1、BRITISH STANDARD BS ISO 6849:1996 Implementation of ISO 6849:1996 Photography Processing wastes Determination of boron ICS 37.040.30BSISO6849:1996 This British Standard, having been prepared under the directionof the Consumer Products and Services Sector Board, was published under theauthority of th
2、e Standards Board and comes into effect on 15 March 1997 BSI 12-1998 The following BSI references relate to the work on this standard: Committee reference CPW/42 Draft for comment 90/44773 DC ISBN 0 580 26634 6 Committees responsible for this British Standard The preparation of this British Standard
3、 was entrusted to Technical Committee CPW/42, Photography, upon which the following bodies were represented: British Photographic Association British Institute of Non-destructive Testing Chemical Industries Association Department of the Environment Ministry of Defence PICON Royal Photographic Societ
4、y Amendments issued since publication Amd. No. Date CommentsBSISO 6849:1996 BSI 12-1998 i Contents Page Committees responsible Inside front cover National foreword ii Foreword ii 1 Scope 1 2 Normative references 1 3 Principle 1 4 Safety and operational precautions 2 4.1 Hazard warnings 2 4.2 Hazard
5、information code system 2 4.3 Safety precautions 2 5 Materials and reagents 2 5.1 General 2 5.1.1 Handling and labelling 2 5.1.2 Purity 2 5.1.3 Water 2 5.1.4 Strength of solutions 2 5.2 Reagents for method using boric acid-mannitol complex 3 5.3 Reagents for methylene blue method 3 6 Apparatus 4 6.1
6、 Special apparatus for method using boric acid-mannitol 4 6.2 Special apparatus for methylene blue method 4 7 Sampling and sample preparation 4 8 Procedure4 8.1 Procedure for method using boric acid-mannitol complex for levelsofboron from 0,1mg/l to 5 mg/l 4 8.1.1 Removal of phosphate 4 8.1.2 Remova
7、l of carbonate 4 8.1.3 Preparation for titration 4 8.1.4 Titration 4 8.1.5 Obtaining a blank reading 5 8.2 Procedure for method using boric acid-mannitol complex for highlevelsof boron from (5mg/l to 100 mg/l 5 8.2.1 Removal of carbonate 5 8.2.2 Preparation for titration 5 8.2.3 Titration 5 8.2.4 Ob
8、taining a blank reading 5 8.2.5 Expression of results; method using boric acid-mannitol complex 5 8.2.6 Precision 5 8.3 Procedure for methylene blue method 5 8.3.1 Direct sample preparation 5 8.3.2 Fusion sample preparation 6 8.3.3 Completion of sample preparation 6 8.3.4 Calibration curve 6 8.3.5 E
9、xpression of results 6 9 Test report 6 Annex (informative) Bibliography Inside back coverBSISO 6849:1996 ii BSI 12-1998 National foreword This British Standard reproduces verbatim ISO 6849:1996 and implements it as theUKnationalstandard. This British Standard is published under the direction of the
10、Consumer Products and Services Sector Board whose Technical Committee CPW/42 has the responsibility to: aid enquirers to understand the text; present to the responsible international committee any enquiries on interpretation, or proposals for change, and keep UK interests informed; monitor related i
11、nternational and European developments and promulgate them in the UK. NOTEInternational and European Standards, as well as overseas standards, are available from Customer Services, BSI, 389 Chiswick High Road, London W4 4AL. A British Standard does not purport to include all the necessary provisions
12、 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. Summary of pages This document comprises a front cover, an inside front cover, pages i and ii, theISO title page, pa
13、ge ii, pages 1 to 6, an inside back cover and a back cover. This standard has been updated (see copyright date) and may have had amendments incorporated. This will be indicated in the amendment table on theinside front cover.BSISO6849:1996 ii BSI 12-1998 Foreword ISO (the International Organization
14、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 has t
15、he 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. Draft I
16、nternational 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 the member bodies casting a vote. International Standard ISO 6849 was prepared by Technical Committee ISO/TC 42, P
17、hotography. Annex A of this International Standard is for information only.BSISO6849:1996 BSI 12-1998 1 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. This Internatio
18、nal 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 of safety glass
19、es 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. Hazard warnings des
20、ignated by a letter enclosed in angle brackets, , are used as a reminder in those steps detailing handling operations and are defined in clause4. More detailed information regarding hazards, handling and use of these chemicals may be available from the manufacturer. In the case of effluents, the pho
21、tographic 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. 1 Scope This International Standard specifies two methods for the determination of boron
22、 in photographic processing wastes. The first method is the estimation of borates by titration of the boric acid-mannitol complex, which is a stronger acid than the boric acid from which it is formed. It is suitable for boron concentrations of 0,1 mg/l and higher. In the range 0,1 mg/l to 5 mg/l, ph
23、osphate is removed by precipitation by lead acetate. In the range1 mg/l to 100 mg/l, the sample is diluted25times; this eliminates phosphorous interference if the phosphorous concentration is below500mg/l. The second and alternative method is a spectrophotometric technique using methylene blue and i
24、s useful in the boron range of 0,1 ml/l to 1,0 mg/l, this being the concentration likely to be encountered in photographic processing wastes. 2 Normative references The following International Standards contain provisions which, through reference in this text, constitute provisions of this Internati
25、onal Standard. At the time of publication, the editions indicated were valid. All standards are subject to revision, and parties to agreements based on this International Standard are encouraged to investigate the possibility of applying the most recent editions of the standards indicated below. Mem
26、bers ofIEC and ISO maintain registers of currently valid International Standards. ISO 5667-1:1980, Water quality Sampling Part1: Guidance on the design of sampling programmes. ISO 5667-2:1991, Water quality Sampling Part2: Guidance on sampling techniques. ISO 5667-3:1994, Water quality Sampling Part
27、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 3: Specifications Second se
28、ries. ISO 10349-1:1992, Photography Photographic-grade chemicals Test methods Part 1: General. 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, t
29、he pH is adjusted to 7 with sodium hydroxide. Mannitol is added to form a complex acid with any boric acid present. The mixture is then titrated back topH7 with 0,02 mol/l sodium hydroxide. Interference by atmospheric carbondioxide is minimized by titrating both the sample and a blank in a specified
30、 time. This method should not be used in the presence of ammoniagas, aceticacid vapours, or hydrochloric acid fumes since these may be absorbed into the sample and change the pH.BSISO6849:1996 2 BSI 12-1998 In the spectrophotometric method using methyleneblue, sulfuricacid and hydrofluoricacid are a
31、dded to form the tetrafluoroborateion(BF 4 ). Methyleneblue 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 th
32、e test procedures are caustic, toxic or otherwise hazardous. 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
33、will be indicated by the word “DANGER” followed by a symbol 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 t
34、hese 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 paragraph. Hazard symbols will not be used for common organic solvents when used in quantities of less
35、 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 provide training and health and safety information in conformance with legal requirements. The hazard symbol
36、 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 these chemicals obtain from the manufacturer perti
37、nent information about the hazards, handling, use and disposal of these chemicals. 4.2 Hazard information code system 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 labor
38、atory work. 5 Materials 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 of prep
39、aration, 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 shall mee
40、t appropriate standards or be chemicals of a purity acceptable for the analysis. For details seeISO6353-1, ISO 6353-2 and ISO 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 Strength o
41、f 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 (mol/l). The number of significant figures to which themolarity (mol/l) is known shall be sufficient to e
42、nsure 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 ingramsper litre (g/l) to the appropriate number of significant figures. B Harmful if inhaled. Avoid breathing dust, vapour, mist or gas. Use
43、 only with adequate ventilation. C Harmful if contact occurs. Avoid contact with eyes, skin or clothing. Wash thoroughly after handling. S Harmful if swallowed. Wash thoroughly after handling. If swallowed, obtain medical attention immediately. S May be fatal if swallowed. If swallowed, obtain medic
44、al attention immediately. 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.BSISO6849:1996 BSI 12-1998 3 5.1.4.4 When a solution is to be diluted, its solution is ind
45、icated 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(C 2 H 3 O 2 ) 2 3H 2 O 0,5 mol/l. Add approximately 750 ml of w
46、ater to a 1 litre volumetric flask. Add and dissolve 190 g 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 100 ml prefiltered water in 55 s; medium porosity 8m particle retention). 5.
47、2.2 Mannitol (C 6 H 14 O 6 ). 5.2.3 Sodium acetate solution, c(NaC 2 H 3 O 2 ) 0,1 mol/l. Add approximately 750 ml of water to a 1 litre volumetric flask. Add and dissolve 8,2 g 0,1 g of sodiumacetate (anhydrous), dilute to volume with water, stopper and mix well. 5.2.4 Sodium hydroxide, standard vo
48、lumetric solution, c(NaOH) = 0,020 0 mol/l. Pipette 100,0 ml of standard sodium hydroxide solution (0,100 0 mol/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 ab
49、out one week. 5.2.5 Sodium hydroxide, saturated solution. Slowly dissolve 60 g of sodium hydroxide (DANGER: C) in 50 ml 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 amount 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 hy
