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1、 Reference number ISO 7766:2003(E) ISO 2003 INTERNATIONAL STANDARD ISO 7766 First edition 2003-06-15 Processing photographic wastes Analysis of cyanides Determination of hexacyanoferrate(ll) and hexacyanoferrate(lll) by spectrometry Effluents de traitement photographiques Analyse des cyanures Dtermi
2、nation de lhexacyanoferrate(ll) et de lhexacyanoferrate(lll) par spectromtrie Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/22/2007 08:06:30 MDTNo reproduction or networking permitted
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6、l Secretariat at the address given below. ISO 2003 All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized in any form or by any means, electronic or mechanical, including photocopying and microfilm, without permission in writing from either ISO at
7、the address below or ISOs member body in the country of the requester. ISO copyright office Case postale 56 CH-1211 Geneva 20 Tel. + 41 22 749 01 11 Fax + 41 22 749 09 47 E-mail copyrightiso.org Web www.iso.org Published in Switzerland ii ISO 2003 All rights reserved Copyright International Organiza
8、tion for Standardization Provided by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/22/2007 08:06:30 MDTNo reproduction or networking permitted without license from IHS -,-,- ISO 7766:2003(E) ISO 2003 All rights reserved iii Contents Page Forewordiv Intr
9、oduction v 1 Scope1 2 Normative references .1 3 Safety and operational precautions1 4 Principle.2 5 Reactions.3 6 Reagents and materials3 7 Apparatus.4 8 Sampling and sample preparation 4 9 Procedure.5 10 Expression of results6 11 Test report6 Bibliography .7 Copyright International Organization for
10、 Standardization Provided by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/22/2007 08:06:30 MDTNo reproduction or networking permitted without license from IHS -,-,- ISO 7766:2003(E) iv ISO 2003 All rights reserved Foreword ISO (the International Organi
11、zation for 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. Each member body interested in a subject for which a technical committee has been establishe
12、d 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 standardization.
13、International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 2. The main task of technical committees is to prepare International Standards. Draft International Standards adopted by the technical committees are circulated to the member bodies for voting. Pub
14、lication as an International Standard requires approval by at least 75 % of the member bodies casting a vote. Attention is drawn to the possibility 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
15、 rights. ISO 7766 was prepared by Technical Committee ISO/TC 42, Photography. Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/22/2007 08:06:30 MDTNo reproduction or networking permitted
16、without license from IHS -,-,- ISO 7766:2003(E) ISO 2003 All rights reserved v Introduction This International Standard is devoted to the analysis of photographic wastes; it encompasses the analysis of complexed iron cyanides (hexacyanoferrates) in photographic effluents. Some of the chemicals speci
17、fied in the test procedures are caustic, toxic, or otherwise hazardous. Specific warning, caution and danger notices are noted but, in addition, the normal precautions required during the performance of any chemical procedure should be exercised at all times. In the case of effluents, the photograph
18、ic laboratory can best establish conformity to regulations by appropriate chemical analysis. In some cases, in-house analyses will be possible; but the use of an outside laboratory will often be required. Complexed cyanides are used in the bleaching stage of colour photographic processing and it is,
19、 therefore, possible for the cyanide portion of the resulting photographic effluent to reach a reportable level. Complexed cyanides contribute to the total cyanides in those tests in which the sample preparation breaks down the complexed cyanides. It is the purpose of this International Standard to
20、provide a method giving an independent determination of the cyanide present as hexacyanoferrate complexes. Due to the chemical behaviour of cyanide complexes, it is not possible to specify a single method for the quantitative determination of complexed cyanides in these effluents. The analysis of cy
21、anide is covered in various aspects in the following International Standards: ISO 6703-1:1984, Water quality Determination of cyanide Part 1: Determination of total cyanide; ISO 6703-2:1984, Water quality Determination of cyanide Part 2: Determination of easily liberatable cyanide. NOTE 1 Easily lib
22、eratable cyanides are defined as substances with cyanide groups and a measurable hydrocyanic acid vapour pressure at pH 4 and room temperature. NOTE 2 Cyanide diffuses as hydrogen cyanide (HCN) at room temperature from a solution at pH 6; the procedure determines cyanide from simple compounds of cya
23、nide and easily dissociated complexes. Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/22/2007 08:06:30 MDTNo reproduction or networking permitted without license from IHS -,-,- Copyrigh
24、t International Organization for Standardization Provided by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/22/2007 08:06:30 MDTNo reproduction or networking permitted without license from IHS -,-,- INTERNATIONAL STANDARD ISO 7766:2003(E) ISO 2003 All ri
25、ghts reserved 1 Processing photographic wastes Analysis of cyanides Determination of hexacyanoferrate(ll) and hexacyanoferrate(lll) by spectrometry 1 Scope This International Standard establishes a test method for the determination of hexacyanoferrate(II) (ferrocyanide) and hexacyanoferrate(III) (fe
26、rricyanide), referred to hereafter as Fe(CN)6, in photographic processing effluents1). Results are reported as hexacyanoferrate, Fe(CN)6. 2 Normative references The following referenced documents are indispensable for the application of this document. For dated references, only the edition cited app
27、lies. For undated references, the latest edition of the referenced document (including any amendments) applies. ISO 5667-1:1980, Water quality Sampling Part 1: Guidance on the design of sampling programmes ISO 5667-2:1991, Water quality Sampling Part 2: Guidance on sampling techniques ISO 5667-3:199
28、4, Water quality Sampling Part 3: Guidance on the preservation and handling of samples ISO 6353-1:1982, Reagents for chemical analysis Part 1: General test methods ISO 6353-2:1983, Reagents for chemical analysis Part 2: Specifications First series ISO 6353-3:1987, Reagents for chemical analysis Part
29、 3: Specifications Second series ISO 10349-1:2002, Photography Photographic-grade chemicals Test methods Part 1: General 3 Safety and operational precautions 3.1 Hazard warnings Some of the chemicals specified in the test procedures are caustic, toxic, or otherwise hazardous. Safe laboratory practic
30、e for the handling of chemicals requires the use of safety glasses or goggles and, in some cases, other protective apparel such as rubber gloves, face masks and aprons. Specific danger notices are given in the text for particularly dangerous materials, but normal precautions are required during the
31、performance of any chemical procedure at all times. 1) Significant levels of thiosulfate (hypo) can result in interference. Significant levels of thiosulfate in processing-machine effluents result in oxidation of the thiosulfate by iron (III). Sulfur will form, increasing the spectrophotometric abso
32、rbance which is measured. Also, thiosulfate may deplete the added iron (III) leaving nothing for the colour reaction. The method is applicable to effluents from buildings where the thiosulfate would be diluted by the rest of the building wastes and this would eliminate the interference. Copyright In
33、ternational Organization for Standardization Provided by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/22/2007 08:06:30 MDTNo reproduction or networking permitted without license from IHS -,-,- ISO 7766:2003(E) 2 ISO 2003 All rights reserved The first t
34、ime that a hazardous material is noted in the test procedures, the hazard will be indicated by the word “DANGER” followed by a symbol consisting of angle brackets “ ” containing a letter that designates the specific hazard. A double bracket “ ” will be used for particularly perilous situations. In s
35、ubsequent statements involving handling of these hazardous materials, only the hazard symbol consisting of the brackets and letter(s) will be displayed. Furthermore, for a given material, the hazard symbol will be used only once in a single paragraph. Hazard warning symbols will not be used for comm
36、on organic solvents when used in quantities of less than 1 l, unless they are particularly hazardous. Detailed warnings for handling chemicals and their diluted solutions are beyond the scope of this International Standard. Employers shall provide training and health and safety information in accord
37、ance with legal requirements. The hazard code system used in this International Standard is intended to provide information to the users and is not meant for compliance with any legal requirements for labelling, as these vary from country to country. It is strongly recommended that anyone using thes
38、e chemicals obtain pertinent information from the manufacturer about the hazards, handling, use and disposal of these chemicals. 3.2 Hazard information code system B Harmful if inhaled. Avoid breathing dust, vapour, mist or gas. Use only with adequate ventilation. C Harmful if contact occurs. Avoid
39、contact with eyes, skin or clothing. Wash thoroughly after handling. F Will burn. Keep away from heat, sparks and open flame. Use with adequate ventilation. O Oxidizer. Contact with other material may cause fire. Do not store near combustible materials. S Harmful if swallowed. Wash thoroughly after
40、handling. If swallowed, obtain medical attention immediately. S May be fatal if swallowed. If swallowed, obtain medical attention immediately. 3.3 Safety precautions ALL PIPETTE OPERATIONS SHALL BE PERFORMED WITH A PIPETTE BULB OR PLUNGER PIPETTE. Failure to observe this warning notice can result in
41、 cyanide poisoning. THIS IS A CRITICAL SAFETY WARNING! Digestion procedures shall be performed in a fume hood. Hydrogen cyanide or other toxic substances may be evolved. Safety glasses shall be worn for all laboratory work. 4 Principle A sample of effluent, or diluted effluent, is treated with a mix
42、ture of iron(II) and iron(III) ions. If Fe(CN)6 is present, a blue suspension will form. In the range 1,0 mg/l to 10,0 mg/l of Fe(CN)6, this suspension is stable and its absorbance is linear with its concentration. The absorbance is measured with a spectrometer, and the concentration determined from
43、 a previously established calibration. Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/22/2007 08:06:30 MDTNo reproduction or networking permitted without license from IHS -,-,- ISO 7766
44、:2003(E) ISO 2003 All rights reserved 3 5 Reactions 3Fe(II)(CN)64 + 4Fe3+ Fe4Fe(CN)63 2Fe(III)(CN)63 + 3Fe2+ Fe3Fe(CN)62 6 Reagents and materials 6.1 General 6.1.1 Handling and labelling Reagents shall be handled in accordance with health and safety precautions as shown on containers, or as given in
45、 other sources of such information. Proper labelling of prepared reagents includes chemical name, date of preparation, expiration date, restandardization date, name of preparer and adequate health and safety precautions. The discharge of reagents shall conform to applicable environmental regulations
46、. 6.1.2 Purity Reagents used in the test procedures shall be certified reagent-grade chemicals and shall meet appropriate standards or be chemicals of a purity acceptable for the analysis, as specified in ISO 6353-1, ISO 6353-2 and ISO 6353-3. 6.1.3 Water Whenever water is specified without other qu
47、alifiers in the test procedures, only distilled water or water of equal purity shall be used. 6.1.4 Strength of solutions 6.1.4.1 Acids and ammonium hydroxide are full strength unless otherwise specified. 6.1.4.2 When a standardized solution is required, its concentration is expressed as molarity (m
48、ol/l). The number of significant figures to which the molarity is known shall be sufficient to ensure that the reagent does not limit the reliability of the test method. 6.1.4.3 When a standardized solution is not required, its concentration is expressed, in grams per litre (g/l), to the appropriate number of significant figures. 6.1.4.4 When a solution is to be diluted, its dilution is indicated by (X + Y), meaning