ASTM D5958-99(2011)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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 (Reapproved 2011)
StandardPractices 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-
Test MethodsD56 and D1310) is exceeded in the heating cycle
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
(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. No other units of measurement are included in this
bath procedure (Practice D5597) where possible. standard.
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.
2. Referenced Documents
1.4 These procedures are for use with ink resins intended
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 TestMethodforFlashPointandFirePointofLiquids
or glycerine esters, phenolic modified rosin esters, maleic
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
Volumetric/Gravimetric Determination
1.5 The typical high boiling solvents to be used include C
to C petroleum distillates, 2,2,4 trimethyl 1,3-pentanediol D5597 Practice for Preparation of Oil-Based Ink Resin
Solutions Using a Hot Oil Bath (Withdrawn 1999)
di-isobutyrate, alkali refined linseed oil, tridecyl alcohol, or
combinations of the above. E1 Specification for ASTM Liquid-in-Glass Thermometers
E230 Specification and Temperature-Electromotive Force
1.6 To avoid fire or injury, or both, to the operator, these
(EMF) Tables for Standardized Thermocouples
practices should not be used with low flash point solvents such
as toluene or xylene. The minimum flash point of the solvents
3. Terminology
used should be 60°C (140°F) as determined by Test Method
3.1 Definitions of Terms Specific to This Standard:
3.1.1 cold cut, 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 June 1, 2011. Published June 2011. Originally clear, homogeneous, and stable solution.
ϵ1
approved in 1996. Last previous edition approved in 2005 as D5958 - 99 (2005) .
DOI: 10.1520/D5958-99R11.
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 (Reapproved 2011)
3.1.3 dissolution, n—the point at which all resin completely 6.5 Stirrer/Hot Plate, with a range of 38 to 371°C.
dissolves in the solvent.
6.6 Condenser, with ground glass joints.
3.1.4 incompatibility, n—resin and solvent mixture is not
6.7 Erlenmeyer Flask, 250-mLwith 24/40 joint top and side
compatible, an opaque or two-phase mixture results.
arm.
3.1.5 oil bath, n—non-volatile, silicone fluid contained in a
6.8 Silicone Oil.
large heat resistant crystallizing dish heated by a temperature
6.9 Auxiliary Equipment, (that is, a 76-mm stir bar, lab jack,
controlled stirrer hot-plate.
lab stand, flask clamp, glass bubbler filled with mineral oil,
3.1.6 solution, n—resin and solvent form a clear, compat-
inert gas source, etc.).
ible, and homogeneous mixture.
3.1.6.1 Discussion—Industrial practice may use the term 6.10 Assembly of Hot Oil Bath Set-Up— Place a stirrer/hot
“solution” loosely to describe what may actually be a clear plate in an aluminum tray on a lab jack. Put the crystallization
“dispersion.” For the sack of simplification, the terms solution dish filled approximately ⁄3 with silicone oil on top of the hot
and dispersion have been used interchangeably in this practice. plate. Arrange the condenser above the center of the bath.
ClamptheErlenmeyerflaskcontainingthesolutioningredients
HOT OIL BATH
on to the condenser. Adjust the flow of nitrogen to flow down
the condenser into the Erlenmeyer flask. Lower the flask into
4. Summary of Hot Oil Bath Practice
the oil bath.
4.1 Place the required amount of resin and solvent in a
250-mL Erlenmeyer flask.
7. Reagents
4.2 A hot oil bath is heated to the required dissolution
7.1 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, hydrocarbon petroleum distillate C to C and
12 16
vegetable oils.
4.3 The Erlenmeyer flask containing the mixture of resin
and solvent is placed into the hot oil bath with inert gas purge
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 .
12 16
5. Significance and Use
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
8.4 Standard Ink Oils.
atmosphere using uniform, controlled heating).
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).
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.
concentration requirements for preparation of a 30 to 100-g
sample. Typically 100 g of solution is prepared.
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; (email: napim@napim.org) for assistance.
D5958 − 99 (Reapproved 2011)
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
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
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
and 25 mm in length.
243°C (470°F) IBP ink oil 25
100.0
13.3 Thermometer, No. 42°C, conforming to Specification
Solution No. 4 Percent
E1, or other accurate temperature measuring device capable of
measuring to 220°C or greater, in 1°C increments.
resin 50
TXIB 50
13.4 Cork Stopper, high quality, designed to fit the flask
100.0
used. This cork is then bored out appropriately to receive the
9.4 Weighconcentrationofsolventneededtothenearest0.1
thermometer in 13.3 in a snug fashion. The hole should be
g.
drilled at an angle of approximately 25° so the tip of the
9.5 Place flask containing resin mixture into ground glass
thermometer comes to rest at the inside edge of the flask. Place
fittingonwater-cooledcondenser,secureflaskwithclamp,jack
a small groove on the side of the cork to prevent pressure
up hot oil bath under flask until the bottom of the flask is close
build-up.
enough to the bottom of the bath (but not touching the bottom)
13.5 Hot Plate Stirrer, capable of a surface temperature of
for the stir bar to mix efficiently. Maintain inert gas flow over
300°C.
the resin-solvent mixture at approximately 1 bubble per 5 s
13.6 Stop Watch.
through the outlet mineral oil bubbler. If lab jack not available,
lower flask manually.
14. Calibration and Standardization
9.6 Allow the mixture to continue mixing until all resin is
dissolved. 14.1 The setting of the hot plate surface temperature must
be calibrated by making a blank run in the following manner.
9.7 Check to see that all resin is dissolved.
14.2 Determine the total mass of the intended solution
9.8 After all the resin is in solution, and if the solution is
described in 12.1 (Note: the mass should be between 30 and 45
clear, lower the hot oil bath and allow the solution to cool
g). Weigh into the 125-mL Erlenmeyer flask a quantity of
under the inert gas atmosphere.
ARLO equal to the intended solution mass described in 12.2.
10. Evaluation
Next, add the stirring bar and affix the thermometer/cork
10.1 During solution preparation, observe the dissolution of assembly described in 13.4 to the Erlenmeyer flask.
resin and, if desired, record the time and temperature at which
14.3 Turnonthehotplatetemperaturecontrollertoasetting
dissolution occurred or the maximum temperature at which the
that will give a surface temperature of approximately 300°C.
mixture was heated if the resin did not dissolve.
Allow the hot plate 10 min to heat up and equilibrate.
10.2 Upon cooling, samples can be tested for viscosity
14.4 Settheflaskonthepreheatedhotplatestirrerandbegin
following Test Method D1725, dilutability following Test
stirring.
Method D5062, color, etc.
14.5 Start the stop watch.
11. Report
14.6 Measure the time required for the ARLO to reach a
11.1 Report on solution preparation the following informa-
temperature of 215°C.
tion:
14.7 The hot plate surface temperature is correct when the
11.1.1 Dissolution time and temperature,
ARLO heats from room temperature to 215°C in 11 min 615
11.1.2 Solution clarity,
s. On a hot plate, this is usually at a setting between 5 and 6 on
11.1.3 Failure of resin dissolution, if necessary, and
the temperature-controller dial.
11.1.4 Maximum temperature at which resin failed to dis-
solve.
15. Procedure
STIRRER—HOT PLATE
15.1 Crush large size pieces of resin sample and pass the
crushed resin through a 16-mesh sieve.
12. Summary of Stirrer/Hot Plate Practice
12.1 Small samples of ink resin and aliphatic ink oil or ink 15.2 Weigh to 60.02 g into the Erlenmeyer flask, the ink
resin and alkali-refined linseed oil (ARLO) are cut into resin and solvent at the ratio agreed upon between producer
D5958 − 99 (Reapproved 2011)
and user. Typical resin solutions are noted in 9.3.1. The total aliphatic petroleum distillate. Using this practice to make the
mass of ink resin solids and solvent should be between 30 and solution, the operators then measured the viscosity of the
45 g. dispersion in accordance with Test Method D1725.
15.3 Carefully place the stirring bar into the flask to avoid 16.2 Each operator ran duplicate samples on Day 1 and Day
splashing the solvent. 2. The overall ave
...