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1、BRITISH STANDARD BS ISO 6850:1994 Implementation of ISO 6850:1994 Photography Processing wastes Determination of nitrate by a spectrometric method using brucine Licensed Copy: sheffieldun sheffieldun, na, Sun Nov 26 03:15:27 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS ISO 6850:1994 This British St
2、andard, 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 April 1995 BSI 12-1999 The following BSI references relate to the work on this standard: Committee reference CPM/1
3、4 Draft for comment 90/44774 DC ISBN 0 580 23960 8 Committees responsible for this British Standard The preparation of this British Standard was entrusted to Technical Committee CPM/14, Photographic chemicals and processing, upon which the following bodies were represented: British Institute of Non-
4、Destructive Testing British Photographic Association Chemical Industries Association Department of the Environment (Water Directorate) Royal Photographic Society Amendments issued since publication Amd. No.DateComments Licensed Copy: sheffieldun sheffieldun, na, Sun Nov 26 03:15:27 GMT+00:00 2006, U
5、ncontrolled Copy, (c) BSI BS ISO 6850:1994 BSI 12-1999i Contents Page Committees responsibleInside front cover National forewordii Forewordiii Text of ISO 68501 Licensed Copy: sheffieldun sheffieldun, na, Sun Nov 26 03:15:27 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS ISO 6850:1994 ii BSI 12-1999
6、National foreword This British Standard reproduces verbatim ISO 6850:1994 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 CPM/14, has the responsibility to: aid enquirer
7、s 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 w
8、ell 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
9、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, pages ii to iv, pages 1 to 6 and a back cover. This standard has been updated (see copyright date) and may have had a
10、mendments incorporated. This will be indicated in the amendment table on the inside front cover. Licensed Copy: sheffieldun sheffieldun, na, Sun Nov 26 03:15:27 GMT+00:00 2006, Uncontrolled Copy, (c) BSI Licensed Copy: sheffieldun sheffieldun, na, Sun Nov 26 03:15:27 GMT+00:00 2006, Uncontrolled Cop
11、y, (c) BSI ISO 6850:1994(E) ii BSI 12-1999 Contents Page Forewordiii Introduction1 1Scope1 2Normative references1 3Principle1 4Safety and operational precautions1 5Materials and reagents2 6Apparatus3 7Sampling and sample preparation3 8Procedure4 9Expression of results5 10Precision5 Annex A (informat
12、ive) Bibliography6 Licensed Copy: sheffieldun sheffieldun, na, Sun Nov 26 03:15:27 GMT+00:00 2006, Uncontrolled Copy, (c) BSI ISO 6850:1994(E) BSI 12-1999iii Foreword ISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies).
13、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-g
14、overnmental, 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 fo
15、r voting. Publication as an International Standard requires approval by at least 75 % of the member bodies casting a vote. International Standard ISO 6850 was prepared by Technical Committee ISO/TC 42, Photography. Licensed Copy: sheffieldun sheffieldun, na, Sun Nov 26 03:15:27 GMT+00:00 2006, Uncon
16、trolled Copy, (c) BSI iv blank Licensed Copy: sheffieldun sheffieldun, na, Sun Nov 26 03:15:27 GMT+00:00 2006, Uncontrolled Copy, (c) BSI ISO 6850:1994(E) BSI 12-19991 Introduction This International Standard is one a series devoted to the analysis of photographic wastes; it encompasses the field of
17、 analysis of nitrate ions 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 pra
18、ctice 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 ta
19、ken 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
20、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 Intern
21、ational Standard specifies a spectrometric method for the determination of nitrates in photographic processing wastes. Pretreatment of the sample is necessary to remove interferences present in photographic processing wastes. This method can be applied to samples containing nitrate in the concentrat
22、ion range 4,4 mg/l to 88 mg/l of nitrate (1 mg/l to 20 mg/l of nitrogen). 2 Normative references The following 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
23、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.
24、 ISO 6353-1:1982, Reagents for chemical analysis Part 1: General requirements. 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 c
25、hemicals Test methods Part 1: General. 3 Principle The reaction between nitrate and brucine produces a yellow colour, the intensity of which is measured at 410 nm. The reaction rate between brucine and nitrate ions and hence the intensity of the colour formed is affected significantly by the amount
26、of heat generated during the test. Thus the procedure seeks to control the heat by optimizing the reagent addition sequence and by subsequent incubation of the reaction mixture for a precise interval of time at a known temperature. The sample is pretreated to remove interferences in photographic pro
27、cessing wastes. Sodium arsenite solution is added to the sample to eliminate any residual chlorine present in the sample. Sulfanilic acid in the brucine reagent eliminates nitrite interference. The sample is then reacted with brucine reagent, acidified with sulfuric acid, and incubated for exactly 2
28、0 min in a boiling water bath. The absorbance of the coloured sample is measured at 410 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 test and foo
29、tnotes 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 test procedures, the hazard will be indicated by the word “DANGER” followed by a symbol consisting
30、of angle brackets “” containing a letter which designates the specific 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 disp
31、layed. Furthermore, for a given material, the hazard symbol will be used only once in a single paragraph. Detailed warnings for handling chemicals and their diluted solutions are beyond the scope of this International Standard. Licensed Copy: sheffieldun sheffieldun, na, Sun Nov 26 03:15:27 GMT+00:0
32、0 2006, Uncontrolled Copy, (c) BSI ISO 6850:1994(E) 2 BSI 12-1999 Employers shall provide training and health and safety information in conformance with legal requirements. The hazard code system defined in this International Standard is intended to provide information to the users and is not meant
33、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 cod
34、e 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 co
35、nformity 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 precaution
36、s. 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,
37、ISO 6353-2 and ISO 6353-3. Whenever water is specified without other qualifiers in the test procedures, only distilled water or water of equal purity shall be used. 5.1.3 Strength of solutions 5.1.3.1 Acids and ammonium hydroxide are full strength unless otherwise specified. 5.1.3.2 When a standardi
38、zed solution is required, its concentration is expressed as molarity (mol/l). 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. 5.1.3.3 When a standardized solution is not required, its c
39、oncentration is expressed in grams per litre (g/l) to the appropriate number of significant figures. 5.1.3.4 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 distilled or deionized
40、 water. 5.2 Reagents 5.2.1 Brucine reagent 5.2.1.1 Brucine/sulfanilic acid stock solution Dissolve 1,00 g 0,01 g of brucine sulfate (C23H26N2O4)2.2H2SO47H2O (DANGER: ) and 0,10 g 0,01 g of sulfanilic acid (C6H7NSO3H2O) in 70 ml of hot water in a 150 ml beaker. Then add, from a tip-up pipette (6.6),
41、3 ml of hydrochloric acid, 1,18 g/ml (DANGER: ), cool and dilute to 100 ml. This stock solution shall be stored in a refrigerator, where it is stable for several months. 5.2.1.2 Preparation Prepare the brucine reagent by mixing 25 ml of the brucine/sulfanilic acid stock solution (DANGER: Harmful if
42、inhaled. Avoid breathing dust, vapour, mist or gas. Use only with adequate ventilation. Harmful if contact occurs. Avoid contact with eyes, skin or clothing. Wash thoroughly after handling. Harmful if swallowed. Wash thoroughly after handling. If swallowed, obtain medical attention immediately. May
43、be fatal if swallowed. If swallowed, obtain medical attention immediately. Will burn. Keep away from heat, sparks and open flame. Use with adequate ventilation. Oxidizer. Contact with other material may cause fire. Do not store near combustible materials. Licensed Copy: sheffieldun sheffieldun, na,
44、Sun Nov 26 03:15:27 GMT+00:00 2006, Uncontrolled Copy, (c) BSI ISO 6850:1994(E) BSI 12-19993 5.2.4 Standard nitrate solutions Prepare these from a stock solution of potassium nitrate containing 4,4 g/l nitrate ion (1 g/l of nitrogen) which is prepared from 7,175 g 0,001 g of dried potassium nitrate
45、(KNO3). (This should be dried in an oven at 100 C to 105 C for 2 h.) Transfer quantitatively to a 1 litre one-mark volumetric flask, dissolve in about 800 ml of water, and dilute to the mark. This solution is stable for 6 months. NOTE 1Experience in one laboratory shows that nitrate standards are su
46、bject to biodegradation (nitrification or denitrification) even with refrigeration and can be stabilized by the addition of 1 ml to 2 ml of chloroform per litre. Samples are stabilized by the adjustment of the pH to the range 1 to 2 by the addition of sulfuric acid. Prepare the following standard so
47、lutions by dilution from the stock solution using one-mark pipettes and one-mark volumetric flasks. 5.2.4.1 Nitrate standard, 440 mg/l of nitrate ion. Dilute 50 ml of stock solution (5.2.4) to 500 ml. 5.2.4.2 Nitrate standard, 8,8 mg/l of nitrate ion. Dilute 10 ml of 440 mg/l standard solution (5.2.
48、4.1) to 500 ml. 5.2.4.3 Nitrate standard, 44 mg/l of nitrate ion. Dilute 50 ml of 440 mg/l standard solution (5.2.4.1) to 500 ml. 5.2.4.4 Nitrate standard, 79,2 mg/l of nitrate ion. Dilute 90 ml of 440 mg/l standard solution (5.2.4.1) to 500 ml. 5.2.5 Silver sulfate/ammonia solution Add 23 g of silv
49、er sulfate (Ag2SO4), weighed to the nearest 0,1 g, to 250 ml of water in a 1 litre one-mark volumetric flask. Stir on a magnetic stirrer, and add 700 ml of ammonium hydroxide (NH4OH), 0,91 g/ml (DANGER: ), stirring until all is dissolved. Remove the stirring bar and dilute to the mark with ammonium hydroxide, 0,91 g/ml (). This reagent shall be stored in a tightly stoppered brown reagent bottle. 5.2.6 Sodium arsenite, NaAsO2, 5 g/l solution. Weigh, to the nearest 0,1 g, 5 g of sodium arsenite (DANGER: ) and add to 800 ml of wat
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