1、Reference number ISO 6851:2001(E) ISO 2001 INTERNATIONAL 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 K
2、jeldahl)ISO 6851:2001(E) PDF disclaimer This PDF file may contain embedded typefaces. In accordance with Adobes licensing policy, this file may be printed or viewed but shall not be edited unless the typefaces which are embedded are licensed to and installed on the computer performing the editing. I
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5、dress given below. ISO 2001 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 the address below or IS
6、Os 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.ch Web www.iso.ch Printed in Switzerland ii ISO 2001 All rights reservedISO 6851:2001(E) ISO 2001 All rights reserved iii Contents P
7、age Foreword.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
8、 ISO 2001 All rights reserved Foreword 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 interes
9、ted in a subject for which a technical 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 C
10、ommission (IEC) on all matters of electrotechnical 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
11、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 International Standard may be the subject of patent rights. ISO shall not be held responsible for identifying any or all such p
12、atent rights. International Standard 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) ISO 2001 All rights reserved v Introduction This Interna
13、tional Standard is one of a series devoted to the analysis of photographic 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
14、analytical techniques. Some of the procedures use caustic, toxic or 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 pre
15、cautions for the safe performance of any chemical procedure must be 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. Mor
16、e detailed information on hazards, handling and use of these chemicals 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.INTERNATIONAL STA
17、NDARD ISO 6851:2001(E) ISO 2001 All rights reserved 1 Photography Processing waste Determination 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, pr
18、esent in photographic processing wastes by the Kjeldahl method. Total Kjeldahl nitrogen can 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
19、separately and subtracted, the concentration of organic amino nitrogen can be established. 2 Normative references The following normative documents contain provisions which, through reference in this text, constitute provisions of this International Standard. For dated references, subsequent amendme
20、nts to, or revisions of, any of these publications do not apply. However, parties to agreements 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 editi
21、on of the normative document referred to applies. Members of ISO and IEC maintain registers 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
22、: 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 and handling of samples. ISO 6353-1:1982, Reagents for chemical analysis Part 1: General test
23、 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 6853:2001, Photography Processing waste Determination of ammoniacal nitrogen (microdiffusion method). ISO 10349-1:1
24、992, Photography Photographic-grade chemicals Test methods Part 1: General.ISO 6851:2001(E) 2 ISO 2001 All rights reserved 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
25、 ammonium hydrogen sulfate. The ammonia is then liberated by treatment with a suitable alkali and absorbed into a solution 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 wit
26、h 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 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 fo
27、r 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 perfo
28、rmance of any chemical procedure at all times. The first time that a hazardous material is noted in the 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 “ “ wi
29、ll be used for particularly perilous situations. In subsequent 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 symbols will be used only once in a single parag
30、raph. Hazard warning symbols will not be used for common organic solvents when used in quantities of less than 1 litre, unless they are particularly hazardous. Detailed warnings for handling chemicals and their diluted solutions are beyond the scope of this International Standard. Employers shall pr
31、ovide training and health and safety information in conformance 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
32、 country. It is strongly recommended that anyone using these chemicals obtain pertinent information from the manufacturer 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 wit
33、h adequate ventilation.ISO 6851:2001(E) ISO 2001 All rights reserved 3 C Harmful if contact occurs. Avoid 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 materi
34、al may cause fire. Do not store near combustible materials. S Harmful if swallowed. Wash thoroughly after handling. If swallowed, obtain medical attention immediately. S May be fatal if swallowed. If swallowed, obtain medical attention immediately. 5.3 Safety precautions ALL PIPETTE OPERATIONS SHALL
35、 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 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 cont
36、ainers, or as given in other sources of such information. Proper labelling of prepared reagents includes the 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 applicabl
37、e environmental regulations. 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. For details, see ISO 6353-1, ISO 6353-2 and ISO 6353-3. 6.1.3 Water Whenever water
38、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 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-
39、of-substance concentration is expressed in moles per litre. 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 ex
40、pressed 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 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 ISO 200
41、1 All rights reserved 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 potassium sulfate, K 2 SO 4 , and transfer it quantitatively to a 1 litre volumetric flask conforming to Class A of ISO 1042. A
42、dd 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. Weigh 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 soluti
43、on (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 volume when cool, and mix well. Store this solution at a temperature above 14 C to prevent crystallization. 6.2.2 Potassi
44、um 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 potassium hydroxide, KOH (DANGER: C ), and dissolve it in the tetraborate solution. Boil on a hotplate for 5 min, cool
45、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 the beaker into the flask several times. When cool, dilute to volume and mix well. Note that the wetting agent will separa
46、te 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. 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
47、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 , keeping the contents of the flask stirred until all the constituents are dissolved. Dilute to within about 15 ml of t
48、he 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 microdiff
49、usion cell. Check that excess sodium hydroxide is absent by adding 0,10 ml of 0,002 50 mol/l sulfuric acid (6.2.7) 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. 6.2.4 Sulfuric acid solution, c(H 2 SO 4 ) 3mo l / l( DA N G E R : C ). Carefully add 170 ml
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