1、INTERNATIONAL STANDARD ISO 3617 Second edition 1994-12-15 Photography - Processing chemicals - Specifications for sodium hydroxide Photographie - Produits Ihydroxyde de sodium chimiques de traitemen t - Spkifica tions pour Reference number ISO 3617:1994(E) ISO 3617:1994(E) Foreword ISO (the Internat
2、ional Organization for Standardization) is federation of national Standards bodies (ISO member bodies) preparing International Standards is normally carried out technical committees. Esch member body interested in a sub a worldwide . The work of through ISO ject for which a technicai committee has b
3、een established has the 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 sta
4、ndardization. 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. International Standard ISO 3617 was prepared by Technical C
5、ommittee ISO/TC 42, Photography. This second edition cancels and replaces the first edition (ISO 3617:1976), which has been technically revised. Annex A of this International Standard is for information only. 0 ISO 1994 All rights reserved. Unless otherwise specified, no part of this publication may
6、 be reproduced or utilized in any form or by any means, electronie or mechanical, including photocopying and mrcrofilm, without Permission in writing from the publisher. International Case postale Organization for Standardization 56 l CH-l 211 Geneve 20 l Swit Printed in Switzerland 0 ISO ISO 3617:1
7、994(E) Introduction 0.1 This International Standard is one of a series that establishes 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, 5, 6 and 7 of ISO 10349. This Internat
8、ional Standard is intended for use by individuals with a working knowledge of analytical 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 glas
9、ses or goggles, rubber gloves and other protective apparel such as face masks or 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
10、designated by a letter enclosed in angle brackets, c, are used as a reminder in those 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 St
11、andard provides Chemical and physical require- ments for the suitability of a photographit-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 r
12、equirements necessary to assure sufficient purity for use in photographic processing 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 ta
13、ke advantage of the availability of the higher-quality material. Every effort has 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 ma
14、terials furnished for use. Although the ultimate criterion for suitability of such 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 al
15、l cases where a satisfactory method is available. An effective assay requirement 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 cou
16、ld pass the other tests. All requirements listed in clause 4 are mandatory. The physical appearance of the material and any footnotes are for general Information only and are not part 0% the requirements. ISO 3617:1994(E) 0 ISO 0.3 Efforts have been made to employ tests which are capable of being ru
17、n in any normally equipped laboratory and, wherever possible, to avoid tests 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
18、, great improvements have been made in instrumentation for various analyses. 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 responsibi
19、lity of the User. In case of disagreement in results, the method called for in the specification shall prevail. Where a requirement states “to pass test”, however, alternative methods shall not be used. INTERNATIONAL STANDARD o ISO ISO 3617:1994(E) Photography - Processing chemicals - Specifications
20、 for sodium hydroxide 1 Scope This International Standard establishes criteria for the purity of photographit-grade sodium hydroxide (DANGER: )l) and specifies the tests to be used to determine the purity. 2 Normative references The following Standards contain provisions which, through reference in
21、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 Standard are encouraged to investigate the possibility of applying the most rec
22、ent editions of the Standards indicated below. Members of IEC and ISO maintain registers of currently valid International Standards. ISO 10349-1: 1992, Photography - Photographic- grade chemicals - Test methods - Part 1: General. ISO 10349-5: 1992, Photography - Photographic- grade chemicals - Test
23、methods - Part 5: Determi- nation of heavy metals and iron content. ISO 10349-6: 1992, Photography - Photographic- grade chemicals - Test methods - Part 6: Determi- nation of halide con tent. ISO 10349-7: 1992, Photography - Photographic- grade chemicals - Test methods - Part 7: Determi- nation of a
24、lkalinity or acidity. 3 General 3.1 Physical properties Sodium hydroxide, NaOH, exists in the form of white sticks, pellets, flakes, granules or powder. lt has a relative molecular mass of 40,OO. 3.2 Hazardous properties Sodium hydroxide is corrosive (DANGER:). Avoid contact with eyes, skin and clot
25、hing. Avoid breathing dust. Refer to the manufacturers Material Safety Data Sheet (MSDS) for additional information. 3.3 Handling and storage Sodium hydroxide shall be stored in a properly labelled and tightly sealed plastic Container. Sodium hydroxide readily absorbs moisture with the liberation of
26、 heat and reacts violently with acids. 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 10349-1 unless otherwise noted. The hazard warning Symbols used as a reminder in
27、those Steps detailing handling oper- ations 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 from country to country. 6 Sampling See ISO 10349-1. 7 Test methods 7.1 Assay
28、 7.1.1 Specification Content of NaOH sha II be 95,0 % (m/m ) min 1) Hazard warning Codes are defined in ISO 10349-1:1992, clause 4. ISO 3617:1994(E) 0 ISO Table 1 - Summary of requirements Test Assay (as NaOH) Heavy metals (as Pb) Iran (Fe) Halides (as Cl-) Carbonate (as Na V is the volume, in milli
29、litres, of the hydrochloric acid used to resch the titration endpoint (7.1.4); m is the mass, in grams, of the test Portion; 2) Commercially available analysed reagent is recommended. 16 solutions are to be prepared, see any quantitative anafyticaf chemistry text. 3) This Solution tan be prepared fr
30、om concentrated hydrochloric acid, p = 1 ,18 g/ml (DANGER: cB). 4) This Solution tan be prepared from solid sodium hydroxide (DANGER: ). 2 0 ISO ISO 3617:1994(E) 40,OO is the conversion factor obtained from the mass of sodium hydroxide equivalent to 1 mole of hydrochloric acid (i.e. 40,O) x the conv
31、ersion factor for millilitres to litres (i.e. 0,001) x the sampling factor (i.e. IO) x 100 (for percentage). 7.5 Carbonate content (as Na2C03) 75.1 Specification Maximum content of carbonate shall be 2,5 % (mlm), as Na2C03. 7.5.2 Reagents 7.2 Heavy metals content 7.5.2.1 Hydrochlorit acid, HCI, Stan
32、dard volumetric Solution of 0,l mol/l, (3,646 g/l)2)5). 7.2.1 Specification Maximum content of heavy metals shall be 0,003 % (mlm). 7.5.2.2 Methyl orange indicator. 7.2.2 Procedure Dissolve 0,l g of methyl orange indicator in 250 ml of water. NOTE 1 The Standard for the iron test (7.3) is prepared i
33、n the same way as the heavy metals Standard. 7.5.3 Apparatus Determine the percentage of heavy metals in accordance with ISO 10349-5. Use a test Portion of 0,90 g to 1 ,IO g prepared in accordance with ISO 10349-5:1992, 7.3. Use 3 ml of the heavy metals Standard prepared in accordance with ISO 10349
34、-5: 1992, 8.1.2. 7.5.3.1 Burette, of 50 ml capacity. 7.5.4 Procedure Add two drops of methyl orange indicator (7.5.2.2) to the Solution from the assay titration in 7.1.4 and continue the titration with hydrochloric acid (7.5.2.1) to a permanent pink colour. The additional acid used represents carbon
35、ate. 7.3 Iron content 7.3.1 Specification Maximum content of iron shall be 0,002 % (m/m). 7.5.5 Expression of results 7.3.2 Procedure The carbon ate content, as N percentage bY mass of Na0 H I a2C03, expressed as a is given by Determine the percentage of iron in accordance with ISO 10349-5. Use a te
36、st Portion of 0,90 g to 1 ,IO g of the Sample prepared in accordance with ISO 10349-5: 1992, 7.3. Use 2 ml of the iron Standard prepared in accordance with ISO 10349-5:1992, 8.1.2. 52,99dWm where C is the actual concentration, in moles per litre, of the hydrochloric acid (7.5.2.1); 7.4 Halides conte
37、nt (as Cl-) V is the volume, in millilitres, of the hydrochloric acid used to resch the titration endpoint (7.5.4); 7.4.1 Specification Maximum content of halides shall be 0,3 % (m/m) as m is the mass, in grams, of the test Portion; 52,99 is the conversion factor obtained from the mass of sodium car
38、bonate equivalent to 1 mole of hydrochloric acid (i.e. 52,99) x the conversion factor for millilitres to litres (i.e. 0,001) x the sampling factor (i.e. IO) x 100 (for percentage). 7.4.2 Procedure Determine the percentage of halides (expressed as Cl-) in accordance with ISO 10349-6. Use a 10 ml aliq
39、uot of the Solution and 15 ml of the Halide A Standard. 5) This tan be prepared by diluting 100 ml of hydrochloric acid (7.1.2.1) to 1 Oitre with carbon-dioxide-free water. ISO 3617:1994(E) 0 ISO 7.6 Calcium and magnesium content (as Mg) 7.6.1 Specification Maximum Calcium and magnesium content shal
40、l be 0,06 % (m/m) as Mg. 7.6.2 Reagents 7.6.2.1 Ammonium hydroxide, NH,OH, p= 0,91 g/ml (DANGER: cC). 7.6.2.2 Buffer solution, pH 9,5 to 10,O. Dissolve 54 g of ammonium chloride (NH,CI) in 200 ml of water. Add 350 ml of ammonium hydroxide (7.6.2.1) () and dilute to 1 litre. 7.6.2.3 EDTA solution, St
41、andard volumetric Solution of 0,Ol mol/1 (3,36 g/l of the disodium salt, C-,0H14Na2N208) 2i . 7.6.2.4 Hydrochlorit acid, HCI, p = Ill8 g/ml (DANGER: ). 7.6.2.5 Magnesium Standard Solution (1 ml con- tains 1 mg Mg). Dissolve 1 Oll 41 g of magnesium sulfate heptahydrate (MgS04*7H20) in water containin
42、g 1 ml of hydro- chloric acid (7.6.2.4) () in a 1 litre volumetric flask (7.6.3.1). Dilute to the mark and mix. 7.6.2.6 Mordant black indicator. Grind 0,25 g of Mordant black 11 7, with 25 g of sodium chloride (NaCI) in a mortar. 7.6.3 Apparatus 7.6.3.1 One-mark volumetric flask, of 1 litre ca- paci
43、ty. 7.6.3.2 Burette, of 50 ml capacity. 7.6.4 Procedure Weigh, to the nearest 0,Ol g, a test Portion of about 2 g and dissolve it in 75 ml of water. Using Iitmus Paper, neutralize the Solution with hydrochloric acid (7.6.2.4) (), boil for 5 min and cool. Prepare a ten-fold dilution (1 + 9) of a Port
44、ion of the magnesium Standard Solution (7.6.2.5) and add 1 ml of this diluted Solution, followed by 5 ml of the buffer Solution (7.6.2.2) and Oll g of the Mordant black 11 indicator (7.6.2.6). Titrate with the EDTA Solution (7.6.2.3) to the colour Change from violet-red to blue. Carry out a similar
45、titration on a blank Solution which is treated the same way except for the addition of the test Portion. 7.6.5 Expression of results The Calcium and magnesium content, as Mg, expressed as a percentage by mass of the NaOH, is given by 0,024 3(Vl - Vz)/m where VI is the volume, in millilitres, of the
46、EDTA Solution (7.6.2.3) used to resch the titration endpoint of the test Solution; v2 is the volume, in millilitres, of the EDTA Solution (7.6.2.3) used to resch the titration endpoint of the blank; m is the mass, in grams, of the test Portion; 0,024 3 is the conversion factor obtained from the mass
47、 of magnesium equivalent to 1 mole of EDTA (i.e. 24,3) x the concentration of the EDTA Solution (i.e. 0,Ol) x the con- Version factor for millilitres to litres (i.e. 0,001) x 100 (for percentage). 7.7 Appearance of Solution 7.7.1 Specification The Solution shall be clear and free from insoluble matt
48、er except for a slight flocculence. 7.7.2 Procedure Dissolve a test Portion of IO,0 g in 50 ml of water and dilute to 100 ml with water. Observe the Solution for colour and clarity. 6) A procedure for the preparation and standardization of EDTA solution is given in annex A. 7) histed in colour index
49、 as C.I. 14645. Chrome Fast Black CAT, KlT*TS, Eriochrome Black DW, T and TDW, and Potting Black C are examples of suitable products available commercially. Thrs information is given for the convenience of users of this international Standard and does not constitute an endorsement by OS0 of these products. 4 0 ISO ISO 3617:1994(E) Annex A (informative) Preparation of EDTA solution: Standard volumetric solution of 0,Ol mol/1 (3,36 g/l) A. 1 Reagents A.l.1 Ethylenediaminetetraacetic acid (EDTA) dihydrate, disodium salt, C,0H14N2Na208m2H20. NOTE 2 The relative molecular mass for the dihydr
