1、 ANSI/I3A IT4.129-2002for Photography Processing Chemicals Specifications for p-Aminophenol HydrochlorideANSI/I3AIT4.129-2002ANSI/I3A IT4.129-2002Revision and redesignation ofANSI/NAPM IT4.129-1985 (R1995)American National Standardfor Photography Processing Chemicals Specifications for p-Aminophenol
2、 HydrochlorideSecretariatInternational Imaging Industry Association, Inc. (I3A)Approved February 13, 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 have
3、been met by the standards developer.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. C
4、onsensus requires that allviews and 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 manufact
5、uring, marketing, purchasing, or 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
6、or authority to issue aninterpretation 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 S
7、tandard may be revised orwithdrawn 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
8、writing the AmericanNational Standards 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 a
9、nyform, in an electronic retrieval 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
10、methods 2Table1 Summary of requirements 2Figure1 Reference infrared spectrum of p-aminophenol hydrochloride (KBr plate) 7AnnexA Preparation of standard ammonium cerium (IV) hexanitrate solution 8iiForeword (This foreword is not part of American National Standard ANSI/I3A IT4.129-2002.)This standard
11、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 updated and revised in format. Many of the standards inthis series, but not all, also exist as standards of the In
12、ternational 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 international stan-dardization, references to ISO standards have been left in place.This standard contains one annex, which i
13、s informative and is not considered part ofthis standard.Suggestions for the improvement of this standard will be welcome. They should besent to the International Imaging Industry Association (I3A), 550 Mamaroneck Ave-nue, Suite 307, Harrison, NY 10528-1216, e-mail: i3astdsi3a.org.This standard was
14、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 Committee had the follow
15、ingmembers:Joseph M Rao, ChairmanJohn Gignac, SecretaryOrganization Represented Name of RepresentativeInternational Imaging Industry Association (I3A) . Jan CarlockLinda CrosbyKunihiro FujiwaraRonald A. KleinLaszlo PapaiAnthony JarkowskiGeneral Chemical Corporation. Mark DulikPhoto Marketing Associa
16、tion International . Herb SteinPhotographic Society of America, Inc. . Grant HaistIndividual ExpertsPeter KrauseNorman NewmanJoseph M. RaoSubcommittee IT4-1 on Specifications for Photographic Chemicals, which was re-sponsible for this edition, had the following members:Joseph M. Rao, Chairman-protem
17、 Jan CarlockLinda CrosbyMark DulikKunihiro FujiwaraNorman NewmanLaszlo PapaiJoseph M. RaoHerb 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 procedurescited in this standa
18、rd are compiled in Parts 1, 4, 5, and 8 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 practice for the
19、handling of chemicals requires the use of safety glasses or goggles, and other pro-tective 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 in this st
20、andard 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 these chemicals
21、 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-graphic ef
22、fects. 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 penalty in its
23、 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 on samples
24、 “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.Assay procedur
25、es 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 havebeen included whenever a possibility exists that another chemical or
26、 mixture ofchemicals could 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 being run
27、in any nor-mally equipped laboratory and, wherever possible, to avoid tests that require highlyspecialized equipment or techniques. Instrumental methods have been specifiedonly as alternative methods or alone in those cases where no other satisfactorymethod is available.Over the past few years, grea
28、t 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 al-ternative procedures with the given method is the responsibility of the user. In
29、caseof disagreement 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 IT4.129-2002American National Standard for Photography Processing Chemicals Specificat
30、ions for p-Aminophenol Hydrochloride 1 1 Scope This standard establishes criteria for the purity of photographic-grade p-aminophenol (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
31、 this text, constitute provi-sions 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 in-vestigate the possibility of applying the most recent editions of the stand
32、ards indicated below. Members of IEC and ISO maintain registers of currently valid standards. ISO 10349-1:1992, Photography Photographic-grade chemicals Test methods Part 1: Gen-eral ISO 10349-4:1992 (R1999), Photography Photographic-grade chemicals Test methods Part 4: Determination of residue afte
33、r ignition ISO 10349-5:1992 (R1999), Photography Photographic-grade chemicals Test methods Part 5: Determination of heavy metals and iron content ISO 10349-8:1992, Photography Photographic-grade chemicals Test methods Part 8: De-termination of volatile matter 3 General 3.1 Physical properties p-Amin
34、ophenol hydrochloride (HOC6H4NH2HCI), exists as a white to light-tan crystalline powder. It has a relative molecular mass of 145.59. 3.2 Hazardous properties p-Aminophenol hydrochloride is moderately toxic and can act as an allergen and skin irritant. 3.3 Storage -Aminophenol hydrochloride shall be
35、stored in a closed container at room temperature away from strong oxidizing agents. 4 Requirements A summary of the requirements is shown in Table 1. _ 1)Hazard warning codes are defined in ISO 10349-1, clause 4. ANSI/I3A IT4.129-2002 2 Table 1 Summary of requirements Test Limit Subclause Standard i
36、n which test method is given Assay: Ceric titration or Alkali titration 98.0% (m/m) min. 99.0% (m/m) min. 7.1.4.1 7.1.4.2 ANSI/I3A IT4.129 ANSI/I3A IT4.129 Solubility in water To pass test. 7.2 ANSI/I3A IT4.129 Sulfate To pass test. 7.3 ANSI/I3A IT4.129 Ammonia To pass test. 7.4 ANSI/I3A IT4.129 Res
37、idue after ignition 2.0% (m/m) max. 7.5 ISO 10349-4 Heavy metals (as Pb) 0.001% (m/m) max. 7.6 ISO 10349-5 Iron (Fe) 0.005% (m/m) max. 7.7 ISO 10349-5 Volatile matter 0.5% (m/m) max. 7.8 ISO 10349-8 Identity: Mixed melting point or Infrared spectrum To pass test. Equivalent to Figure 1. 7.9.4.1 7.9.
38、4.2 ANSI/I3A IT4.12 ANSI/I3A IT4.129 NOTE m/m = mass/mass 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 detailing handling operations,
39、are defined in ISO 10349-1. These symbols are used to pro-vide 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 Specification 7.1.1.1 Minimum conten
40、t of p-aminophenol hydrochloride (HOC6H4NH2HCl) by ceric titration shall be 98.0% (m/m). 7.1.1.2 Minimum content of p-aminophenol hydrochloride (HOC6H4NH2HCl) by alkali titration shall be 99.0% (m/m). ANSI/I3A IT4.129-2002 3 7.1.2 Reagents 7.1.2.1 Ammonium cerium (IV) hexanitrate, (NH4)2Ce(NO3)6, 0.
41、100 mol/l (54.82 g/l)2),3)7.1.2.2 Sulfuric acid solution, H2SO4, (1+70) With constant stirring, slowly add 2 ml of sulfuric acid 1.84 g/ml (DANGER:) to 140 ml of water. 7.1.2.3 Ferrous sulfate, FeSO4, 0.025 mol/l (3.80 g/l) Dissolve 4.25 g of FeSO4H2O in 1 liter of water. Alternatively, either 5.60
42、g of FeSO44H2O, 6.05 g of FeSO45H2O or 6.95 g of FeSO47H2O may be used. 7.1.2.4 Ferroin indicator, tris(1,10-phenathroline) iron (II) ion. Dissolve 1.48 g of 1,10-phenanthroline in 100 ml of the 0.025 mol/l ferrous sulfate solution (7.1.2.3). 7.1.2.5 Sodium hydroxide, NaOH, standard volumetric solut
43、ion of 0.1 mol/l (4.0 g/l)2), 4)7.1.2.6 Acetone, CH3COCH3, 100% (DANGER: ) 7.1.3 Apparatus 7.1.3.1 Glass electrode 7.1.3.2 Calomel electrode 7.1.4 Procedure 7.1.4.1 Ceric titration Weigh about 0.28 g of a test portion of the sample (DANGER:, ) to the nearest 0.1 mg, and quantitatively transfer it to
44、 a 250-ml Erlenmeyer flask containing 100 ml of dilute sulfuric acid (7.1.2.2). After the sample is dissolved, add 1 drop of ferroin indicator (7.1.2.4) and titrate with ammonium cerium (IV) hexanitrate (7.1.2.1) to a change in color from orange to blue. 7.1.4.2 Alkali titration Weigh about 0.4 g of
45、 a test portion of the sample (, ) to the nearest 0.1 mg and quantita-tively transfer it to a 250-ml beaker containing 10 ml of water. After the sample is dissolved, add 90 ml of acetone (7.1.2.6) () and titrate potentiometrically with 0.1 mol/l standard sodium hydroxide solution (7.1.2.5) using gla
46、ss (7.1.3.1) and calomel (7.1.3.2) electrodes. In a similar manner, titrate a blank consisting of 10 ml of water and 90 ml of acetone (7.1.2.6) () as above without the sample. Plot the titration curves and determine the inflection points. _ 2)Commercially available analyzed reagent solutions are rec
47、ommended. If solutions are to be prepared, see any quantitative chemistry text. 3)See annex A for preparation and standardization of this solution. 4)This solution can be prepared from solid sodium hydroxide (DANGER: ). ANSI/I3A IT4.129-2002 4 7.1.5 Expression of results 7.1.5.1 Ceric titration The
48、assay, expressed as a percentage by mass, of p-aminophenol hydrochloride (HOC6H4NH2HCl) is given by 7.28 cV/m where c is the actual concentration, expressed in moles per liter, of the ammonium cerium (IV) hexanitrate (7.1.2.1); V is the volume, in milliliters, of the ammonium cerium (IV) hexanitrate
49、 (7.1.2.1) used to reach the titration endpoint; m is the mass, in grams, of the test portion; 7.28 is the conversion factor obtained from the mass of ammonium cerium (IV) hex-anitrate equivalent to 1 mole of p-aminophenol hydrochloride (i.e., 72.80) x the conversion for milliliters to liters (i.e., 0.001) x 100 (for percentage). 7.1.5.2 Alkali titration The assay, expressed as a percentage by mass, of p-aminophenol hydrochloride (HOC6H4NH2HCl) is given by 14.56c (V1 - V2) /m where c is the actual concentration, expressed in mol
