1、BRITISH STANDARD BS ISO 10349-13:2002 Photography Photographic-grade chemicals Test methods Part 13: Determination of pH ICS 37.040.30 BS ISO 10349-13:2002 This British Standard, having been prepared under the direction of the Consumer Products and Services Sector Policy and Strategy Committee, was
2、published under the authority of the Standards Policy and Strategy Committee on 11 December 2002 BSI 11 December 2002 ISBN 0 580 40929 5 National foreword This British Standard reproduces verbatim ISO 10349-13:2002 and implements it as the UK national standard. The UK participation in its preparatio
3、n was entrusted to Technical Committee CPW/42, Photography, which has the responsibility to: A list of organizations represented on this committee can be obtained on request to its secretary. Cross-references The British Standards which implement international publications referred to in this docume
4、nt may be found in the BSI Catalogue under the section entitled “International Standards Correspondence Index”, or by using the “Search” facility of the BSI Electronic Catalogue or of British Standards Online. This publication does not purport to include all the necessary provisions of a contract. U
5、sers are responsible for its correct application. Compliance with a British Standard does not of itself confer immunity from legal obligations. aid enquirers to understand the text; present to the responsible international/European committee any enquiries on the interpretation, or proposals for chan
6、ge, and keep the UK interests informed; monitor related international and European developments and promulgate them in the UK. Summary of pages This document comprises a front cover, an inside front cover, the ISO title page, pages ii to iv, pages 1 to 4, an inside back cover and a back cover. The B
7、SI copyright date displayed in this document indicates when the document was last issued. Amendments issued since publication Amd. No. Date CommentsINTERNATIONAL STANDARD ISO 10349-13 First edition 2002-11-15 Reference number ISO 10349-13:2002(E) Photography Photographic-grade chemicals Test methods
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13、11 Fxa + 14 47 2290 9 74 E-liam cpoyrigthsio.ch Web wwwsi.oc.h BSISO1034913:2002iiContents Page 1 Scope . 1 2 Normative reference . 1 3 Term and definition . 1 4 Hazards 1 5 Reagents 1 6 Apparatus . 2 7 Sampling . 2 8 Procedure . 2 8.1 Calibration and standardization . 2 8.2 pH measurement . 3 9 Tes
14、t report 3 Annex A Electrode care. 4 BSISO1034913:2002iiiForeword 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 committee
15、s. 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 Inter
16、national Electrotechnical Commission (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 bodi
17、es for voting. Publication 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 part of ISO 10349 may be the subject of patent rights. ISO shall not be held responsible for identif
18、ying any or all such patent rights. International Standard ISO 10349-13 was prepared by Technical Committee ISO/TC 42, Photography. ISO 10349 consists of the following parts, under the general title Photography Photographic-grade chemicals Test methods: Part 1: General Part 2: Determination of matte
19、r insoluble in water Part 3: Determination of matter insoluble in ammonium hydroxide solution Part 4: Determination of residue after ignition Part 5: Determination of heavy metals and iron content Part 6: Determination of halide content Part 7: Determination of alkalinity or acidity Part 8: Determin
20、ation of volatile matter Part 9: Reaction to ammoniacal silver nitrate Part 10: Determination of sulfide content Part 11: Determination of specific gravity Part 12: Determination of density Part 13: Determination of pH Annex A of this part of ISO 10349 is for information only. BSISO1034913:2002ivANR
21、ETNIITOTS LANDNADRA OSI 11-94302002:3)E( Photography Photographic-grade chemicals Test methods Part 13: Determination of pH 1 Scope This part of ISO 10349 specifies a general test method for the determination of pH of solutions of photographic-grade chemicals to within units. This method is not inte
22、nded to monitor the pH of formulated solutions used directly in photographic processing, e.g. developers. 2 Normative reference The following normative document contains provisions which, through reference in this text, constitute provisions of this part of ISO 10349. For dated references, subsequen
23、t amendments to, or revisions of, this publication do not apply. However, parties to agreements based on this part of ISO 10349 are encouraged to investigate the possibility of applying the most recent edition of the normative document indicated below. For undated references, the latest edition of t
24、he normative document referred to applies. Members of ISO and IEC maintain registers of currently valid International Standards. ISO 10349-1: 1) , Photography Photographic-grade chemicals Test methods Part 1: General 3 Term and definition For the purposes of this part of ISO 10349, the following ter
25、m and definition apply. 3.1 calibration buffers materials, purchased from various chemical supply sources, that are used to calibrate the pH meter in preparation for measuring samples 4 Hazards General hazard warnings for the handling of chemicals are specified in ISO 10349-1. 5R e a g e n t s 5.1 C
26、alibration buffers 5.1.1 pH 4,0 buffer solution Potassium hydrogen phthalate based, with an accuracy of units. Available from several vendors. 1) To be published. (Revision of ISO 10349-1:1992) 0,1 pH 0,01 pH BSISO1034913:200215.1.2 pH 7,0 buffer solution Potassium/sodium phosphate based, with an ac
27、curacy of units. Available from several vendors. 5.1.3 pH 10,0 buffer solution Potassium carbonate/borate hydroxide based, with an accuracy of units. Available from several vendors. 6 Apparatus All glassware subject to heating shall be of heat-resistant borosilicate glass 2) . Pipettes and other vol
28、umetric glassware shall meet the requirements specified in ISO 10349-1. 6.1 pH meter, with resolution/accuracy of at least units. 6.2 Electrodes, pH glass electrode with a range of 0 to 14; an accuracy of units minimum; a sodium error of units minimum; and a suitable reference electrode with appropr
29、iate filling solutions. The choice of the reference electrode can be critical to the application and shall be chosen accordingly. For routine measurements of solutions with a pH value greater than 10, a sodium-corrected electrode is strongly recommended. NOTE A combination electrode may be used in p
30、lace of a glass/reference pair. The same considerations apply when choosing the electrode. 6.3 Constant temperature water-bath, with pump and heating system designed to maintain a circulating current and constant temperature ( ). The bath shall be deep enough to keep the part of the sample container
31、 that is filled with the sample below the surface of the water. The bath temperature shall be set at . 7 Sampling Sampling shall be in accordance with ISO 10349-1. 8 Procedure 8.1 Calibration and standardization 8.1.1 Consult the manufacturers instruction manual for proper set-up and initial conditi
32、ons of the pH meter (6.1). 8.1.2 Rinse the electrodes (6.2) with water and blot excess water from the tip of the electrode with a soft tissue, taking care not to rub the tissue against the electrode membrane surface. It should be sufficient to hold the tissue near the surface of the electrode and al
33、low water to be drawn into it. Immerse the electrodes into the pH 7,0 buffer solution (5.1.2). Wait for the electrodes to equilibrate and the pH- meter reading to stabilize. If needed, adjust the “calibration control” of the pH meter to obtain the assigned buffer value. 2) Pyrex is an example of sui
34、table glassware available commercially. This information is given for the convenience of the users of this part of ISO 10349 and does not constitute an endorsement by ISO of this product. 0,01 pH 0,01 pH 0,01 pH 0,02 pH 0,05 pH 1 C 25 C 2 min BSISO1034913:200228.1.3 Rinse the electrodes with water a
35、nd blot dry. For low pH samples, immerse the electrodes into the pH 4,0 buffer solution (5.1.1). For high pH samples, immerse the electrodes into the pH 10,0 buffer solution (5.1.3). Wait for the electrodes to equilibrate and the pH-meter reading to stabilize. If needed, adjust the “slope control” o
36、f the pH meter to obtain the assigned buffer value. Note the slope value for this electrode pair. If this value drops below , repeat the calibration. If the slope remains below , corrective action should be performed before any samples are tested (see annex A). 8.1.4 Rinse the electrodes with water;
37、 blot dry and proceed with sample measurements or properly store the electrodes for future use. 8.1.5 Calibration of the pH meter shall be done just prior to sample measurement. 8.1.6 Calibration buffers (5.1) shall be replaced daily. 8.2 pH measurement 8.2.1 After temperature equilibration and cali
38、bration of the pH meter for the desired pH range, the pH of the sample may be determined. 8.2.2 Weigh the test portion specified in the appropriate International Standard, transfer it to a beaker, and dissolve the sample in of freshly boiled and cooled water. 8.2.3 Rinse the electrodes with water an
39、d blot dry. Immerse the electrodes into the sample to be measured and waitfor the electrodes to equilibrate and the pH meter reading to stabilize. 8.2.4 Record the pH of the solution to the nearest 0,1 pH units. 9 Test report The test report shall specify the method used and the test result obtained
40、. It shall also mention all operating details not specified in this part of ISO 10349, or regarded as optional, together with details of any incidents which may have influenced the test result. The test report shall include all information necessary for the complete identification of the sample. 2 m
41、in 95 % 95 % 100 ml 50 ml 2 min BSISO1034913:20023Annex A (informative) Electrode care A.1 Storage There is much conflicting information on suitable storage solutions for glass electrodes. Follow the manufacturers recommendation for electrode care when possible. When the electrode pair is out of ser
42、vice, it is recommended that the pH 7 phosphate buffer be used for glass- electrode storage, and the potassium chloride buffer for reference electrode storage. For temporary storage of the electrode pair between measurements, use a storage buffer consisting of potassium chloride in a pH 7 phosphate
43、buffer. A.2 pH electrodes Preconditioning/rejuvenation Follow the manufacturers recommendations for preconditioning the glass pH electrodes. A minimum soaking time ofin the pH 7 phosphate buffer is recommended before use for pH measurement; overnight soaking is better. Take the following rejuvenatin
44、g steps if an electrode fails to meet the slope criterion, cannot achieve the assigned buffer values, or gives an unsatisfactory value when the control buffer is measured. a) Detach the electrode leads from the pH meter (6.1). b) Place the glass electrode tip in hydrochloric acid for , followed by i
45、n sodium hydroxide. Return the electrode (6.2) to hydrochloric acid for an additional . Rinse the electrode with water. c) Soak the electrode in the pH 7,0 buffer solution (5.1.2) for . d) Reconnect the electrode and try another calibration. If there is no improvement, discard the electrode. NOTE Mo
46、re severe reconditioning procedures are not recommended, due to both the toxicity of required reagents and the cost in analyst time versus the cost of electrode replacement. e) If there is an improvement but the electrode is still not reading the required values, repeat the sodium hydroxide and hydr
47、ochloric acid soaks and try another calibration. If there is no improvement, discard the electrode. A.3 Reference electrode Care/rejuvenation A.3.1 Calomel reference electrode Before putting a new calomel reference electrode into service, withdraw the saturated potassium chloride filling solution an
48、d refill with potassium chloride solution. The lower salt concentration produces less crystallization inside the electrodes and in the reference junction. At the beginning of each shift or day, withdraw the potassium chloride filling solution and refill the electrode with freshpotassium chloride sol
49、ution. A.3.2 Silver/silver chloride electrodes Before putting a new silver/silver chloride reference electrode into service, withdraw the saturated potassium chloride filling solution and refill with potassium chloride solution saturated with silver chloride (the potassium 3,5 mol/l 0,1 mol/l 2h 1,0 mol/l 5 min 5 min 1,0 mol/l 1,0 mol/l 5 min 2h 3,5 mol/l 3,5 mol/l 3,5 mol/l BSISO10349
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