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D EUTSCHE NORM October 2000

Photography
Processed silver-gelatin type black-and-white film {
Specifications for stability
(ISO 10602 : 1995) ISO 10602
ICS 37.040.20 Supersedes DIN 19070-1,
September 1985 edition.

Photographie – Verarbeitete Schwarzweißfilme vom Silber-Gelatine-Typ


– Festlegungen für die Haltbarkeit (ISO 10602 : 1995)

This standard incorporates International Standard


ISO 10602 Photography – Processed silver-gelatin type black-and-white film – Specifications for stability.

A comma is used as the decimal marker.

National foreword
This standard has been prepared by ISO/TC 42 ‘Photography’, WG 5 ‘Physical properties and storage of
photographic materials’.
The responsible German body involved in its preparation was the Normenausschuss Bild und Film
(Cinematography and Photography Standards Committee), Technical Committee Physikalische Eigen-
schaften und Lagerung von strahlungsempfindlichen Materialien sowie Photochemikalien.
The DIN Standards corresponding to the International Standards referred to in clause 2 of the ISO Standard
are as follows:
ISO Standard DIN Standard(s)
ISO 5-1 DIN 4512-7, DIN 4512-8, and DIN 4512-9
ISO 5-2 DIN 4512-8
ISO 5-3 DIN 4512-8 and DIN 4512-9
ISO 527-3 DIN EN ISO 527-3
ISO 543 DIN 15551-1
ISO 5466 DIN 19070-3
ISO 10214 DIN ISO 10214
ISO 18917 DIN 19069

Amendments
DIN 19070-1, September 1985 edition, has been superseded by the specifications of DIN ISO 10602.

Previous editions
DIN 19070-1: 1978-08, 1985-09; DIN 19070-2: 1978-08.

Continued overleaf.
ISO Standard comprises 22 pages.

© No part of this standard may be reproduced without the prior permission of Ref. No. DIN ISO 10602 : 2000-10
DIN Deutsches Institut für Normung e. V., Berlin. Beuth Verlag GmbH, 10772 Berlin, Germany, English price group 15 Sales No. 0415
has the exclusive right of sale for German Standards (DIN-Normen).
04.01
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DIN ISO 10602 : 2000-10

National Annex NA
Standards referred to
(and not included in Normative references)
DIN 4512-7 Determination of optical density in photographic sensitometry – Concepts, symbols and
notations
DIN 4512-8 Determination of optical density in photographic sensitometry – Geometric conditions for
transmission density
DIN 4512-9 Determination of optical density – Spectral conditions
DIN 15551-1 Radiation-sensitive safety films – Concepts, requirements and testing
DIN 19069 Determination of thiosulphate and other residual chemicals in processed photographic
films, plates and papers – Iodine amylose method, methylene blue method and silver
densitometric method
DIN 19070-3 Storage quality of processed photosensitive materials – Preservation of processed safety
films
DIN EN ISO 527-3 Plastics - Determination of tensile properties – Part 3: Test conditions for films and sheets
(ISO 527-3 : 1995)
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ISO 10602 : 1995

Photography
Processed silver-gelatin type black-and-white film
Specifications for stability

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ISO 10602 : 1995

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ISO 10602 : 1995

Foreword
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 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-governmental, in liaison with ISO, also take part in the work. ISO
collaborates closely with the International Electrotechnical Commission
(lEC) on all matters of electrotechnical standardization.

Draft International Standards adopted by the technical committees are


circulated to the member bodies for voting. Publication as an International
Standard requires approval by at least 75 % of the member bodies casting
a vote.

International Standard ISO 10602 was prepared by Technical Committee


ISOfTC 42, Photography.

This second edition cancels and replaces the first edition


(ISO 10602: 1993), which has been technically revised .

Annex A forms an integral part of this International Standard. Annexes B,


C, D, E, F and G are tor information only.
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ISO 10602 : 1995

Introduction

Since 1930 great advances have been made in the use of photographic
films for the preservation of records. The preservation of film records by
governments, banks, insurance companies, industry and other enterprises
has been stimulated by a recognition of the economies in storage space,
organization, accessibility and ease of reproduction that result from the
use of film records.

During the early development period of the art of copying documents,


35 mm nitrate motion-picture film was sometimes used. This material is
highly flammable and is not a safety film as specified in ISO 543. Nitrate
film is not acceptable for any record film. The manufacture of nitrate
film declined after World War II and was discontinued in most countries
in the 1950's.

For many years the only safety films in commercial use were made on
some type of cellulose ester base, such as cellulose acetate, cellulose
acetate propionate or cellulose acetate butyrate. The useful life of safety
cellulose-ester-type films is somewhat conjectural, since actual experience
with commercial material extends back only to about 1908. However,
these materials show severe degradation when exposed to high tem-
peratures and particularly to high humidities. Laboratory incubation studies
predict a usefullife of at least a century when sto red under recommended
conditions[1]. [2]. [3]. [4J.

A second type of polymer safety film base belonging to the polyester


class, known chemically as poly(ethylene terephthalatel. was introduced
commercially in 1956. This material has a number of advantages over the
cellulose ester base such as greater strength, stiffness, tear resistance,
flexibility, dimensional stability and other characteristics, which make it
superior for many photographic applications[5], [6J. Actual experience with
polyester film is considerably less than with cellulose ester film although
this material has been used for over 35 years.

Practical experience to date and accelerated ageing tests indicate that this
film support is more stable than safety cellulose ester film base and is
expected to have a useful life of 500 years[1], [4J.

This second edition eliminates the film classifications of "archival",


"Iong-term" and "medium-term" and replaces them with the LE (Iife ex-
pectancy) rating. In addition, residual hypo limits and image-stability tests
are given for radiographic film, microfilm and all other films.

Studies on the stability of silver-gelatin-type films have investigated the


effect of residual hypo on the image permanence of radiographic films[7],
microfilms[8] and aerial films[9J. This work suggested modifications to the
residual hypo limits and a more quantitative image-stability test was in-
cluded in the first edition of ISO 10602. Residual hypo limits and image-
stability tests are now included for all film categories.
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ISO 10602 : 1995

Former annex O, "Microsocopic spots and blemishes", and annex E,


"Emulsion adhesion", have been eliminated; an annex F, "Accelerated
image-stability test for aerial films", has been added.
This International Standard identifies certain hazards to permanence at-
tributable to the chemical or physical characteristics of processed film and
gives methods of evaluating them. So me of these characteristics are the
responsibility of the film manufacturer, some of the film processor, and
some are influenced by both. However, specifying the chemical and
physical characteristics of the material does not, by itself, ensure satis-
factory keeping behaviour. It is essential to provide proper storage tem-
perature and humidity, and protection from the hazards of fire, water,
fungus and certain atmospheric pollutants. It is important that films be
sto red under the conditions specified in ISO 5466 and ISO 10214.

1 Scope 2 Normative references

1.1 This International Standard establishes the


specifications for photographic films intended for the The following standards contain provlslons which,
storage of records. through reference in this text, constitute provisions
of this International Standard. At the time of publi-
1.2 It applies specifically to films with a base of cation, the editions indicated were valid. AII standards
safety cellulose ester or polyester [poly(ethylene are subject to revision, and parties to agreements
terephthalate)] having silver-gelatin emulsions, pro- based on this International Standard are encouraged
cessed to produce a black-and-white silver image by to investigate the possibility of applying the most re-
negative or full-reversal processing . It applies to film cent editions of the standards indicated below.
processed by a monobath which includes thiosulfate Members of lEC and ISO maintain registers of cur-
as the fixing agent followed by a conventional wash. rently valid International Standards.
It also applies to silver films given a stabilizing treat-
ment by partial or full conversion to silver sulfide, sil- ISO 5-1 : 1984, Photography - Density measurements
- Part 1: Terms, symbo/s and notations.
ver selenide or gold.
ISO 5-2: 1991, Photography - Density measurements
1.3 This International Standard does not apply to - Part 2: Geometric conditions for transmission
films with colour images of any type, nor to films with density.
a magnetic recording track. It does not apply to films
with silver images produced by dry or thermal pro- ISO 5-3:-2), Photography - Density measurements
cessing or by diffusion-reversal processing . It does - Part 3: Spectra/ conditions.
not apply to films that have been processed by a
monobath using other than a thiosulfate-type fixing ISO 417: 1993, Photography - Determination of re-
solution . It is not applicable to films where the silver sidua/ thiosu/fate and other re/ated chemica/s in pro-
salts are removed by means other than thiosulfate cessed photographic materia/s - Methods using
solutions[10J. iodine-amy/ose, methy/ene b/ue and si/ver su/fideo

ISO 543: 1990, Photography - Photographic fi/ms -


1.4 This International Standard does not apply to
Specifications for safety film.
films to which lacquers have been applied .
ISO 1184: 1983, P/astics - Determination of tensi/e
1.5 This 1nternational Standard applies to films properties of fi/ms.
having ultrasonic or dielectric (induction heated)
splices. It does not cover films with splices made by ISO 5466:1992, Photography - Processed safety
means of adhesive tape or solvent-type splices.1) photographic fi/ms - Storage practices.

1) Solvent-type splices are suspect since they may retain traces of residual solvents containing peroxide which can pose some
risk of oxidative attack on the silver image.
2) To be published. (Revision of ISO 5-3: 1984)
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ISO 10602 : 1995

ISO 10214:1991, Photography - Processed photo- NOTE 4 Antihalation or other layers removed in process-
graphic materials - Filing ene/osures for storage. ing are excluded from this definition.

3.9 safety photographic film: Photographic film


which passes the ignition time test and burning time
3 Definitions
test as specified in ISO 543.
For the purposes of this International Standard, the
3.10 safety cellulose-ester base: A film base com-
definitions given in ISO 5-1 and the following defi-
posed mainly of the cellulose esters of acetic,
nitions apply.
propionic or butyric acids, or mixtures thereof.
3.1 archival medium: A recording material that can
3.11 safety poly(ethylene terephthalate) base: A
be expected to retain information forever so that it
polyester film base composed mainly of a polymer of
can be retrieved without significant loss when prop-
ethylene glycol and terephthalic acid .
erly stored.
3.12 full-reversal processing: Processing that in-
NOTE 1 There is, however, no such material and it is not
a term to be used in International Standards or system
eludes development, bleach, clear, re-exposure and
specifications. second development, followed by fi xing and washing.

3.2 life expectancy (LE): The length of time that 4 Safety and hazards
information is predicted to be retrievable in a system
under extended-term storage conditions. 4.1 Hazard warnings
NOTE 2 However, the actual useful life of film is very
Some of the chemicals specified in the test pro-
dependent upon the existing storage conditions (see
cedures are caustic, toxic or otherwise hazardous.
ISO 5466 and ISO 10214).
Safe laboratory practice for the handling of chemicals
requires the use of safety glasses or goggles, rubber
3.3 LE designation: A rating for the "Iife
gloves and other protective apparel such as face
expectancy" of recording materials and associated
masks or aprons where appropriate. Specific danger
retrieval systems. The number following the LE sym-
notices are given in the text and footnotes for par-
bol is a prediction of the minimum life expectancy, in
ticularly dangerous materials, but normal precautions
years, for which information can be retrieved without
are required during the performance of any chemical
significant loss when stored under extended term
procedures at all times . The first time that a hazardous
storage conditions.
material is noted in the test procedure section, the
NOTE 3 For example, LE-100 indicates that information hazard will be indicated by the word "DANGER" fol-
can be retrieved for at least 100 years' storage. lowed by a symbol consisting of angle brackets
"< >" containing a letter which designates the
3.4 extended-ter m storage conditions: Storage specific hazard. A double bracket " « »" will be
conditions suitable for the preservation of recorded used for particularly perilous situations . In subsequent
information having permanent value. statements involving handling of these hazardous
materials, only the hazard symbol consisting of the
3.5 medium-term storage conditions: Storage brackets and letter(s) will be displayed. Furthermore,
conditions suitable for the preservation of recorded for a given material, the hazard symbol will be used
information for a minimum of 10 years. only once in a single paragraph.

Detailed warnings for handling chemicals and their


3.6 film base: The plastic support for the emulsion
diluted solutions are beyond the scope of this Inter-
and backing layers.
national Standard .
3.7 emulsion layers(s): The image or image- Employers shall provide training and health and
forming layer(s) of photographic films, papers and safety information in conformance with legal re-
plates. quirements.

3.8 noncurl backing layer: A layer, usually made The hazard symbol system used in this International
of gelatin, applied to the side of the film base opposite Standard is intended to provide information to the
that of the emulsion layer, for the purpose of pre- users and is not meant for compliance with any legal
venting curl. It is comparable to the emu lsion layer in requirements for labelling as these vary from country
thickness and is not removed in processing . to country.
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ISO 10602 : 1995

It is strongly recommended that anyone using 6 Requirements for processed film


these chemicals obtain from the manufacturer
pertinent information about the hazards, hand- Films shall be stored under the conditions specified in
ling, use and disposal of these chemicals. ISO 5466 and ISO 10214.

4.2 Hazard information code system

<B> Harmful if inhaled. Avoid breathing dust,


vapour, mist or gas. Use only with ad-
equate ventilation. 6.1 Safety film

<C> Harmful if contact occurs. Avoid contact The film shall meet the requirements specified in
with eyes, skin or clothing. Wash ISO 543.
thoroughly after handling.

<s> Harmful if swallowed. Wash thoroughly


after handling. If swallowed, obtain medi-
cal attention immediately.
6.2 Amount of free acid
« S» May be fatal if swallowed. If swallowed,
obtain medical attention immediately. Oifferent specifications and test methods are given
for polyester base and cellulose-ester base films. The
<F> Will burn. Keep away from heat, sparks
polyester base shall not have an amount of free acid
and open flame. Use with adequate venti-
greater than the equivalent of 1,0 mi of 0,1 mol/l
lation 31 • sodium hydroxide solution per gram of film, and the
< O> Oxidizer. Contact with other material may cellulose-ester base shall not have an amount of free
cause fire. Do not store near combustible acid greater than the equivalent of 0,5 mi of
materials. 0,1 mol/l sodium hydroxide solution per gram of film.
The amount of free acidity shall be measured in ac-
cordance with 9.3.
4.3 Safety precautions
The volume of 0,1 mol/l sodium hydroxide equivalent
AII pipette operations shall be performed with a
to the amount of free acid of the processed film shall
pipette bulb or plunger pipette.
not increase by more than 0,5 mili over its original
Safety glasses shall be worn for all laboratory value after the accelerated ageing described in 9.2.
work.

5 Requirements for film bases


The base used for record films, as specified in this 6.3 Tensile properties and loss in tensile
International Standard, shall be of a safety polyester properties
[i.e. poly(ethylene terephthalate}] or a cellulose-ester
type, and can be identified by the method described
The film samples shall be processed and dried under
in 9.1.
the conditions used for the film records. Processed
So me films on a cellulose-ester-type base can have a films shall be tested for tensile properties as de-
maximum LE rating of 100. Some films on a polyester scribed in 9.4 and shall have a tensile stress and
base can have a maximum LE rating of 500. elongation at break as specified in table 1 (unheated
film). The loss in tensile properties after accelerated
NOTE 5 These limitations are based on historical experi- ageing as described in 9.2 shall not exceed the per-
ences as discussed in the introduction. centage specified in table 1 (heated film).

3) The flammable warning symbol < F > will not be used for quantities of common solvents under 1 litre.
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ISO 10602 : 1995

7.2 Emulsion flow


Table 1 - Limits for tensile properties and loss The processed film shall not show any visual evidence
in tensile properties on ageing of emulsion flow (caused by partial emulsion remelt-
ing) as a result of accelerated ageing of the processed
Tensile
Elongation film . Emulsion flow shall be determined as described
Film type stress at
at break in 9.7 when the accelerated ageing is performed as
break
described in 9.2.
Unheated film
Minimum permissible 7.3 Blocking
tensile properties:
Cellulose-ester base 80 MPa 1) 15 % Processed film shall show no evidence of blocking
(stickingl. delamination or surface damage when
Polyester base 140 MPa 75 %
tested as described in 9.8. A slight sticking of the film
Heated film samples that does not result in physical damage or a
Maximum permissible change in the gloss of the surface shall be acceptable .
loss in tensile properties
compared with unheated 7.4 Thiosulfate concentration
film :
Cellulose-ester base 15 % 30 % Films shall be fixed in solutions containing either
Polyester base 15 % 30% sodium thiosulfate (hypo) or ammonium thiosul-
fate[10J. Hypo-eliminating agents containing oxidizing
2
1) 1 MPa = 106 N/m agents such as peroxides or hypochlorites shall not
be used.

NOTE 6 Hypo-eliminating agent contains chemicals,


7 Requirements for the emulsion and usually strong oxidizing agents, which decompose thiosul-
backing layers of processed film fa te (see annexes B and D). These are to be distinguished
from hypo-clearing baths, which are high ionic strength salt
solutions. These facilitate the washing of thiosulfate from
7.1 layer adhesion the film, but do not chemically alter the thiosulfate .

After processing, the film shall not contain a greater


7.1.1 Tape-stripping adhesion
concentration of residual thiosulfate calculated as
thiosulfate ions (S2032 -) than that specified in table 2
The processed film shall not show any removal of the
when determined by one of the test methods de-
emulsion layer or backing layer when tested as de-
scribed in ISO 417 41 .
scribed in 9.5.
The analysis for thiosulfate shall be made on a film
7.1.2 Humidity-cycling adhesion sample from a clear area and shall be made within
2 weeks after processing (see annex B). The test
The emulsion layer or backing layer of the processed method does not measure any change in the sample
film shall not show separation or cracking that can between the time of processing and the time of
impair its intended use, when tested as described in analysis, but is used to judge the keeping of the film
9.6. following the time of the test.

4) Three methods for measuring residual thiosulfate based chemicals in film are described in ISO 417 . AII three methods are
considered sufficiently reliable to report thiosulfate concentrations at the level of 0,014 g/m 2 of S20/ -. The methylene blue
2
method is considered reliable for thiosulfate concentrations of 0,007 g/m . The methylene blue and iodine amylose methods
measure thiosulfate ions only. They must be run within 2 weeks of processing. The silver sulfide densitometric test method
measures polythionate decomposition products and other residual chemicals in addition to thiosulfate. The method may be run
more than 2 weeks after processing. To determine thiosulfate levels accurately with this method, a calibration curve for the
particular film is necessary.
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ISO 10602 : 1995

Table 2 - Limits for thiosulfate (S02 2 -) concentration


Maximum permissible concentration
Film type Film classification 1) of thiosulfate 2 ) 3)

g/m 2

Radiographic films LE-10 0,100


LE-100 0,050
LE-500 0,020

Microfilms LE-100 0,030


LE-500 0,014

Other films LE-10 0,100


LE-100 0,050
LE-500 0,014

1) LE-500 film only applies to polyester base film.


2) Values are for each si de of the film which has a photographic layer or a noncurl backing layer.
3) The concentration of thiosulfate is expressed in grams per square metre, which conforms to SI units.
° 2
0,01 g/m = 1¡lg/cm
2

7.5 Residual silver compounds 8.2.1 LE-100 film

The processed film shall not show more than a barely The area of minimum density shall have a visual dif-
perceptible tint when tested in accordance with 9.9 fuse density of less than 0.4 after incubation. The
(see annex e). difference in visual density between the two test
areas shall be at least 0,8 after incubation.

8 Requirements for image stability 8.2.2 LE-SOO film

The specifications and test methods for image stab- Neither the minimum-density nor the high-density
ility are different for the different product types. ISO area shall change by more than ± 0,1 in visual diffuse
visual diffuse density or status A blue density shall be density units after incubation.
measured on a densitometer which has spectral con-
formance to ISO 5-3 and geometric conformance to
8.3 Other films
ISO 5-2. Processed film samples shall be incubated
as described in 9.10. A minimum-density area and a 1,0 ± 0,1 status A blue
density patch of processed film shall be tested.
8.1 Radiographic films Neither the minimum-density area nor the high-
density patch shall change by more than ± 0,1
An area of unexposed processed film shall be tested. status A blue density units after incubation. This re-
The status A blue density change of the unexposed quirement shall apply to LE-10, LE-100 and LE-500
area shall be no greater than 0,05 density units after films.
incubation. This requirement shall apply to LE-10,
LE-100 and LE-500 films. 9 Test methods

8.2 Microfilms 9.1 Identification of film base

An area of minimum density and another having a Remove all emulsion and backing layers from a
visual diffuse density of 1,2 ± 0,1 on the processed sample of unknown film, either by scraping or by the
film sample shall be tested. The criteria given in 8.2.1 use of enzyme solution. Then remove all sublayers by
and 8.2.2 shall apply to the different film categories. scraping. Prepare a sample of the base material by
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ISO 10602 : 1995

scuffing the surface with a suitable tool such as a NOTE 8 In the subsequent text, samples subjected to
razor blade. The general procedure is to move the these accelerated ageing conditions are designated "heated
scuffing device back and forth over the sample film" . Comparison samples kept at room conditions are
designated "unheated film ".
manually while exerting a very slight pressure. This
removes the top layer of the base as a very fine dust.
Carefully brush this into a mortar. 9.3 Determination of the amount of free acid
Mix the sample with about 100 times its mass of
potassium bromide. previously ground to about 9.3.1 Specimen preparation
75 11m. Prepare a strip or pellet as described in refer-
ence [11]. Measurements shall be made on two unheated and
two heated specimens of imaged film that weigh ap-
Obtain an infrared absorption curve from the prepared proximately 1 9 to 2 9 each . Weigh the specimens to
pellet by means of an infrared absorption spec- the nearest 0,01 g. Heat the films in accordance with
trometer. By comparing the infrared absorption curve 9.2. Remove all coatings from the film base by
for the unknown with curves for known polymers, the scraping. Cut each specimen into small pieces and
identity of the unknown can be established[ 121 accurately weigh it prior to dissolving it in the appro-
priate solvents.
NOTE 7 It is difficult. although not impossible. to dis-
tinguish between cellulose acetate, cellulose acetate
9.3.2 Solution preparation
propionate and cellulose acetate butryate bases by this
method. but such separation is not necessary for the pur-
poses of this International Standard. The polyester base and the cellulose-ester base re-
quire different solvents.

Immerse the polyester specimens in 30 mi of a


70/30 (m/m) mixture of purified o-cresol/chloroform
9.2 Accelerated ageing conditions
(DANGER : < B > < C > < S».
Processed film shall be subjected to accelerated age- WARNING - Chloroform is harmful if inhaled.
ing conditions to meet the requirements for increase
Avoid breathing vapour, mist or gas. Use with
in the amount of free acid, loss in tensile properties,
adequate ventilation. If inhaled, move to fresh air.
and emulsion flow. Contact should be avoided between chloroform
and the eyes, skin or clothing. In case of contact,
The test specimens shall be conditioned at
obtain medical attention immediately.
(23 ± 1) oC and (50 ± 2) % relative humidity for at
least 15 h. After conditioning, place the specimens in o-Cresol is toxic if swallowed. Contact should be
a moisture-proof envelope and heat-seal the envel- avoided between o-cresol and the eyes, skin or
ope 51 . To prevent sticking between adjacent speci- clothing. Wash after handling. In case of contact,
mens, it may be necessary to interleave them with flush eyes and skin thoroughly with water. Obtain
aluminium foil. Ensure a high ratio of film to air vol- medical attention immediately.
ume by squeezing out excess air prior to heat-sealing.
Use a separate envelope for each film sample. Double Take care to dispose of chloroform and o-cresol in
bagging is recommended to reduce any effect of accordance with national and local hazardous
pinholes in the envelopes. Heat the envelopes in an waste disposal regulations.
oven for 72 h at (100 ± 2) °C61.
Dissolve the polyester support by heating it at
An alternative method of incubating the specimens in (93 ± 2) oC for 30 min or until the specimen has dis-
a closed environment is by placing them in 25 mm solved. Precautions should be taken to prevent ex-
borosilicate glass tubes[ 131 Each tube shall have two cessive evaporation of the solvent. Cool the dissolved
flanged sections separated by a gasket to provide a specimens to room temperature .
moisture seaFI and shall be he Id together by a metal
clamp. Sufficient film specimens shall be used to Immerse the cellulose ester specimens in approxi-
provide a high ratio of film to air volume. mately 80 mi of methylene chloride (DANGER : < B >

5) A suitable moisture-proof envelope is a metal foil bag that is coated on the inside with polyethylene for heat-sealing.
6) Incubation is accomplished in a closed environment to prevent escape of any acid that may be produced during incubatian.
Such acid may catalyse further film base degradation.
7) A suitable inert gasket can be made from polytetrafluoroethylene.
Page 11
ISO 10602 : 1995

< C > < S >), then slowly add 40 mi of denatured m is the mass, in grams, of the specimen.
ethanol.
Carry out the titration in duplicate on separately pre-
WARNING - Methylene chloride is harmful if pared solutions. The average amount of free acid for
inhaled. Avoid breathing vapour, mist or gas. Use the unheated and heated film specimens shall be cal-
with adequate ventilation. If inhaled, move to culated and reported separately.
fresh airo Contact should be avoided between
methylene chloride and the eyes, ski n or clothing.
In case of contact, obtain medical attention im- 9.4 Tensile property test for processed film
mediately.

Take care to dispose of methylene chloride in ac- 9.4.1 Specimen preparation


cordance with national and local hazardous waste
disposal regulations. Processed film already in 16 mm format may be
tested in this width. In the case of perforated 16 mm
film, specimens shall be cut from between the per-
9.3.3 Titration forations. Film in other sizes shall be cut into sections
15 mm to 16 mm wide and at least 150 mm long,
Titrate the polyester solution potentiometrically with using a sharp tool that does not nick the edges of the
standardized 0,1 mol/l tetrabutylammonium hydroxide specimen. Five specimens are required for the un-
using an automatic recording titrimeter and a heated film and five specimens for the heated film.
glass/calomel electrode system. The electrodes shall The specimens to be heated and the control speci-
have been preconditioned for 24 h in the mens shall be cut alternately and contiguously from
o-cresol/chloroform solvent mixture « B > < C > a single piece of film. The thickness of each specimen
< S » to prevent excessive instrumentation noise. shall be measured with a suitable gauge to the near-
est 0,002 mm and the width to the nearest 0,1 mm.
During titration, the burette tip shall be immersed into
the solution as far as possible, and shall also be as far
from the electrodes as is practical. The stirring rate 9.4.2 Accelerated ageing
shall be as rapid as can be maintained without causing
bubbles. Also titrate 30 mi of a blank solution which Five specimens shall be subjected to accelerated
has been heated for the same length of time as the ageing as described in 9.2.
polyester solution. Details of the preparation of
standardized tetrabutylammonium hydroxide are given
in annex A. 9.4.3 Conditioning

Titrate the cellulose ester solution with 0,1 mol/l AII specimens, both unheated and heated, shall be
sodium hydroxide, using cresol purple as indicator. conditioned at (23 ± 1) oC and at (50 ± 2) % relative
Also carry out a blank titration on the solvent mixture. humidity for at least 15 h. This can be accomplished
by means of an air-conditioned room or a
conditioning-air cabinet. The specimens shall be sup-
9.3.4 Calculation ported in such a way as to permit free circulation of
air around the film and the linear air velocity shall be
The amount of free acid, A, expressed in equivalent
at least 150 mm/s.
millilitres of 0,1 mol/l sodium hydroxide per gram of
film base, is calculated as follows for each specimen:
9.4.4 Procedure
(VS - VS)CT
A = -'---''------''-'-
O,lm
The film specimens shall not be removed from the
conditioning atmosphere for testing. The tensile
where
stress and percent elongation at break of unheated
Vs is the volume, in millilitres, of titrant used and heated film specimens shall be tested alternately
for the specimen; by means of a tensile machine, as specified in
ISO 1184.
is the volume, in millilitres, of titrant used
for the blank; The initial grip separation shall be 100 mm and the
rate of grip separation shall be 50 mm/min. The
is the concentration, in moles per litre, of tensile stress and elongation at break shall be calcu-
the titrant; lated separately for the unheated and heated film.
Page 12
ISO 10602 : 1995

9.5 Tape-stripping adhesion test 9.6 Humidity-cycling adhesion test

9.6.1 Specimen preparation


9.5.1 Specimen preparation
Two specimens of processed film shall be selected
Although the dimensions of the processed film from an area of high silver density. The specimens
specimen are not critical, one dimension shall be at should be 50 mm x 50 mm or 50 mm long x the film
least 150 mm. Four specimens shall be used for the width where the size of the film permits, but the di-
emulsion surface and four specimens for the backing mensions are not critical provided all specimens are
layer, if present. of uniform size .

9.6.2 Procedure
9.5.2 Conditioning
Mount the test specimens in a specimen rack and
Specimens shall be conditioned as described in place them in a glass laboratory desiccator jar in such
9.4.3. a way that they are freely exposed to the required
conditioning atmosphere. Place the jar in a forced-air
circulating oven for 8 h at (50 ± 2) oC. The atmos-
9.5.3 Procedure phere within the jar shall be maintained at 96 % rela-
tive humidity, which can be obtained by keeping a
The film specimens shall not be removed from the saturated solution of potassium sulfate in water[14] in
conditioning atmosphere for testing. Apply a strip of the bottom of the jara) Take care to ensure that the
pressure-sensitive plastic-base adhesive tape about saturated solution contains an ex ces s of undissolved
150 mm long to the surface of the processed film . crystals at 50 oC. The undissolved crystals shall be
Press the tape down with thumb pressure to ensure completely covered by a layer of saturated salt sol-
adequate contact, leaving enough tape at one end to ution and the surface area of the solution should be
grasp. No portion of the tape shall extend to the as large as practical. The jar and salt solution shall be
edges of the film specimens or extend to film perfor- kept at 50 oC for at least 20 h prior to use to ensure
ations. Hold the specimen firmly on a flat surface and adequate equilibrium .
remove the tape rapidly from the film surface. This
shall be accomplished by peeling the tape back on it- After 8 h, place the specimens and specimen rack for
self and pulling the end so that it is removed from the 16 h in a second desiccator jar that is also in the same
film at an angle of approximately 180°. Removal by oven. The atmosphere within the second jar shall be
the tape of any portion of the surface layer on any of maintained at 11 % relative humidity, which can be
the specimens shall be considered failure . obtained by keeping a saturated solution of lithium
chloride in water[14] in the bottom of the jarBl.
The results of the tape-stripping test may be very de-
pendent upon the adhesive tape used if the bonding Time periods of 8 h at the high humidity and 16 h at
force between it and the particular film surface under the low humidity constitute one cycle 91• Each film
test is not sufficiently high. For this reason, a mini- specimen shall be subjected to 12 humidity cycles.
mum bonding force is specified for this test. This After this, remove the film specimens from the
bonding force shall be determined by applying the specimen rack and examine the emulsion and any
adhesive tape to the film surface in the same manner backing layer for any evidence of peeling, flaking or
as described in the tape-stripping test. The tape shall cracking produced as a result of the humidity-cycling
be rapidly peeled back from the film surface at an treatment.
angle of approximately 180°. The peelback force re-
NOTE 9 Films may sometimes exhibit what appear to be
quired to separate the tape from the film shall be
small pinholes in the image after processing. These can be
measured by a suitable device such as a strain gauge caused by dirt or dust particles on the emulsion surface at
or spring scale capable of reading the maximum force the time the raw film is exposed and should not be con-
used. A bonding force of at least 0,9 N per millimetre fused with holes or cracks in the emulsion layer. The exist-
of tape width is required . ence of such pinholes in the image prior to humidity cycling

8) The relative humidity is based on the normal vapour pressure of the salt solution but the relative humidity tolerances cannot
be specified.
9) This can be most easily accomplished by placing the specimens in the 96 % relative humidity jar in the morning and in the
11 % relative humidity jar in the evening.
Page 13
ISO 10602 : 1995

should be noted so that their presence does not lead to a Alternatively, the temperature and humidity conditions
false interpretation of adhesion weakness. can be achieved by means of conditioning-air cabinets
or air-conditioned rooms.
The film shall be examined under magnification and
lighting conditions that are normal for the end use of Remove the film stack from the oven and allow it to
the product. During an interruption in the cycling pro- cool. Individually remove the film specimens from the
cedure, the film specimens shall be kept at stack and observe each for evidence of film blocking
(50 ± 2) oC and 11 % relative humidity. (sticking) (see 7.3).

9.9 Residual silver compound test


9.7 Emulsion flow test
Two specimens of processed film of any available size
Measurements shall be made on two heated speci- shall be tested on both sides. These specimens shall
mens of processed film. Each specimen shall contain be taken from the end of the processing run o Blot the
a photographic image of a grid pattern or of printed film dry, if necessary, and spot a clean image-free
material. Subject the film specimens to accelerated area with a freshly prepared 0,2 % aqueous solution
ageing as described in 9.2. After incubation, visually of sodium sulfide. Wash away or blot up the reagent
examine the photographic images on the heated after 3 mino
samples for any image change caused by flow of the
If there is more than a barely perceptible tint, a refer-
emulsion. This visual examination can be facilitated
ence specimen shall be prepared. The reference
by comparison with the images on unheated speci-
specimen shall be
mens.
- of the same film type, preferably the same lot,

9.8 Blocking test - fixed successively for 5 min in each of two dupli-
cate fresh fixing baths containing 240 gIl of
At least five specimens of processed film shall be sodium thiosulfate (Na2S203·5H201. and
conditioned at 62 % relative humidity and
(40 ± 2) oC. The preferred specimen size is - washed for 30 min in running water that is flowing
50 mm x 50 mm but the dimensions are not critical at arate that will fill the vessel once every 5 mino
provided all specimens are of uniform size. Place the
specimens in a glass laboratory desiccator jar so that Air-dry the film and test it with the sodium sulfide
they are freely exposed to the required conditioning solution as stated in the previous paragraph. Any stain
atmosphere for at least 15 h. Place the jar containing in the test specimen greater than that of the refer-
the specimens in a forced-air circulating oven at ence specimen is an indication of residual silver salts.
(40 ± 2) oC. A relative humidity of approximately
62 % can be obtained by keeping a saturated solution 9.10 Image-stability test
of sodium nitrite[1S] in water at the bottom of the
jarlll . Take care to ensure that the saturated solution 9.10.1 Specimen preparation
contains an excess of undissolved crystals at 40 oC.
The undissolved crystals shall be completely covered Specimens of film shall be exposed to the specified
by a layer of saturated salt solution and the surface densities as indicated in table 3. These differ for the
area of the solution should be as large as is practical. different film types . An appropriate specimen size is
The jar and salt solution shall be kept at 40 oC for at 50 mm x 50 mm for sheet film products or 50 mm in
least 20 h prior to use to ensure adequate equilibrium. length x the film width for roll film products.

After moisture equilibrium is attained, remove the jar 9.10.2 Specimen incubation
from the oven. Without removing the film specimens
from the jar, stack at least five film specimens so that The specimens shall be conditioned at 60 % relative
the emulsion surface of one specimen is against the humidity for at least 8 h at ambient temperature. This
back surface of the adjacent specimen. Place the can be accomplished by means of an air-conditioning
stack under a uniform pressure of 35 kPa. This can room or a conditioning-air cabinet. Support the speci-
be accomplished by placing a weight on the film mens in the conditioning-air cabinet in such a way as
stack, the dimensions of the weight being greater to permit free circulation of air around the film . The
than those of the film specimens. The jar containing linear air velocity shall be at least 150 mm/s. Then
the weighted stack shall be put back into the forced- heat-seal the film in a moisture-proof metallic-foil en-
air circulating oven for 3 days at 40 oC. velope after the air has been squeezed out. Double
Page 14
ISO 10602 : 1995

bagging is recommended to reduce any effect of 9.10.4 Measurements


pinholes in the bags.
80th befo re and after incubation, microfilms shall be
9.10.3 Incubation conditions measured for visual diffuse density and all other film
shall be measured for status A blue density. Densities
Film specimens shall be incubated at the tempera- shall be measured on a densitometer having spectral
tures and times specified in table 3. A description of conformance to ISO 5-3, and geometric conformance
how these conditions were chosen appears in an- to ISO 5-2. The specimen shall meet the density cri-
nexes D, E and F. teria given in 8.1 to 8.3.

Table 3 - Conditions for image-stability test

Incubation conditions

Film type Sample density Film classification Time Temperature Humidity

days oC %
Radiographic films Unexposed area LE-lO 14 68 60
LE-lOO 14 77 60
LE-500 14 85 60

Microfilms Area of minimum density LE-lOO 14 60 60


and LE-5úO 30 60 60

D = 1,2 ± 0,1

Other films Unexposed area and LE-lO 7 60 60


LE-lOO 14 60 60
D = 1,0 ± 0,1 LE-500 30 60 60
Page 15
ISO 10602 : 1995

Annex A
(normative)

Preparation of standard solution of tetrabutylammonium hydroxide

Polyester bases inherently have carboxyl groups in- Then use the primary standard to determine the
corporated in their molecular structure. In chemical molarity of the TBAH base titrant.
terminology, this is referred to as "free acids" and is
expressed as the volume of a standard solution of Prepare a 25 % (m/m) solution of TBAH by dissolving
sodium hydroxide required to neutralize 1 9 of poly- 25 9 of TBAH in 75 9 of water. Prepare a nominal
ester base. The intent of the test specified in 6.2 is 0,10 mol/l TBAH titrant solution by adding 90 mi
to ensure that the base is chemically stable and also isopropanol to 10 mi of the 25 % (m/m) aqueous
that it will not be adversely affected by the image- TBAH solution . Standardize this against the primary
bearing or other layers . Thus, the entire film shall be benzoic acid solution by pipetting exactly 1 mi of the
heated in accordance with 9.2 to simulate longtime 0,1 mol/l benzoic acid solution into a 50 mi beaker and
ageing . However, remove all the layers from the base adding 30 mi of the 70/30 (mlm) mixture of
prior to determining the acidity to simplify the analyti- o-cresol/chloroform « B > < C > < S» . Titrate this
cal procedure. solution with TBAH base titrant using an automatic-
recording titrimeter in the specified manner. Carry out
Use a primary 0,1 mol/l standard solution of benzoic a similar titration with a blank 30 mi sample of the
acid to standardize the tetrabutylammonium hydrox- o-cresol/chloroform mixture. Make both titrations in
ide (TBAH) titrant. Then titrate the TBAH against the duplicate.
polyester base to determine the amount of free acid.
Prepare the nominal 0,1 mol/l primary standard sol- The concentration, cT' in moles per litre, of the TBAH
ution of benzoic acid by weighing (1,22 ± 0,01) 9 of base titrant is calculated from:
benzoic acid into a 100 mi volumetric flask. Make up
to the mark with a 70/30 (mlm) mixture of purified
o-cresol/chloroform (DANGER : < B > < C > < S».
where
WARNING - Chloroform is harmful if inhaled.
Avoid breathing vapour, mist or gas. Use with is the volume, in millilitres, of the
adequate ventilation. If inhaled, move to fresh airo 0,1 mol/l benzoic acid solution;
Contact should be avoided between chloroform
and the eyes, ski n or clothing. If contact occurs, Cp is the concentration, in moles per litre, of
obtain medical attention immediately. the 0,1 mol/l benzoic acid solution;

o-Cresol is toxic if swallowed. Contact should be is the volume, in millilitres, of TBAH titrant
avoided between o-cresol and the eyes, skin or used in the titration of the primary stan-
clothing. Wash after handling. In case of contact, dard;
flush eyes and ski n thoroughly with water. Obtain
medical attention immediately. is the volume, in millilitres, of TBAH titrant
used in the titration of the blank.
Take care to dispose of chloroform and o-cresol in
accordance with national and local hazardous EXAMPLE
waste disposal regulations.
If 1,00 mi of 0,102 mol/l primary standard is titrated
with 1,147 mi of TBAH titrant and 30 mi of blank is
The concentration, Cp, in moles per litre, of the primary
titrated with 0,032 mi of TBAH titrant, then the con-
benzoic acid standard is calculated from :
centration of TBAH is
0, 1mB
cp=1.22 1,00xO,102
CT = 1,147 _ 0,032 = 0,091 mol/l

where mB is the mass, in grams, of benzoic acid used.


Page 16
ISO 10602 : 1995

Annex B
(informative)

Washing and the effect of residual thiosulfate on the developed silver image

NOTE 10 The term "residual thiosulfate" is used in this b) bleaching or loss of density in the image areas;
annex to include its decomposition products, polythionates, or
including those complexed with silver.
c) increase in density of the image areas[5J, [6J.
The preseNation of silver-gelatin-type photographic
film is dependent on the products which are still The test for residual thiosulfate ions is specified to be
present after washing. The maximum content of re- made on non-image or clear areas of the film beca use
sidual thiosulfate and residual silver compounds is this is where the thiosulfate ion concentration, as
specified in 7.4 and 7.5. Water used for washing measured by the methylene blue method, will not
should be colourress and free from substances in change appreciably over a period of 2 weeks .
suspension . Drinking water is generally pure enough
for washing purposes. Tests have shown that even at fairly high levels of
residual thiosulfate ions, adverse changes are quite
The temperature of the water used for washing gradual for incubations at 60 % relative humidity. The
should be maintained between 15 oC and 25 oC as limits of residual thiosulfate ions permitted in this
this is generally suitable and strikes a balance be- International Standard are based on the incubations
tween the danger of swelling introduced by higher described in annexes D, E and F and are sufficiently
temperatures and the decrease in the rate of solubility low to minimize changes under recommended
of the salts being removed at lower temperatures. storage conditions.
Some films can tolerate higher temperatures. Wash-
ing in well-agitated running water for 15 min at a The amount of thiosulfate ions retained in a processed
temperature of 20 oC is generally satisfactory, pro- film is dependent to a considerable degree on the
vided that the films are not in contact with one composition of the fixing bath[16J, [171 Acid-hardening
another and that water is renewed at their surface. fixing baths (which contain aluminium salts) condition
For most automatic machines (droplet jets, etc.). the the gelatin in the emulsion so that the thiosulfate ions
washing time is shorter and the water temperature is are retained more tenaciously than in a non-hardening
higher. The temperature of the water used for wash- bath. However, a non-hardening fixing bath should be
ing should be within 3 oC of the temperature of the used with caution beca use the gelatin may become
developer. soft. Ammonia or hypo eliminators which contain
oxidizing agents (such as hypochlorite and peroxides)
lon-exchange washing accelerators may be used. For should not be used.
instance, films may be soaked in a bath containing
20 gIl of anhydrous sodium sulfite before washing. The degree of change that can be tolerated in films
depends upon their intended use. For textual records,
Excessive thiosulfate ions retained by the film pro- legibility can be the sole consideration. For picture
duce one or more of the following phenomena: records, even a slight amount of discoloration or
bleaching, particularly if non-uniform, can be unac-
a) yellow-brown discoloration in the low-density ceptable. It is believed that the residual thiosulfate ion
areas of the film ; level specified provides a sufficient margin of safety
for all levels of life expectancy under the storage
conditions specified in ISO 5466.
Page 17
ISO 10602 : 1995

Annex e
(informative)

Effect of residual silver compounds on the developed silver image

Residual silver compounds and complexes are an im- To ensure that the fixing bath is suitable, it is rec-
portant cause of image layer degradation in aged pro- ommended that the amount of silver be less than
cessed photographic films. Silver ions from the 0,5 % (m/m) in the case of a bath containing sodium
complex ions can combine with the sulfur produced thiosulfate (Na 2S20 3), or less than 0,8 % (m/m) in the
by decomposition of the thiosulfate ions or can react case of a bath containing ammonium thiosulfate
with atmospheric contaminants to produce discolor- [(NH4)2S203]. In order to minimize in microfilms de-
ation. At the present state of knowledge, it is not fects known as "ageing blemish microspots", the
possible to specify a safe maximum for residual silver iodide content (as KI) in the fixing bath for such prod-
compounds in quantitative terms . However, it is be- ucts shall be between 0,1 g/I and 0,5 g/1.
lieved that the quantity of residual silver compounds
will be satisfactorily low when the film passes the test A high concentration of silver complexes in the fixing
for residual silver compounds specified in 7.5. bath, oxidants in the water used for washing, and
Thorough washing of the film to reduce the residual film-drying conditions that provide an unclean atmos-
thiosulfate ion level also has the important effect of phere or impart a case-hardening effect on the
reducing the level of residual silver compounds. emulsion, are considered undesirable factors in the
processing of film .
Page 18
ISO 10602 : 1995

Annex D
(informative)

Accelerated image-stability test tor radiographic tilms

The experimental method used to derive the residual celerated tests given in 9.10 were based on results
thiosulfate ion levels and film lifetimes is based on of the eight radiographic films mentioned previously.
data that appear in reference [7]. Eight radiographic The times were based on the least stable of these
films were exposed and processed in suitable films and are conservative estimates.
processors by adding various amounts of fixer to the
wash tanks of the processors. This non-
recommended processing cycle yielded processed 6 ResiduaL thiosuLfate ions: • 0,035 g/m 2
10
film specimens with a wide range of residual thiosul- ... 0,11 g/m 2 I

fate levels . The methylene blue method described in Days Years


. 0,30 g/m 2 / /
ISO 417 was used to measure residual thiosulfate 1000 / /
levels. The processed film specimens were incubated / /
for a series of times in dark chambers at 60 % relative / /
humidity and temperatures from 93 oC to 52 oC. AII 10 5 / /
specimens were hung freely in chambers where / /
temperature and humidity were both controlled.
100
/ /
Status A blue density measurements were made be- / /
fore and after the keeping periods for all specimens. / /
QJ

Status A blue density change in the area of minimum


0\
e
el 10
4 / /
density was shown to be the sensitometric para meter
.J::.
u
e
/ /
most sensitive to increasing residual thiosulfate ion 'E
c:¡ / /
levels. Practical radiographs that had been incubated
lI'
O
O
10
/ /
were examined by people with experience in X-ray <...
.....O
diagnosis. They concluded that a yellow-brown stain QJ
E 10 3
increase of 0,05 status A blue density units would be ¡::
just noticeable to a diagnostician. For each film and for
each temperature, the storage time to produce this
sensitometric change was determined for each re-
sidual thiosulfate ion level.

The log of the time for the stain build-up to occur for
each incubation temperature was plotted against the
reciprocal of the thermodynamic (absolute) tempera-
ture. Curves are plotted in figure D.1 for experiments
which showed density change . Extrapolation down to
a room temperature of 23 oC indicated the time for
the stain build-up to occur for room-temperature 23 'C
storage at 60 % relative humidity. The results of these
2,7 2,8 2,9 3,0 3,1 3,2 3,3 3,4
extrapolations justify the limits specified in table 2.
The limits are conservative and are based on extra- 1000/ T
polations of the experimental data. The limits are also
conservative beca use the experiment was carried out NOTE - Temperatures have been plotted as reciprocals of
at 60 % relative humidity, which is higher than the thermodynamic temperatures, T (in kelvins) .
maximum recommended storage relative humidity for
radiographic film . The incubation criteria for the ac- Figure D.1 - Time versus temperature for
radiographic films
Page 19
ISO 10602 : 1995

Annex E
(informative)

Accelerated image-stability test for microfilms

The experimental method used to derive the residual


thiosulfate ion levels and film lifetimes is based on
data that appear in reference [8]. Ten microfilms were
exposed and processed by adding seasoned fixes to
10 6 .
Days Years
/
a stagnant wash in the wash tank of the processor.
This non-recommended processing cycle gave pro- 1000 /
cessed film specimens with a wide range of residual /
thiosulfate ion levels with values from less than /
2
0,003 g/m 2 to 0,15 g/m . The methylene blue method 10 5 /
of ISO 417 was used to measure residual thiosulfate
oC
.::c:I /
ion levels. The processed film specimens were incu-
~
c.
100 /
bated for a series of times in dark chambers at 60 % VI
/
c:
relative humidity and temperatures from 77 oC to QJ

32 oC. AII specimens were hung freely in chambers


"O
.....
o
/
10 4
where both temperature and humidity were con- c:I /
.S
trolled. Density measurements were made befo re and QJ /
after the keeping periods for all specimens. '"c:I
QJ 10 /
'-

The density change criteria specified in 8.2.2 were


u
.S /
1:
.¡¡;
used. A low-density patch and a 1,2 density patch c:
QJ
10)
should not change by more than 0,1 density units. "O
.....
o
(This level of change is greater than the measurement '-
error.) ....o
QJ
E
¡::
The logarithm of the time for a 0,1 density unit in-
crease for each incubation temperature was plotted 10 2
versus the reciprocal of the thermodynamic (absolute)
temperature, using the approach of Arrhenius.
Although the thiosulfate ion levels were as high as
0,15 g/m 2 , only the film at the lowest thiosu lfate ion
level for one of the products changed enough to plot 23 ·C
~~~~--r4~-r~-,~~.-~-.~~
1
(see figure E.1). 10

Extrapolation of high-temperature data down to a


2.7 2.8 2.9 3.0 3.1 3.2 3.3 3.'
room temperature of 23 oC indicated that the time for 1000/ T

a 0,1 density change at 60 % relative humidity ex-


ceeded 1 500 years. Therefore the limits specified in NOTE - Temperatures have been plotted as reciprocals of
table 2 are conservative. The limits are also conserva- thermodynamic temperatures, T (in kelvins) .
tive beca use the experiment was carried out at 60 %
relative humidity, and this is higher than the maximum Figure E.1 - Time versus temperature for
recommended storage relative humidity of 30 % for microfilms
microfilm.
Page 20
ISO 10602 : 1995

Annex F
(informative)

Accelerated image-stability test for aerial films

The experimental method used for determining re- ommended relative humidity for extended-life storage
sidual thiosulfate ion levels and film lifetimes was of aerial films.
based on the study reported in reference [9]. In three
separate experiments, ten aerial films were exposed, NOTE 11 Similar experiments were carried out for other
developed and fixed, but were washed either in a films but separate annexes are not presented.
stagnant water bath to which various amounts of
seasoned fixer had been added, or were immersed
after normal washing in a solution of diluted, Residual thiosulfate ions: 0,18 g/m 2
seasoned fixer. These unorthodox treatments re- Days Years
sulted in the retention of residual thiosulfate ions in 1000
2
the emulsion layers ranging from 0,003 g/m to
2
0,28 g/m , as measured by the methylene blue
method given in ISO 417. The processed film speci-
mens were conditioned at 60 % relative humidity, ~

then sealed in foil bags and incubated for different ~

times at temperatures ranging from 32 oC to 77 oC. 'o." 100


~
Density and resolving power measurements were 'Vi
e
QJ
made befo re and after incubation. D
,...
o 10 4
The resolving power values were determined in ac- '"
.<::=
/
cordance with ISO 6328, which involves a visual as- QJ
1/) /
sessment of target images. None of these resolving '"
QJ
'-
10 /
power values changed by more than one element. u
.<::= /
~ /
'Vi
The changes in density were determined by status A e
QJ 10 3 /
blue densitometry (ISO 5-3 and ISO 5-2). The per- D
,... /
missible change in blue density was set at 0,1 for o /
'-
both the high- and minimum-density patches of the ....o /
QJ

specimens. This amount of change is greater than the E


¡::
test system error. Investigation of the density
changes as a function of residual thiosulfate level 10 2
showed that the density change of the high-density
patch was the most sensitive parameter.

The log of the time for a 0,1 status A blue density in-
crease for the high-density patch for each incubation
temperature was plotted versus the reciprocal of the
thermodynamic (absolute) temperature, using the ap- 2,7 2,8 2,9 3,0 3,1 3,2 3,3 3,4
proach of Arrhenius. A sample curve is shown in fig-
1000/ T
ure F.l. (The example represents a film containing
approximately twice the level of thiosulfate ions per-
NOTE - Temperatures have been plotted as reciprocals of
mitted in LE-10 aerial film.) The thiosulfate ion limits
thermodynamic temperatures, T (in kelvins).
for LE-10, LE-lOO and LE-500 films are conservative
beca use the experiment was at 60 % relative hu-
Figure F.1 - Time versus temperature for aerial
midity, and this is higher than the maximum rec-
films
Page 21
ISO 10602 : 1995

Annex G
(informative)

Bibliography

[1] ADELSTEIN, P.Z. and MCCREA, J.L. Stability of [8] KOPPERL, D.F. and HUTIEMANN, T.J. Effect of
processed polyester base photographic films. residual thiosulfate ion on the image stability of
Journal of Applied Photographic Engineering, microfilms . Journal of Image Technology, 12,
7(6), December 1981, pp. 160-167. August 1986, pp. 173-180.

[2] RAM, A.T. and MCCREA. J.L. Stability of pro- [9] KOPPERL, D.F., GOETIl NG, R.R., HUTIEMANN, T.J .
cessed cellulose ester photographic films . and SCHICKLlNG, M .L. Use of Arrhenius testing
Journal of the Society of Motion Picture and to evaluate the thiosulfate tolerance of black-
Television Engineers, 97, June 1988, and-white aerial film . Journal of Imaging Science
pp. 474-483. and Technology, 36, January/February 1992,
pp. 42-45.
[3] ADELSTEIN, P.Z., REILLY, J.M., NISHIMURA, D.W .
and ERBLAND, C.J . Stability of cellulose ester [10] HENN, R.W . and KING, N.H. A comparison of the
base photographic film : Part I - Laboratory effect of residual sodium and ammonium thio-
testing procedures. Journal of the Society of sulfate on image permanence. Photographic
Motion Picture and Television Engineers, 101, Science and Engineering, 5, January 1961,
May 1992, pp. 336-346. pp . 46-47.

[4] ADELSTEI N, P.Z., RE ILLY, J.M ., NISHIMURA, D.W . [11] ANDERSON, D.H. and WOODALL, N.B. Infrared
and ERBLAND, C.J. Stability of cellulose ester identification of materials in the fractiona l milli-
base photographic film : Part 11 - Practical gram range . Analytical Chemistry, 25, December
storage consideration . Journal of the Society of 1953, pp . 1906-1909.
Motion Picture and Television Engineers, 101,
May 1992, pp. 347-353. [12] Infrared Spectra Plastics and Resins, P.B.
111438. US Department of Commerce, Office
[5] CENTA, J.M . Performance characteristics of of Technical Services, Washington, DC, 1954.
Cronar polyester photographic film base. Photo-
grammetric Engineering, 21, September 1955, [13] RICHTER, S.G . and WELLS, F.L. Influence of
pp. 539-542 . moisture in accelerated aging of cellulose .
TAPPI, 39, 1956, pp. 603-608.
[6] WHITE, D.R ., GASS, C.J., MESCHTER, E and
HOLM, W.R . Polyester photographic film base. [14] WEXLER, A. and HASEGAWA, S. Relative
Journal of the Society of Motion Picture and humidity-temperature relationships of so me
Television Engineers, 64, December 1955, saturated salt solutions in the temperature range
pp. 674-678. O to 50 oC. Research Paper RP2512 . Journal of
Research of the National Bureau of Standards,
[7] KOPPERL, D.F., LARSON, G.W ., HUTCHINS, BA 53(1), July 1954, pp . 19-26.
and BARD, C.C. A method to predict the effect
of residual thiosulfate content on the long-term [15] CARR, DS and HARRIS, B.L. Solutions for main-
image-stability characteristics of radiographic taining constant relative humidity. Journal of In-
films . Journal of Applied Photographic Engin- dustrial Engineering Chemistry, 41, September
eering, 8, April 1982, pp. 83-89. 1949, pp . 2014~015 .
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[16] CRABTREE, J.!., EATON, G.T. and MUEHLER, L.E. [17] HENN, R.W., KING, N.H. and CRABTREE, J.!. The
The removal of hypo and silver salts from effect of salt baths on hypo and silver elim-
photographic materials as affected by the com- ination. Photographic Engineering, 7, 1956,
position of the processing solutions. Journal of pp. 153-164.
the Society of Motion Picture Engineers, 41,
July 1943, pp. 9-68.

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