1、BRITISH STANDARD BS EN 14397-2:2004 Fertilizers and liming materials Determination of carbon dioxide Part 2: Method for liming materials The European Standard EN 14397-2:2004 has the status of a British Standard ICS 65.080 BS EN 14397-2:2004 This British Standard was published under the authority of
2、 the Standards Policy and Strategy Committee on 14 July 2004 BSI 14 July 2004 ISBN 0 580 44086 9 National foreword This British Standard is the official English language version of EN 14397-2:2004. The UK participation in its preparation was entrusted to Technical Committee CII/37, Fertilizers and r
3、elated chemicals, which has the responsibility to: 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 Cat
4、alogue under the section entitled “International Standards Correspondence Index”, or by using the “Search” facility of the BSI Electronic Catalogue or of British Standards Online. This publication does not purport to include all the necessary provisions of a contract. Users are responsible for its c
5、orrect application. Compliance with a British Standard does not of itself confer immunity from legal obligations. aid enquirers to understand the text; present to the responsible international/European committee any enquiries on the interpretation, or proposals for change, and keep the UK interests
6、informed; monitor related international and European 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 10, an inside back cover and a back cover. The BSI copyright notice displayed in this document
7、 indicates when the document was last issued. Amendments issued since publication Amd. No. Date CommentsEUROPEANSTANDARD NORMEEUROPENNE EUROPISCHENORM EN143972 July2004 ICS65.080 Englishversion FertilizersandlimingmaterialsDeterminationofcarbondioxide Part2:Methodforlimingmaterials Engraisetamendeme
8、ntsminrauxbasiques DterminationdelateneurendioxidedecarbonePartie 2:Mthodeapplicableauxamendementsminraux basiques DngemittelundCalcium/Magnesium BodenverbesserungsmittelBestimmungvon KohlenstoffdioxidTeil2:VerfahrenfrCalcium /MagnesiumBodenverbesserungsmittel ThisEuropeanStandardwasapprovedbyCENon1
9、April2004. CENmembersareboundtocomplywiththeCEN/CENELECInternalRegulationswhichstipulatetheconditionsforgivingthisEurope an Standardthestatusofanationalstandardwithoutanyalteration.Uptodatelistsandbibliographicalreferencesconcernings uchnational standardsmaybeobtainedonapplicationtotheCentralSecreta
10、riatortoanyCENmember. ThisEuropeanStandardexistsinthreeofficialversions(English,French,German).Aversioninanyotherlanguagemadebytra nslation undertheresponsibilityofaCENmemberintoitsownlanguageandnotifiedtotheCentralSecretariathasthesamestatusast heofficial versions. CENmembersarethenationalstandards
11、bodiesofAustria,Belgium,Cyprus,CzechRepublic,Denmark,Estonia,Finland,France, Germany,Greece,Hungary,Iceland,Ireland,Italy,Latvia,Lithuania,Luxembourg,Malta,Netherlands,Norway,Poland,Portugal, Slovakia, Slovenia,Spain,Sweden,SwitzerlandandUnitedKingdom. EUROPEANCOMMITTEEFORSTANDARDIZATION COMITEUROPE
12、NDENORMALISATION EUROPISCHESKOMITEEFRNORMUNG ManagementCentre:ruedeStassart,36B1050Brussels 2004CEN Allrightsofexploitationinanyformandbyanymeansreserved worldwideforCENnationalMembers. Ref.No.EN143972:2004:EEN 14397-2:2004 (E) 2 Contents Foreword3 1 Scope 4 2 Normative references 4 3 Terms and defi
13、nitions .4 4 Principle4 5 Reagents.4 6 Apparatus .5 7 Sampling.7 8 Procedure .7 9 Expression of results 8 10 Precision.8 11 Test report 9 Bibliography 10 EN 14397-2:2004 (E) 3 Foreword This document (EN 14397-2:2004) has been prepared by Technical Committee CEN/TC 260 “Fertilizers and liming materia
14、ls”, 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 identical text or by endorsement, at the latest by January 2005, and conflicting national standards shall be withdrawn at the latest by January 2005. EN
15、14397 “Fertilizers and liming materials Determination of carbon dioxide“ consists of two parts: - Part 1: Method for solid fertilizers (prCEN/TS 14397-1) - Part 2: Method for liming materials According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following cou
16、ntries are bound to implement this European Standard: Austria, Belgium, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Slovakia, Slovenia, Spain, Sweden, Switze
17、rland and United Kingdom. EN 14397-2:2004 (E) 4 1 Scope This document specifies a method for the determination of carbon dioxide in all liming materials. 2 Normative references The following referenced documents are indispensable for the application of this document. For dated references, only the e
18、dition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies. EN 1482, Sampling of solid fertilizers and liming materials. EN 12944-3:2001, Fertilizers and liming materials Vocabulary Part 3: Terms relating to liming materials. EN ISO
19、 3696, Water for analytical laboratory use Specification and test methods (ISO 3696:1987). 3 Terms and definitions For the purposes of this document, the terms and definitions given in EN 12944-3:2001 apply. 4 Principle The carbon dioxide contained in liming materials in the form of carbonates is li
20、berated by reaction with hydrochloric acid and determined volumetrically. 5 Reagents 5.1 General During the analysis, unless otherwise stated, use only reagents of recognized analytical grade and water conforming to grade 3 in accordance with EN ISO 3696. 5.2 Concentrated hydrochloric acid, 20(HCl)
21、= 1,18 g/ml to 1,19 g/ml 5.3 Diluted hydrochloric acid, 20(HCl) = 1,09 g/ml Dilute one part by volume of concentrated hydrochloric acid (5.2) with one part by volume of water. 5.4 Concentrated sulfuric acid, 20(H 2 SO 4 ) = 1,84 g/ml 5.5 Sodium sulfate, Na 2 SO 45.6 Sealing liquid Add 20 g of sodium
22、 sulfate (5.5) and 5 ml of concentrated sulfuric acid (5.4) to water and make up to 100 ml. Colour with a few drops of methyl red solution (5.8). The sealing liquid shall be saturated with carbon dioxide. EN 14397-2:2004 (E) 5 5.7 Ethanol, w (C 2 H 5 OH) = 95,6 % (mass fraction) 5.8 Methyl red solut
23、ion Dissolve 0,1 mg of methyl red in 50 ml of ethanol (5.7). Dilute with water up to 100 ml and homogenize. 5.9 Potassium hydroxide solution, w (KOH) = 50 % (mass fraction) 5.10 Calcium carbonate, CaCO 3 , pre-dried to constant mass at 250 C 5.11 Copper sulfate, CuSO 4 5 H 2 O 6 Apparatus 6.1 Appara
24、tus for liberation and determination of carbon dioxide as shown in Figure 1 6.2 Laboratory balance capable of weighing to the nearest 0,0001 g 6.3 Heating device, electrical or gas-burning EN 14397-2:2004 (E) 6 Key 1 Dropping funnel with a volume of 25 ml 2 Stopcock 1 3 Stopcock 2 4 Capillary tubes
25、5 Three-way tap 6 Heated decomposition flask with a volume of 50 ml 7 Absorption vessel with a volume of 100 ml containing KOH solution 8 Measuring burette with a volume of 100 ml 9 Levelling bottle with a volume of 200 ml containing sealing liquid 10 Tube filled with water 11 Heating device Figure
26、1 Apparatus for liberation and determination of carbon dioxide EN 14397-2:2004 (E) 7 7 Sampling Sample the liming material in accordance with EN 1482. 8 Procedure 8.1 Test portion The test portion used depends on the expected carbon dioxide content and shall be chosen according to Table 1. Table 1 T
27、est portion Expected carbon dioxide content mass fraction Test portion g 15 % 50 % 0,1 10 % 15 % 0,3 5 % 10 % 0,5 2 % 5 % 1,0 0 % 2 % 2,0 8.2 Determination Weigh the test portion (8.1) to the nearest 0,1 mg into the decomposition flask. Bond any hydrogen sulfide formed by adding a spatula-tip of cop
28、per sulfate (5.11) and suspend in a little water. Connect the decomposition flask to the rest of the apparatus (see Figure 1) with a double-bored stopper. A dropping funnel and the feed tube to the measuring burette pass through the stopper. Open the stopcocks in these two lines. Bring the three-way
29、 tap to the position such that it connects the flask and measuring burette with one another. Fill the burette with sealing liquid (5.6) up to the three-way tap by raising the levelling bottle. Now close stopcock 1 and fill the funnel with diluted hydrochloric acid (5.3). Add diluted hydrochloric aci
30、d (5.3) to the flask through the dropping funnel until the flask is half full. With stopcock 1 closed a little acid remains as sealing liquid in the funnel. Allow the mixture to react for about 3 min and then heat it to the boiling point and boil for about 3 min. Fill the decomposition flask complet
31、ely with diluted hydrochloric acid (5.3) up to stopcock 2 through the dropping funnel to transfer the remaining gas mixture into the burette. Take care that no diluted hydrochloric acid overflows. Close the burette with the three-way tap. After about 5 min, bring the sealing liquid (5.6) in the bure
32、tte and in the levelling bottle to the same level and record the gas volume V 1 . Turn the three-way tap to connect the measuring burette with the absorption vessel and wash out the air-carbon dioxide-mixture collected. For this, raise the levelling bottle so that all the gas is forced through the p
33、otassium hydroxide solution (5.9) in the absorption vessel. The carbon dioxide is thereby absorbed. Repeat the absorption operation by raising the levelling bottle seven or eight times until, finally, the measuring burette contains only the residual gas. Close the three-way tap, bring the sealing li
34、quid (5.6) in the burette and in the levelling bottle to the same level and record the gas volume V 2 . NOTE The volume difference V 1- V 2corresponds to the carbon dioxide content of the sample. 8.3 Calibration of the apparatus Weigh 0,1 g of calcium carbonate (5.10) to the nearest 0,0001 g into th
35、e decomposition flask (see Figure 1). Carry out the determination as described in 8.2. NOTE The volume difference V 3- V 4corresponds to the carbon dioxide content of the calibration material. EN 14397-2:2004 (E) 8 Calculate the correction factor F 1of the absorption apparatus from equation (1): p V
36、 V T F ) ( 96 , 82 4 3 1 = (1) where T is the measurement temperature, in Kelvins; V 3 is the volume of the gas before absorption related to the calibration material, in millilitres; V 4 is the volume of the gas after absorption related to the calibration material, in millilitres; p is the corrected
37、 barometer reading, in hectopascals. F 1shall be in the range from 1,00 to 1,04. Otherwise the apparatus shall be checked for gas-tightness and proper functioning and the calibration repeated. 9 Expression of results Calculate the carbon dioxide content w CO 2 , given as mass fraction in percent, fr
38、om equation (2): m T p V V F w CO ) ( 053 , 0 2 1 1 2 = (2) where F 1 is the correction factor in accordance with equation (1); V 1 is the volume of the gas before absorption related to the test portion, in millilitres; V 2 is the volume of the gas after absorption related to the test portion, in mi
39、llilitres; p is the corrected barometer reading, in hectopascals. T is the measurement temperature, in Kelvins; m is the mass of the test portion, in grams. If the calibration and determination are carried out directly after one another, the temperature and atmospheric pressure need not be taken int
40、o consideration. For this case, equation (2) is simplified to m V V V V w CO ) ( ) ( 397 , 4 4 3 2 1 2 = (3) 10 Precision 10.1 General The values of the repeatability limit r and the reproducibility limit R are derived from inter-laboratory tests with building lime products in accordance with EN 459
41、-2. EN 14397-2:2004 (E) 9 10.2 Repeatability The absolute difference between two single test results found on identical test material by one operator using the same apparatus within the shortest feasible time interval will exceed the repeatability limit r in not more than 5 % of cases. The repeatabi
42、lity limit r is calculated from r = 2,8 s r , where s ris the repeatability standard deviation. The value of s r is given by the following equation: s r = 0,065 w CO 210.3 Reproducibility The absolute difference between two single test results, obtained with the same method on identical test materia
43、l in different laboratories with different operators using different equipment, will exceed the reproducibility limit R in not more than 5 % of the cases. The reproducibility limit R is calculated from R = 2,8 s R , where s Ris the reproducibility standard deviation. The value of s R is given by the
44、 following equation: s R = 0,09 w CO 211 Test report The test report shall contain at least the following information: a) all data necessary for the complete identification of the sample; b) a reference to this document; c) the results and the units in which the results have been expressed; d) any p
45、articular points observed in the course of the test; e) any operations not specified in the method or regarded as optional which might have affected the results. EN 14397-2:2004 (E) 10 Bibliography EN 196-21, Methods of testing cement Part 21: Determination of the chloride, carbon dioxide and alkali
46、 content of cement. EN 459-2, Building lime Part 2: Test methods VDLUFA, Manual II of analysing methods for fertilisers. (VDLUFA-Verlag, Bismarckstrae 41 A, D-64293 Darmstadt). BS EN 14397-2:2004 BSI 389 Chiswick High Road London W4 4AL BSI British Standards Institution BSI is the independent nation
47、al body responsible for preparing British Standards. It presents the UK view on standards in Europe and at the international level. It is incorporated by Royal Charter. Revisions British Standards are updated by amendment or revision. Users of British Standards should make sure that they possess the
48、 latest amendments or editions. It is the constant aim of BSI to improve the quality of our products and services. We would be grateful if anyone finding an inaccuracy or ambiguity while using this British Standard would inform the Secretary of the technical committee responsible, the identity of which can be found on the inside front cover. Tel: +44 (0)20 8996 9000. Fax: +44 (0)20 8996 7400. BSI offers members an individual updating service called PLUS which ensures that subscribers automatically receive the la
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