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1、BRITISH STANDARD BS ISO 422:1994 Implementation of ISO 422:1994 Photography Processing chemicals Specifications for p-methylaminophenol sulfate ICS 37.040.30 Licensed Copy: sheffieldun sheffieldun, na, Sun Nov 26 12:36:13 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS ISO 422:1994 This British Standa
2、rd, having been prepared under the direction of the Consumer Products and Services Sector Board (W/-), was published under the authority of the Standards Board and comes into effect on 15 March 1995 BSI 01-2000 The following BSI references relate to the work on this standard: Committee reference CPM
3、/14 Draft for comment 92/38216 DC ISBN 0 580 23903 9 Committees responsible for this British Standard The preparation of this British Standard was entrusted to Technical Committee CPM/14, Photographic chemicals and processing, upon which the following bodies were represented: British Institute of No
4、n-destructive Testing British Photographic Association Chemical Industries Association Department of the Environment (Water Directorate) Royal Photographic Society Amendments issued since publication Amd. No.DateComments Licensed Copy: sheffieldun sheffieldun, na, Sun Nov 26 12:36:13 GMT+00:00 2006,
5、 Uncontrolled Copy, (c) BSI BS ISO 422:1994 BSI 01-2000i Contents Page Committees responsibleInside front cover National forewordii Forewordiv Text of ISO 4221 Licensed Copy: sheffieldun sheffieldun, na, Sun Nov 26 12:36:13 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS ISO 422:1994 ii BSI 01-2000 Na
6、tional foreword This British Standard reproduces verbatim ISO 422:1994 and implements it as the UK national standard. It supersedes BS 3105:1978 which is withdrawn. This British Standard is published under the direction of the Consumer Products and Services Sector Board whose Technical Committee CPM
7、/14 has the responsibility to: aid enquirers to understand the text; present to the responsible international committee any enquiries on interpretation, or proposals for change, and keep UK interests informed; monitor related international and European developments and promulgate them in the UK. NOT
8、EInternational and European Standards, as well as overseas standards, are available from Customer Services, BSI, 389 Chiswick High Road, London W4 4AL. A British Standard does not purport to include all the necessary provisions of a contract. Users of British Standards are responsible for their corr
9、ect application. 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 and ii, the ISO title page, pages ii to iv, pages 1 to 7 and a back cover. This standard has been upda
10、ted (see copyright date) and may have had amendments incorporated. This will be indicated in the amendment table on the inside front cover. Licensed Copy: sheffieldun sheffieldun, na, Sun Nov 26 12:36:13 GMT+00:00 2006, Uncontrolled Copy, (c) BSI Licensed Copy: sheffieldun sheffieldun, na, Sun Nov 2
11、6 12:36:13 GMT+00:00 2006, Uncontrolled Copy, (c) BSI ISO 422:1994(E) ii BSI 01-2000 Contents Page Forewordiv Introduction1 1Scope1 2Normative references1 3General2 3.1Physical properties2 3.2Hazardous properties2 3.3Handling and storage2 4Requirements2 5Reagents and glassware2 6Sampling2 7Test meth
12、ods3 7.1Assay Cerate titration3 7.1.1Specification3 7.1.2Reagents3 7.1.3Apparatus3 7.1.4Procedure3 7.1.5Expression of results3 7.2Assay Alkali titration3 7.2.1Specification3 7.2.2Reagents3 7.2.3Apparatus3 7.2.4Procedure3 7.2.5Expression of results3 7.3Identity tests4 7.3.1Melting point of nitroso de
13、rivative4 7.3.2Infrared spectrum4 7.4Residue after ignition4 7.4.1Specification4 7.4.2Procedure4 7.5Heavy metals content4 7.5.1Specification4 7.5.2Procedure4 7.6Iron content4 7.6.1Specification4 7.6.2Procedure5 7.7Volatile matter5 7.7.1Specification5 7.7.2Procedure5 7.8p-Aminophenol content5 7.8.1Sp
14、ecification5 7.8.2Reagents5 7.8.3Apparatus5 7.8.4Procedure5 7.9p-Amino-N,N-dimethylaniline sulfate content5 7.9.1Specification5 7.9.2Reagents5 7.9.3Apparatus5 7.9.4Procedure5 Licensed Copy: sheffieldun sheffieldun, na, Sun Nov 26 12:36:13 GMT+00:00 2006, Uncontrolled Copy, (c) BSI ISO 422:1994(E) BS
15、I 01-2000iii Page 7.10Solubility in diethyl ether6 7.10.1 Specification6 7.10.2 Reagent6 7.10.3 Apparatus6 7.10.4 Procedure6 7.10.5 Expression of results6 7.11Appearance of solution6 7.11.1 Specification6 7.11.2 Reagent6 7.11.3 Procedure6 Annex A (informative) Preparation of standard ammonium cerium
16、(IV) hexanitrate solution, c(NH4)2Ce(NO3)6 = 0,100 mol/l (54,82 g/l)7 Figure 1 Reference infrared spectrum of p-methylaminophenol sulfate (KBr plate)6 Table 1 Summary of requirements2 Descriptors: Photography, photographic materials, photographic chemicals, p-methylaminophenol sulphate, specificatio
17、ns, materials specifications, purity criteria, tests, chemicals analysis. Licensed Copy: sheffieldun sheffieldun, na, Sun Nov 26 12:36:13 GMT+00:00 2006, Uncontrolled Copy, (c) BSI ISO 422:1994(E) iv BSI 01-2000 Foreword ISO (the International Organization for Standardization) is a worldwide federat
18、ion of national standards bodies (ISO member bodies). The work of preparing International Standards 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 committe
19、e. International organizations, governmental and non-governmental, in liaison with ISO, also take part in the work. ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization. Draft International Standards adopted by the techn
20、ical 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. International Standard ISO 422 was prepared by Technical Committee ISO/TC 42, Photography. This second edition cancels and
21、replaces the first edition (ISO 422:1976) which has been technically revised. Licensed Copy: sheffieldun sheffieldun, na, Sun Nov 26 12:36:13 GMT+00:00 2006, Uncontrolled Copy, (c) BSI ISO 422:1994(E) BSI 01-20001 Introduction 0.1 This International Standard is one of a series that establishes crite
22、ria of purity for chemicals used in processing photographic materials. General test methods and procedures cited in this International Standard are compiled in parts 1, 4, 5 and 8 of ISO 10349. This International Standard is intended for use by individuals with a working knowledge of analytical tech
23、niques, which may not always be the case. Some of the procedures utilize caustic, toxic or otherwise hazardous chemicals. Safe laboratory practice for the handling of chemicals requires the use of safety glasses or goggles, rubber gloves and other protective apparel such as face masks or aprons wher
24、e appropriate. Normal precautions required in the performance of any chemical procedure are to be exercised at all times but care has been taken to provide warnings for hazardous materials. Hazard warnings designated by a letter enclosed in angle brackets, , are used as a reminder in those steps det
25、ailing handling operations and are defined in ISO 10349-1. More detailed information regarding hazards, handling and use of these chemicals may be available from the manufacturer. 0.2 This International Standard provides chemical and physical requirements for the suitability of a photographic-grade
26、chemical. The tests correlate with undesirable photographic effects. Purity requirements are set as low as possible consistent with these photographic effects. These criteria are considered the minimum requirements necessary to assure sufficient purity for use in photographic processing solutions, e
27、xcept that if the purity of a commonly available grade of chemical exceeds photographic processing requirements and if there is no economic penalty in its use, the purity requirements have been set to take advantage of the availability of the higher-quality material. Every effort has been made to ke
28、ep the number of requirements to a minimum. Inert impurities are limited to amounts which will not unduly reduce the assay. All tests are performed on samples “as received” to reflect the condition of materials furnished for use. Although the ultimate criterion for suitability of such a chemical is
29、its successful performance in an appropriate use test, the shorter, more economical test methods described in this International Standard are generally adequate. Assay procedures have been included in all cases where a satisfactory method is available. An effective assay requirement serves not only
30、as a safeguard of chemical purity but also as a valuable complement to the identity test. Identity tests have been included whenever a possibility exists that another chemical or mixture of chemicals could pass the other tests. All requirements listed in clause 4 are mandatory. The physical appearan
31、ce of the material and any footnotes are for general information only and are not part of the requirements. 0.3 Efforts have been made to employ tests which are capable of being run in any normally equipped laboratory and, wherever possible, to avoid tests which require highly specialized equipment
32、or techniques. Instrumental methods have been specified only as alternative methods or alone in those cases where no other satisfactory method is available. Over the past few years, great improvements have been made in instrumentation for various analyses. Where such techniques have equivalent or gr
33、eater precision, they may be used in place of the tests described in this International Standard. Correlation of such alternative procedures with the given method is the responsibility of the user. In case of disagreement in results, the method called for in the specification shall prevail. Where a
34、requirement states “to pass test”, however, alternative methods shall not be used. 1 Scope This International Standard establishes criteria for the purity of photographic-grade p-methylaminophenol sulfate and specifies the test methods to be used to determine the purity. 2 Normative references The f
35、ollowing International Standards contain provisions which, through reference in this text, constitute provisions of this International Standard. At the time of publication, the editions indicated were valid. All standards are subject to revision, and parties to agreements based on this International
36、 Standard 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 565:1983, Test sieves Woven metal wire cloth, perforated plate and electroformed she
37、et Nominal sizes of openings. Licensed Copy: sheffieldun sheffieldun, na, Sun Nov 26 12:36:13 GMT+00:00 2006, Uncontrolled Copy, (c) BSI ISO 422:1994(E) 2 BSI 01-2000 ISO 10349-1:1992, Photography Photographic-grade chemicals Test methods Part 1: General. ISO 10349-4:1992, Photography Photographic-g
38、rade chemicals Test methods Part 4: Determination of residue after ignition. ISO 10349-5:1992, Photography Photographic-grade chemicals Test methods Part 5: Determination of heavy metals and iron content. ISO 10349-8:1992, Photography Photographic-grade chemicals Test methods Part 8: Determination o
39、f volatile matter. 3 General 3.1 Physical properties p-Methylaminophenol sulfate, HOC6H4NHCH3“H2SO4, exists in the form of a white crystalline powder. It has a relative molecular mass of 172,20. 3.2 Hazardous properties p-Methylaminophenol sulfate is not hazardous when handled with normal precaution
40、s. 3.3 Handling and storage p-Methylaminophenol sulfate shall be stored in a closed container at room temperature. 4 Requirements A summary of the requirements is shown in Table 1. 5 Reagents and glassware All reagents, materials and glassware shall conform to the requirements specified in ISO 10349
41、-1 unless otherwise noted. The hazard warning symbols used as a reminder in those steps detailing handling operations are defined in ISO 10349-1. These symbols are used to provide information to the user and are not meant to provide conformance with hazardous labelling requirements, as these vary fr
42、om country to country. 6 Sampling See ISO 10349-1. Table 1 Summary of requirements TestLimitSubclause International Standard in which test method is given Assay cerate titration or alkali titration Identity melting point of nitroso derivative mixed melting point of nitroso derivative infrared spectr
43、um (optional) Residue after ignition Heavy metals (as Pb) Iron (Fe) Volatile matter p-Aminophenol p-Amino-N,N-dimethylaniline sulfate Solubility in diethyl ether Appearance of solution 99,0 % (m/m) min. 102,0 % (m/m) max. 97,5 % (m/m) min. 130 C to 135 C Not less than sample or standard Equivalent t
44、o Figure 1 0,10 % (m/m) max. 0,002 % (m/m) max. 0,005 % (m/m) max. 0,3 % (m/m) max. 2,5 % (m/m) max. To pass test 0,2 % (m/m) max. Clear and not more than slightly yellow 7.1 7.2 7.3.1 7.3.1 7.3.2 7.4 7.5 7.6 7.7 7.8 7.9 7.10 7.11 ISO 422 ISO 422 ISO 422 ISO 422 ISO 422 ISO 10349-4 ISO 10349-5 ISO 1
45、0349-5 ISO 10349-8 ISO 422 ISO 422 ISO 422 ISO 422 NOTEm/m = mass/mass Licensed Copy: sheffieldun sheffieldun, na, Sun Nov 26 12:36:13 GMT+00:00 2006, Uncontrolled Copy, (c) BSI ISO 422:1994(E) BSI 01-20003 7 Test methods 7.1 Assay Cerate titration 7.1.1 Specification Content of HOC6H4NHCH3“H2SO4 sh
46、all be between 99,0 % (m/m) min. and 102,0 % (m/m) max. 7.1.2 Reagents 7.1.2.1 Ammonium cerium(IV) hexanitrate, (NH4)2Ce(NO3)6, standard volumetric solution of 0,100 mol/l (54,82 g/l)1)2). 7.1.2.2 Iron(II) sulfate solution, 0,025 mol/l (3,80 g/l). Dissolve 4,25 g of FeSO4H2O in 1 litre of water. (Al
47、ternatively 5,60 g of FeSO44H2O, 6,05 g of FeSO45H2O or 6,95 g FeSO47H2O may be used.) 7.1.2.3 Ferroin indicator tris(1,10-phenanthroline) iron(II) ion. Dissolve 1,48 g of 1,10-phenanthroline in 100 ml of the iron(II) sulfate solution (7.1.2.2). 7.1.2.4 Sulfuric acid, H2SO4, 0,050 mol/l (4,9 g/l)1)3
48、)4). 7.1.3 Apparatus 7.1.3.1 Watch glass 7.1.3.2 Burette, of 50 ml capacity. 7.1.4 Procedure Weigh, to the nearest 0,000 1 g, a test portion of about 0,25 g on to a watch glass (7.1.3.1). Transfer the watch glass and test portion to a 250 ml wide-mouth conical flask containing 100 ml of water and 10
49、 ml of the sulfuric acid (7.1.2.4). Dissolve the sample add 3 drops of the ferroin indicator (7.1.2.3) and titrate with the ammonium cerate solution (7.1.2.1) to a light green colour which persists for 15 s. 7.1.5 Expression of results The assay, expressed as a percentage by mass, for p-methylaminophenol sulfate (HOC6H4NHCH3“H2SO4), is given by 7.2 Assay Alkali titration 7.2.1 Specification Content of HOC6H4NHCH3“H2SO4 shall be 97,5 % (m/m) min. 7.2.2 Reagents 7.2.2.1 Acetone, (CH3)2CO. 7.2.2.2 Sodium hydroxide