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1、BRITISH STANDARD BS EN ISO 21078-1:2008 Determination of boron (III) oxide in refractory products Part 1: Determination of total boron (III) oxide in oxidic materials for ceramics, glass and glazes ICS 81.040.01; 81.060.01 ? Licensed Copy: London South Bank University, South Bank University, 16/11/2
2、008 11:27, Uncontrolled Copy, (c) BSI BS EN ISO 21078-1:2008 This British Standard was published under the authority of the Standards Policy and Strategy Committee on 30 September 2008 BSI 2008 ISBN 978 0 580 54934 2 National foreword This British Standard is the UK implementation of EN ISO 21078-1:
3、2008. It supersedes BS 1902-2.3: Addendum No. 1:1976 which is withdrawn. The UK participation in its preparation was entrusted to Technical Committee RPI/1, Refractory products and materials. A list of organizations represented on this committee can be obtained on request to its secretary. This publ
4、ication does not purport to include all the necessary provisions of a contract. Users are responsible for its correct application. Compliance with a British Standard cannot confer immunity from legal obligations. Amendments/corrigenda issued since publication DateComments Licensed Copy: London South
5、 Bank University, South Bank University, 16/11/2008 11:27, Uncontrolled Copy, (c) BSI EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 21078-1 January 2008 ICS 81.040.01; 81.060.01 English Version Determination of boron (III) oxide in refractory products - Part 1: Determination of total boro
6、n (III) oxide in oxidic materials for ceramics, glass and glazes (ISO 21078-1:2008) Dosage de loxyde de bore (III) dans les produits rfractaires - Partie 1: Dtermination de loxyde de bore (III) total dans les matriaux oxydants pour les cramiques, les verres et les maux (ISO 21078-1:2008) Bestimmung
7、des Gehaltes an Bor(III)-oxid in feuerfesten Erzeugnissen - Teil 1: Bestimmung des Gesamtgehaltes an Bor(III)-oxid in oxidischen Werkstoffen fr Keramik, Glas und Glasuren (ISO 21078-1:2008) This European Standard was approved by CEN on 28 December 2007. CEN members are bound to comply with the CEN/C
8、ENELEC 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 bibliographical references concerning such national standards may be obtained on application to the CEN Management Centre or to
9、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 responsibility of a CEN member into its own language and notified to the CEN Management Centre has the same status as the official version
10、s. CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spai
11、n, Sweden, Switzerland and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG Management Centre: rue de Stassart, 36 B-1050 Brussels 2008 CENAll rights of exploitation in any form and by any means reserved worldwide for CEN national M
12、embers. Ref. No. EN ISO 21078-1:2008: E Licensed Copy: London South Bank University, South Bank University, 16/11/2008 11:27, Uncontrolled Copy, (c) BSI Foreword This document (EN ISO 21078-1:2008) has been prepared by Technical Committee ISO/TC 33 “Refractories“ in collaboration with Technical Comm
13、ittee 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 standard, either by publication of an identical text or by endorsement, at the latest by July 2008, and conflicting national standards shall be
14、 withdrawn at the latest by July 2008. Attention is drawn to the possibility that some of the elements of this document may be the 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 Regulatio
15、ns, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlan
16、ds, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and the United Kingdom. Endorsement notice The text of ISO 21078-1:2008 has been approved by CEN as a EN ISO 21078-1:2008 without any modification. BS EN ISO 21078-1:2008 Licensed Copy: London South Bank University
17、, South Bank University, 16/11/2008 11:27, Uncontrolled Copy, (c) BSI Reference number ISO 21078-1:2008(E) INTERNATIONAL STANDARD ISO 21078-1 First edition 2008-01-15 Determination of boron(III) oxide in refractory products Part 1: Determination of total boron(III) oxide in oxidic materials for cera
18、mics, glass and glazes BS EN ISO 21078-1:2008 Licensed Copy: London South Bank University, South Bank University, 16/11/2008 11:27, Uncontrolled Copy, (c) BSI ii Licensed Copy: London South Bank University, South Bank University, 16/11/2008 11:27, Uncontrolled Copy, (c) BSI iii Contents Page Forewor
19、d iv 1 Scope . 1 2 Normative references. 1 3 Terms and definitions. 2 4 Preparation of the test sample 2 5 Number of determinations. 2 6 Determination of boron(III) oxide by alkaline titrimetry 3 7 Determination of boron(III) oxide by azomethine H absorption spectrophotometry. 5 8 Determination of b
20、oron(III) oxide by curcumin absorption spectrophotometry 8 9 Determination of boron(III) oxide by inductively coupled plasma atomic emission spectrometry (ICP-AES). 12 10 Expression of test results 14 11 Test report . 15 Annex A (informative) Interlaboratory test results . 16 BS EN ISO 21078-1:2008
21、Licensed Copy: London South Bank University, South Bank University, 16/11/2008 11:27, Uncontrolled Copy, (c) BSI iv Foreword ISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). The work of preparing International Standa
22、rds is normally carried out through ISO technical committees. 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 liaison with ISO, also tak
23、e 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 2. The main task of technical committees is
24、 to prepare International Standards. Draft International Standards adopted 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 possibilit
25、y that some of the elements of this document may be the subject of patent rights. ISO shall not be held responsible for identifying any or all such patent rights. ISO 21078-1 was prepared by Technical Committee ISO/TC 33, Refractories, in collaboration with Technical Committee CEN/TC 187, Refractory
26、 products and materials. ISO 21078 consists of the following parts, under the general title Determination of boron(III) oxide in refractory products: Part 1: Determination of total boron(III) oxide in oxidic materials for ceramics, glass and glazes Part 2: Acid extraction method for the determinatio
27、n of boron(III) oxide in binder components BS EN ISO 21078-1:2008 Licensed Copy: London South Bank University, South Bank University, 16/11/2008 11:27, Uncontrolled Copy, (c) BSI 1 Determination of boron(III) oxide in refractory products Part 1: Determination of total boron(III) oxide in oxidic mate
28、rials for ceramics, glass and glazes 1 Scope This part of ISO 21078 specifies methods of determining boron(III) oxide in refractory products and raw materials, in mass fractions of 0,01 % or greater. It is applicable to the determination of total boron(III) oxide in oxidic materials for ceramics, gl
29、ass and glazes. The determination of boron(III) oxide is carried out using one of the following four methods: a) alkaline titrimetry, which is applied to samples containing more than 0,5 % by mass of boron(III) oxide; b) azomethine H absorption spectrophotometry, which is applied to samples containi
30、ng from 0,01 % by mass to 2,5 % by mass of boron(III) oxide; c) curcumin absorption spectrophotometry (rothocyanine method), which is applied to samples containing from 0,01 % by mass to 1,0 % by mass of boron(III) oxide; d) inductively coupled plasma atomic emission spectrometry (ICP-AES), which is
31、 applied to samples containing from 0,01 % by mass to 15 % by mass of boron(III) oxide. NOTE 1 The method can be extended to 30 % boron(III) oxide using modified oxidic fluxes. NOTE 2 Interlaboratory test results for this part of ISO 21078 are given in Annex A. 2 Normative references The following r
32、eferenced documents are indispensable for the application of this document. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies. ISO 31-0, Quantities and units Part 0: General principles ISO 83
33、6, Refractories Vocabulary ISO 3310-1, Test sieves Technical requirements and testing Part 1: Test sieves of metal wire cloth ISO 3696, Water for analytical laboratory use Specification and test methods ISO 6353-2, Reagents for chemical analysis Part 2: Specifications First series ISO 6353-3, Reagen
34、ts for chemical analysis Part 3: Specifications Second series BS EN ISO 21078-1:2008 Licensed Copy: London South Bank University, South Bank University, 16/11/2008 11:27, Uncontrolled Copy, (c) BSI 2 3 Terms and definitions For the purposes of this document, the terms and definitions given in ISO 83
35、6 and the following apply. 3.1 dry unshaped refractories dry particles and/or powder of unshaped refractories 3.2 wet unshaped refractories wet particles and/or powder of unshaped refractories with liquid such as mortar and a mixture of refractory-aggregate and pitch or resin 4 Preparation of the te
36、st sample 4.1 Refractory brick or its raw material Carry out sampling in accordance with the contract between the user and producer. Take a specified quantity from a lot of the sample and crush to pass through a 6,7 mm sieve (see ISO 3310-1). Reduce to about 100 g by riffling or coning and quarterin
37、g, then grind all the reduced sample to pass through a 300 m sieve (ISO 3310-1). 4.2 Unshaped refractories Prepare two portions of approximately 100 g each of the sample for analysis (both dry and wet) and crush to pass through a 300 m sieve (see ISO 3310-1) in accordance with the following procedur
38、e. 4.3 Dry unshaped refractories Take one bag or 5 kg of the sample from a lot, reduce to about 100 g as described in 4.1 and crush to pass through a 300 m sieve. 4.4 Wet unshaped refractories Take a specified quantity from the sample and spread on a heat-resistant plate that does not react with the
39、 sample (for example, a polyethylene tetrafluoride plate) to form a charge of 10 mm thickness. Dry the sample in an air-bath or oven at 110C 5C for a minimum of 10 h. Then crush to pass through a 6,7 mm sieve, reduce to about 100 g by riffling or coning and quartering, and grind to pass through a 30
40、0 m sieve (see ISO 3310-1). 4.5 Laboratory sample Reduce the laboratory sample from 4.1 or 4.2 to approximately 25 g by coning and quartering, and grind to pass through a 106 m sieve. This is the test sample for analysis. Transfer it into a container (e.g. a flat weighing bottle (50 mm 30 mm) or sam
41、ple tube (50 mm 25 mm), dry in an oven at 110C 5C for a minimum of 2 h, cool and store it in a desiccator. 4.6 Weighing of test portion Weigh the quantity of the test portion for the chemical analysis specified for the particular procedure, to the nearest 0,1 mg, using an analytical balance and reco
42、rd the actual mass. 5 Number of determinations Carry out simultaneous duplicate determinations. Carry out a blank test on the reagents and make appropriate deductions from the results. BS EN ISO 21078-1:2008 Licensed Copy: London South Bank University, South Bank University, 16/11/2008 11:27, Uncont
43、rolled Copy, (c) BSI 3 6 Determination of boron(III) oxide by alkaline titrimetry 6.1 Principle The sample is fused with sodium hydroxide in a dish placed in a furnace at about 600 C. After cooling, the melt is dissolved in water and the sample solution made up to about 100 ml with water. The interf
44、ering ions left in the sample solution are precipitated by adding calcium carbonate. After first adjusting the pH value to 6,5 with sodium hydroxide solution, mannitol is added and the H+ ions liberated as the result are titrated with sodium hydroxide to obtain a pH value of 6,8. 6.2 Reagents Use on
45、ly reagents of known analytical purity and water conforming to the requirements of grade 2 of ISO 3696 (e.g. double-distilled water). The boron and borate ion concentrations in the water and the reagents shall be negligible compared with the lowest concentration to be determined. All solutions are a
46、queous, unless otherwise specified. 6.2.1 Sodium hydroxide (ISO 6353-2 R 34), assay, minimum mass fraction 98 %. 6.2.2 Hydrochloric acid (concentrated), (ISO 6353-2 R 13), mass fraction 35 %. 6.2.3 Hydrochloric acid (1+1), add 1 volume of hydrochloric acid (concentrated) to 1 volume of water. 6.2.4
47、Calcium carbonate (ISO 6353-3 R 53), assay, minimum mass fraction 99,5 %. 6.2.5 Bromocresol purple solution, C21H16Br2O5S, 1 g/l. Dissolve 0,1 g of bromocresol purple in water and dilute to approximately 100 ml. Keep this solution in the dark at low temperature. 6.2.6 Boron(III) oxide standard solut
48、ion, 0,1 mg B2O3/ml. Transfer approximately 0,5 g of boric acid into a 100 ml beaker, spread it as a thin layer and dry for 24 h in a desiccator. Weigh 0,177 6 g of this dry boric acid and transfer into a 200 ml plastic beaker. Dissolve in approximately 100 ml of water and dilute precisely to 1 000
49、ml in a volumetric flask. 6.2.7 D( )-mannitol, C6H14O6. 6.2.8 Sodium hydroxide standard volumetric solution. Transfer 50 g of sodium hydroxide into a polyethylene bottle, add 50 ml of water, and dissolve with cooling. Allow to stand for several days with a cover, pipette 4,0 ml of the supernatant fraction, and dilute to 2 000 ml in a volumetric flask. Transfer this solution into a polyethylene bottle using a 25 ml automatic filling burette with soda-lim