should be of an analytical grade in accordance with the manufacturers instruction ma
27、nual for the instrument used. 4.1Oxygen-containing combustion gas, free of sulfur and its compounds, in accordance with the instructions of the equipment manufacturer. 4.2Calibration substances, such as sulfanilic acid (C6H7NO3S) or other compounds of known sulfur content or soil samples with certif
28、ied sulfur contents. NOTEStandard reference materials (SRM) or other commercially available reference soils with a certified sulfur content can be obtained and used for calibration purposes in this test method. Examples of such materials are given in annex A. Users of SRMs are urged to use these mat
29、erials to develop their own internal reference materials and associated quality assurance procedures. 5Apparatus 5.1Analytical balance. The resolution of the balance should be less than or equal totimes the mass of sample or calibration sub- stance in accordance with the following table: 5.2Measurem
30、ent apparatus, to determine the total sulfur content of a sample by burning it at a temperature of at leastand detecting the SO2generated. 5.3Accessories and consumables. Accessories and consumables in accordance with the manufacturers instructions. 6Preparation of sample Pulverize the sample to pas
31、s asieve and mix thoroughly in accordance with ISO 11464. A separate portion of the sample should be analysed for moisture content in accordance with ISO 11465 for recalculation of results to an oven-dry basis. Care should be exercised to minimize, during handling, the probability of altering the mo
32、isture content of the SRM through desiccation or absorption of atmospheric moisture. All standard reference materials should be used in ac- cordance with the information given in the certificate of analysis. 7Procedure 7.1Instrument preparation Assemble the apparatus according to the manufacturers i
33、nstructions and condition it to eliminate drift in the sensitivity. Table 1 Mass of sample or calibration substanceBalance resolution gmg 1 to 0,1 0,000 1 160,1 60,01 0,160,001 1 150 C 250m Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=NASA
34、Technical Standards 1/9972545001 Not for Resale, 04/24/2007 21:42:25 MDTNo reproduction or networking permitted without license from IHS -,-,- ISO 15178:2000(E) ISO 2000 All rights reserved 3 7.2Calibration Analyse sufficient samples or calibration substances (4.2) with sulfur contents covering the
35、range of values to be ex- pected in the unknown samples. Widely accepted quality control procedures may be employed to establish the required number of calibrated samples and the precision and frequency of calibration. A minimum of four calibration points is strongly recommended. 7.3Analysis Weigh a
36、 test portion into a suitable crucible. Choose the mass of the test portion so that the expected sulfur content falls within the range of values covered by the calibration curve. If the sulfur content is greater than the maximum cal- ibration value, repeat the analysis with a smaller mass of test sa
37、mple. Operate the instrument in accordance with the manufacturers instructions. 8Calculation and expression of the results Calculate the total content of sulfur, in grams per kilogram, on the basis of the oven-dried soil according to the following formula: where is the molar conversion factor from S
38、O2to S; is the mass of the soil sample, in grams; is the mass of the sulfur dioxide released by the sample, in milligrams; is the mass fraction of water content (expressed as a percentage) on the basis of the oven-dried soil (clause 6). NOTEAutomatic instruments may give sulfur contents directly, al
39、though these data may need correction to an oven-dried basis. 9Test report The test report shall contain the following information: a)a reference to this International Standard; b)all necessary information for the complete identification of the sample; c)the results of the determination, in grams su
40、lfur per kilogram of oven-dried soil; d)details of any operation not specified in this International Standard or which is optional, as well as any factor which may have affected the results. Report the result to the nearest. 10Precision and comparison with other methods 10.1General The quantitative
41、limit of this method is estimated to be about. wts wts=0,500 5(m2/m1) (100+ w)/100 0,505 5 m1 m2 w 0,1 g/kg 0,2 g/kg Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/24/2007 21:42:25 MDTN
42、o reproduction or networking permitted without license from IHS -,-,- ISO 15178:2000(E) 4 ISO 2000 All rights reserved This method is highly dependent upon the calibration of the equipment. The reference materials should be as close as possible to the samples in sulfur content, chlorine content, iro
43、n content, etc. 10.2Precision This method was tested in an interlaboratory trial in 1998. Four soil samples were analysed by eight laboratories. In accordance with ISO 5725-2:1994,Accuracy (trueness and precision) of measurement methods and results Part 2: Basic method for the determination of repea
44、tability and reproducibility of a standard measurement method, the results in Table 2 were obtained. 10.3Comparison with other methods The samples from the interlaboratory trial were analysed by two other methods, X-ray fluorescence, XRF, and induc- tively coupled plasma spectrometry, ICP. The ICP d
45、etermination was performed after extraction with concentrated ni- tric acid. The results in Table 3 were obtained. Table 2 SampleMean sulfur contentRepeatability conditionsReproducibility conditions g/kg 11,620,050,130,160,46 20,460,100,280,210,58 30,250,050,130,100,28 40,280,060,180,130,37 is the r
46、epeatability standard deviation. is the repeatability value. is the reproducibility standard deviation. is the reproducibility value. Table 3 Sample Method1234 Mean value from ring test1,620,460,250,28 XRF1,500,560,270,46 ICP1,520,450,200,32 srrsRR sr r sR R Copyright International Organization for
47、Standardization Provided by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/24/2007 21:42:25 MDTNo reproduction or networking permitted without license from IHS -,-,- ISO 15178:2000(E) ISO 2000 All rights reserved 5 Annex A (informative) Examples of Stand
48、ard Reference Materials (SRM) The following standard reference materials are available. The list is not exhaustive. a)US Geological Survey GXR-4sulfur b)BCR CRM 101sulfur c)Soils from the National Institute of Science and Technology, NIST, USA SRM 2710sulfur SRM 2711sulfur 17,7 g/kg 1,70 g/kg 2,4 g/kg 0,420 g/kg Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/24/2007 21:42:25 MDTNo reproduction or n