ASTM D5958-99(2012)e1
(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 and health practices and determine the applicability of regulatory limitations prior to use. For specific hazard statement see 25.11.
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Designation: D5958 − 99 (Reapproved 2012)
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.
ε NOTE—Thermometer references and Footnote 5 were editorially corrected in November 2012.
1. Scope* as toluene or xylene. The minimum flash point of the solvents
used should be 60°C (140°F) as determined by Test Method
1.1 These practices describe laboratory procedures for pre-
D56.(Warning—Users of this practice should be aware that
paring an oil-based ink resin solution in a high-boiling solvent
the flash point of many solvents used for this test (as defined in
using four pieces of lab equipment; (1) a hot oil bath (Sections
TestMethodsD56andD1310)isexceededintheheatingcycle
4 to 11),
of this test method. Take safety precautions since there is the
(2) a stirrer/hot plate (Sections 12 to 16),
potential for vapor ignition. Do the methods outlined in a
(3) an industrial blender (Sections 17 to 22), and
shielded exhaust hood, where there is access to a fire extin-
(4) a hot air gun (Sections 23 to 27).
guisher if needed.)
ASTM Subcommittee D01.37 recommends using the hot oil
bath procedure (Practice D5597) where possible. 1.7 The values stated in SI units are to be regarded as
standard. The values given in parentheses are for information
1.2 These practices use laboratory equipment generally
only.
available in a normal, well-equipped laboratory.
1.8 This standard does not purport to address all of the
1.3 One or several of these practices allows for rapid resin
safety concerns, if any, associated with its use. It is the
solution preparation (under 30 min, typical), can regulate the
responsibility of the user of this standard to establish appro-
maximum temperature, can be done under an inert atmosphere,
priate safety and health practices and determine the applica-
and can prevent the random solvent loss during preparation.
bility of regulatory limitations prior to use. For specific hazard
1.4 These procedures are for use with ink resins intended
statement see 25.11.
mainly for oil-based offset and letterpress inks. The type of
2. Referenced Documents
resins are typically, but not limited to C aromatic hydrocarbon
resins, modified dicyclopentadiene resins, rosin pentaerythritol
2.1 ASTM Standards:
or glycerine esters, phenolic modified rosin esters, maleic
D56 Test Method for Flash Point by Tag Closed Cup Tester
anhydride modified rosin esters, and naturally occurring resins
D1310 TestMethodforFlashPointandFirePointofLiquids
such as gilsonite.
by Tag Open-Cup Apparatus
D1725 Practice for Preparing Resin Solutions for Viscosity
1.5 The typical high boiling solvents to be used include C
Measurement by Bubble Time Method
to C petroleum distillates, 2,2,4 trimethyl 1,3-pentanediol
D5062 Test Method for Resin Solution Dilutability by
di-isobutyrate, alkali refined linseed oil, tridecyl alcohol, or
Volumetric/Gravimetric Determination
combinations of the above.
D5597 Practice for Preparation of Oil-Based Ink Resin
1.6 To avoid fire or injury, or both, to the operator, these
Solutions Using a Hot Oil Bath (Withdrawn 1999)
practices should not be used with low flash point solvents such
E1 Specification for ASTM Liquid-in-Glass Thermometers
E230 Specification and Temperature-Electromotive Force
(EMF) Tables for Standardized Thermocouples
These practices are under the jurisdiction of ASTM Committee D01 on Paint
and Related Coatings, Materials, and Applications and are the direct responsibility
3. Terminology
of Subcommittee D01.37 on Ink Vehicles.
Current edition approved Nov. 1, 2012. Published November 2012. Originally
3.1 Definitions of Terms Specific to This Standard:
approved in 1996. Last previous edition approved in 2011 as D5958 – 99 (2011).
DOI: 10.1520/D5958-99R12E01.
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.
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.
*A Summary of Changes section appears at the end of this standard
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
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D5958 − 99 (2012)
3.1.1 cold cut, n—dispersionofresinintosolventusinghigh ing devices such as liquid-in-glass thermometers, thermistors,
shear dispersion without external heating. thermocouples, or platinum resistance thermometers that pro-
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
compatible, an opaque or two-phase mixture results.
6.6 Condenser, with ground glass joints.
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
“dispersion.” For the sake of simplification, the terms solution
6.10 Assembly of Hot Oil Bath Set-Up—Place a stirrer/hot
and dispersion have been used interchangeably in this practice.
plate in an aluminum tray on a lab jack. Put the crystallization
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
4.1 Place the required amount of resin and solvent in a
the condenser into the Erlenmeyer flask. Lower the flask into
250-mL Erlenmeyer flask.
the oil bath.
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
until all of the resin is completely dissolved.
8.1 Nonvolatile Resins, (for example, hydrocarbon resins,
rosin ester resins).
4.5 Remove the flask from the hot oil bath and allow it to
cool while still under an inert atmosphere for 10 to 15 min.
8.2 Solvents, used in this procedure will be those most often
Save the sample for future testing. used in the manufacture of lithographic ink vehicles, for
example, alkali refined linseed oil (ARLO), hydrocarbon
5. Significance and Use petroleum distillate C to C .
12 16
5.1 These practices provide means of preparing small quan-
8.3 The resins and solvents agreed upon between producer
tities of resin solution (in some procedures in an inert gas
and user.
atmosphere using uniform, controlled heating). 5
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
resin solutions and vehicles. Samples can usually be prepared
9.1 Set the hot oil bath to heat at the specified temperature.
in approximately 30 to 45 minutes or less.
Set the temperature, if possible, at 10°C above the softening
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
is, C to C hydrocarbon petroleum distillate with initial
9.2 Crush large size pieces of resin sample and pass the
12 16
boiling point (IBP) about 470°F).
crushed resin through a 16-mesh sieve.
9.3 Weigh to the nearest 0.02 g, an appropriate amount of
6. Apparatus
the screened resin into a 250-mL Erlenmeyer flask to meet the
6.1 Balance, capable of weighing to 60.01 g accuracy.
6.2 Sieve, 16-mesh. 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
6.3 Thermometer, capable of reading 0 to 250°C and con-
lot to ensure consistent data. Sources and ordering information are available at
forming to Specification E1. Alternately, temperature measur- www.napim.org/testmethods/standardstest.aspx.
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D5958 − 99 (2012)
concentration requirements for preparation of a 30 to 100-g STIRRER—HOT PLATE
sample. Typically 100 g of solution is prepared.
12. Summary of Stirrer/Hot Plate Practice
9.3.1 Examples of common ink resin solutions are as
12.1 Small samples of ink resin and aliphatic ink oil or ink
follows:
resin and alkali-refined linseed oil (ARLO) are cut into
Solution No. 1 Percent Solution No. 2 Percent
dispersion in an Erlenmeyer flask to a specific temperature, at
resin 33.3 resin 50
a specified rate, with stirring.
alkali refined linseed oil 66.7 470°F IBP ink oil 50
12.2 The resulting fluid dispersion can be used to measure
100.0 100
parameters such as viscosity and aliphatic solubility or com-
9.3.2 High-viscosity, high-molecular weight, (“structured”
patibility of a printing ink resin.
or “self-gelling”) resins may require a stronger solvent system.
Possibleresinsolutionsforusewiththeseresinsareasfollows:
13. Apparatus
Solution No. 3 Percent
13.1 Erlenmeyer Flask, 125-mL, fitting the following de-
scription: a height of 114 mL, an outside base diameter of 67
resin 45
TXIB 30
mL, and an opening of 27 mL.
243°C (470°F) IBP ink oil 25
100.0 13.2 Magnetic Stirring Bar, polytetrafluoroethylene-coated,
Solution No. 4 Percent and 25 mm in length.
13.3 Thermometer, capable of reading 0 to 250°C and
resin 50
TXIB 50 conforming to Specification E1. Alternately, temperature mea-
100.0
suring devices such as liquid-in-glass thermometers,
thermistors, thermocouples, or platinum resistance thermom-
9.4 Weighconcentrationofsolventneededtothenearest0.1
g. eters that provide equivalent or better accuracy and precision,
that cover the temperature range specified, may be used.
9.5 Place flask containing resin mixture into ground glass
13.4 Cork Stopper, high quality, designed to fit the flask
fittingonwater-cooledcondenser,secureflaskwithclamp,jack
used. This cork is then bored out appropriately to receive the
up hot oil bath under flask until the bottom of the flask is close
thermometer in 13.3 in a snug fashion. The hole should be
enough to the bottom of the bath (but not touching the bottom)
drilled at an angle of approximately 25° so the tip of the
for the stir bar to mix efficiently. Maintain inert gas flow over
thermometer comes to rest at the inside edge of the flask. Place
the resin-solvent mixture at approximately 1 bubble per 5 s
a small groove on the side of the cork to prevent pressure
through the outlet mineral oil bubbler. If lab jack not available,
build-up.
lower flask manually.
13.5 Hot Plate Stirrer, capable of a surface temperature of
9.6 Allow the mixture to continue mixing until all resin is
300°C.
dissolved.
13.6 Stop Watch.
9.7 Check to see that all resin is dissolved.
14. Calibration and Standardization
9.8 After all the resin is in solution, and if the solution is
clear, lower the hot oil bath and allow the solution to cool 14.1 The setting of the hot plate surface temperature must
under the inert gas atmosphere. be calibrated by making a blank run in the following manner.
14.2 Determine the total mass of the intended solution
10. Evaluation
described in 12.1 (Note: the mass should be between 30 and 45
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.
resin and, if desired, record the time and temperature at which
Next, add the stirring bar and affix the thermometer/cork
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
10.2 Upon cooling, samples can be tested for viscosity
that will give a surface temperature of approximately 300°C.
following Test Method D1725, dilutability following Test
Allow the hot plate 10 min to heat up and equilibrate.
Method D5062, color, etc.
14.4 Settheflaskonthepreheatedhotplatestirrerandbegin
11. Report stirring.
14.5 Start the stop watch.
11.1 Report on solution preparation the following informa-
tion:
14.6 Measure the time required for the ARLO to reach a
11.1.1 Dissolution time and temperature,
temperature of 215°C.
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 temperature to 215°C in 11 min 615
11.1.4 Maximum temperature at which resin failed to dis- s. On a hot plate, this is usually at a setting between 5 and 6 on
solve. the temperature-controller dial.
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D5958 − 99 (2012)
15. Procedure 16. Precision and Bias
16.1 Precis
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