1、BRITISH STANDARD BS ISO 6853:2001 Photography Processing waste Determination of ammoniacal nitrogen (microdiffusion method) ICS 13.030.20; 37.040.30 NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBS ISO 6853:2001 This British Standard, having been prepared under the direction
2、of the Consumer Products and Services Policy and Strategy Committee, was published under the authority of the Standards Policy and Strategy Committee on 18 January 2002 BSI 18 January 2002 ISBN 0 580 37505 6 National foreword This British Standard reproduces verbatim ISO 6853:2001 and implements it
3、as the UK national standard. The UK participation in its preparation was entrusted to Technical Committee CPW/42, Photography, which has the responsibility to: A list of organizations represented on this committee can be obtained on request to its secretary. Cross-references The British Standards wh
4、ich implement international publications referred to in this document may be found in the BSI Standards Catalogue under the section entitled “International Standards Correspondence Index”, or by using the “Find” facility of the BSI Standards Electronic Catalogue. A British Standard does not purport
5、to include all the necessary provisions of a contract. Users of British Standards are responsible for their correct application. Compliance with a British Standard does not of itself confer immunity from legal obligations. aid enquirers to understand the text; present to the responsible internationa
6、l/European committee any enquiries on the interpretation, or proposals for change, and keep the UK interests informed; monitor related international and European developments and promulgate them in the UK. Summary of pages This document comprises a front cover, an inside front cover, the ISO title p
7、age, pages ii to v, a blank page, pages 1 to 8, an inside back cover and a back cover. The BSI copyright date displayed in this document indicates when the document was last issued. Amendments issued since publication Amd. No. Date CommentsReference number ISO 6853:2001(E) OSI 1002 INTERNATIONAL STA
8、NDARD ISO 6853 Second edition 2001-12-15 Photography Processing waste Determination of ammoniacal nitrogen (microdiffusion method) Photographie Effluents de traitement Dtermination de lazote ammoniacal (mthode par microdiffusion)ii ISO 6853:2001(E)iii Contents Page Foreword.iv Introduction.v 1 Scope
9、 1 2 Normative references 1 3 Principle1 4 Reaction2 5 Safety and operational precautions.2 6 Materials and reagents3 7 Apparatus .5 8 Sampling and sample preparation.5 9 Procedure .6 10 Expression of results 7 11 Test report 7 Bibliography8ISO 6853:2001(E) iv Foreword ISO (the International Organiz
10、ation 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 established
11、 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. I
12、nternational Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 3. 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 th
13、e member bodies casting a vote. Attention is drawn to the possibility that some of the elements of this International Standard may be the subject of patent rights. ISO shall not be held responsible for identifying any or all such patent rights. International Standard ISO 6853 was prepared by Technic
14、al Committee ISO/TC 42, Photography. This second edition cancels and replaces the first edition (ISO 6853:1987), of which it constitutes a technical revision.ISO 6853:2001(E)v Introduction This International Standard is one of a series devoted to the analysis of photographic wastes; it encompasses t
15、he field of analysis of the ammoniacal nitrogen content in a photographic effluent. This International Standard is intended for use by individuals with a working knowledge of analytical techniques. Some of the procedures use caustic, toxic or otherwise hazardous chemicals. Safe laboratory practice f
16、or 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 or aprons. Normal precautions for the safe performance of any chemical procedure must be exercised at all times, but specific details have been pr
17、ovided for hazardous materials. Hazard warnings are designated by a letter enclosed in angle brackets “ .“ These are defined in clause 5 and then used throughout the text. More detailed information on hazards, handling and use of these chemicals may be available from the manufacturer. Photographic l
18、aboratories can establish conformity to effluent regulations only by chemical analysis. If this cannot be done in-house, an outside laboratory should be used.blankINTERNATIONAL STANDARD ISO 6853:2001(E)1 Photography Processing waste Determination of ammoniacal nitrogen (microdiffusion method) 1 Scop
19、e This International Standard specifies a method for the determination of ammonia and other volatile amines that can be liberated from photographic processing wastes by strong alkali, the results being expressed in terms of nitrogen. The method is applicable for the determination of the ammonia conc
20、entration of typical photoprocessing wastes in the range of 10 mg/l to 200 mg/l of ammonia or 8 mg/l to 160 mg/l of nitrogen. Other volatile amines are determined as ammonia, but their concentrations in photoprocessing wastes are usually very low. 2 Normative references The following normative docum
21、ents contain provisions which, through reference in this text, constitute provisions of this International Standard. For dated references, subsequent amendments to, or revisions of, any of these publications do not apply. However, parties to agreements based on this International Standard are encour
22、aged to investigate the possibility of applying the most recent editions of the normative documents indicated below. For undated references, the latest edition of the normative document referred to applies. Members of ISO and IEC maintain registers of currently valid International Standards. ISO 648
23、:1977, Laboratory glassware One-mark pipettes. 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 5667-3:1994, Water quality Sampling Part 3: Guidance on the preservation
24、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 3: Specifications Second series. ISO 10349-1:1992, Photogra
25、phy Photographic-grade chemicals Test methods Part 1: General. 3P r i n c i p l e Ammonia is liberated from the sample by treatment with potassium metaborate and is absorbed into boric acid. The absorbed ammonia is then determined by titration with standard sulfuric acid. The liberation and absorpti
26、on are carried out in a microdiffusion cell, which is a small covered dish with concentric chambers for sample, sealant and absorbing solution. When the sample and the metaborate are mixed in the sample chamber, ammonia is evolved and absorbed into the boric acid chamber. The gaseous free path from
27、sample to absorbent is short, in order to ensure a room temperature distillation in a reasonable time. Scale-up of this method or alteration of the sample to buffer ratio should be avoided, as these modifications change the rate of ammonia diffusion.ISO 6853:2001(E) 2 4 Reaction 43 2 NH X OH NH H O
28、+ X 5 Safety and operational precautions 5.1 Hazard warnings Some of the chemicals specified in the test procedures are caustic, toxic or otherwise hazardous. Safe laboratory practice for the handling of chemicals requires the use of safety glasses or goggles, and in some cases other protective appa
29、rel 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 performance of any chemical procedure at all times. The first time that a hazardous material is noted in the procedures
30、, 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 subsequent statements involving handling of these hazardous ma
31、terials, only the hazard symbol consisting of the brackets and letter(s) will be displayed. Furthermore, for a given material, the hazard symbols will be used only once in a single paragraph. Hazard warning symbols will not be used for common organic solvents when used in quantities of less than 1 l
32、itre, 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 conformance with legal requirements. The hazard code system us
33、ed 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 these chemicals obtain pertinent information from the manuf
34、acturer about the hazards, handling, use and disposal of these chemicals. 5.2 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 contact with eyes, skin or clothing. Wash thoroughly af
35、ter 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 handling. If swallowed, obtain medical attention immedi
36、ately. S May be fatal if swallowed. If swallowed, obtain medical attention immediately. 5.3 Safety precautions ALL PIPETTE OPERATIONS SHALL BE PERFORMED WITH A PIPETTE BULB OR PLUNGER PIPETTE. THIS IS A CRITICAL SAFETY WARNING! Safety glasses shall be worn for all laboratory work.ISO 6853:2001(E)3 6
37、 Materials and reagents 6.1 General 6.1.1 Handling and labelling Reagents shall be handled in conformity with health and safety precautions as shown on containers, or as given in other sources of such information. Proper labelling of prepared reagents includes the chemical name, date of preparation,
38、 expiration date, restandardization date, name of preparer, and adequate health and safety precautions. The discharge of reagents shall conform to applicable environmental regulations. 6.1.2 Purity Reagents used in the test procedures shall be certified reagent-grade chemicals and shall meet appropr
39、iate standards, or be chemicals of a purity acceptable for the analysis. For details, see ISO 6353-1, ISO 6353-2 and ISO 6353-3. 6.1.3 Water Whenever water is specified without other qualifiers in the test procedures, only distilled water or water of equivalent purity shall be used. 6.1.4 Strength o
40、f 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 amount-of-substance-concentration is expressed in moles per litre. The number of significant figures to which the molarity is known shall be sufficient
41、 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 ind
42、icated by (X + Y), meaning that X volumes of reagent, or concentrated solution, are to be diluted with Y volumes of water (6.1.3). 6.2 Reagents 6.2.1 Potassium tetraborate solution,5 14g /l . Weigh 673 g 0,1 g of potassium tetraborate, K 2 B 4 O 7 4H 2 O, and dissolve it in 550 ml of water in a 1 li
43、tre beaker. Then weigh 247 g 0,1 g of potassium hydroxide, KOH (DANGER: C ), and dissolve it in the tetraborate solution. Boil on a hotplate for 5 min, cool and add 5 ml of a 10 % aqueous solution of nonylphenoxypoly (610) ethylene oxide, NPPO, or similar wetting agent 1 . Transfer to a 1 litre volu
44、metric flask, rinsing the beaker into the flask several times. When cool, dilute to volume and mix well. Note that the wetting agent will separate out on standing; therefore, the flask must be shaken vigorously before each use. 6.2.2 Boric acid absorbent solution Add about 800 ml of water to a 1 lit
45、re volumetric flask. Stir, using a magnetic stirrer, and add 2 mg to 3 mg of xylene cyanole FF, weighed to the nearest 1 mg, followed by 0,5 ml of NPPO, followed by 5,0 ml of methyl red indicator solution prepared by dissolving 0,125 g of methyl red in 250 ml of methanol (DANGER: F S ). Add 6g 0,1 g
46、 of boric acid, H 3 BO 3 , keeping the contents of the flask stirred until all the constituents are dissolved. 1 Non-ionic detergent with a hydrophilic lipophilic balance in the range of 13 to 14.ISO 6853:2001(E) 4 Dilute to within about 15 ml of the mark and mix. Place 1,5 ml of this solution in th
47、e centre of a microdiffusion cell and observe the colour. If the colour in the cell is pink, add just sufficient 0,1 mol/l sodium hydroxide (6.2.7) to the solution in the 1 litre flask to obtain a neutral colour when 1 ml is viewed in the microdiffusion cell. Check that excess sodium hydroxide is ab
48、sent by adding 0,10 ml of 0,002 50 mol/l sulfuric acid (6.2.5) to 1 ml of the solution, at which point a pink colour should be produced. Note that the solution in the 1 litre flask will appear red, even when the 1 ml in the microdiffusion cell looks neutral. 6.2.3 Sulfuric acid solution, c(H 2 SO 4
49、) 0,5 mol/l. Carefully add 28,3 ml of sulfuric acid (DANGER: C ), 1,84 g/ml, to 500 ml of water in a 1 litre volumetric flask while mixing and cooling. Dilute to the mark with water. 6.2.4 Sulfuric acid solution, c(H 2 SO 4 ) 0,05 mol/l. Pipette 100,0 ml of 0,5 mol/l sulfuric acid (6.2.3) into a 1 litre volumetric flask and dilute to the mark with water. NOTE This solution is not the standard volumetric solution that is required in 6.2.5. 6.2.5 Sulfuric acid solution
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