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1、BRITISH STANDARD BS 7709-1: 1993 ISO 10136-1: 1993 Analysis of extract solutions of glass Part 1: Method for determination of silicon dioxide by molecular absorption spectrometry UDC 666.11/.18.01.2:543.422:546.284-31 Licensed Copy: London South Bank University, London South Bank University, Fri Dec
2、 08 13:34:02 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 7709-1:1993 This British Standard, having been prepared under the direction of the Laboratory Apparatus Standards Policy Committee, was published under the authority of the Standards Board and comes into effect on 15 September 1993 BSI 11-19
3、99 The following BSI references relate to the work on this standard: Committee reference LBC/36 Draft for comment 90/56734 DC ISBN 0 580 22277 2 Committees responsible for this British Standard The preparation of this British Standard was entrusted by the Laboratory Apparatus Standards Policy Commit
4、tee (LBC/-) to Technical Committee LBC/36, upon which the following bodies were represented: Association for Science Education BLWA Ltd. (The Association of the Laboratory Supply Industry) British Glass Manufacturers Confederation CLEAPSS School Science Service Department of Trade and Industry (Labo
5、ratory of the Government Chemist) Institute of Medical Laboratory Sciences The following body was also represented in the drafting of the standard, through a subcommittee: Society of Glass Technology Amendments issued since publication Amd. No.DateComments Licensed Copy: London South Bank University
6、, London South Bank University, Fri Dec 08 13:34:02 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 7709-1:1993 BSI 11-1999i Contents Page Committees responsibleInside front cover National forewordii Introduction1 1Scope1 2Normative references1 3Definitions2 4Principle2 5Reagents2 6Apparatus3 7Samplin
7、g and samples3 8Procedure4 9Expression of results4 10Test report4 Annex A (informative) Bibliography5 List of referencesInside back cover Licensed Copy: London South Bank University, London South Bank University, Fri Dec 08 13:34:02 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 7709-1:1993 ii BSI 11
8、-1999 National foreword This Part of BS 7709 has been prepared under the direction of the Laboratory Apparatus Standards Policy Committee and is identical with ISO 10136-1:1993 Glass and glassware Analysis of extract solutions Part 1: Determination of silicon dioxide by molecular absorption spectrom
9、etry, published by the International Organization for Standardization (ISO). ISO 10136-1 has been prepared by Subcommittee 5 of Technical Committee ISO/TC 48, with the active participation and approval of the UK. BS 7709 is published in six Parts as follows: Part 1: Method for determination of silic
10、on dioxide by molecular absorption spectrometry; Part 2: Method for determination of sodium oxide and potassium oxide by flame spectrometric methods; Part 3: Method for determination of calcium oxide and magnesium oxide by flame atomic absorption spectrometry; Part 4: Method for determination of alu
11、minium oxide by molecular absorption spectrometry; Part 5: Method for determination of iron(III) oxide by molecular absorption spectrometry and flame atomic absorption spectrometry; Part 6: Method for determination of boron(III) oxide by molecular absorption spectrometry. BS 2649 Methods for analysi
12、s of glass Part 1:1988 Glasses of the soda-lime-magnesia-silica type and Part 3:1988 Glasses of the potassium oxide-lead oxide-silica type describe methods of determination primarily of the gravimetric type. The methods given in BS 7709 should be considered complementary to those of BS 2649. The Tec
13、hnical Committee has reviewed the provisions of ISO 385-2, ISO 648, ISO 835-3, ISO 6955 and ISO 7056, to which normative reference is made in the text, and has decided that they are acceptable for use in conjunction with this standard. Cross-references International StandardCorresponding British Sta
14、ndard BS 700 Graduated pipettes ISO 835-1:1981Part 1:1982 Specification for general requirements (Identical) ISO 835-2:1981Part 2:1982 Specification for pipettes for which no waiting time is specified (Identical) ISO 1042:1983BS 1792:1982 Specification for one-mark volumetric flasks (Identical) ISO
15、3585:1991BS 2598 Glass plant, pipeline and fittings Part 1:1991 Specification for properties of borosilicate glass 3.3 (Identical) ISO 3696:1987BS 3978:1987 Specification for water for laboratory use (Identical) ISO 3819:1985BS 6523:1984 Specification for glass beakers for laboratory use (Technicall
16、y equivalent) Licensed Copy: London South Bank University, London South Bank University, Fri Dec 08 13:34:02 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 7709-1:1993 BSI 11-1999iii This British Standard describes a method of test only and should not be used or quoted as a specification defining lim
17、its of performance. Reference to this British Standard should indicate that the method of test used is in accordance with BS 7709-1:1993. A British Standard does not purport to include all the necessary provisions of a contract. Users of British Standards are responsible for their correct applicatio
18、n. Compliance with a British Standard does not of itself confer immunity from legal obligations. Summary of pages This document comprises a front cover, an inside front cover, pages i to iv, pages 1 to 6, an inside back cover and a back cover. This standard has been updated (see copyright date) and
19、may have had amendments incorporated. This will be indicated in the amendment table on the inside front cover. Licensed Copy: London South Bank University, London South Bank University, Fri Dec 08 13:34:02 GMT+00:00 2006, Uncontrolled Copy, (c) BSI iv blank Licensed Copy: London South Bank Universit
20、y, London South Bank University, Fri Dec 08 13:34:02 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 7709-1:1993 BSI 11-19991 Introduction The determination of silica (SiO2) in durability extract solutions has not, hitherto, been included in classifications of glass or glassware according to chemical
21、resistance. Indeed, in many applications the concentrations of silica found in such extract solutions, normally very low, are not significant and are of little interest. There are occasions where such releases could be important, for example from glassware used in the determination of small concentr
22、ations of silica in solutions or, in some cases, releases from medical and pharmaceutical ware. Then again, in examining the properties of new glass compositions it could be an advantage to know the full analysis of the durability extract solutions. Technical Committee 2, Chemical Durability and Ana
23、lysis, of the International Commission on Glass (ICG), investigated two procedures for determining silica (see 6 in Annex A) by the molecular absorption spectrometric technique. Both were based on the formation of colour complexes in the presence of ammonium molybdate, one using the yellow colour of
24、 the complex formed, the other using the blue colour produced when a suitable reducing agent is added. In collaborative experimental work, twelve laboratories analysed silica in two synthetic solutions and in extract solutions produced by the test described in ISO 480234. It was agreed that whilst d
25、eterminations using the yellow complex were more consistent, they were also less sensitive and, since the concentrations of silica in extract solutions are normally very low, the blue complex method was preferred. The results of investigations on turbidities, especially in grain test solutions, show
26、ed that acidification to dissolve possible hydroxides and/or carbonates is necessary prior to the analytical determination. This is achieved by using spectroscopic buffer solutions, which are normally strongly acidic, or by addition of acids. 1 Scope This part of ISO 10136 specifies an analytical pr
27、ocedure, using molecular absorption spectrometry, for measuring the concentrations of silicon, expressed as silicon dioxide or silica (SiO2), released into extract solutions during hydrolytic resistance test procedures. This part of ISO 10136 applies to the analysis of extract solutions obtained fro
28、m any kind of glass or glassware, including laboratory and pharmaceutical ware made, for example, from borosilicate glass (such as borosilicate glass 3.3 according to ISO 3585), neutral glass, or soda-lime-silica glass as defined in ISO 480234, food and drink packaging ware, tableware and kitchenwar
29、e. The extract solution may be obtained from glass articles, for example according to ISO 4802, or from glass as material, for example when tested according to ISO 7191 or ISO 7202. In addition, it may be applied to the extract solutions produced by any method for measuring the hydrolytic resistance
30、 of glass or glassware. 2 Normative references The following standards contain provisions which, through reference in this text, constitute provisions of this part of ISO 10136. At the time of publication, the editions indicated were valid. All standards are subject to revision, and parties to agree
31、ments based on this part of ISO 10136 are encouraged to investigate the possibility of applying the most recent editions of the standards indicated below. Members of IEC and ISO maintain registers of currently valid International Standards. ISO 385-2:1984, Laboratory glassware Burettes Part 2: Buret
32、tes for which no waiting time is specified. ISO 648:1977, Laboratory glassware One-mark pipettes. ISO 835-1:1981, Laboratory glassware Graduated pipettes Part 1: General requirements. ISO 835-2:1981, Laboratory glassware Graduated pipettes Part 2: Pipettes for which no waiting time is specified. ISO
33、 835-3:1981, Laboratory glassware Graduated pipettes Part 3: Pipettes for which a waiting time of 15 s is specified. ISO 1042:1983, Laboratory glassware One-mark volumetric flasks. ISO 3585:1991, Borosilicate glass 3.3 Properties. ISO 3696:1987, Water for analytical laboratory use Specification and
34、test methods. ISO 3819:1985, Laboratory glassware Beakers. ISO 6955:1982, Analytical spectroscopic methods Flame emission, atomic absorption, and atomic fluorescence Vocabulary. ISO 7056:1981, Plastics laboratory ware Beakers. Licensed Copy: London South Bank University, London South Bank University
35、, Fri Dec 08 13:34:02 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 7709-1:1993 2 BSI 11-1999 3 Definitions For the purposes of this part of ISO 10136, the following definitions apply. 3.1 extract solution the aqueous solution obtained from the reaction of glass with water under specific conditions
36、3.2 sample measuring solution the solution actually used for measuring the concentration of the analyte. It may be the undiluted, diluted or modified extract solution 3.3 analyte the element or constituent to be determined 3.4 stock solution a solution of appropriate composition containing the analy
37、te, expressed as its oxide, in a known but high concentration 3.5 standard solution a solution containing the analyte, expressed as its oxide, in a known concentration suitable for the preparation of reference or calibration solutions 3.6 set of calibration solutions; set of reference solutions a se
38、t of simple or synthetic reference solutions having different analyte concentrations. The zero member is, in principle, the solution having zero concentration of the analyte ISO 6955 3.7 molecular absorption spectrometry (MAS) a technique for determining the concentration of an analyte in solution b
39、y measuring the optical density of a colour complex of the analyte 3.8 blank test solution a solution prepared in the same way as the sample measuring solution but so that it does not contain the analyte to be determined 4 Principle Conditioning of the extract solution to be analysed and developing
40、of the blue silicomolybdate complex using ammonium molybdate and a reducing solution. Measurement of the optical density of the colour complex, when measuring the sample measuring solution, by means of a molecular absorption spectrometer at 800 nm using 10 mm optical cells. 5 Reagents During the ana
41、lysis, unless otherwise stated, use only reagents of recognized analytical grade, and grade 1 or grade 2 water as specified in ISO 3696. When acids and ammonium hydroxide are specified only by name or chemical formula, the concentrated reagent is intended. The concentrations of diluted acids or ammo
42、nium hydroxide are specified as a ratio, stating the number of volumes of the concentrated reagent to be added to a given number of volumes or water. For example, 1 + 3 means that 1 volume of the concentrated reagent shall be diluted with 3 volumes of water. Commercially available standard solutions
43、 for spectrometry may be used for the preparation of the stock or standard solutions. 5.1 4-Amino-3-hydroxynaphthalene-1-sulfonic acid or 1-amino-2-hydroxynaphthalene-4-sulfonic acid NH2C10H5(OH)SO3H 5.2 Ammonium molybdate (NH4)6Mo7O24.4H2O, 60 g/l aqueous solution. 5.3 Boric acid (H3BO3), 50 g/l so
44、lution. 5.4 2,4-Dinitrophenol 2,4-(NO2)2C6H3OH, 1 g/l indicator solution. 5.5 Hydrochloric acid (HCl), = 1,19 g/ml. 5.5.1 Hydrochloric acid, diluted 1 + 5. 5.5.2 Hydrochloric acid, diluted 1 + 24. 5.6 Hydrofluoric acid (HF) solution, = 1,13 g/ml. 5.7 Reducing solution Dissolve 0,7 g of sodium sulfit
45、e (5.15) in 20 ml of water, add 0,15 g of 4-amino-3-hydroxynaphthalene-1-sulfonic acid or 1-amino-2-hydroxynaphthalene-4-sulfonic acid (5.1) and stir to dissolve. Dissolve 9 g of sodium metabisulfite (5.14) in 160 ml of water and transfer both solutions to the same 200 ml one-mark volumetric flask (
46、6.7). Make up to the mark and mix. This solution shall be discarded if the faintest blue coloration appears. Licensed Copy: London South Bank University, London South Bank University, Fri Dec 08 13:34:02 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 7709-1:1993 BSI 11-19993 5.8 Silicon dioxide (also
47、 called silica) (SiO2). Use finely ground silica sand containing at least 99,9 % (m/m) SiO2, dried at 110 C at least. 5.9 Silica, stock solution. Weigh, to the nearest 0,1 mg, about 1 g of silica (5.8) into a platinum dish (6.6). Add 4,5 g of sodium carbonate (5.11) and intimately mix using a dry ro
48、d (do not use a glass rod). Ease the mixture into the centre of the dish and flatten it to cover an area of diameter about 30 mm. Cover the mixture as evenly as possible with a further 0,5 g of sodium carbonate (5.11), then gently brush any particles adhering to the rod into the dish. Cover the dish
49、 with a platinum lid (6.6) and place it in a muffle furnace at 300 C to 400 C. Gradually increase the temperature to 1 100 C and maintain this for about 10 min or until fusion is complete. Remove the dish from the furnace and gently swirl the melt to incorporate any remaining particles. Allow to cool, wash any material adhering to the underside of the lid into the dish using hot water, then dissolve the fused mass in hot water. Cool, transfer the solution to a 1 000 ml one-mark volumetric flask (6.