ASTM D5958-99(2005)e1

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
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Designation:D5958–99(Reapproved2005)
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.
´ NOTE—Footnote 5 was editorially corrected in September 2005.
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; (1) a hot oil bath (Sections
potential for vapor ignition. Do the methods outlined in a
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
1.7 The values stated in SI units are to be regarded as
(4) a hot air gun (Sections 23 to 27).
standard. No other units of measurement are included in this
ASTM Subcommittee D01.37 recommends using the hot oil
standard.
bath procedure (Practice D5597) where possible.
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 and health practices and determine the applica-
solution preparation (under 30 min, typical), can regulate the
bility of regulatory limitations prior to use. For specific hazard
maximum temperature, can be done under an inert atmosphere,
statement see 25.11.
and can prevent the random solvent loss during preparation.
1.4 These procedures are for use with ink resins intended
2. Referenced Documents
mainly for oil-based offset and letterpress inks. The type of
2.1 ASTM Standards:
resins are typically, but not limited to C aromatic hydrocarbon
D56 Test Method for Flash Point by Tag Closed Cup Tester
resins, modified dicyclopentadiene resins, rosin pentaerythritol
D1310 Test Method for Flash Point and Fire Point of
or glycerine esters, phenolic modified rosin esters, maleic
Liquids by Tag Open-Cup Apparatus
anhydride modified rosin esters, and naturally occurring resins
D1725 Test Method for Viscosity of Resin Solutions
such as gilsonite.
D5062 Test Method for Resin Solution Dilutability by
1.5 The typical high boiling solvents to be used include C
Volumetric/Gravimetric Determination
to C petroleum distillates, 2,2,4 trimethyl 1,3-pentanediol
2 D5597 Practice for Preparation of Oil-Based Ink Resin
di-isobutyrate, alkali refined linseed oil, tridecyl alcohol, or
Solutions Using a Hot Oil Bath
combinations of the above.
E1 Specification for ASTM Liquid-in-Glass Thermometers
1.6 To avoid fire or injury, or both, to the operator, these
E230 Specification and Temperature-Electromotive Force
practices should not be used with low flash point solvents such
(EMF) Tables for Standardized Thermocouples
as toluene or xylene. The minimum flash point of the solvents
used should be 60°C (140°F) as determined by Test Method
3. Terminology
3.1 Definitions of Terms Specific to This Standard:
3.1.1 coldcut,n—dispersionofresinintosolventusinghigh
These practices are under the jurisdiction of ASTM Committee D01 on Paint
shear dispersion without external heating.
and Related Coatings, Materials, and Applications and are the direct responsibility
3.1.2 compatibility, n—resin and solvent mixture forms a
of Subcommittee D01.37 on Ink Vehicles.
Current edition approved Sept. 1, 2005. Published September 2005. Originally
clear, homogeneous, and stable solution.
approved in 1996. Last previous edition approved in 1999 as D5958 - 99. DOI:
10.1520/D5958-99R05E01.
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 Withdrawn. The last approved version of this historical standard is referenced
you may attend. on www.astm.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
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D5958–99 (2005)
3.1.3 dissolution, n—the point at which all resin completely 6.6 Condenser, with ground glass joints.
dissolves in the solvent. 6.7 Erlenmeyer Flask, 250-mLwith 24/40 joint top and side
3.1.4 incompatibility, n—resin and solvent mixture is not arm.
compatible, an opaque or two-phase mixture results. 6.8 Silicone Oil.
3.1.5 oil bath, n—non-volatile, silicone fluid contained in a 6.9 Auxiliary Equipment, (that is, a 76-mm stir bar, lab jack,
large heat resistant crystallizing dish heated by a temperature lab stand, flask clamp, glass bubbler filled with mineral oil,
controlled stirrer hot-plate. inert gas source, etc.).
3.1.6 solution, n—resin and solvent form a clear, compat- 6.10 Assembly of Hot Oil Bath Set-Up— Place a stirrer/hot
ible, and homogeneous mixture. plate in an aluminum tray on a lab jack. Put the crystallization
3.1.6.1 Discussion—Industrial practice may use the term dish filled approximately ⁄3 with silicone oil on top of the hot
“solution” loosely to describe what may actually be a clear plate. Arrange the condenser above the center of the bath.
“dispersion.” For the sack of simplification, the terms solution ClamptheErlenmeyerflaskcontainingthesolutioningredients
and dispersion have been used interchangeably in this practice. on to the condenser. Adjust the flow of nitrogen to flow down
the condenser into the Erlenmeyer flask. Lower the flask into
HOT OIL BATH
the oil bath.
4. Summary of Hot Oil Bath Practice
7. Reagents
4.1 Place the required amount of resin and solvent in a
7.1 Solvents used in this procedure will be those most often
250-mL Erlenmeyer flask.
used in the manufacture of lithographic ink vehicles, for
4.2 A hot oil bath is heated to the required dissolution
example, hydrocarbon petroleum distillate C to C and
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temperature (150 to 200°C, typically about 180°C or slightly
vegetable oils.
higher for high softening point or poorly solvated resins).
4.3 The Erlenmeyer flask containing the mixture of resin
8. Reagents and Materials
and solvent is placed into the hot oil bath with inert gas purge
8.1 Nonvolatile Resins, (for example, hydrocarbon resins,
and a cold water condenser.
rosin ester resins).
4.4 Allow the mixture to mix at the desired temperature
8.2 Solvents, used in this procedure will be those most often
until all of the resin is completely dissolved.
used in the manufacture of lithographic ink vehicles, for
4.5 Remove the flask from the hot oil bath and allow it to
example, alkali refined linseed oil (ARLO), hydrocarbon
cool while still under an inert atmosphere for 10 to 15 min.
petroleum distillate C to C .
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Save the sample for future testing.
8.3 The resins and solvents agreed upon between producer
and user.
5. Significance and Use
8.4 Standard Ink Oils.
5.1 These practices provide means of preparing small quan-
tities of resin solution (in some procedures in an inert gas
9. Procedure
atmosphere using uniform, controlled heating).
9.1 Set the hot oil bath to heat at the specified temperature.
5.2 This practice provides quick ways to prepare a resin
Set the temperature, if possible, at 10°C above the softening
solution for quality control testing during the manufacture of
point of the resin, but below the initial boiling point of the
resin solutions and vehicles. Samples can usually be prepared
solvent. (180°C is a common starting temperature for many
in approximately 30 to 45 minutes or less.
high-melting-point ink resins.)
5.3 These practices can be used to prepare commonly
9.2 Crush large size pieces of resin sample and pass the
specified ink test solutions such as 33.3 % resin in alkali
crushed resin through a 16-mesh sieve.
refined linseed oil, and 50 % resin in heat-set ink solvent (that
9.3 Weigh to the nearest 0.02 g, an appropriate amount of
is, C to C hydrocarbon petroleum distillate with initial
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the screened resin into a 250-mL Erlenmeyer flask to meet the
boiling point (IBP) about 470°F).
concentration requirements for preparation of a 30 to 100-g
sample. Typically 100 g of solution is prepared.
6. Apparatus
9.3.1 —Examples of common ink resin solutions are as
6.1 Balance, capable of weighing to 60.01 g accuracy.
follows:
6.2 Sieve, 16-mesh.
6.3 Thermometer (see Specification E1)or Thermocouple
(see Specification E230),AP style with a range of 0 to 250°C.
Suitable standard ink oils are available from several suppliers. Please contact
6.4 Heat Resistant Crystallizing Dish, 150 by 75 mm in
the NationalAssociation of Printing Ink Manufacturers, Inc., (NAPIM) at 581 Main
size.
St., Woodbridge, NJ 07095; Phone: 732–855–1525 (email: napim@napim.org) for
6.5 Stirrer/Hot Plate, with a range of 38 to 371°C. assistance.
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D5958–99 (2005)
12.2 The resulting fluid dispersion can be used to measure
Solution No. 1 Percent Solution No. 2 Percent
parameters such as viscosity and aliphatic solubility or com-
resin 33.3 resin 50
patibility of a printing ink resin.
alkali refined linseed oil 66.7 470°F IBP ink oil 50
100.0 100
13. Apparatus
9.3.2 High-viscosity, high-molecular weight, (“structured”
13.1 Erlenmeyer Flask, 125-mL, fitting the following de-
or “self-gelling”) resins may require a stronger solvent system.
scription: a height of 114 mL, an outside base diameter of 67
Possibleresinsolutionsforusewiththeseresinsareasfollows:
mL, and an opening of 27 mL.
Solution No. 3 Percent
13.2 Magnetic Stirring Bar, polytetrafluoroethylene-coated,
resin 45
and 25 mm in length.
TXIB 30
13.3 Thermometer, No. 42°C, conforming to Specification
243°C (470°F) IBP ink oil 25
E1, or other accurate temperature measuring device capable of
100.0
Solution No. 4 Percent measuring to 220°C or greater, in 1°C increments.
13.4 Cork Stopper, high quality, designed to fit the flask
resin 50
used. This cork is then bored out appropriately to receive the
TXIB 50
100.0 thermometer in 13.3 in a snug fashion. The hole should be
drilled at an angle of approximately 25° so the tip of the
9.4 Weighconcentrationofsolventneededtothenearest0.1
thermometer comes to rest at the inside edge of the flask. Place
g.
a small groove on the side of the cork to prevent pressure
9.5 Place flask containing resin mixture into ground glass
build-up.
fittingonwater-cooledcondenser,secureflaskwithclamp,jack
13.5 Hot Plate Stirrer, capable of a surface temperature of
up hot oil bath under flask until the bottom of the flask is close
300°C.
enough to the bottom of the bath (but not touching the bottom)
13.6 Stop Watch.
for the stir bar to mix efficiently. Maintain inert gas flow over
the resin-solvent mixture at approximately 1 bubble per 5 s
14. Calibration and Standardization
through the outlet mineral oil bubbler. If lab jack not available,
14.1 The setting of the hot plate surface temperature must
lower flask manually.
be calibrated by making a blank run in the following manner.
9.6 Allow the mixture to continue mixing until all resin is
14.2 Determine the total mass of the intended solution
dissolved.
described in 12.1 (Note: the mass should be between 30 and 45
9.7 Check to see that all resin is dissolved.
g). Weigh into the 125-mL Erlenmeyer flask a quantity of
9.8 After all the resin is in solution, and if the solution is
ARLO equal to the intended solution mass described in 12.2.
clear, lower the hot oil bath and allow the solution to cool
Next, add the stirring bar and affix the thermometer/cork
under the inert gas atmosphere.
assembly described in 13.4 to the Erlenmeyer flask.
14.3 Turnonthehotplatetemperaturecontrollertoasetting
10. Evaluation
that will give a surface temperature of approximately 300°C.
10.1 During solution preparation, observe the dissolution of
Allow the hot plate 10 min to heat up and equilibrate.
resin and, if desired, record the time and temperature at which
14.4 Settheflaskonthepreheatedhotplatestirrerandbegin
dissolution occurred or the maximum temperature at which the
stirring.
mixture was heated if the resin did not dissolve.
14.5 Start the stop watch.
10.2 Upon cooling, samples can be tested for viscosity
14.6 Measure the time required for the ARLO to reach a
following Test Method D1725, dilutability following Test
temperature of 215°C.
Method D5062, color, etc.
14.7 The hot plate surface temperature is correct when the
ARLO heats from room temperature to 215°C in 11 min 615
11. Report
s. On a hot plate, this is usually at a setting between 5 and 6 on
11.1 Report on solution preparation the following informa-
the temperature-controller dial.
tion:
11.1.1 Dissolution time and temperature,
15. Procedure
11.1.2 Solution clarity,
15.1 Crush large size pieces of resin sample and pass the
11.1.3 Failure of resin dissolution, if necessary, and
crushed resin through a 16-mesh sieve.
11.1.4 Maximum temperature at which resin failed to dis-
15.2 Weigh to 60.02 g into the Erlenmeyer flask, the ink
solve.
resin and solvent at the ratio agreed upon between producer
and user. Typical resin solutions are noted in 9.3.1. The total
STIRRER—HOT PLATE
mass of ink resin solids and solvent should be between 30 and
12. Summary of Stirrer/Hot Plate Practice 45 g.
15.3 Carefully place the stirring bar into the flask to avoid
12.1 Small samples of ink resin and aliphatic ink oil or ink
splashing the solvent.
resin and alkali-refined linseed oil (ARLO) are cut into
dispersion in an Erlenmeyer flask to a specific temperature, at
NOTE 1—It is not recommended that the stirring bar be added to the
a specified rate, with stirring. tared flask while on an electronic balance. The magnetic field associated
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D5958–99 (2005)
with the stirring bar can affect weighing accuracies.
16.4 Based
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