1、 ANSI/I3A IT4.101-2002for Photography Processing Chemicals Specifications for Sulfuric AcidANSI/I3AIT4.101-2002ANSI/I3A IT4.101-2002Revision and redesignation ofANSI/NAPM IT4.101-1985 (R1995)American National Standardfor Photography Processing Chemicals Specifications for Sulfuric AcidSecretariatInt
2、ernational Imaging Industry Association, Inc. (I3A)Approved May 16, 2002 American National Standards Institute, Inc.Approval of an American National Standard requires review by ANSI that therequirements for due process, consensus, and other criteria for approval havebeen met by the standards develop
3、er.Consensus is established when, in the judgement of the ANSI Board ofStandards Review, substantial agreement has been reached by directly andmaterially affected interests. Substantial agreement means much more thana simple majority, but not necessarily unanimity. Consensus requires that allviews a
4、nd objections be considered, and that a concerted effort be madetowards their resolution.The use of American National Standards is completely voluntary; theirexistence does not in any respect preclude anyone, whether he has approvedthe standards or not, from manufacturing, marketing, purchasing, or
5、usingproducts, processes, or procedures not conforming to the standards.The American National Standards Institute does not develop standards andwill in no circumstances give an interpretation of any American NationalStandard. Moreover, no person shall have the right or authority to issue aninterpret
6、ation of an American National Standard in the name of the AmericanNational Standards Institute. Requests for interpretations should beaddressed to the secretariat or sponsor whose name appears on the titlepage of this standard.CAUTION NOTICE: This American National Standard may be revised orwithdraw
7、n at any time. The procedures of the American National StandardsInstitute require that action be taken periodically to reaffirm, revise, orwithdraw this standard. Purchasers of American National Standards mayreceive current information on all standards by calling or writing the AmericanNational Stan
8、dards Institute.American National StandardPublished byAmerican National Standards Institute, Inc.25 West 43rd Street, New York, NY 10036Copyright 2002 by American National Standards Institute, Inc.All rights reserved.No part of this publication may be reproduced in anyform, in an electronic retrieva
9、l system or otherwise,without prior written permission of the publisher.Printed in the United States of AmericaiContentsPageForeword ii0 Introduction. iii1 Scope . 12 Normative references . 13 General. 14 Requirements . 15 Reagents and glassware 26 Sampling. 27 Test methods 2Table1 Summary of requir
10、ements 2iiForeword (This foreword is not part of American National Standard ANSI/I3A IT4.101-2002.)This standard is one of a series of standards establishing criteria of purity for chemi-cals used in processing photographic materials. In the current review process, thisseries of standards is being u
11、pdated and revised in format. Many of the standards inthis series, but not all, also exist as standards of the International Organization forStandardization (ISO). The current updates and revisions are in accord with thatdone for the ISO standards. In an effort to promote the concept of internationa
12、l stan-dardization, references to ISO standards have been left in place.Suggestions for the improvement of this standard will be welcome. They should besent to the International Imaging Industry Association, Inc. (I3A), 550 MamaroneckAvenue, Suite 307, Harrison, NY 10528-1615, e-mail: i3astdsi3a.org
13、.This standard was processed and approved for submittal to ANSI by I3A TechnicalCommittee IT4 on Photographic Processing. Committee approval of the standarddoes not necessarily imply that all committee members voted for its approval. At thetime it approved this edition of the standard, the IT4 Commi
14、ttee had the followingmembers:Joseph M. Rao, ChairmanJohn Gignac, SecretaryOrganization Represented Name of RepresentativeInternational Imaging Industry Association, Inc. (I3A) Jan CarlockLinda CrosbyKunihiro FujiwaraRonald A. KleinLaszlo PapaiAnthony Jarkowsky General Chemical Corporation. Mark Dul
15、ikPhotographic Society of America, Inc. . Grant HaistPhoto Marketing Association International Herb SteinIndividual ExpertsPeter KrauseNorman NewmanJoseph M. RaoSubcommittee IT4-1 on Specifications for Photographic Chemicals, which was re-sponsible for this edition, had the following members:Joseph
16、M. Rao, Chairman-protem Jan CarlockLinda CrosbyMark DulikKunihiro FujiwaraNorman NewmanLaszlo PapaiHerb Steiniii0 Introduction0.1 This standard is one of a series that establishes criteria of purity for chemicalsused in processing photographic materials. General test methods and procedures cit-ed in
17、 this standard are compiled in Parts 1, 4, 5, and 6 of ISO 10349.This standard is intended for use by individuals with a working knowledge of analyti-cal techniques, which may not always be the case. Some of the procedures utilizecaustic, toxic, or otherwise hazardous chemicals. Safe laboratory prac
18、tice for thehandling of chemicals requires the use of safety glasses or goggles and other protec-tive apparel such as rubber gloves, face masks or aprons where appropriate.Normal precautions required in the performance of any chemical procedure shall beexercised at all times, but care has been taken
19、 in this standard to provide warningsfor hazardous materials. Hazard warnings designated by a letter enclosed in anglebrackets, , are used as a reminder in those steps detailing handling operationsand are defined in ISO 10349-1. More detailed information regarding hazards, han-dling, and use of thes
20、e chemicals may be available from the manufacturer.0.2 This standard provides chemical and physical requirements for the suitability of aphotographic-grade chemical. The tests correlate with undesirable photographic ef-fects. Purity requirements are set as low as possible consistent with these photo
21、-graphic effects. These criteria are considered the minimum requirements necessaryto assure sufficient purity for use in photographic processing solutions, except that ifthe purity of a commonly available grade of chemical exceeds photographic process-ing requirements and if there is no economic pen
22、alty in its use, the purity require-ments have been set to take advantage of the availability of the higher qualitymaterial.Every effort has been made to keep the number of requirements to a minimum. Inertimpurities are limited to amounts that will not unduly reduce the assay. All tests areperformed
23、 on samples “as received“ to reflect the condition of materials furnished foruse. Although the ultimate criterion for suitability of such a chemical is its successfulperformance in an appropriate use test, the shorter, more economical test methodsdescribed in this standard are generally adequate.Ass
24、ay procedures have been included in all cases where a satisfactory method isavailable. An effective assay requirement serves not only as a safeguard of chemicalpurity, but also as a valuable complement to the identity test. Identity tests have beenincluded whenever a possibility exists that another
25、chemical or mixture of chemicalscould pass the other tests.All requirements listed in clause 4 are mandatory. The physical appearance of thematerial and any footnotes are for general information only and are not part of the re-quirements.0.3 Efforts have been made to employ tests that are capable of
26、 being run in any nor-mally equipped laboratory and, wherever possible, to avoid tests that require highlyspecialized equipment or techniques. Instrumental methods have been specified onlyas alternative methods or alone in those cases where no other satisfactory method isavailable.Over the past few
27、years, great improvements have been made in instrumentation forvarious analyses. Where such techniques have equivalent or greater precision, theymay be used in place of the tests described in this standard. Correlation of such alter-native procedures with the given method is the responsibility of th
28、e user. In case ofdisagreement in results, the method called for in the specification shall prevail.Where a requirement states “to pass test“, however, alternative methods shall not beused.AMERICAN NATIONAL STANDARD ANSI/I3A IT4.101-20021 American National Standard for Photography Processing Chemica
29、ls Specifications for Sulfuric Acid 1 Scope This standard establishes criteria for the purity of photographic-grade sulfuric acid (DANGER:)1)and specifies the tests to be used to determine the purity. 2 Normative references The following standards contain provisions which, through reference in this
30、text, constitute provisions of this standard. At the time of publication, the editions indicated were valid. All standards are subject to revision, and parties to agreements based on this standard are encouraged to investigate the possibility of applying the most recent editions of the standards ind
31、icated below. Members of IEC and ISO maintain registers of currently valid standards. ISO 10349-1:1992, Photography Photographic-grade chemicals Test methods Part 1: General. IS0 10349-4:1992 (R1999), Photography Photographic-grade chemicals Test methods Part 4: Determination of residue after igniti
32、on. ISO 10349-5:1992 (R1999), Photography Photographic-grade chemicals Test methods Part 5: Determination of heavy metals and iron content. ISO 10349-6:1992 (R1999), Photography Photographic-grade chemicals Test methods Part 6: Determination of halide content. 3 General 3.1 Physical properties Sulfu
33、ric acid, H2SO4, is a viscous oily liquid. It has a relative molecular mass of 98.08. 3.2 Hazardous properties Sulfuric acid causes severe skin burns on contact. Refer to the manufacturer for additional information. 3.3 Storage Sulfuric acid shall be stored away from combustible materials. 4 Require
34、ments A summary of the requirements is shown in Table 1. _ 1)Hazard warning codes are defined in ISO 10349-1, clause 4. ANSI/I3A IT4.101-2002 2 Table 1 - Summary of requirements Test Limit Subclause Standard in which test method is given Assay Minimum: 93.0% Maximum: 98.0% 7.1 ANSI/I3A IT4.101 Mass
35、fraction of residue after ignition Maximum: 0.01% 7.2 ISO 10349-4 Mass fraction of heavy metals (as Pb) Maximum: 0.005% 7.3 ISO 10349-5 Mass fraction of iron (Fe) Maximum: 0.005% 7.4 ISO 10349-5 Mass fraction of halides (as Cl-) Maximum: 0.001% 7.5 ISO 10349-6 Substances reducing permanganate To pas
36、s test 7.6 ANSI/I3A IT4.101 Appearance of solution To pass test 7.7 ANSI/I3A IT4.101 5 Reagents and glassware All reagents, materials, and glassware shall conform with the requirements specified in ISO 10349-1 unless otherwise noted. The hazard warning symbols, used as a reminder in those steps deta
37、iling handling operations, are defined in ISO 10349-1. These symbols are used to provide information to the user and are not meant to provide conformance with hazardous labeling requirements, as these vary from country to country. 6 Sampling See ISO 10349-1. 7 Test methods 7.1 Assay 7.1.1 Specificat
38、ion The minimum mass fraction of sulfuric acid shall be 93.0%; the maximum mass fraction shall be 98.0%. 7.1.2 Reagents 7.1.2.1 Methanol, CH3OH 7.1.2.2 Phenolphthalein indicator, 1% alcoholic solution Dissolve 1 g of phenolphthalein in 100 ml of methanol (7.1.2.1). Filter if necessary. 7.1.2.3 Sodiu
39、m hydroxide, NaOH, (DANGER: ), standard volumetric solution of 1 mol/l (40 g/l).2),3)_ 2)Commercially available analyzed reagent solutions are recommended. If solutions are to be prepared, see any quantitative chemistry text. 3)This solution can be prepared from solid sodium hydroxide (DANGER: ). AN
40、SI/I3A IT4.101-2002 3 7.1.3 Procedure Transfer about 30 ml of water to a glass-stoppered flask and weigh to the nearest 0.1 mg. Add about 1 ml of a test portion of the sulfuric acid sample () to the flask and reweigh to the nearest 0.1 mg. Add 2 to 3 drops of phenolphthalein indicator (7.1.2.2) to t
41、he flask. While stirring the solution in the flask without splashing, titrate with 1 mol/l standard sodium hydroxide solution (7.1.2.3) () to the appearance of a pink color that persists for 15 seconds. 7.1.4 Expression of results The assay, expressed as a percentage by mass, of sulfuric acid is giv
42、en by 4.90 cV/m where c is the actual concentration, expressed in moles per liter, of the sodium hydroxide solution (7.1.2.3); V is the volume, expressed in milliliters, of the sodium hydroxide solution used to reach the titration endpoint; m is the mass, expressed in grams, of the test portion; 4.9
43、0 is the conversion factor obtained from the mass of sulfuric acid equivalent to 1 mole of sodium hydroxide (i.e., 49.04) x the conversion factor for milliliters to liters (i.e., 0.001) x 100 (for percentage). 7.2 Mass fraction of residue after ignition 7.2.1 Specification The maximum mass fraction
44、of residue after ignition shall be less than 0.01%. 7.2.2 Procedure Determine the residue after ignition in accordance with ISO 10349-4. Use a test portion of 10 g 0.1 g of the sample () weighed to the nearest 0.1 mg, and incinerate at 600C 50C for 4 hours. Cool the residue in a desiccator and then
45、weigh to the nearest 0.1 mg. Retain this residue for the iron test (7.4). 7.3 Mass fraction of heavy metals 7.3.1 Specification The maximum mass fraction of heavy metals shall be 0.005%. 7.3.2 Procedure NOTE The standard for the iron test (7.4) is prepared in the same way as the heavy metals standar
46、d. Determine the percentage of heavy metals in accordance with ISO 10349-5. Use a test portion corresponding to 1 g 0.1 g of the sample prepared in accordance with ISO 10349-5:1992, 7.2. Use 5 ml of the heavy metal standard prepared in accordance with ISO 10349-5:1992, 8.1.1. 7.4 Mass fraction of ir
47、on 7.4.1 Specification The maximum mass fraction of iron shall be 0.005%. 7.4.2 Procedure Determine the percentage of iron in accordance with ISO 10349-5. Use a test portion of the residue after ignition corresponding to 4 g 0.1 g of the sample prepared in accordance with ISO 10349-5:1992, 7.1, i.e.
48、, 10 ml of the 25 ml residue solution. Use 20 ml of the iron standard prepared in accordance with ISO 10349-5:1992, 8.1.1. ANSI/I3A IT4.101-2002 4 7.5 Mass fraction of halides (as Cl-) 7.5.1 Specification The maximum mass fraction of halides as Cl-shall be 0.001%. 7.5.2 Procedure Determine the perce
49、ntage of halides (expressed as Cl-) in accordance with ISO 10349-6. 7.6 Substances reducing permanganate 7.6.1 Specification The material shall pass the test. 7.6.2 Reagent 7.6.2.1 Potassium permanganate solution, KMnO4(DANGER: ) Dissolve 3.16 g of potassium permanganate () in 1 liter of water. 7.6.3 Procedure Cautiously add 20 ml of the sample () to 60 ml of water in a 100-ml beaker. Cool to room temperature and add 0.05 ml of potassium permanganate solution (), (7.6.2.1). The treated sample solution should remain pink for at lea
