Standard Practice for Laboratory Preparation of Gelled Vehicle Samples Using a Microwave Oven

SIGNIFICANCE AND USE
This practice provides a means of preparing a number of gel vehicle samples with minimum use of materials and time. It provides a means of quickly characterizing and comparing the gelability or reactivity of resins, vehicles, and gelling agents.
SCOPE
1.1 This practice outlines a procedure for preparing gelled vehicle samples using a microwave oven.
1.2 The test samples can be used for characterizing the gelability or reactivity of resins, gelling agents, and vehicles used in the manufacture of oil based printing inks, or both.
1.3 Evaluation of the gelled vehicles may, depending upon preference, be either visual or instrumental.
1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.5 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.

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Publication Date
31-May-2008
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ASTM D5166-97(2008) - Standard Practice for Laboratory Preparation of Gelled Vehicle Samples Using a Microwave Oven
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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:D5166–97(Reapproved2008)
Standard Practice for
Laboratory Preparation of Gelled Vehicle Samples Using a
Microwave Oven
This standard is issued under the fixed designation D 5166; 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 3.1.1 gel, n—Any resin solution, or more complex blend of
resinsandalkydsthathasbeencookedorreactedwithagelling
1.1 This practice outlines a procedure for preparing gelled
or cross-linking agent to build molecular weight and that
vehicle samples using a microwave oven.
exhibits a pseudoplastic rheology. (Also called “gelled ve-
1.2 The test samples can be used for characterizing the
hicle.”)
gelability or reactivity of resins, gelling agents, and vehicles
3.1.2 gelling agent, n—in the context of ink resins and
used in the manufacture of oil based printing inks, or both.
vehicles, gelling agents or gellants are typically organo-
1.3 Evaluation of the gelled vehicles may, depending upon
aluminum compounds that react with carboxylic acid and
preference, be either visual or instrumental.
hydroxyl groups present on the backbone of resins and alkyds
1.4 The values stated in SI units are to be regarded as
to form cross-linked networks. (Also called “gellant.”)
standard. No other units of measurement are included in this
3.1.3 gel length, n—References to long, medium, and short
standard.
gel length refer to the length of a string of gelled vehicle
1.5 This standard does not purport to address all of the
observed when pulling apart a small sample of vehicle with a
safety concerns, if any, associated with its use. It is the
spatula (that is, a long gel is very fluid and forms a “long”
responsibility of the user of this standard to establish appro-
filament; a short gel has little flow and forms a “short”
priate safety and health practices and determine the applica-
filament).
bility of regulatory limitations prior to use.
3.1.4 pregel, n—The resin solution or vehicle components
2. Referenced Documents comprising the vehicle prior to the addition of gelling agent
and viscosity adjusting solvent. (Also called “pregel vehicle.”)
2.1 ASTM Standards:
D 154 Guide for Testing Varnishes
4. Summary of Practice
D 1545 Test Method for Viscosity of Transparent Liquids
4.1 Prepare a pregel resin solution or vehicle.
by Bubble Time Method
4.2 Separate the pregel vehicle into five or more aliquots to
D 1725 Test Method for Viscosity of Resin Solutions
which various levels of gellant are added. Alternately, various
D 4040 Test Method for Rheological Properties of Paste
gellants can be added at a given concentration to compare their
Printing and Vehicles by the Falling-Rod Viscometer
effectiveness.
E1 Specification forASTM Liquid-in-Glass Thermometers
4.3 Place the test samples on a turntable in the microwave
3. Terminology oven and heat the samples at full power until the desired test
temperature is attained.
3.1 Definitions of Terms Specific to This Standard:
4.4 After the prescribed waiting period, test and rate
samples for gelability.
This practice is under the jurisdiction of ASTM Committee D01 on Paint and
Related Coatings, Materials, and Applications and is the direct responsibility of
5. Significance and Use
Subcommittee D01.37 on Ink Vehicles.
5.1 Thispracticeprovidesameansofpreparinganumberof
Current edition approved June 1, 2008. Published June 2008. Originally
approved in 1991. Last previous edition approved in 2003 as D 5166 – 97 (2003).
gel vehicle samples with minimum use of materials and time.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
It provides a means of quickly characterizing and comparing
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
the gelability or reactivity of resins, vehicles, and gelling
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. agents.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D5166–97 (2008)
TABLE 1 Microwave Gelability Test, Weights and Concentrations
6. Apparatus
for 50-g Samples
6.1 Mercury Thermometer, capable of reading from 0 to
Weight Gellant
250°C and conforming to SpecificationE1.
A
Gellant Actual Gellant Solution, g
A
3 Weight Ink Oil, g
6.2 Jars, (40 mm in diameter by 83 mm in height), 70 cm Solution, % Concentration, % (at 33.3 %
Gellant in Ink Oil)
with nonmetallic screw-on lids.
0 0.00 0.0 5.0
6.3 Microwave Oven, common 750-watt.
1 0.33 0.5 4.5
6.4 Microwave Oven Carousel, if not contained in the
2 0.67 1.0 4.0
microwave oven.
3 1.00 1.5 3.5
4 1.33 2.0 3.0
6.5 Glass Dish, 15.2 cm in diameter.
5 1.67 2.5 2.5
6.6 Balance or Scale, capable of weighing to 60.1 g
6 2.00 3.0 2.0
accuracy.
7 2.33 3.5 1.5
8 2.67 4.0 1.0
6.7 Ink Knife or Rigid Spatula.
9 3.00 4.5 0.5
6.8 Rheology Testing Apparatus, at the discretion of the
10 3.33 5.0 0.0
user.
A
Weight added to 45-g pregel sample.
7. Reagents and Materials
7.1 Nonvolatile materials including resins, alkyds, gellants,
50 % gellant in major vehicle solvent recommended) in 1 %
etc., consistent with those used in the manufacture of litho-
increments plus additional solvent to adjust the vehicle to a
graphic ink vehicles, for example, aromatic hydrocarbon res-
100 % formula. If the amount of gellant required can not be
ins, modified rosin ester resins, long oil linseed isophthalic
estimated, use a larger range of gellant concentration.
alkyds, and aluminum compounds.
8.2.1 If using the pregel formula as just recommended, the
7.2 Solvents typically used in the manufacture of litho-
required amount of gellant can be estimated from Table 1.
graphic ink vehicles, for example, hydrocarbon petroleum
8.2.2 A sample containing no (0 %) gellant solution is
distillate
...

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