ASTM D5958-99(2020)
(Practice)Standard Practices for Preparation of Oil-Based Ink Resin Solutions
Standard Practices for Preparation of Oil-Based Ink Resin Solutions
SIGNIFICANCE AND USE
5.1 These practices provide means of preparing small quantities of resin solution (in some procedures in an inert gas atmosphere using uniform, controlled heating).
5.2 This practice provides quick ways to prepare a resin solution for quality control testing during the manufacture of resin solutions and vehicles. Samples can usually be prepared in approximately 30 to 45 minutes or less.
5.3 These practices can be used to prepare commonly specified ink test solutions such as 33.3 % resin in alkali refined linseed oil, and 50 % resin in heat-set ink solvent (that is, C12 to C16 hydrocarbon petroleum distillate with initial boiling point (IBP) about 470°F).
SCOPE
1.1 These practices describe laboratory procedures for preparing an oil-based ink resin solution in a high-boiling solvent using four pieces of lab equipment:
(1) A hot oil bath (Sections 4 to 11),
(2) A stirrer/hot plate (Sections 12 to 16),
(3) An industrial blender (Sections 17 to 22), and
(4) A hot air gun (Sections 23 to 27).
ASTM Subcommittee D01.37 recommends using the hot oil bath procedure (Practice D5597) where possible.
1.2 These practices use laboratory equipment generally available in a normal, well-equipped laboratory.
1.3 One or several of these practices allows for rapid resin solution preparation (under 30 min, typical), can regulate the maximum temperature, can be done under an inert atmosphere, and can prevent the random solvent loss during preparation.
1.4 These procedures are for use with ink resins intended mainly for oil-based offset and letterpress inks. The type of resins are typically, but not limited to C9 aromatic hydrocarbon resins, modified dicyclopentadiene resins, rosin pentaerythritol or glycerine esters, phenolic modified rosin esters, maleic anhydride modified rosin esters, and naturally occurring resins such as gilsonite.
1.5 The typical high boiling solvents to be used include C12 to C16 petroleum distillates, 2,2,4 trimethyl 1,3-pentanediol di-isobutyrate,2 alkali refined linseed oil, tridecyl alcohol, or combinations of the above.
1.6 To avoid fire or injury, or both, to the operator, these practices should not be used with low flash point solvents such as toluene or xylene. The minimum flash point of the solvents used should be 60°C (140°F) as determined by Test Method D56. (Warning—Users of this practice should be aware that the flash point of many solvents used for this test (as defined in Test Methods D56 and D1310) is exceeded in the heating cycle of this test method. Take safety precautions since there is the potential for vapor ignition. Do the methods outlined in a shielded exhaust hood, where there is access to a fire extinguisher if needed.)
1.7 The values stated in SI units are to be regarded as standard. The values given in parentheses are for information only.
1.8 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use. For specific hazard statement see 25.11.
1.9 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
General Information
Relations
Standards Content (Sample)
This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
Designation: D5958 − 99 (Reapproved 2020)
Standard Practices for
Preparation of Oil-Based Ink Resin Solutions
This standard is issued under the fixed designation D5958; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope D56.(Warning—Users of this practice should be aware that
the flash point of many solvents used for this test (as defined in
1.1 These practices describe laboratory procedures for pre-
TestMethodsD56andD1310)isexceededintheheatingcycle
paring an oil-based ink resin solution in a high-boiling solvent
of this test method. Take safety precautions since there is the
using four pieces of lab equipment:
potential for vapor ignition. Do the methods outlined in a
(1) A hot oil bath (Sections 4 to 11),
shielded exhaust hood, where there is access to a fire extin-
(2) A stirrer/hot plate (Sections 12 to 16),
guisher if needed.)
(3) An industrial blender (Sections 17 to 22), and
(4) A hot air gun (Sections 23 to 27). 1.7 The values stated in SI units are to be regarded as
ASTM Subcommittee D01.37 recommends using the hot oil standard. The values given in parentheses are for information
bath procedure (Practice D5597) where possible. only.
1.8 This standard does not purport to address all of the
1.2 These practices use laboratory equipment generally
safety concerns, if any, associated with its use. It is the
available in a normal, well-equipped laboratory.
responsibility of the user of this standard to establish appro-
1.3 One or several of these practices allows for rapid resin
priate safety, health, and environmental practices and deter-
solution preparation (under 30 min, typical), can regulate the
mine the applicability of regulatory limitations prior to use.
maximum temperature, can be done under an inert atmosphere,
For specific hazard statement see 25.11.
and can prevent the random solvent loss during preparation.
1.9 This international standard was developed in accor-
1.4 These procedures are for use with ink resins intended
dance with internationally recognized principles on standard-
mainly for oil-based offset and letterpress inks. The type of
ization established in the Decision on Principles for the
resins are typically, but not limited to C aromatic hydrocarbon
9 Development of International Standards, Guides and Recom-
resins, modified dicyclopentadiene resins, rosin pentaerythritol
mendations issued by the World Trade Organization Technical
or glycerine esters, phenolic modified rosin esters, maleic
Barriers to Trade (TBT) Committee.
anhydride modified rosin esters, and naturally occurring resins
such as gilsonite.
2. Referenced Documents
1.5 The typical high boiling solvents to be used include C 2.1 ASTM Standards:
to C petroleum distillates, 2,2,4 trimethyl 1,3-pentanediol D56 Test Method for Flash Point by Tag Closed Cup Tester
di-isobutyrate, alkali refined linseed oil, tridecyl alcohol, or D1310 TestMethodforFlashPointandFirePointofLiquids
combinations of the above. by Tag Open-Cup Apparatus
D1725 Practice for Preparing Resin Solutions for Viscosity
1.6 To avoid fire or injury, or both, to the operator, these
Measurement by Bubble Time Method
practices should not be used with low flash point solvents such
D5062 Test Method for Resin Solution Dilutability by
as toluene or xylene. The minimum flash point of the solvents
Volumetric/Gravimetric Determination
used should be 60°C (140°F) as determined by Test Method
D5597 Practice for Preparation of Oil-Based Ink Resin
Solutions Using a Hot Oil Bath (Withdrawn 1999)
These practices are under the jurisdiction of ASTM Committee D01 on Paint
E1 Specification for ASTM Liquid-in-Glass Thermometers
and Related Coatings, Materials, and Applications and are the direct responsibility
E230 Specification for Temperature-Electromotive Force
of Subcommittee D01.37 on Ink Vehicles.
(emf) Tables for Standardized Thermocouples
CurrenteditionapprovedJune1,2020.PublishedJuly2020.Originallyapproved
ɛ1
in 1996. Last previous edition approved in 2012 as D5958 – 99 (2012) . DOI:
10.1520/D5958-99R20.
2 3
The sole source of supply of the plasticizer TXIB known to the committee at For referenced ASTM standards, visit the ASTM website, www.astm.org, or
this time is Eastman Chemical Company, / Texas E. M. Division, P.O. Box 7444, contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Longview,TX 75607-7444. If you are aware of alternative suppliers, please provide Standards volume information, refer to the standard’s Document Summary page on
this information to ASTM International Headquarters. Your comments will receive the ASTM website.
1 4
careful consideration at a meeting of the responsible technical committee, which The last approved version of this historical standard is referenced on
you may attend. www.astm.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D5958 − 99 (2020)
3. Terminology 6.3 Thermometer, capable of reading 0 to 250°C and con-
forming to Specification E1. Alternately, temperature measur-
3.1 Definitions of Terms Specific to This Standard:
ing devices such as liquid-in-glass thermometers, thermistors,
3.1.1 cold cut, n—dispersionofresinintosolventusinghigh
thermocouples, or platinum resistance thermometers that pro-
shear dispersion without external heating.
vide equivalent or better accuracy and precision, that cover the
3.1.2 compatibility, n—resin and solvent mixture forms a
temperature range specified, may be used.
clear, homogeneous, and stable solution.
6.4 Heat Resistant Crystallizing Dish, 150 by 75 mm in
3.1.3 dissolution, n—the point at which all resin completely
size.
dissolves in the solvent.
6.5 Stirrer/Hot Plate, with a range of 38 to 371°C.
3.1.4 incompatibility, n—resin and solvent mixture is not
6.6 Condenser, with ground glass joints.
compatible, an opaque or two-phase mixture results.
3.1.5 oil bath, n—non-volatile, silicone fluid contained in a 6.7 Erlenmeyer Flask, 250-mLwith 24/40 joint top and side
large heat resistant crystallizing dish heated by a temperature arm.
controlled stirrer hot-plate.
6.8 Silicone Oil.
3.1.6 solution, n—resin and solvent form a clear,
6.9 Auxiliary Equipment, (that is, a 76-mm stir bar, lab jack,
compatible, and homogeneous mixture.
lab stand, flask clamp, glass bubbler filled with mineral oil,
3.1.6.1 Discussion—Industrial practice may use the term
inert gas source, etc.).
“solution” loosely to describe what may actually be a clear
6.10 Assembly of Hot Oil Bath Set-Up—Place a stirrer/hot
“dispersion.” For the sake of simplification, the terms solution
plate in an aluminum tray on a lab jack. Put the crystallization
and dispersion have been used interchangeably in this practice.
dish filled approximately ⁄3 with silicone oil on top of the hot
HOT OIL BATH
plate. Arrange the condenser above the center of the bath.
ClamptheErlenmeyerflaskcontainingthesolutioningredients
4. Summary of Hot Oil Bath Practice
on to the condenser. Adjust the flow of nitrogen to flow down
the condenser into the Erlenmeyer flask. Lower the flask into
4.1 Place the required amount of resin and solvent in a
the oil bath.
250-mL Erlenmeyer flask.
4.2 A hot oil bath is heated to the required dissolution
7. Reagents
temperature (150 to 200°C, typically about 180°C or slightly
7.1 Solvents used in this procedure will be those most often
higher for high softening point or poorly solvated resins).
used in the manufacture of lithographic ink vehicles, for
4.3 The Erlenmeyer flask containing the mixture of resin
example, hydrocarbon petroleum distillate C to C and
12 16
and solvent is placed into the hot oil bath with inert gas purge
vegetable oils.
and a cold water condenser.
8. Reagents and Materials
4.4 Allow the mixture to mix at the desired temperature
8.1 Nonvolatile Resins, (for example, hydrocarbon resins,
until all of the resin is completely dissolved.
rosin ester resins).
4.5 Remove the flask from the hot oil bath and allow it to
8.2 Solvents, used in this procedure will be those most often
cool while still under an inert atmosphere for 10 to 15 min.
used in the manufacture of lithographic ink vehicles, for
Save the sample for future testing.
example, alkali refined linseed oil (ARLO), hydrocarbon
petroleum distillate C to C .
5. Significance and Use
12 16
8.3 The resins and solvents agreed upon between producer
5.1 These practices provide means of preparing small quan-
and user.
tities of resin solution (in some procedures in an inert gas
atmosphere using uniform, controlled heating).
8.4 Standard Ink Oils.
5.2 This practice provides quick ways to prepare a resin
9. Procedure
solution for quality control testing during the manufacture of
9.1 Set the hot oil bath to heat at the specified temperature.
resin solutions and vehicles. Samples can usually be prepared
Set the temperature, if possible, at 10°C above the softening
in approximately 30 to 45 minutes or less.
point of the resin, but below the initial boiling point of the
5.3 These practices can be used to prepare commonly
solvent. (180°C is a common starting temperature for many
specified ink test solutions such as 33.3 % resin in alkali
high-melting-point ink resins.)
refined linseed oil, and 50 % resin in heat-set ink solvent (that
9.2 Crush large size pieces of resin sample and pass the
is, C to C hydrocarbon petroleum distillate with initial
12 16
crushed resin through a 16-mesh sieve.
boiling point (IBP) about 470°F).
6. Apparatus
The use of ink industry recognized standard test oils (petroleum distillates) is
recommended for evaluating resins. The test oils are closely controlled from lot to
6.1 Balance, capable of weighing to 60.01 g accuracy.
lot to ensure consistent data. Sources and ordering information are available at
6.2 Sieve, 16-mesh. www.napim.org/testmethods/standardstest.aspx.
D5958 − 99 (2020)
9.3 Weigh to the nearest 0.02 g, an appropriate amount of STIRRER—HOT PLATE
the screened resin into a 250-mL Erlenmeyer flask to meet the
12. Summary of Stirrer/Hot Plate Practice
concentration requirements for preparation of a 30 to 100-g
12.1 Small samples of ink resin and aliphatic ink oil or ink
sample. Typically 100 g of solution is prepared.
resin and alkali-refined linseed oil (ARLO) are cut into
9.3.1 Examples of common ink resin solutions are as
dispersion in an Erlenmeyer flask to a specific temperature, at
follows:
a specified rate, with stirring.
Solution No. 1 Percent Solution No. 2 Percent
12.2 The resulting fluid dispersion can be used to measure
resin 33.3 resin 50
parameters such as viscosity and aliphatic solubility or com-
alkali refined linseed oil 66.7 470°F IBP ink oil 50
100.0 100
patibility of a printing ink resin.
9.3.2 High-viscosity, high-molecular weight, (“structured”
13. Apparatus
or “self-gelling”) resins may require a stronger solvent system.
13.1 Erlenmeyer Flask, 125-mL, fitting the following de-
Possibleresinsolutionsforusewiththeseresinsareasfollows:
scription: a height of 114 mL, an outside base diameter of 67
Solution No. 3 Percent
mL, and an opening of 27 mL.
resin 45
13.2 Magnetic Stirring Bar, polytetrafluoroethylene-coated,
TXIB 30
243°C (470°F) IBP ink oil 25 and 25 mm in length.
100.0
13.3 Thermometer, capable of reading 0 to 250°C and
Solution No. 4 Percent
conforming to Specification E1. Alternately, temperature mea-
resin 50
suring devices such as liquid-in-glass thermometers,
TXIB 50
thermistors, thermocouples, or platinum resistance thermom-
100.0
eters that provide equivalent or better accuracy and precision,
9.4 Weighconcentrationofsolventneededtothenearest0.1
that cover the temperature range specified, may be used.
g.
13.4 Cork Stopper, high quality, designed to fit the flask
9.5 Place flask containing resin mixture into ground glass
used. This cork is then bored out appropriately to receive the
fittingonwater-cooledcondenser,secureflaskwithclamp,jack
thermometer in 13.3 in a snug fashion. The hole should be
up hot oil bath under flask until the bottom of the flask is close
drilled at an angle of approximately 25° so the tip of the
enough to the bottom of the bath (but not touching the bottom)
thermometer comes to rest at the inside edge of the flask. Place
for the stir bar to mix efficiently. Maintain inert gas flow over
a small groove on the side of the cork to prevent pressure
the resin-solvent mixture at approximately 1 bubble per 5 s
build-up.
through the outlet mineral oil bubbler. If lab jack not available,
13.5 Hot Plate Stirrer, capable of a surface temperature of
lower flask manually.
300°C.
9.6 Allow the mixture to continue mixing until all resin is
13.6 Stop Watch.
dissolved.
14. Calibration and Standardization
9.7 Check to see that all resin is dissolved.
14.1 The setting of the hot plate surface temperature must
9.8 After all the resin is in solution, and if the solution is
be calibrated by making a blank run in the following manner.
clear, lower the hot oil bath and allow the solution to cool
under the inert gas atmosphere.
14.2 Determine the total mass of the intended solution
described in 12.1 (Note: the mass should be between 30 and 45
10. Evaluation
g). Weigh into the 125-mL Erlenmeyer flask a quantity of
10.1 During solution preparation, observe the dissolution of ARLO equal to the intended solution mass described in 12.2.
Next, add the stirring bar and affix the thermometer/cork
resin and, if desired, record the time and temperature at which
dissolution occurred or the maximum temperature at which the assembly described in 13.4 to the Erlenmeyer flask.
mixture was heated if the resin did not dissolve.
14.3 Turnonthehotplatetemperaturecontrollertoasetting
that will give a surface temperature of approximately 300°C.
10.2 Upon cooling, samples can be tested for viscosity
Allow the hot plate 10 min to heat up and equilibrate.
following Test Method D1725, dilutability following Test
Method D5062, color, etc.
14.4 Settheflaskonthepreheatedhotplatestirrerandbegin
stirring.
11. Report
14.5 Start the stop watch.
11.1 Report on solution preparation the following informa-
14.6 Measure the time required for the ARLO to reach a
tion:
temperature of 215°C.
11.1.1 Dissolution time and temperature,
11.1.2 Solution clarity, 14.7 The hot plate surface temperature is correct when the
11.1.3 Failure of resin dissolution, if necessary, and ARLO heats from room tempera
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