ISO 6849-1996 Photography - Processing wastes - Determination of boron《摄影 冲洗废液 硼的测定》.pdf

1、IS0 6849 96 4853903 0685709 IT3 = I NTERNATI ONAL STANDARD IS0 First edition 1996-1 1-01 Photography - Processing wastes - Determination of boron Photographie - Effluents de traitement - Dtermination du bore This material is reproduced from IS0 documents under International Organization for Standard

2、ization (SO) Copyright License number IHSIICCI1996. Not for resale. No pari of these IS0 documents may be reproduced in any form, electronic retrieval system or otherwise, except as allowed in the copyright law of the country of use, or with the prior written consent of IS0 (Case postale 56,1211 Gen

3、eva 20, Switzerland, Fax +41 22 734 IO 79), IHS or the IS0 Licensors members. Reference number IS0 6849:1996(E) IS0 b849 96 4853903 Ob85730 935 IS0 6849:1996(E) Foreword IS0 (the International Organization for Standardization) is a worldwide federation of national standards bodies (IS0 member bodies

4、). The work of preparing International Standards is normally carried out through IS0 technical committees. Each member body interested in a subject for which a technical committee has been established has the right to be represented on that committee. International organizations, governmental and no

5、n-governmental, in liaison with 60, also take part in the work. IS0 collaborates closely with the International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization. Draft International Standards adopted by the technical committees are circulated to the member bodies

6、for voting. Publication as an International Standard requires approval by at least 75 YO of the member bodies casting a vote. International Standard IS0 6849 was prepared by Technical Committee ISOTTC 42, Photography. Annex A of this International Standard is for information only. O IS0 1996 All rig

7、hts 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 the publisher. International Organization for Standardization Case Posta

8、le 56 CH-1 21 1 Genve 20 Switzerland Printed in Switzerland II 0 IS0 IS0 6849 96 4853903 Ob85711 851 W IS0 6849:1996(E) Introduction This International Standard is one of a series devoted to the analysis of photographic wastes; it encompasses the field of analysis of boron in photographic effluents.

9、 This International 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

10、 of safety glasses or goggles, rubber gloves and other protective apparel such as face masks or aprons where appropriate. Normal precautions 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. Haz

11、ard warnings designated by a letter enclosed in angle brackets, ( ), are used as a reminder in those steps detailing handling operations and are defined in clause 4. More detailed information regarding hazards, handling and use of these chemicals may be available from the manufacturer. In the case o

12、f effluents, the photographic laboratory can best establish its conformity to regulations by appropriate chemical analysis. In some cases, in-house analyses will be possible; often the use of an outside laboratory will be required. . 111 IS0 6849 96 4853903 Ob85732 798 E INTERNATIONAL STANDARD 0 IS0

13、 IS0 6849:1996(E) Photography - Processing wastes - Determination of boron 1 Scope This International Standard specifies two methods for the determination of boron in photographic processing wastes. The first method is the estimation of borates by titration of the boric acid-mannitol complex, which

14、is a stronger acid than the boric acid from which it is formed. It is suitable for boron concentrations of 0,l mg/l and higher. In the range 0,l mg/l to 5 mg/l, phosphate is removed by precipitation by lead acetate. In the range 1 mg/l to 100 mg/l, the sample is diluted 25 times; this eliminates pho

15、sphorous interference if the phosphorous concentration is below 500 mg/l. The second and alternative method is a spectrophotometric technique using methylene blue and is useful in the boror range of 0,l ml/l to 1 ,O mg/, this being the concentration likely to be encountered in photographic processin

16、g wastes. 2 Normative references The following International Standards contain provisions which, through reference in 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

17、agreements based on this International Standard are encouraged to investigate the possibility of applying the most recent editions of the standards indicated below. Members of IEC and IS0 maintain registers of currently valid International Standards. IS0 5667-1 :I 980, Water quality - Sampling - Par

18、t 7: Guidance on the design of sampling programmes. IS0 5667-2:1991, Water quality - Sampling - Part 2: Guidance on sampling techniques. IS0 5667-3:1994, Water quality - Sampling - fart 3: Guidance on the preservation and handling of samples IS0 6353-1 :I 982, Reagents for chemical analysis - Part 1

19、: General test methods. IS0 6353-2:1983, Reagents for chemical analysis - Part 2: Specifications - First series. IS0 6353-3:1987, Reagents for chemical analysis - Part 3: Specifications - Second series. IS0 1 0349-1 :I 992, Photography - Photographic-grade chemicals - Test methods - Parr I: General

20、3 Principle In the method using boric acid-mannitol complex, sodium acetate is added to stabilize the pH. The sample is then acidified with sulfuric acid and boiled to expel carbon dioxide. Upon cooling, the pH is adjusted to 7 with sodium 1 IS0 6847 76 = 4853703 0685733 624 IS0 6849:1996(E) Q IS0 h

21、ydroxide. Mannitol is added to form a complex acid with any boric acid present. The mixture is then titrated back to pH 7 with 0,02 mol/l sodium hydroxide. Interference by atmospheric carbon dioxide is minimized by titrating both the sample and a blank in a specified time. This method should not be

22、used in the presence of ammonia gas, acetic acid vapours, or hydrochloric acid fumes since these may be absorbed into the sample and change the pH. In the spectrophotometric method using methylene blue, sulfuric acid and hydrofluoric acid are added to form the tetrafluoroborate ion (BF4-1. Methylene

23、 blue is then added and the complex formed is extracted with 1,2-dichloroethane. The absorbance of the extract is measured at a wavelength near 660 nm. 4 Safety and operational precautions 4.1 Hazard warnings Some of the chemicals specified in the test procedures are caustic, toxic or otherwise haza

24、rdous. Specific danger notices are given in the text and footnotes, but normal precautions are required during the performance of any chemical procedure at all times. The first time that a hazardous material is handled in a procedure, the hazard will be indicated by the word “DANGER“ followed by a s

25、ymbol consisting of angle brackets “( )“ containing a letter which designates the specific hazard and a statement of the hazard. A double bracket “( )“ will be used for particularly perilous situations. In subsequent statements involving handling of these hazardous materials, only the hazard symbol

26、consisting of the brackets and letterk) will be displayed. Furthermore, for a given material, the hazard symbols will be used only once in a single paragraph. Hazard symbols will not be used for common organic solvents when used in quantities of less than 1 litre unless they are particularly hazardo

27、us. 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 symbol system used in this International Standard is int

28、ended 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 from the manufacturer pertinent information about the hazards, handling, use

29、and disposal of these chemicals. 4.2 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 after handling. (S) Harmful if swallowe

30、d. Wash thoroughly after handling. If swallowed, obtain medical attention immediately. (S) May be fatal if swallowed. If swallowed, obtain medical attention immediately. (F) Will burn. Keep away from heat, sparks and open flame. Use with adequate ventilation. (O) Oxidizer. Contact with other materia

31、l may cause fire. Do not store near combustible materials. 4.3 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. 2 0 IS0 IS0 6849 96 = 4853903 Ob857LLi 5b0 W IS

32、0 6849: 1996( E) 5 Nlaterials and reagents 5.1 General 5.1.1 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 chemical name, date o

33、f preparation, expiration date, restandardization date, name of preparer, and adequate health and safety precautions. The discharge of reagents shall comply with applicable environmental regulations. 5.1.2 Purity Reagents used in the test procedures shall be certified reagent-grade chemicals and sha

34、ll meet appropriate standards or be chemicals of a purity acceptable for the analysis. For details see IS0 6353-1, IS0 6353-2 and IS0 6353-3. 5.1.3 Water Whenever water is specified without other qualifiers in the test procedures, only distilled water or water of equal purity shall be used. 5.1.4 St

35、rength of solutions 5.1.4.1 Acids and ammonium hydroxide are full strength unless otherwise specified. 5.1.4.2 When a standardized solution is required, its concentration is expressed in moles per litre (moi/i). The number of significant figures to which the molarity (mol/l) is known shall be suffic

36、ient to ensure that the reagent does not limit the reliability of the test method. 5.1.4.3 When a standardized solution is not required, its concentration is expressed in grams per litre (g/I) to the appropriate number of significant figures. 5.1.4.4 When a solution is to be diluted, its solution is

37、 indicated by (X + Y), meaning that X volumes of reagent, or concentrated solution, are to be diluted with Y volumes of distilled or deionized water. 5.2 Reagents for method using boric acid-mannitol complex 5.2.1 Lead acetate solution, cPb(C2H302)2 . 3H201 = 0,5 mol/l. Add approximately 750 ml of w

38、ater to a 1 litre volumetric flask. Add and dissolve 190 g k 1 g of lead acetate trihydrate (DANGER: (S) and dilute to volume with water. If the solution is not clear, filter it through a filter paper 1) (prefolded; medium flow - 1 O0 ml prefiltered water in 55 s; medium porosity - 8 pm particle ret

39、ention). 5.2.3 Sodium acetate solution, c(NaC2H302) = 0.1 mol/l. Add approximately 750 ml of water to a 1 litre volumetric flask. Add and dissolve 8,2 g f 0,l g of sodium acetate (anhydrous), dilute to volume with water, stopper and mix well. 1) Whatman 2V is an example of a suitable filter paper av

40、ailable commercially. This information is given for the convenience of users of this International Standard and does not constitute an endorsement by IS0 of this product. 3 IS0 6849 96 9 4853703 Ob85735 4T7 = IS0 6849:1996(E) Q IS0 5.2.4 Sodium hydroxide, standard volumetric solution, c(Na0H) = 0,02

41、0 O mol/l. Pipette 100,O ml of standard sodium hydroxide solution (0,100 O mo/l) into a 500 ml volumetric flask. Dilute to volume with boiled distilled water which has been cooled to room temperature. Avoid unnecessary exposure to air. This solution is stable for about one week. 5.2.5 Sodium hydroxi

42、de, saturated solution. Slowly dissolve 60 g of sodium hydroxide (DANGER: (C) in 50 mI of freshly boiled, distilled water in a polyethylene or polypropylene bottle. Allow this solution to stand for 48 h before using it. When using this solution, care should be taken not to disturb it. Decant the amo

43、unt needed to avoid contamination from sodium carbonate which has settled to the bottom of the container. DANGER- If the water has not cooled before adding the sodium hydroxide, the heat of solution may cause the mixture to boil and erupt. 5.2.6 Sodium hydroxide, approximately 0,5 mol/l solution (ca

44、rbonate free). Add from a graduated cylinder, 3 ml of the decanted saturated sodium hydroxide (DANGER: (C) (5.2.5) to a 150 ml beaker. Dilute to approximately 100 ml with freshly boiled distilled water and store in a polyethylene or polypropylene bottle. Avoid prolonged and unnecessary exposure to a

45、ir. The solution is stable for two days only. 5.2.7 Sodium sulfate solution, c(Na2S04) = 0.5 mol/l. Add approximately 750 ml of water to a 1 litre volumetric flask. Add and dissolve 71 g f 1 g of sodium sulfate (anhydrous), dilute to volume with water, stopper and mix well. 5.2.8 Sulfuric acid solut

46、ion, c(H2S04) = 0.05 mol/l. 5.2.9 Thymol blue solution, 0.04 YO in water. 5.3 Reagents for methylene blue method 5.3.1 Boron standard solution, boron = O, 1 g/1. Dissolve 0,572 g f 0,001 g of orthoboric acid in water, transfer to a 1 litre volumetric flask, add water up to the mark, stopper and mix

47、well. This solution can be kept for 6 months after preparation. 5.3.2 Boron standard solution, boron = 0,001 g/I. Pipette 10 ml of boron standard solution (0,l 9/11 (5.3.1) into a 1 litre volumetric flask, add water up to the mark, stopper and mix well. This solution should be used within 1 O days a

48、fter preparation. 5.3.3 Boron standard solution, boron = 0,000 1 gA. Pipette 10 ml of boron standard solution (0,001 9/11 (5.3.2) into a 100 ml volumetric flask, add water up to the mark, stopper and mix well. Prepare this solution at the time of use. This solution should be used within 8 h after pr

49、eparation. 5.3.4 12-Dichloroethane (DANGER: (F)(C). 5.3.5 Hydrofluoric acid (1 + 9). Prepare the solution in a fume hood. (EXTREME Dl extremely corrosive.) GER: (C)(S). Concentrated hydrofluoric ac S 4 Q IS0 IS0 6849 96 m L;851903 0685736 333 m IS0 6849:1996(E) 5.3.6 Methylene blue solution. Dissolve 0.40 g k 0,Ol g of methylene blue in water to make 100 ml of solution. Add 10 ml of this solution to a 1 O0 ml volumetric flask, add water to the mark, stopper and mix well. 5.3.7 Silver sulfate solution, 0,3 g/I. Dissolve 0,15 g f 0,Ol g of silver sulfate in water to make 5