1、BRITISH STANDARDSoil quality Determination ofcarbonate content Volumetric methodBS EN ISO10693:2014ICS 13.080.10 National forewordThis British Standard is the UK implementation of EN ISO 10693:2014. It is identical to ISO 10693:1995. It supersedes BS 7755-3.10:1995 (dual numbered as ISO 10693:1995),
2、 which is withdrawn.The UK participation in its preparation was entrusted to Technical Committee EH/4, Soil quality.A list of organizations represented on this committee can be obtained on request to its secretary.Additional information. References to labelled parts of the apparatus refer exclusivel
3、y to Figure 1.In paragraph 1 of 7.2 it is recommended that the variation in temperature is no more than 1 C and the variation in pressure is no more than 0.5 kPa.In paragraph 2 of 7.2 the phrase “two standards of respectively 0,200 g and 0,400 g” means that one sample of each should be prepared.Text
4、ual errors. In note 2 in clause 3, “Annex A ” should read “Annex B”. In paragraph 4 of 7.2 “tube H” should read “tube E”.This publication does not purport to include all the necessary provisions of a contract. Users are responsible for its correct application.Compliance with a British Standard canno
5、t confer immunity from legal obligations.BS EN ISO 10693:2014This British Standard, havingbeen prepared under thedirection of the Health andEnvironment Sector Board, waspublished under the authorityof the Standards Board andcomes into effect on15 October 1995Amendments/corrigenda issued since public
6、ationDate Comments 30 June 2014 This corrigendum renumbers BS 7755-3.10:1995 (dual numbered as ISO 10693:1995) as BS EN ISO 10693:2014ISBN 978 0 580 83738 8 The British Standards Institution 2014. Published by BSI Standards Limited 2014EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 10693 M
7、arch 2014 ICS 13.080.10 English Version Soil quality - Determination of carbonate content - Volumetric method (ISO 10693:1995) Qualit du sol - Dtermination de la teneur en carbonate - Mthode volumtrique (ISO 10693:1995) Bodenbeschaffenheit - Bestimmung des Carbonatgehaltes -Volumetrisches Verfahren
8、(ISO 10693:1995) This European Standard was approved by CEN on 13 March 2014. CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this European Standard the status of a national standard without any alteration. Up-to-date lists and bibl
9、iographical references concerning such national standards may be obtained on application to the CEN-CENELEC Management Centre or to any CEN member. This European Standard exists in three official versions (English, French, German). A version in any other language made by translation under the respon
10、sibility of a CEN member into its own language and notified to the CEN-CENELEC Management Centre has the same status as the official versions. CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Repu
11、blic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMA
12、LISATION EUROPISCHES KOMITEE FR NORMUNG CEN-CENELEC Management Centre: Avenue Marnix 17, B-1000 Brussels 2014 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN ISO 10693:2014 EForeword The text of ISO 10693:1995 has been prepared by
13、Technical Committee ISO/TC 190 “Soil quality” of the International Organization for Standardization (ISO) and has been taken over as EN ISO 10693:2014 by Technical Committee CEN/TC 345 “Characterization of soils” the secretariat of which is held by NEN. This European Standard shall be given the stat
14、us of a national standard, either by publication of an identical text or by endorsement, at the latest by September 2014, and conflicting national standards shall be withdrawn at the latest by September 2014. Attention is drawn to the possibility that some of the elements of this document may be the
15、 subject of patent rights. CEN and/or CENELEC shall not be held responsible for identifying any or all such patent rights. According to the CEN-CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgiu
16、m, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerl
17、and, Turkey and the United Kingdom. Endorsement notice The text of ISO 10693:1995 has been approved by CEN as EN ISO 10693:2014 without any modification. iiBS EN ISO 10693:2014 EN ISO 10693:2014 (E)ContentsPage1 Scope 12 Normative references 13 Principle 14 Reagents 15 Apparatus and glassware 16 Lab
18、oratory sample 37 Procedure 48 Calculation 49 Repeatability 510 Test report 5Annex A (informative) Results of an interlaboratory trial for the determination of the carbonate content of soils 6Annex B (informative) Bibliography 6Figure 1 Example of a Scheibler unit for a single sample determination 2
19、Figure 2 Example of a single Scheibler unit 3Table 1 Relationship between intensity and time of effervescence, estimated carbonate content of the soil and mass of test portion 4Table 2 Repeatability 5Table A.1 Results of the interlaboratory trial for the determination of the carbonate content 6iiiBS
20、 EN ISO 10693:2014 ISO 10693:1995BS EN ISO 10693:2014 ISO 10693:199511 ScopeThis International Standard specifies a method for the determination of carbonate content in soil samples.It is applicable to all types of air-dried soil samples.2 Normative referencesThe following standards contain provisio
21、ns 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 possi
22、bility of applying the most recent editions of the 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 11464:1994, Soil quality Pretreatment of samples f
23、or physico-chemical analyses. ISO 11465:1993, Soil quality Determination of dry matter and water content on a mass basis Gravimetric method. 3 PrincipleHydrochloric acid is added to a soil sample to decompose any carbonates present. The reaction in simplified form reads as follows (Me means metal):M
24、eCO3 + 2H+ F Me2+ + H2CO3H2CO3 F H2O + CO2 (gaseous state)The volume of the carbon dioxide produced is measured by using a Scheibler apparatus (5.1), and is compared with the volume of carbon dioxide produced by pure calcium carbonate. To avoid making corrections for differences in temperature and p
25、ressure, all determinations are carried out under the same conditions. The determination should be carried out in a temperature-controlled room.NOTE 1The carbonate content is expressed as an equivalent concentration of calcium carbonate (CaCO3). In fact all carbonates and bicarbonates present in the
26、 sample are measured. Many carbonates appear in the form of calcite and aragonite (CaCO3), dolomite CaMg(CO3)2, siderite (FeCO3) and rhodochrosite (MnCO3). In soils in dry (arid) regions, soda (Na2CO3.10 H2O) may be present. When it is known that a certain form of carbonate, other than calcium carbo
27、nate, is mainly present in the soil under study, the final concentration of this form can be used.NOTE 2Other gases that are produced e.g. hydrogen sulfide (H2S) in samples of anaerobic soil containing sulfides may result in an overestimate of the carbonate content. In these cases the gas produced s
28、hould be purified and its volume measured in another way (see 1 in Annex A). When sulfides are known to be present in the soil samples, mercury(II) chloride (HgCl2) is added to the hydrochloric acid solution to form insoluble mercury(II) sulfide (HgS).4 ReagentsUse only reagents of recognized analyt
29、ical grade.4.1 Water, with a specific electrical conductivity not higher than 0,2 mS/m at25C (conforming to grade2 of ISO 3696).4.2 Hydrochloric acid, c(HCl) = 4 mol/l.Dilute 340ml of concentrated hydrochloric acid ( = 1,19 g/ml) to 1000ml with water (4.1).4.3 Calcium carbonate (CaCO3), powder.5 App
30、aratus and glassware5.1 Scheibler apparatus, adapted for carrying out a single sample determination (see Figure 1). An example of a single unit of apparatus, together with an indication of the water level before and after the measurement, is given in Figure 2.BS EN ISO 10693:2014 ISO 10693:19952KeyA
31、BCD1D2EFGHReaction vessel (5.3)Plastics cup (5.4) with hydrochloric acid (4.2)Rubber stopperStop-cockStop-cockU-shaped calibration tubeStorage vessel with waterShaking beamAir-inlet tubeFigure 1 Example of a Scheibler unit for a single sample determinationBS EN ISO 10693:2014 ISO 10693:19953NOTE 3Fo
32、r the determination specified in this International Standard, a Scheibler apparatus with two glass U-shaped calibration tubes each having a volume of100ml is used. It is also possible to use tubes with a different volume (i.e.50ml or200ml). In this case the mass of the test portion used for the meas
33、urement has to be adapted.NOTE 4The temperature of the water in the system should be equal to the ambient temperature.NOTE 5When only a few soil samples have to be analysed, a minimum of five Scheibler units is sufficient. In this case the reaction vessels can be shaken by hand. However, it is then
34、necessary to take into account the temperature variations in the air inside the vessels.NOTE 6By lowering the water level in the tube on the left (seeFigure 2) with the stop-cock closed, an underpressure is created in the tube on the right. By creating such an underpressure for some time, the unit c
35、an be checked for leaks.5.2 Analytical balance, with an accuracy of at least0,1 mg.5.3 Reaction vessels, of capacity150ml and with a wide neck.5.4 Plastics cup, of capacity about10ml, which can pass through the neck of the reaction vessel (5.3).5.5 Tongs, acid-proof.5.6 Watch glass6 Laboratory sampl
36、eUse the 160 u 1w(CaCO3) is the carbonate content, in grams per kilogram, of the oven-dried soil;m1 is the mass, in grams, of the test portion;m2 is the mean mass, in grams, of the calcium carbonate standards;V1 is the volume, in millilitres, of carbon dioxide produced by the reaction of the test po
37、rtion;V2 is the mean volume, in millilitres, of carbon dioxide produced by the calcium carbonate standards;BS EN ISO 10693:2014 ISO 10693:199559 RepeatabilityThe repeatability of the determination of carbonate content carried out in two separate, consecutive measurements shall satisfy the conditions
38、 given in Table 2.Table 2 Repeatability10 Test reportThe test report shall contain the following information:a) a reference to this International Standard;b) all information necessary for the complete identification of the sample;c) the results of the determination in whole numbers, in grams per kil
39、ogram, calculated on the basis of oven-dried soil expressed as calcium carbonate or as another specified form of carbonate, when it is known to be the main form present;d) details of any operation not specified in this International Standard or regarded as optional, as well as any factor which may h
40、ave affected the results.V3 is the volume change, in millilitres, in the blank determinations (this value can be negative);w(H2O) is the water content, expressed as a percentage by mass, of the dried sample, determined according to ISO11465.Carbonate contentg/kg Acceptable variation0 to 50 3 g/kg 50
41、 to 150 6 % of the value 150 to 180 9 g/kg 180 5 % of the valueBS EN ISO 10693:2014 ISO 10693:19956Annex A (informative) Results of an interlaboratory trial for the determination of the carbonate content of soilsAn interlaboratory trial was organized in1993 by the Wageningen Agricultural University
42、(Netherlands), to verify the procedure specified in this International Standard.For this interlaboratory trial, the determination of the carbonate content of five soils was carried out by nine laboratories.The summary of the results of the interlaboratory trial is presented inTable A.1.The repeatabi
43、lities (r) and the reproducibilities (R) listed inTable A.1 were calculated according to ISO5725:1986, Precision of test methods Determination of repeatability and reproducibility for a standard test method by inter-laboratory tests.Table A.1 Results of the interlaboratory trial for the determinatio
44、n of the carbonate contentAnnex B (informative) Bibliography1 ALLISON, L.E. Wet combustion apparatus and procedure for organic and inorganic carbon in soils. Soil Science Society of America Proc. 24 (1960), pp. 36-40.Soil No. Origin Mean Valueg/kg r R n1 Great Britain 662 31,8 94,8 92 France 540 28,
45、4 55,0 93 France 158 7,6 18,6 84 Netherlands 66 3,8 19,2 95 Argentina 1 2,0 3,3 9n = number of laboratories retained after eliminating outliers.BS EN ISO 10693:2014 ISO 10693:1995This page deliberately set blankBSI389 Chiswick High RoadLondonW4 4ALBSIBritishStandardsInstitutionBSI is the independent
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