1、INTERNATIONAL ISO STANDARD 3618 Second edition 1994-12-15 - Photography - Processing chemicals - Specifications for benzotriazole Photographie - Produits chimiques de traitemen t - Specifica tions pour Ie benzo triazole Reference number ISO 3618:1994(E) Foreword ISO (the international Organization f
2、or Standardization) is a worldwide federation of national Standards bodies (ISO member bodies). The work of preparing International Standards is normally carried out through ISO technical committees. Esch member body interested in a subject for which a technical committee has been established has th
3、e right to be represented on that committee. 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 In
4、ternational 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. International Standard ISO 3618 was prepared by Technical Committee lSO/TC 42, Ph
5、otography. This second edition cancels and replaces the first edition (ISO 3618:1976), which has been technically revised. 0 ISO 1994 All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized in any form or by any means, electronie or mechanical, incl
6、uding photocopyrng and microfilm, without Permission in writing from the publisher. International Organization for Standardization Case postale 56 l CH-l 211 Geneve 20 l Switzerland Pnnted in Switzerland ii 0 ISO ISO 3618:1994(E) Introduction 0.1 This International Standard is one of a series that e
7、stablishes criteria 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 and 8 of ISO 10349. This International Standard is intended for use by individuals with a working knowledge of an
8、alytical techniques 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
9、 aprons where appropriate. Normal pre- cautions 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 t
10、hose Steps detailing 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 require- ments for the suitability of a pho
11、tographit-grade 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 process
12、ing solutions, except 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
13、 been made to keep 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 suc
14、h a Chemical is 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
15、serves not only 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 p
16、hysical appearance of the material and any footnotes are for general Information only and are not part of the requirements. Ill ISO 3618:1994(E) 0 ISO 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
17、which require highly specialized equipment 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.
18、Where such techniques have equivalent or greater 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 i
19、n the specification shall prevail. Where a requirement states “to pass test”, however, alternative methods shall not be used. INTERNATIONAL STANDARD o ISO ISO 3618:1994(E) Photography - Processing chemicals - Specifications for benzotriazole 1 Scope This International Standard establishes criteria f
20、or the purity of photographit-grade benzotriazole and speci- fies the tests to be used to determine the purity. 2 Normative references The following Standards contain provisions which, through reference in this text, constitute provisions of this International Standard. At the time of publication, t
21、he editions indicated were valid. All Standards are subject to revision, and Parties to agreements based on this International 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 cu
22、rrently valid International Standards. ISO 565:1990, Test sieves - Metal wire cloth, perforated metal plate and electroformed sheet - Nominal sizes of openings. ISO 10349-1: 1992, Photography - Photographic- grade chemicals - Test methods - Part 7: General. ISO 10349-4: 1992, Photography - Photograp
23、hic- grade chemicals - Test methods - Part 4: Determi- nation of residue after ignition. ISO 10349-8: 1992, Photography - Photographic- grade chemicak - Test methods - Part 8: Determi- na tion of vola tile matter. 3 General 3.1 Physical properties Benzotriazole, C6H5N3, Comes in the form of white to
24、 light-tan needles or powder. lt has a relative molecular mass of 119,13. 3.2 Hazardous properties Benzotriazole is not hazardous when handled with normal precautions. 3.3 Storage Benzotriazole requires no special storage conditions other than a cool, dry environment. 4 Requirements A summary of the
25、 requirements is shown in table 1. Table 1 - Summary of requirements Test Assay Identity Melting Point Mixed melting Point Infrared spectrum Residue after ignition Volatile matter Appearance of Solution NOTE - m/m = mass/mass Limit Subclause International Standard in which test method is given 98 %
26、(/wz) min. 7.1 ISO 3618 101 % (m/m) max. ISO 3618 94 “C to 99 “C 7.2.1 Not lower than Sample or Standard 7.2.1 Match reference spectrum 7.2.2 0,5 % (m/m) max. 7.3 ISO 10349-4 015 % (m/m) max. 7.4 ISO 10349-8 Clear and colourless 7.5 ISO 3618 ISO 3618:1994(E) 0 ISO 5 Reagents and glassware All reagen
27、ts, materials and glassware shall conform to the requirements specified in ISO 10349-1 unless otherwise noted. The hazard warning Symbols used as a reminder in those Steps detailing handling oper- ations are defined in ISO 10349-1. These Symbols are used to provide information to the user and are no
28、t meant to provide conformance with hazardous labelling requirements as these vary from country to country. 6 Sampling See ISO 10349-1. 7 Test methods 7.1 Assay 7.1 .l Specification Content of benzotriazole (C6H5N3) shall be between 98,0 % (m/m) and 101 % ( is the mass, in grams, of the precipitate;
29、 is the conversion factor for the relative mol- ecular mass of benzotriazole (119) equiv- alent to the relative molecular mass of the benzotriazole silver salt (226) x 100 (for percentage). 7.2 Identity tests 7.21 Melting Point 72.1 .l Specifications The melting Point shall be from 94 “C to 99 “C. A
30、 mixed melting Point shall be from 94 “C to 99 “C and shall not be less than either that of the Sample or the Standard. 7.2.1.2. Apparatus 7.2.1.2.1 Capillary-tube melting Point apparatus, complete with thermometer for the range 50 “C to 100 “C. 7.2.1.3 Procedure Prepare three capillary tubes contai
31、ning: a) the Sample to be tested; b) a Sample known to be benzotriazole; c) a finely ground mixture of a) and b) mixed in equal proportions. ldentify the tubes and attach them to the thermometer. Heat the apparatus (7.2.1.2.1) to about 85 “C. Insert the thermometer with the samples attached, and the
32、reafter heat at a constant rate of 2 “C/min. Note the melting Point of each Sample as indicated by the first appearance of Iiquefaction. 7.2.2 Infrared spectrum 7.2.2.1 Specification To pass test. 1) Wazard waming Codes are defined in ISO 10349-1 :1992, clause 4. 3) This Solution tan be prepared fro
33、m concentrated ammonium hydroxide solution, p= 0,91 g/ml (DANGER: ). 3) This Solution tan be prepared from solid silver nitrate (DANGER: ). 2 0 ISO ISO 3618:1994(E) Wave number, cm- 4000 3000 2500 2000 1500 1400 1300 1200 1100 1000 900 800 700 80 60 8 9 Wavelength, Pm Figure 1 - Reference infrared s
34、pectrum of benzotriazole (KBr plate) The infrared absorption curve shall be essentially the same as that of the reference spectrum (figure 1). This optional recommendation is supplementary to that of 7.2.1. 7.2.2.2 Apparatus 7.2.2.2.1 Test sieve, of 63 um aperture size, con- forming to ISO 565. 7.2.
35、2.2.2 Infrared spectrometer, equipped for the 2 um to 16 um regions, and accessory equipment for using potassium bromide plates or mineral oil mull. 7.2.2.3 Procedure Grind about 1 g of the Sample to a homogeneous fine powder and prepare a 0,5 % (m/m) mixture of the Sample in finely ground potassium
36、 bromide. Grind together thoroughly to pass through the test sieve (7.2.2.2.1). Prepare a pressed plate of the mixture containing 0,13 g to 0,16 g of the mixture per Square centimetre. Record the infrared spectrum from 2 um to 16 um. Compare with the reference spectrum given in figure 1. NOTE 1 As a
37、n alternative procedure, the Sample may be ground and dispersed in mineral Oil. lt will then be necess- ary to take into account the absorption bands of the Oil. 7.3 Residue after ignition 7.3.1 Specification Maximum residue after ignition shall be 0,5 % (m/m). 7.3.2 Procedure Determine the percenta
38、ge residue after ignition in accordance with ISO 10349-4. Weigh 2,0 g of the test Sample and ignite in a platinium crucible (600 “C t 50 OC, 4 h, 0,000 1 g)4. 7.4 Volatile matter 7.4.1 Specification Maximum percentage of volatile matter shall be 0,5 % (mlm). 7.4.2 Procedure Determine the percentage
39、of volatile matter at 70 “C in accordance with ISO 10349-8. Weigh 2,0 g of the test Sample and dry in a weighing bottle (70 OC, 1 h, 0,000 1 ,)4). 7.5 Appearance of solution 7.5.1 Specification The Solution shall be clear and colourless. 7.5.2 Procedure Prepare a Solution of 10 g t 0,5 g of the Samp
40、le in 1 litre of water. Examine at 50 “C for clarity and colour. 4) The notation System used for the drying procedure is described in ISO 10349-1:1992, clause 1. This page intentionally left blank This page intentionally left blank This page intentionally left blank This page intentionally left blank ISO 3618:1994(E) 0 ISO ICS 37.040.30 Descriptors: photography, photographic matenals, photographic chemicals, benzotriazole, specifications, matenak specifications, purity criteria, tests, Chemical analysis. Price based on 3 pages
