1、BRITISH STANDARD BS ISO 6851:2001 Photography Processing waste Determination of total amino nitrogen (microdiffusion Kjeldahl method) ICS 13.030.20; 37.040.30 NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBS ISO 6851:2001 This British Standard, having been prepared under the
2、direction 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 37508 0 National foreword This British Standard reproduces verbatim ISO 6851:2001 and impl
3、ements it 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 St
4、andards which 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 no
5、t purport 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 in
6、ternational/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 I
7、SO title page, pages ii to v, a blank page, pages 1 to 10, 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 6851:2001(E) OSI 1002 INTERN
8、ATIONAL STANDARD ISO 6851 Second edition 2001-12-15 Photography Processing waste Determination of total amino nitrogen (microdiffusion Kjeldahl method) Photographie Effluents de traitement Dtermination de lazote amino total (mthode de microdiffusion Kjeldahl)ii ISO 6851:2001(E)iii Contents Page Fore
9、word.iv Introduction.v 1 Scope 1 2 Normative references 1 3 Principle2 4 Reactions2 5 Safety and operational precautions.2 6 Materials and reagents3 7 Apparatus .6 8 Sampling and sample preparation.6 9 Procedure .7 10 Expression of results 8 11 Test report 9 Bibliography10ISO 6851:2001(E) iv Forewor
10、d ISO (the International Organization 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 technica
11、l committee has been 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 ele
12、ctrotechnical standardization. International 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
13、 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 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
14、ISO 6851 was prepared by Technical Committee ISO/TC 42, Photography. This second edition cancels and replaces the first edition (ISO 6851:1987), of which it constitutes a technical revision.ISO 6851:2001(E)v Introduction This International Standard is one of a series devoted to the analysis of photo
15、graphic wastes; it encompasses the field of analysis of the total amino nitrogen (microdiffusion Kjeldahl method) 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
16、 otherwise hazardous chemicals. Safe laboratory practice 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 or aprons. Normal precautions for the safe performance of any chemical procedure must be
17、 exercised at all times, but specific details have been provided 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 chemic
18、als may be available from the manufacturer. Photographic laboratories 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 6851:2001(E)1 Photography Processing waste Determina
19、tion of total amino nitrogen (microdiffusion Kjeldahl method) 1 Scope This International Standard specifies a method for the determination of the total organic nitrogen, as well as any ammoniacal nitrogen, present in photographic processing wastes by the Kjeldahl method. Total Kjeldahl nitrogen can
20、be determined in photographic processing wastes in the range of 10 mg/l to 200 mg/l as ammonia, or in the range of 8 mg/l to 160 mg/l in terms of nitrogen. If ammoniacal nitrogen (see ISO 6853) is determined separately and subtracted, the concentration of organic amino nitrogen can be established. 2
21、 Normative references The following normative documents 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 agreeme
22、nts based on this International Standard are encouraged 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
23、of currently valid International Standards. ISO 648:1977, Laboratory glassware One-mark pipettes. ISO 1042:1998, Laboratory glassware One-mark volumetric flasks. ISO 5667-1:1980, Water quality Sampling Part 1: Guidance on the design of sampling programmes. ISO 5667-2:1991, Water quality Sampling Par
24、t 2: Guidance on sampling techniques. ISO 5667-3:1994, 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 serie
25、s. ISO 6353-3:1987, Reagents for chemical analysis Part 3: Specifications Second series. ISO 6853:2001, Photography Processing waste Determination of ammoniacal nitrogen (microdiffusion method). ISO 10349-1:1992, Photography Photographic-grade chemicals Test methods Part 1: General.ISO 6851:2001(E)
26、2 3P r i n c i p l e In the presence of sulfuric acid and/or potassium sulfate with mercuric sulfate as a catalyst, the amino nitrogen of most organic substances is converted into ammonium hydrogen sulfate. The ammonia is then liberated by treatment with a suitable alkali and absorbed into a solutio
27、n of boric acid. The liberation and absorption of the ammonia is carried out in a microdiffusion cell. The ammonia absorbed into the boric acid is then determined by titration with standard sulfuric acid. 4 Reactions .NH 2 .NHR+H 2 SO 4 (NH 4 )HSO 4 .NR 2 (NH 4 )HSO 4 +2 OH NH 3 +2 H 2 O+S O 4 2 5 S
28、afety 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 apparel suc
29、h 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, the h
30、azard 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 materials
31、, 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 litre, u
32、nless 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 used in t
33、his 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 manufacturer
34、 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.ISO 6851:2001(E)3 C Harmful if contact occurs. Avoid contact with eyes, skin or clothing. Wash tho
35、roughly 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 handling. If swallowed, obtain medical attent
36、ion immediately. 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. 6 Materi
37、als 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, expira
38、tion 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 appropriate st
39、andards, 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 of solut
40、ions 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 to ens
41、ure 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
42、by (X + Y), meaning that X volumes of reagent, or concentrated solution, are to be diluted with Y volumes of water (6.1.3).ISO 6851:2001(E) 4 6.2 Reagents 6.2.1 Acidified mercury(II) sulfate/potassium sulfate solution (DANGER: C S ), (HgO) = 2 g/l, (K 2 SO 4 ) = 134 g/l. Weigh 134 g 0,1 g of potassi
43、um sulfate, K 2 SO 4 , and transfer it quantitatively to a 1 litre volumetric flask conforming to Class A of ISO 1042. Add about 650 ml of water and dissolve the potassium sulfate. Carefully add 200 ml of sulfuric acid, H 2 SO 4 (DANGER: C ) 1,84 g/ml, from a graduated measuring cylinder and mix. We
44、igh 2 g 0,1 g of red mercury(II) oxide, HgO 1 (DANGER: B C S ), and dissolve it in 25 ml of 3 mol/l sulfuric acid solution (6.2.4) (DANGER: C ) in a small beaker. Add the contents of the beaker to the acidified potassium sulfate solution, and rinse the beaker into the flask. Dilute the solution to v
45、olume when cool, and mix well. Store this solution at a temperature above 14 C to prevent crystallization. 6.2.2 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 litre beaker. Then weigh 247 g 0,1 g of
46、 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 (6-10) ethylene oxide, NPPO, or similar wetting agent 2 . Transfer the mixture to a 1 litre volumetric flask, rinsing th
47、e 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. 6.2.3 Boric acid absorbent solution Add about 800 ml of water to a 1 litre volumetric flask. Sti
48、r, 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 of boric acid, H 3 BO 3
49、 , keeping the contents of the flask stirred until all the constituents are dissolved. Dilute to within about 15 ml of the mark and mix. Place 1,5 ml of this solution in the 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 (6.2.9) to the solution in the 1 litre flask to obtain a neutral colour when 1 ml is viewed in the microdiffusion cell. Chec
