1、 ANSI/I3A IT4.107-2002for Photography Processing Chemicals Specifications for Anhydrous Citric Acid and Citric Acid MonohydrateANSI/I3AIT4.107-2002ANSI/I3A IT4.107-2002Revision and redesignation ofANSI/NAPM IT4.107-1983 (R1995)American National Standardfor Photography Processing Chemicals Specificat
2、ions for Anhydrous Citric Acidand Citric Acid MonohydrateSecretariatInternational Imaging Industry Association, Inc. (I3A)Approved May 21, 2002 American National Standards Institute, Inc.Approval of an American National Standard requires review by ANSI that therequirements for due process, consensus
3、, and other criteria for approval havebeen 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 majo
4、rity, but not necessarily unanimity. Consensus 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 appro
5、vedthe standards or not, from manufacturing, 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. Mor
6、eover, no person shall have the right 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.CA
7、UTION NOTICE: This American National Standard 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 infor
8、mation on all standards by calling or 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 t
9、his publication may be reproduced in anyform, 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 . 25 Reagen
10、ts and glassware 26 Sampling. 27 Test methods 2Table1 Summary of requirements 2iiForeword (This foreword is not part of American National Standard ANSI/I3A IT4.107-2002.)This standard is one of a series of standards establishing criteria of purity for chemi-cals used in processing photographic mater
11、ials. 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 International Organization forStandardization (ISO). The current updates and revisions are in accord with thatdone for
12、 the ISO standards. In an effort to promote the concept of international 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 Mamar
13、oneckAvenue, Suite 307, Harrison, NY 10528-1615; e-mail: i3astdsi3a.org.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 appro
14、val. At thetime it approved this edition of the standard, the IT4 Committee had the followingmembers:Joseph M. Rao, ChairmanJohn Gignac, SecretaryOrganization Represented Name of RepresentativeInternational Imaging Industry Association, Inc. (I3A) Jan CarlockLinda CrosbyKunihiro FujiwaraRonald A. Kl
15、einLaszlo PapaiAnthony Jarkowski General Chemical Corporation. Mark DulikPhotographic Society of America, Inc. . Grant HaistPhoto Marketing Association International Herb SteinIndividual ExpertsPeter KrauseNorman NewmanJoseph M. RaoSubcommittee IT4-1 on Specifications for Photographic Chemicals, whi
16、ch was re-sponsible for this edition, had the following members:Joseph 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 processin
17、g photographic materials. General test methods and procedurescited in this standard are compiled in Parts 1, 4, 5, 6, and 7 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 utili
18、zecaustic, toxic, or otherwise hazardous chemicals. Safe laboratory practice 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 c
19、hemical procedure shall beexercised at all times, but care has been taken 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
20、. More detailed information regarding hazards, han-dling, and use of these 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. P
21、urity requirements are set as low as possible consistent with these photo-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 exce
22、eds photographic process-ing requirements and if there is no economic penalty 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
23、 to amounts that will not unduly reduce the assay. All tests areperformed 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 eco
24、nomical test methodsdescribed in this standard are generally adequate.Assay 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. Ide
25、ntity tests havebeen included whenever a possibility exists that another chemical or 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-
26、quirements.0.3 Efforts have been made to employ tests that are capable of being run 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 thos
27、e cases where no other satisfactorymethod is available.Over the past few 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
28、al-ternative procedures with the given method is the responsibility of the user. In caseof disagreement in results, the method called for in the specification shall prevail.Where a requirement states “to pass test“, however, alterative methods shall not beused.AMERICAN NATIONAL STANDARD ANSI/I3A IT4
29、.107-20021 American National Standard for Photography Processing Chemicals Specifications for Anhydrous Citric Acid and Citric Acid Monohydrate 1 Scope This standard establishes criteria for the purity of photographic-grade citric acid, anhydrous and monohydrate, and specifies the tests to be used t
30、o determine the purity. 2 Normative references The following standards contain provisions which, through reference in this 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 bas
31、ed on this 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 standards. ISO 10349-1:1992, Photography Photographic-grade chemicals Test methods Part 1: General. IS
32、O 10349-4:1992 (R1999), Photography Photographic-grade chemicals Test methods Part 4: Determination of residue after ignition. 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
33、 Photographic-grade chemicals Test methods Part 6: Determination of halide content. ISO 10349-7:1992 (R1999), Photography Photographic-grade chemicals Test methods Part 7: Determination of alkalinity or acidity. 3 General 3.1 Physical properties Anhydrous citric acid, C6H8O7, exists as white or colo
34、rless crystals. It has a relative molecular mass of 192.12. Citric acid monohydrate, C6H8O7H2O, exists as white or colorless crystals. It has a relative molecular mass of 210.14. 3.2 Hazardous properties Anhydrous citric acid and citric acid monohydrate are organic acids that may irritate the eyes.
35、3.3 Storage Citric acid shall be stored in a closed container at room temperature away from combustible material. ANSI/I3A IT4.107-2002 2 4 Requirements A summary of the requirements is shown in Table 1. Table 1 Summary of requirements Test Limit Subclause Standard in which test method is given Assa
36、y Anhydrous Monohydrate Mininum: 99.5% Minimum: 99.5% 7.1 ANSI/I3A IT4.107 Mass fraction of residue after ignition Maximum: 0.05% 7.2 ISO 10349-4 Mass fraction of heavy metals (as Pb) Maximum: 0.001% 7.3 ISO 10349-5 Mass fraction of iron (Fe) Maximum: 0.001% 7.4 ISO 10349-5 Mass fraction of halide (
37、as Cl-) Maximum: 0.005% 7.5 ISO 10349-6 Appearance of solution To pass test 7.6 ANSI/I3A IT4.107 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 thos
38、e steps detailing 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.
39、1 Specification The minimum mass fraction of anhydrous citric acid shall be 99.5%. The minimum mass fraction of citric acid monohydrate shall be 99.5%. 7.1.2 Reagents 7.1.2.1 Carbon-dioxide-free water Prepare carbon-dioxide-free water in accordance with ISO 10349-7:1992, 4.4. 7.1.2.2 Ethanol, C2H5OH
40、, 95% (V/V), denatured 7.1.2.3 Phenolphthalein indicator, ethanol solution Dissolve 0.5 g of phenolphthalein in 50 ml of ethanol (7.1.2.2), then dilute to 100 ml with water. Filter if necessary. ANSI/I3A IT4.107-2002 3 7.1.2.4 Sodium hydroxide, NaOH, (DANGER: )1)standard volumetric solution of 1 mol
41、/l (40/gl). 2), 3)7.1.3 Aparatus 7.1.3.1 Erlenmeyer flask, capacity 125 ml. 7.1.3.2 Pipette, capacity 50 ml. 7.1.3.3 Burette, capacity 50 ml. 7.1.4 Procedure Weigh 2 g of a test portion of the sample to the nearest 0.001 g in a tared 125 ml Erlenmeyer flask (7.1.3.1). Using a pipette (7.1.3.2), add
42、50 ml of carbon dioxide-free water (7.1.2.1) to dissolve the sample. Add 3 drops of phenolphthalein indicator (7.1.2.3) and using the burette (7.1.3.3), titrate with 1 mol/l sodium hydroxide solution (7.1.2.4) () to the first change to a pink color that persists for 30 seconds. 7.1.5 Expression of r
43、esults 7.1.5.1 Anhydrous citric acid The assay, expressed as a percentage by mass, of anhydrous citric acid (C6H8O7) is given by 6.40 cV/m where c is the actual concentration, expressed in moles per liter, of the sodium hydroxide solution (7.1.2.4); V is the volume, expressed in milliliters, of the
44、sodium hydroxide solution (7.1.2.4) used to reach the titration endpoint; m is the mass, expressed in grams, of the test portion; 6.40 is a conversion factor obtained from the mass of anhydrous citric acid equivalent to 1 mole of sodium hydroxide (i.e., 64.04) x the conversion factor for milliliters
45、 to liters (i.e., 0.001) x 100 (for percentage). 7.1.5.2 Citric acid monohydrate The assay, expressed as a percentage by mass, of citric acid monohydrate (C6H8O7H2O) is given by 7.01 cV/m where c is the actual concentration, expressed in moles per liter, of the sodium hydroxide solution (7.1.2.4); V
46、 is the volume, expressed in milliliters, of the sodium hydroxide solution (7.1.2.4) used to reach the titration endpoint; m is the mass, expressed in grams, of the test portion; 7.01 is a conversion factor obtained from the mass of citric acid monohydrate equivalent to 1 mole of sodium hydroxide (i
47、.e., 70.05) x the conversion factor for milliliters to liters (i.e., 0.001) x 100 (for percentage). _ 1)Hazard warning codes are defined in ISO 10349-1, clause 4. 2)Commercially available analyzed reagent solutions are recommended. If solutions are to be prepared, see any quantitative chemistry text
48、. 3)This solution can be prepared from solid sodium hydroxide (DANGER: ). ANSI/I3A IT4.107-2002 4 7.2 Mass fraction of residue after ignition 7.2.1 Specification The maximum mass fraction of residue after ignition shall be 0.05%. 7.2.2 Procedure Determine the residue after ignition in accordance wit
49、h 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 600oC + 50oC for 4 hours. Cool the residue in a desiccator and then weigh to the nearest 0.1 mg. Retain this residue for the heavy metals (7.3) and iron (7.4) tests. 7.3 Mass fraction of heavy metals 7.3.1 Specification The maximum mass fraction of heavy metals shall be 0.001%. 7.3.2 Procedure NOTE The standard for the iron test (7.4) is prepared in the same way as the heavy metals standard. Determine the percentage of heavy metals
