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1、BRITISH STANDARD BS EN 13475:2002 Liming materials Determination of calcium content Oxalate method The European Standard EN 13475:2001 has the status of a British Standard ICS 65.080 NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAW Licensed Copy: sheffieldun sheffieldun, na, Mo
2、n Oct 30 01:39:45 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS EN 13475:2002 This British Standard, having been prepared under the direction of the Materials and Chemicals Sector Policy and Strategy Committee, was published under the authority of the Standards Policy and Strategy Committee on 29 Ja
3、nuary 2002 BSI 29 January 2002 ISBN 0 580 38978 2 National foreword This British Standard is the official English language version of EN 13475:2001. The UK participation in its preparation was entrusted to Technical Committee CII/37, Fertilizers and related chemicals, which has the responsibility to
4、: A list of organizations represented on this committee can be obtained on request to its secretary. Cross-references The British Standards which implement international or European publications referred to in this document may be found in the BSI Standards Catalogue under the section entitled “Inte
5、rnational Standards Correspondence Index”, or by using the “Find” facility of the BSI Standards Electronic Catalogue. A British Standard does not purport to include all the necessary provisions of a contract. Users of British Standards are responsible for their correct application. Compliance with a
6、 British Standard does not of itself confer immunity from legal obligations. aid enquirers to understand the text; present to the responsible European committee any enquiries on the interpretation, or proposals for change, and keep the UK interests informed; monitor related international and Europea
7、n developments and promulgate them in the UK. Summary of pages This document comprises a front cover, an inside front cover, the EN title page, pages 2 to 9 and a back cover. The BSI copyright date displayed in this document indicates when the document was last issued. Amendments issued since public
8、ation Amd. No. DateComments Licensed Copy: sheffieldun sheffieldun, na, Mon Oct 30 01:39:45 GMT+00:00 2006, Uncontrolled Copy, (c) BSI EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 13475 November 2001 ICS 65.080 English version Liming materials Determination of calcium content Oxalate method
9、Amendements minraux basiques Dtermination de la teneur en calcium Mthode loxalate Calcium-/Magnesium-Bodenverbesserungsmittel Bestimmung des Calciumgehaltes Oxalatverfahren This European Standard was approved by CEN on 29 September 2001. CEN members are bound to comply with the CEN/CENELEC Internal
10、Regulations which stipulate the conditions for giving this European Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such national standards may be obtained on application to the Management Centre or to any CEN member. This
11、 European Standard exists in three official versions (English, French, German). A version in any other language made by translation under the responsibility of a CEN member into its own language and notified to the Management Centre has the same status as the official versions. CEN members are the n
12、ational standards bodies of Austria, Belgium, Czech Republic, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHE
13、S KOMITEE FR NORMUNG Management Centre: rue de Stassart, 36 B-1050 Brussels 2001 CENAll rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 13475:2001 E Licensed Copy: sheffieldun sheffieldun, na, Mon Oct 30 01:39:45 GMT+00:00 2006, Uncontroll
14、ed Copy, (c) BSI EN 13475:2001 (E) 2 Contents Page Foreword.3 1Scope4 2Normative references .4 3Principle.4 4Reagents4 5Apparatus.5 6Sampling6 7Procedure.6 8Expression of results8 9Precision8 10Test report9 Licensed Copy: sheffieldun sheffieldun, na, Mon Oct 30 01:39:45 GMT+00:00 2006, Uncontrolled
15、Copy, (c) BSI EN 13475:2001 (E) 3 Foreword This European Standard has been prepared by Technical Committee CEN/TC 260, Fertilizers and liming materials, the Secretariat of which is held by DIN. This European Standard shall be given the status of a national standard, either by publication of an ident
16、ical text or by endorsement, at the latest by May 2002, and conflicting national standards shall be withdrawn at the latest by May 2002. According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: A
17、ustria, Belgium, Czech Republic, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and the United Kingdom. Licensed Copy: sheffieldun sheffieldun, na, Mon Oct 30 01:39:45 GMT+00:00 2006, Uncontrolled Copy, (c) BS
18、I EN 13475:2001 (E) 4 1 Scope This European Standard specifies a method for the determination of the calcium content of silicate liming materials including slags. NOTE 1The method has been shown to be suitable for other liming materials too, but there are no precision data available yet. NOTE 2The m
19、ethod is also applicable for the determination of the calcium content of mineral fertilizers. 2 Normative references This European Standard incorporates by dated or undated reference, provisions from other publications. These normative references are cited at the appropriate places in the text, and
20、the publications are listed hereafter. For dated references, subsequent amendments to, or revisions of any of these publications apply to this European Standard only when incorporated in it by amendment or revision. For undated references the latest edition of the publication referred to applies (in
21、cluding amendments). EN 1482, Sampling of solid fertilizers and liming materials. ISO 3310-1, Test sieves Technical requirements and testing Part 1: Test sieves of metal wire cloth. 3 Principle After dissolution of the sample in a mixture of hydrochloric acid and nitric acid, calcium is precipitated
22、 in the form of calcium oxalate at a pH between 4,4 and 4,6. The supernatant solution is removed by means of an immersion filter. The calcium oxalate precipitate is dissolved in sulfuric acid and the calcium content is determined by titration with potassium permanganate. 4 Reagents 4.1 General Comme
23、rcially available standard solutions may be used instead of standard solutions produced in the laboratory. Variations in concentration shall be taken into account for the calculation of the results. 4.2Hydrochloric acid, ?20(HCl) = 1,19 g/ml, c(HCl) = 12,5 mol/l. 4.3Nitric acid, ?20(HNO3) = 1,40 g/m
24、l, c(HNO3) = 14,9 mol/l. 4.4Citric acid solution Dissolve 300 g of citric acid monohydrate in water and make up to 1 l. 4.5Ammonium chloride solution Dissolve 100 g of ammonium chloride in water and make up to 1 l. Mix well. 4.6Bromocresol green Dissolve 5 g of bromocresol green in ethanol with a vo
25、lume concentration of ethanol of 96 % and make up to 1 l. Licensed Copy: sheffieldun sheffieldun, na, Mon Oct 30 01:39:45 GMT+00:00 2006, Uncontrolled Copy, (c) BSI EN 13475:2001 (E) 5 4.7Ammonium oxalate solution, saturated Dissolve sufficient ammonium oxalate monohydrate (approximately 70 g) in 1
26、l of water to produce a saturated solution. After reaching saturation, filter the solution. 4.8Ammonia solution Dilute 400 ml of ammonia solution containing a mass fraction of NH3 of 25 % ?20(NH3) = 0,91 g/ml with water to 1 l. 4.9Ammonium oxalate solution Dissolve 10 g of ammonium oxalate monohydra
27、te in water and make up to 1 l. 4.10 Sulfuric acid, ?20(H2SO4) = 1,84 g/ml, c(H2SO4) = 15,2 mol/l. 4.11 Sulfuric acid solution Dilute one volume of sulfuric acid (4.10) with one volume of water. 4.12 Potassium permanganate solution, c(KMnO4) 0,02 mol/l. Dissolve 3,18 g of potassium permanganate in 1
28、00 ml of water by boiling for 20 min. Subsequently filter the solution through a glass filter crucible (5.3) and transfer the filtrate into a light-protected 1 l volumetric flask. Rinse the filter crucible. Transfer the washing water into the 1 l volumetric flask likewise and dilute to the mark. Aft
29、er a standing time of several days filter the solution through a filter crucible (5.3). Determine the exact amount-of-substance concentration (F) of the potassium permanganate solution using the sodium oxalate (4.13). 4.13 Sodium oxalate Weigh, to the nearest 1 mg, 250 mg to 300 mg of sodium oxalate
30、 into a 300 ml conical flask. Dissolve the salt in approximately 100 ml of water and mix with 30 ml of sulfuric acid (4.10). Heat the solution in a boiling water bath and titrate immediately with the potassium permanganate solution until it turns to a weak pink colour. NOTEAlthough sodium oxalate is
31、 not very hygroscopic it is expedient to dry the salt at 130 C for 1 h prior to use to remove any moisture. Subsequently, the dried salt is cooled to ambient temperature in a desiccator for at least 30 min. 5 Apparatus Usual laboratory equipment and in particular the following: 5.1Water bath 5.2Imme
32、rsion filter, diameter 35 mm, porosity grade P 16 (10 m to 16 m). 5.3Glass filter crucible, porosity grade P 40 (16 m to 40 m). 5.4Electric hot plate 5.5Pipette filler, with a rubber expansion bulb. 5.6Vacuum pump or water jet filter pump 5.7Test sieve with nominal aperture size of 250 m, according
33、to ISO 3310-1. Licensed Copy: sheffieldun sheffieldun, na, Mon Oct 30 01:39:45 GMT+00:00 2006, Uncontrolled Copy, (c) BSI EN 13475:2001 (E) 6 6 Sampling Sampling shall be carried out in accordance with EN 1482. 7 Procedure 7.1 Preparation 7.1.1 Preparation of the test sample Dry the test sample at (
34、105 2) C to constant mass. Record the as-received and dry masses and calculate the moisture content. Grind the sample so that it passes the 250 m sieve (5.7). Mix thoroughly and store the sample in an airtight container. 7.1.2 Preparation of the test solution Weigh to the nearest 0,001 g about 1,0 g
35、 of the test sample (prepared in accordance with 7.1.1) into a 600 ml beaker. NOTEIn the case of materials of low silicic acid content with low amounts of CaO (less than 5 % CaO), the mass of the test portion taken may be increased. Suspend the sample with 100 ml of water and add 25 ml of hydrochlor
36、ic acid (4.2) and 5 ml of nitric acid (4.3). Cover the beaker with a watch glass. Boil gently for 30 min shaking several times and replacing evaporated water. Subsequently cool and transfer the contents of the beaker to a 500 ml volumetric flask. Dilute to the mark with water and mix. Filter through
37、 a dry filter, discarding the initial portion. Store this test solution in a stoppered flask if the determination is not to be carried out immediately. Licensed Copy: sheffieldun sheffieldun, na, Mon Oct 30 01:39:45 GMT+00:00 2006, Uncontrolled Copy, (c) BSI EN 13475:2001 (E) 7 7.2 Determination 7.2
38、.1 Aliquot portion Take an aliquot portion according to Table 1. Table 1 Aliquot portions Expected CaO content % Aliquot ml Volume of burette ml 10 to 30 30 200 100 100 100 10 10 25 50 7.2.2 Titration Place the aliquot portion (7.2.1) into a 400 ml beaker, add 10 ml of citric acid solution (4.4) and
39、 5 ml of ammonium chloride solution (4.5). Heat the solution to boiling, add 10 drops of bromocresol green (4.6) and 30 ml of hot ammonium oxalate solution (4.7), stirring slowly and continuously. Then neutralize with ammonia solution (4.8) under constant stirring until the colour of the indicator c
40、hanges from yellow to blue-green (pH 4,4 to pH 4,6). Allow the beaker to stand on a boiling water bath (5.1) for at least 30 min. Cool and remove the supernatant solution through an immersion filter (5.2). Wash the precipitate with 50 ml of cold ammonium oxalate solution (4.9) and subsequently, thre
41、e times with 50 ml of cold water, sucking off the wash solution each time. Add to the precipitate, without removing the immersion filter, 100 ml of water and subsequently approximately 4 ml of sulfuric acid solution (4.11) and dissolve under heating while blowing twice through the immersion filter b
42、y means of a pipette filler (5.5). Titrate the hot solution (min. 60 C) with potassium permanganate solution (4.12) while blowing air through the immersion filter several times by means of the pipette filler until a lasting pink colour is obtained. 7.2.3 Blank titration Titrate the same amount of wa
43、ter as used in the above titration (see 7.2.2) with the addition of 4 ml of sulfuric acid solution (4.11) but omitting the test solution. Licensed Copy: sheffieldun sheffieldun, na, Mon Oct 30 01:39:45 GMT+00:00 2006, Uncontrolled Copy, (c) BSI EN 13475:2001 (E) 8 8 Expression of results 1 ml of 0,0
44、2 mol/l potassium permanganate solution (4.12) corresponds to 2,002 mg Ca. The calcium content w(CaO), expressed as mass fraction calcium oxide (CaO) in percent, is given by equation (1): m FVV w 02,14)( (CaO) 01? ?(1) where V0is the volume of the potassium permanganate solution (4.12), in millilitr
45、es, used in the blank titration (7.2.3); V1is the volume of the potassium permanganate solution (4.12), in millilitres, used in the titration of the test solution (7.2.2); Fis the amount-of-substance concentration of the potassium permanganate solution (4.12) in moles per litre; mis the mass of the
46、test portion, in grams, contained in the aliquot portion (7.2.1); 14,02is of the molar mass of calcium oxide. The calcium content of the product as received w(CaO)ar is given by equation (2): 100 )100(CaO) (CaO) M ar ww w ? ?(2) where w(CaO)is the calcium content, given as mass fraction calcium oxid
47、e (CaO) in percent, of dry material see equation (1); wMis the moisture content of the test sample (7.1.1), given as mass fraction in percent. To express the results in % Ca use equation (3): 7147, 0)CaO()Ca(? ww (3) 9 Precision 9.1 General The values derived from interlaboratory tests with eight pa
48、rticipating laboratories are shown in 9.2 and 9.3. Licensed Copy: sheffieldun sheffieldun, na, Mon Oct 30 01:39:45 GMT+00:00 2006, Uncontrolled Copy, (c) BSI EN 13475:2001 (E) 9 9.2 Repeatability The absolute difference between two single test results obtained with the same method on identical test
49、material in the same laboratory by the same operator using the same equipment within the shortest feasible time interval will exceed the repeatability limit r in not more than 5 % of cases. The values are r = 0,64 % (mass fraction) for blast furnace slags with w(CaO) = 42,0 %; r = 1,01 % (mass fraction) for converter slags with w(CaO) = 48,6 %. NOTEw(CaO) is the mean mass fraction of calcium oxide. 9.3 Reproducibility The absolute difference between two single test results, obtained with the same method on identical test
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