BS-ISO-6849-1996.pdf

BRITISH STANDARD BS ISO 6849:1996 Implementation of ISO 6849:1996 Photography Processing wastes Determination of boron ICS 37.040.30 Licensed Copy: sheffieldun sheffieldun, na, Sun Nov 26 12:53:31 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS ISO 6849:1996 This British Standard, having been prepared under the direction of the Consumer Products and Services Sector Board, was published under the authority of the 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 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 Society Amendments issued since publication Amd. No.DateComments Licensed Copy: sheffieldun sheffieldun, na, Sun Nov 26 12:53:31 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS ISO 6849:1996 © BSI 12-1998i Contents Page Committees responsibleInside front cover National forewordii Forewordii 1Scope1 2Normative references1 3Principle1 4Safety and operational precautions2 4.1Hazard warnings2 4.2Hazard information code system2 4.3Safety precautions2 5Materials and reagents2 5.1General2 5.1.1Handling and labelling2 5.1.2Purity2 5.1.3Water2 5.1.4Strength of solutions2 5.2Reagents for method using boric acid-mannitol complex3 5.3Reagents for methylene blue method3 6Apparatus4 6.1Special apparatus for method using boric acid-mannitol4 6.2Special apparatus for methylene blue method4 7Sampling and sample preparation4 8Procedure4 8.1Procedure for method using boric acid-mannitol complex for levels of boron from 0,1 mg/l to 5 mg/l4 8.1.1Removal of phosphate4 8.1.2Removal of carbonate4 8.1.3Preparation for titration4 8.1.4Titration4 8.1.5Obtaining a blank reading5 8.2Procedure for method using boric acid-mannitol complex for high levels of boron from (5 mg/l to 100 mg/l5 8.2.1Removal of carbonate5 8.2.2Preparation for titration5 8.2.3Titration5 8.2.4Obtaining a blank reading5 8.2.5Expression of results; method using boric acid-mannitol complex5 8.2.6Precision5 8.3Procedure for methylene blue method5 8.3.1Direct sample preparation5 8.3.2Fusion sample preparation6 8.3.3Completion of sample preparation6 8.3.4Calibration curve6 8.3.5Expression of results6 9Test report6 Annex (informative) BibliographyInside back cover Licensed Copy: sheffieldun sheffieldun, na, Sun Nov 26 12:53:31 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS ISO 6849:1996 ii © BSI 12-1998 National foreword This British Standard reproduces verbatim ISO 6849:1996 and implements it as the UK national standard. This British Standard is published under the direction of the 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 international 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 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, the ISO title page, page 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 the inside front cover. Licensed Copy: sheffieldun sheffieldun, na, Sun Nov 26 12:53:31 GMT+00:00 2006, Uncontrolled Copy, (c) BSI Licensed Copy: sheffieldun sheffieldun, na, Sun Nov 26 12:53:31 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS ISO 6849:1996 ii © BSI 12-1998 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 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 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 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 the member bodies casting a vote. International Standard ISO 6849 was prepared by Technical Committee ISO/TC 42, Photography. Annex A of this International Standard is for information only. Licensed Copy: sheffieldun sheffieldun, na, Sun Nov 26 12:53:31 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS ISO 6849:1996 © BSI 12-19981 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 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 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. Hazard 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 of 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. 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 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, 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 phosphorous 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 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 International 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. Members of IEC and ISO maintain registers of currently valid International Standards. 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 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, 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, the 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 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 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. Licensed Copy: sheffieldun sheffieldun, na, Sun Nov 26 12:53:31 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS ISO 6849:1996 2 © BSI 12-1998 In the spectrophotometric method using methylene blue, sulfuric acid and hydrofluoric acid are added to form the tetrafluoroborate ion (BF4). Methylene 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 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 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 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 paragraph. Hazard 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 provide training and health and safety information in conformance with legal requirements. The hazard symbol 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 pertinent 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 laboratory 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 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 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. 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 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 (mol/l). The number of significant figures to which the molarity (mol/l) is known shall be sufficient 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/l) to the appropriate number of significant figures. BHarmful if inhaled. Avoid breathing dust, vapour, mist or gas. Use only with adequate ventilation. CHarmful if contact occurs. Avoid contact with eyes, skin or clothing. Wash thoroughly after handling. SHarmful if swallowed. Wash thoroughly after handling. If swallowed, obtain medical attention immediately. S May be fatal if swallowed. If swallowed, obtain medical attention immediately. FWill burn. Keep away from heat, sparks and open flame. Use with adequate ventilation. OOxidizer. Contact with other material may cause fire. Do not store near combustible materials. Licensed Copy: sheffieldun sheffieldun, na, Sun Nov 26 12:53:31 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS ISO 6849:1996 © BSI 12-19983 5.1.4.4 When a solution is to be diluted, its solution is 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(C2H3O2)2 · 3H2O 0,5 mol/l. Add approximately 750 ml of water 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 paper1) (prefolded; medium flow 100 ml prefiltered water in 55 s; medium porosity 8 µm particle retention). 5.2.2 Mannitol (C6H14O6). 5.2.3 Sodium acetate solution, c(NaC2H3O2) 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 sodium acetate (anhydrous), dilute to volume with water, stopper and mix well. 5.2.4 Sodium hydroxide, standard volum