ASTM D5958-99

Standard Practices for Preparation of Oil-Based Ink Resin Solutions

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 6 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 hot oil bath procedure (Practice D 5597) 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 letter press 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, 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 degrees C (140 degrees F) as determined by Test Method D 56.  
Note 1- Precaution - Users of this practice should be aware that the flash point of many solvents used for this test (as defined in Test Methods D 56 and D 1310) 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 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 Note 6.

General Information

• Status: Historical
• Publication Date: 09-May-1999
• ICS: 87.080 - Inks. Printing inks
• Technical Committee: D01 - Paint and Related Coatings, Materials, and Applications
• Drafting Committee: D01.37 - Ink Vehicles

Relations

• Replaced By: ASTM D5958-99(2005)e1 - Standard Practices for Preparation of Oil-Based Ink Resin Solutions
• Effective Date: 01-Sep-2005

Standards Content (Sample)

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
Designation:D5958–99
Standard Practices for
Preparation of Oil-Based Ink Resin Solutions
This standard is issued under the fixed designation D 5958; 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 (e) indicates an editorial change since the last revision or reapproval.
NOTE 1—Precaution: Users of this practice should be aware that the
1. Scope *
flash point of many solvents used for this test (as defined in Test Methods
1.1 These practices describe laboratory procedures for pre-
D 56 and D 1310) is exceeded in the heating cycle of this test method.
paring an oil-based ink resin solution in a high-boiling solvent
Take safety precautions since there is the potential for vapor ignition. Do
using four pieces of lab equipment; (1) a hot oil bath (Sections
the methods outlined in a shielded exhaust hood, where there is access to
4to11), a fire extinguisher if needed.
(2) a stirrer/hot plate (Sections 12 to 16),
1.7 This standard does not purport to address all of the
(3) an industrial blender (Sections 17 to 22), and
safety concerns, if any, associated with its use. It is the
(4) a hot air gun (Sections 23 to 27).
responsibility of the user of this standard to establish appro-
ASTM Subcommittee D01.37 recommends using the hot oil
priate safety and health practices and determine the applica-
bath procedure (Practice D 5597) where possible.
bility of regulatory limitations prior to use. For specific hazard
1.2 These practices use laboratory equipment generally
statement see Note 6.
available in a normal, well-equipped laboratory.
1.3 One or several of these practices allows for rapid resin 2. Referenced Documents
solution preparation (under 30 min, typical), can regulate the
2.1 ASTM Standards:
maximum temperature, can be done under an inert atmosphere,
D 56 Test Method for Flash Point by Tag Closed Cup
and can prevent the random solvent loss during preparation.
Tester
1.4 These procedures are for use with ink resins intended
D 1310 Test Method for Flash Point and Fire Point of
mainly for oil-based offset and letterpress inks. The type of
Liquids by the Tag Open-Cup Apparatus
resins are typically, but not limited to C aromatic hydrocarbon
D 1725 Test Method for Viscosity of Resin Solutions
resins, modified dicyclopentadiene resins, rosin pentaerythritol
D 5062 Test Method for Resin Solution Dilutability by
or glycerine esters, phenolic modified rosin esters, maleic
Volumetric/Gravimetric Determination
anhydride modified rosin esters, and naturally occurring resins
D 5597 Practice for Preparation of Oil-Based Ink Resin
such as gilsonite. 6
Solutions Using a Hot Oil Bath
1.5 The typical high boiling solvents to be used include C
E 1 Specification for ASTM Thermometers
to C petroleum distillates, 2,2,4 trimethyl 1,3-pentanediol
16 E 230 Specification for Temperature-Electromotive Force
di-isobutyrate, alkali refined linseed oil, tridecyl alcohol, or
(EMF) Tables for Standardized Thermocouples
combinations of the above.
3. Terminology
1.6 To avoid fire or injury, or both, to the operator, these
practices should not be used with low flash point solvents such
3.1 Definitions:
as toluene or xylene. The minimum flash point of the solvents
3.1.1 cold cut—dispersion of resin into solvent using high
used should be 60°C (140°F) as determined by Test Method
shear dispersion without external heating.
D 56.
3.1.2 compatibility—resin and solvent mixture forms a
clear, homogeneous, and stable solution.
3.1.3 dissolution—the point at which all resin completely
These practices are under the jurisdiction of ASTM Committee D-1 on Paint dissolves in the solvent.
and Related Coatings, Materials, andApplications and is the direct responsibility of
3.1.4 incompatibility—resin and solvent mixture is not
Subcommittee D01.37 on Ink Vehicles.
compatible, an opaque or two phase mixture results.
Current edition approved May 10, 1999. Published July 1999. Originally
published as D 5958-96. Last previous edition D 5958-96.
The sole source of supply of the plasticizer TXIB known to the committee at
this time is Eastman Chemical Company, / Texas E. M. Division, P.O. Box 7444, Annual Book of ASTM Standards, Vol 05.01.
Longview,TX 75607-7444. If you are aware of alternative suppliers, please provide Annual Book of ASTM Standards, Vol 06.01.
this information to ASTM Headquarters. Your comments will receive careful Annual Book of ASTM Standards, Vol 06.03.
consideration at a meeting of the responsible technical committee, which you may Discontinued; see 1998 Annual Book of ASTM Standards, Vol 06.03.
attend. Annual Book of ASTM Standards, Vol 14.03.
*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.
D5958
3.1.5 oil bath—non-volatile, silicone fluid contained in a plate. Arrange the condenser above the center of the bath.
large heat resistant crystallizing dish heated by a temperature ClamptheErlenmeyerflaskcontainingthesolutioningredients
controlled stirrer hot-plate. on to the condenser. Adjust the flow of nitrogen to flow down
3.1.6 solution—resin and solvent form a clear, compatible, the condenser into the Erlenmeyer flask. Lower the flask into
and homogeneous mixture. the oil bath.
3.1.6.1 Discussion—Industrial practice may use the term
7. Reagents
“solution” loosely to describe what may actually be a clear
“dispersion”. For the lack of simplification, the terms solution 7.1 Solvents used in this procedure will be those most often
and dispersion have been used interchangeably in this practice.
used in the manufacture of lithographic ink vehicles, for
example, hydrocarbon petroleum distillate C to C , veg-
12 16
HOT OIL BATH
etable oils.
4. Summary of Hot Oil Bath Practice
8. Reagents and Materials
4.1 Place the required amount of resin and solvent in a
8.1 Nonvolatile Resins, (for example, hydrocarbon resins,
250-mL Erlenmeyer flask.
rosin ester resins).
4.2 A hot oil bath is heated to the required dissolution
8.2 Solvents, used in this procedure will be those most often
temperature (150 to 200°C, typically about 180°C or slightly
used in the manufacture of lithographic ink vehicles, for
higher for high softening point or poorly solvated resins).
example, alkali refined linseed oil (ARLO), hydrocarbon
4.3 The Erlenmeyer flask containing the mixture of resin
petroleum distillate C to C .
12 16
and solvent is placed into the hot oil bath with inert gas purge
8.3 The resins and solvents agreed upon between producer
and a cold water condenser.
and user.
4.4 Allow the mixture to mix at the desired temperature
8.4 Standard Ink Oils.
until all of the resin is completely dissolved.
4.5 Remove the flask from the hot oil bath and allow it to 9. Procedure
cool while still under an inert atmosphere for 10 to 15 min.
9.1 Set the hot oil bath to heat at the specified temperature.
Save the sample for future testing.
Set the temperature, if possible, at 10°C above the softening
point of the resin, but below the initial boiling point of the
5. Significance and Use
solvent. (180°C is a common starting temperature for many
5.1 These practices provide means of preparing small quan-
high-melting-point ink resins.)
tities of resin solution (in some procedures in an inert gas
9.2 Crush large size pieces of resin sample and pass the
atmosphere using uniform, controlled heating).
crushed resin through a 16-mesh sieve.
5.2 This practice provides quick ways to prepare a resin
9.3 Weigh to the nearest 0.02 g, an appropriate amount of
solution for quality control testing during the manufacture of
the screened resin into a 250-mL Erlenmeyer flask to meet the
resin solutions and vehicles. Samples can usually be prepared
concentration requirements for preparation of a 30 to 100-g
in approximately 30 to 45 minutes or less.
sample. Typically 100 g of solution is prepared.
5.3 These practices can be used to prepare commonly
9.3.1 —Examples of common ink resin solutions are as
specified ink test solutions such as 33.3 % resin in alkali
follows:
refined linseed oil, and 50 % resin in heat-set ink solvent (that
Solution No. 1 Percent Solution No. 2 Percent
is, C to C hydrocarbon petroleum distillate with initial
12 16
resin 33.3 resin 50
boiling point (IBP) about 470°F).
alkali refined linseed oil 66.7 470°F IBP ink oil 50
100.0 100
6. Apparatus
9.3.2 High viscosity, high molecular weight, (“structured”
6.1 Balance, capable of weighing to 60.01 g accuracy.
or “self gelling”) resins may require a stronger solvent system.
6.2 Sieve, 16-mesh.
Possibleresinsolutionsforusewiththeseresinsareasfollows:
6.3 Thermometer (see Specification E 1) or Thermocouple
Solution No. 3 Percent
(see Specification E 230),APstyle with a range of 0 to 250°C.
6.4 Heat Resistant Crystallizing Dish, 150 by 75 mm in
resin 45
size. TXIB 30
243°C (470°F) IBP ink oil 25
6.5 Stirrer/Hot Plate, with a range of 38 to 371°C.
100.0
6.6 Condenser, with ground glass joints.
Solution No. 4 Percent
6.7 Erlenmeyer Flask, 250-mLwith 24/40 joint top and side
resin 50
arm.
TXIB 50
6.8 Silicone Oil.
100.0
6.9 Auxiliary Equipment, (that is, a 76-mm stir bar, lab jack,
lab stand, flask clamp, glass bubbler filled with mineral oil,
inert gas source, etc.).
Suitable standard ink oils are available from several suppliers. Please call the
6.10 Assembly of Hot Oil Bath Set-Up— Place a stirrer/hot
National Association of Printing Ink Manufacturers, Inc., (NAPIM) at Heights
plate in an aluminum tray on a lab jack. Put the crystallization
Plaza: 777 TerraceAve., Hasbrouck Heights, NJ 07604; Phone: [phone] for
dish filled approximately ⁄3 with silicone oil on top of the hot assistance.
D5958
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
14. Calibration and Standardization
the resin-solvent mixture at approximately 1 bubble per 5 s
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 D 1725, dilutability following Test
temperature of 215°C.
Method D 5062, color, etc.
14.7 The hot plate surface temperature is correct when the
ARLO heats from room temperature to 215°C in 11 min 6 15
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
45 g.
12. Summary of Stirrer/Hot Plate Practice
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 2—It is not recommended that the stirring bar be added to the
tared flask while on an electronic balance. The magnetic field associated
a specified rate, with stirring.
with the stirring bar can affect weighing accuracies.
12.2 The resulting fluid dispersion can be used to measure
parameters such as viscosity and aliphatic solubility or com- 15.4 Affix the thermometer/cork assembly in the mouth of
patibility of a printing ink resin. the flask.Adjust the thermometer tip so it is just off the bottom
surface of the flask (1 mm).
13. Apparatus
15.5 Place the flask on the hot plate stirrer that has been
13.1 Erlenmeyer Flask, 125-mL, fitting the following de- heated 10 min to the calibrated setting derived in Section 14.
scription: a height of 114 mL, an outside base diameter of 67 15.6 Without stirring, let the ink resin-solvent slurry heat to
mL, and an opening of 27 mL. 100°C.
13.2 Magnetic Stirring Bar, polytetrafluoroethylene-coated, 15.7 When the temperature reaches 100°C, begin stirring
and 25 mm in length. the mixture. Keep the stir rate slow at first (so that resin is
13.3 Thermometer, No. 42°C, conforming to Specification moving in the solvent but does not splash resin up above the
E 1, or other accurate temperature measuring device capable of solvent level). For more efficient dissolution, mixing speed is
measuring to 220°C or greater, in 1°C increments. gradually increased as the resin softens. Avoid over-stirring
13.4 Cork Stopper, high q
...