DIN EN ISO 14719-2012 Chemical analysis of refractory material glass and glazes - Determination of Fe and Fe by the spectral photometric method with 1 10-phenanthroline (ISO 14719 .pdf

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1、March 2012 Translation by DIN-Sprachendienst.English price group 11No part of this translation may be reproduced without prior permission ofDIN Deutsches Institut fr Normung e. V., Berlin. Beuth Verlag GmbH, 10772 Berlin, Germany,has the exclusive right of sale for German Standards (DIN-Normen).ICS

2、81.040.10; 81.060.10; 81.080!$zDp“1873377www.din.deDDIN EN ISO 14719Chemische Analyse von feuerfestem Werkstoff, Glas und Glasuren Spektralphotometrische Bestimmung von Fe und Fe2+ 3+ mit1,10-Phenanthrolin (ISO 14719:2011)Englische bersetzung von DIN EN ISO 14719:2012-03Analyse chimique de matriaux

3、rfractaires, du verre et dmaux Dosage de Fe2+ et Fe par la mthode spectrophotomtrique en3+utilisant la 1,10-phnanthroline (ISO 14719:2011)Traduction anglaise de DIN EN ISO 14719:2012-03SupersedesDIN 51087-1:2005-06www.beuth.deDocument comprises pagesIn case of doubt, the German-language original sha

4、ll be considered authoritative.Chemical analysis of refractory material glass and glazes Determination of Fe2+and Fe3+by the spectral photometric method with 1,10-phenanthroline (ISO 14719:2011) English translation of DIN EN ISO 14719:2012-03 1802.12 DIN EN ISO 14719:2012-03 2 A comma is used as the

5、 decimal marker. National foreword This standard has been prepared by Technical Committee CEN/TC 33 “Refractories” in collaboration with Technical Committee CEN/TC 187 “Refractory products and materials” (Secretariat: BSI, United Kingdom). The responsible German body involved in its preparation was

6、the Normenausschuss Materialprfung (Materials Testing Standards Committee), Working Committee NA 062-02-61 AA Chemische Analyse von oxidischen Roh- und Werkstoffen. The DIN Standards corresponding to the International Standards referred to in this document are as follows: ISO 648 DIN EN ISO 648 ISO

7、1042 DIN EN ISO 1042 ISO 3696 DIN ISO 3696 ISO 12677 DIN EN ISO 12677 ISO 26845 DIN EN ISO 26845 Amendments This standard differs from DIN 51087-1:2005-06 as follows: a) a second method (Method A) has been included. In Method A, ten times more sample is necessary than for Method B;b) the standard ha

8、s been editorially revised. Previous editions DIN 51087-1: 2005-06 National Annex NA (informative) Bibliography DIN EN ISO 648, Laboratory glassware Single-volume pipettes DIN EN ISO 1042, Laboratory glassware One-mark volumetric flasks DIN EN ISO 12677, Chemical analysis of refractory products by X

9、-ray fluorescence (XRF) Fused cast-bead method DIN EN ISO 26845, Chemical analysis of refractories General requirements for wet chemical analysis, atomic absorption spectrometry (AAS) and inductively coupled plasma atomic emission spectrometry (ICP-AES) methods DIN ISO 3696, Water for analytical lab

10、oratory use Specification and test methods EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 14719 December 2011 ICS 81.080; 81.060.01; 81.040.01 English Version This European Standard was approved by CEN on 30 November 2011. CEN members are bound to comply with the CEN/CENELEC Internal Regul

11、ations 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 CEN-CENELEC Management Centre or to any CEN membe

12、r. This 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 CEN-CENELEC Management Centre has the same status as the official versions. CE

13、N members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia,

14、Spain, Sweden, Switzerland and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG Management Centre: Avenue Marnix 17, B-1000 Brussels 2011 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN nationa

15、l Members. Ref. No. EN ISO 14719:2011: EChemical analysis of refractory material glass and glazes - Determination of Fe2+and Fe3+by the spectral photometric method with 1,10-phenanthroline (ISO 14719:2011) Analyse chimique de matriaux rfractaires, du verre et dmaux - Dosage de Fe2+et Fe3+par la mtho

16、de spectrophotomtrique en utilisant la 1,10-phnanthroline (ISO 14719:2011) Chemische Analyse von feuerfestem Werkstoff, Glas und Glasuren - Spektralphotometrische Bestimmung von Fe2+und Fe3+mit 1,10-Phenanthrolin (ISO 14719:2011) Contents DIN EN ISO 14719:2012-03 EN ISO 14719:2011 (E) Page Foreword

17、3 1 Scope 4 2 Normative references 4 3 Terms and definitions .4 4 Principle of Methods A and B .5 5 Sample preparation .5 6 Interferences 5 7 Sample disintegration and measurement .5 8 Calculation and expression of results .12 9 Test report 13 Annex A (informative) Precision 14 Bibliography 16 2 For

18、eword This document (EN ISO 14719:2011) has been prepared by Technical Committee ISO/TC 33 “Refractories” in collaboration with Technical Committee CEN/TC 187 “Refractory products and materials” the secretariat of which is held by BSI. This European Standard shall be given the status of a national s

19、tandard, either by publication of an identical text or by endorsement, at the latest by June 2012, and conflicting national standards shall be withdrawn at the latest by June 2012. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. C

20、EN 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, Belgium, Bulgaria, Croatia, Cyprus

21、, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and the United Kingdom. Endorsement notice The text of ISO 1471

22、9:2011 has been approved by CEN as a EN ISO 14719:2011 without any modification. DIN EN ISO 14719:2012-03 EN ISO 14719:2011 (E) 3 1 Scope This International Standard specifies a spectral photometric method with 1,10-phenanthroline for the quantitative determination of Fe2and Fe3in oxidic raw and bas

23、ic materials for ceramics, glass and glazes, e.g. feldspar, kaolinites, clay, limestone, quartz refractory materials. This International Standard could be extended to other aluminosilicate materials, providing that uncertainty data is produced to support it. However, there might be problems in the d

24、ecomposition of high-purity alumina and chrome ore samples. The method is not suitable for reduced materials, such as silicon carbide, graphite-magnesia, etc. 2 Normative references The following referenced documents are indispensable for the application of this document. For dated references, only

25、the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies. ISO 648, Laboratory glassware Single-volume pipettes ISO 1042, Laboratory glassware One-mark volumetric flasks ISO 3696, Water for analytical laboratory use Specificat

26、ion and test methods ISO 5022, Shaped refractory products Sampling and acceptance testing ISO 6286, Molecular absorption spectrometry Vocabulary General Apparatus ISO 8656-1, Refractory products Sampling of raw materials and unshaped products Part 1: Sampling scheme ISO 10725, Acceptance sampling pl

27、ans and procedures for the inspection of bulk materials ISO 11648-2, Statistical aspects of sampling from bulk materials Part 2: Sampling of particulate materials ISO 12677, Chemical analysis of refractory products by X-ray fluorescence (XRF) Fused cast-bead method ISO 26845, Chemical analysis of re

28、fractories General requirements for wet chemical analysis, atomic absorption spectrometry (AAS) and inductively coupled plasma atomic emission spectrometry (ICP-AES) methods 3 Terms and definitions For the purposes of this document, the terms and definitions given in ISO 26845 apply. DIN EN ISO 1471

29、9:2012-03 EN ISO 14719:2011 (E) 4 4 Principle of Methods A and B Samples are digested in a mixture of hydrofluoric acid and sulfuric acid. In the presence of a complexing agent, 1,10-phenanthroline, Fe2ions form a pink complex. The pink complex is measured photometrically at 510 nm in an aqueous sol

30、ution. Quantitative results are obtained by calibration with reference solutions. The sum of the determination of both iron species corresponds to the total iron content. This International Standard provides two sample dissolution techniquesI. In Method A, ten times more sample (500 mg) is necessary

31、 than for Method B (20 mg to 30 mg). As a consequence, the amount of reagents needed are reduced for Method B. In both methods, a HF-H2SO4dissolution of the sample is carried out. Methods A and B implement different strategies to avoid oxidation of Fe2to Fe3during the sample dissolution and measurem

32、ent: while in Method A the samples react in an air- and light-tight reaction vessel with nitrogen, in Method B the solution is stabilized with nitrilotriacetic acid in simple polystyrene cuvettes cooled by ice. Both methods are applicable for the full range of materials covered by the scope of this

33、International Standard. For samples which appear more heterogeneous, a higher sample mass for the preparation may lead to more reproducible results. In this case, Method A shall be applied. 5 Sample preparation The sampling shall be performed in accordance with ISO 5022 or ISO 8656-1 with reference,

34、 where appropriate, to ISO 10725 and ISO 11648-2. The sample shall be ground to a particle size less than 63 m and stored afterwards in a stoppered sample bottle in a desiccator. The samples shall be dried to constant mass at 110 C before the determination of Fe2/Fe3. Weigh precisely the correct sam

35、ple amount for the dissolution. NOTE The drying of samples will not change the Fe2content in almost all refractory materials; the moisture content might vary with time. 6 Interferences Interferences in the determination of Fe2/Fe3can be caused by other polyvalent ions, e.g. As5/As3, Sb5/Sb3, etc. Th

36、e formation of an insoluble precipitate, e.g. lead and barium sulfate, may also interfere in the determination. 7 Sample disintegration and measurement 7.1 Method A 7.1.1 Reagents Reagents of a recognized analytical grade shall be used for this analysis. 7.1.1.1 Water, according to ISO 3696, at leas

37、t of Grade 2. 7.1.1.2 Sulfuric acid, H2SO4, 1,84 g/cm3. 7.1.1.3 Sulfuric acid (1 1). DIN EN ISO 14719:2012-03 EN ISO 14719:2011 (E) 5 7.1.1.4 Hydrofluoric acid, HF, 1,13 g/cm3. 7.1.1.5 Hydrofluoric acid, without reducing agents. Transfer 50 ml of hydrofluoric acid (7.1.1.4) into a platinum dish. Add

38、 one drop of 0,02 mol/l KMnO4(7.1.1.15) solution. Heat on a steam bath until the permanganate is reduced. Cool for use and store in a polyethylene bottle. 7.1.1.6 Boric acid solution. Add 90 g of boric acid (H3BO3) to 1 800 ml of water. 7.1.1.7 Hydroxylammonium chloride, NH2OH.HCl (100 g/l). 7.1.1.8

39、 1,10-Phenanthroline solution (5 g/l). 7.1.1.9 Ammonium acetate, CH3COONH4(approximately 50 % by mass). Dissolve 50 g of ammonium acetate in 50 ml of water. 7.1.1.10 Ammonium iron(II) sulfate hexahydrate, Fe(NH4)2(SO4)26H2O. 7.1.1.10.1 Iron stock solution (1 ml 1 mg Fe). Weigh 3,510 8 g of ammonium

40、iron(II) sulfate hexahydrate Fe(NH4)2(SO4)26H2O (7.1.1.10) and transfer to a 500 ml volumetric flask. Dissolve in water, add 8 ml to 10 ml of hydrochloric acid ( 1,19 g/cm3), dilute to volume and mix. 7.1.1.10.2 Iron standard solution (1 ml 0,01 mg Fe). Dilute 10 ml of the iron stock solution to 1 0

41、00 ml in a volumetric flask with deionized water. 7.1.1.11 Nitrogen gas, white spot (high quality). The gas cylinder should be provided with a two-stage reducing valve and a gas-flow regulator for a flow rate of 28 l/h to 280 l/h. 7.1.1.12 Hydrochloric acid, HCl, 1,19 g/cm3. 7.1.1.13 Hydrochloric ac

42、id (1 4). 7.1.1.14 Hydrochloric acid (1 12). 7.1.1.15 Potassium permanganate solution, KMnO4, 0,02 mol/l (3,160 64 g/l). 7.1.2 Apparatus For solutions that do not contain hydrofluoric acid, ordinary laboratory apparatus and the usual laboratory glassware made from borosilicate glass and complying wi

43、th the requirements of relevant International Standards shall be used. For solutions containing hydrofluoric acid or any acidic fluoride, plastic apparatus shall be used. Graduated plastic graduated flasks shall be used for sample stock solutions and calibration standards, etc. Beakers, storing bott

44、les, volumetric flasks and pipettes shall be prepared by filling them to 90 % of the overflow capacity with hydrochloric acid (7.1.1.14) overnight. After the soaking, they shall be washed thoroughly with water. DIN EN ISO 14719:2012-03 EN ISO 14719:2011 (E) 6 7.1.2.1 Analytical balance, capable of r

45、eading to the nearest 0,1 mg. 7.1.2.2 Volumetric flasks, complying with the requirements of class A in ISO 1042. 7.1.2.3 Pipettes, of suitable capacities complying with the requirements of class A in ISO 648. 7.1.2.4 Magnetic stirrer. 7.1.2.5 Molecular absorption spectrometer, conforming to the requ

46、irements of ISO 6286. 7.1.2.6 Optical cells, as recommended by the spectrometer manufacturer. 7.1.2.7 Hotplate. 7.1.2.8 Reaction vessel. Plastic or polytetrafluoroethylene (PTFE) bottle or beaker of 250 ml capacity. The vessel will be used to exclude air (oxygen) when reacting the sample with the re

47、agents. The vessel can be fitted with a rubber stopper, as shown in Figure 1, or the vessel can be a beaker with the lip removed and the bottom of another container placed on top, with the appropriate openings for introduction of purge gas, reagents, and vent tubing. In order to exclude light, the v

48、essel shall be covered with black paint on the surface. The vessel comprises the components described in 7.1.2.8.1 to 7.1.2.8.5. 7.1.2.8.1 Plastic or TFE-fluorocarbon bottle or beaker, of 250 ml capacity. 7.1.2.8.2 Plastic tube, used to introduce the purge gas into the vessel. It is advisable to use a connection between the plastic tubing and the gas cylinder that will allow it to be easily connected and disconnected. 7.1.2.8.3 Plastic powder funnel, that allows fo