ASTM D5166-97

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

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 This standard does not purport to address all of the safety problems, 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.

General Information

• Status: Historical
• Publication Date: 09-Dec-1997
• Technical Committee: D01 - Paint and Related Coatings, Materials, and Applications
• Drafting Committee: D01.37 - Ink Vehicles

Relations

• Replaced By: ASTM D5166-97(2003) - Standard Practice for Laboratory Preparation of Gelled Vehicle Samples Using a Microwave Oven
• Effective Date: 10-May-2003

Standards Content (Sample)

NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
Designation: D 5166 – 97
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 (e) indicates an editorial change since the last revision or reapproval.
1. Scope hydroxyl groups present on the backbone of resins and alkyds
to form cross-linked networks. (Also called “gellant”.)
1.1 This practice outlines a procedure for preparing gelled
3.1.3 gel length—References to long, medium, and short gel
vehicle samples using a microwave oven.
length refer to the length of a string of gelled vehicle observed
1.2 The test samples can be used for characterizing the
when pulling apart a small sample of vehicle with a spatula
gelability or reactivity of resins, gelling agents, and vehicles
(that is, a long gel is very fluid and forms a “long” filament; a
used in the manufacture of oil based printing inks, or both.
short gel has little flow and forms a “short” filament).
1.3 Evaluation of the gelled vehicles may, depending upon
3.1.4 pregel—The resin solution or vehicle components
preference, be either visual or instrumental.
comprising the vehicle prior to the addition of gelling agent
1.4 This standard does not purport to address all of the
and viscosity adjusting solvent. (Also called “pregel vehicle”.)
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
4. Summary of Practice
priate safety and health practices and determine the applica-
4.1 Prepare a pregel resin solution or vehicle.
bility of regulatory limitations prior to use.
4.2 Separate the pregel vehicle into five or more aliquots to
2. Referenced Documents which various levels of gellant are added. Alternately, various
gellants can be added at a given concentration to compare their
2.1 ASTM Standards:
effectiveness.
D 154 Guide for Testing Varnishes
4.3 Place the test samples on a turntable in the microwave
D 1545 Test Method for Viscosity of Transparent Liquids
oven and heat the samples at full power until the desired test
by Bubble Time Method
temperature is attained.
D 1725 Test Method for Viscosity of Resin Solutions
4.4 After the prescribed waiting period, test and rate
D 4040 Test Method for Viscosity of Printing Inks and
samples for gelability.
Vehicles by Falling Rod Viscometer
E 1 Specification for ASTM Thermometers
5. Significance and Use
3. Terminology 5.1 This practice provides a means of preparing a number of
gel vehicle samples with minimum use of materials and time.
3.1 Definitions of Terms Specific to This Standard:
It provides a means of quickly characterizing and comparing
3.1.1 gel—Any resin solution, or more complex blend of
the gelability or reactivity of resins, vehicles, and gelling
resins and alkyds that has been cooked or reacted with a gelling
agents.
or cross-linking agent to build molecular weight and that
exhibits a pseudoplastic rheology. (Also called “gelled ve-
6. Apparatus
hicle.”)
6.1 Mercury Thermometer, capable of reading from 0 to
3.1.2 gelling agent—in the context of ink resins and ve-
250°C and conforming to Specification E 1.
hicles, gelling agents or gellants are typically organo-
6.2 Jars, (40 mm in diameter by 83 mm in height), 70 cm
aluminum compounds that react with carboxylic acid and
with nonmetallic screw-on lids.
6.3 Microwave Oven, common 750-watt.
This practice is under the jurisdiction of ASTM Committee D-1 on Paint and 6.4 Microwave Oven Carousel, if not contained in the
Related Coatings, Materials, and Applications and is the direct responsibility of
microwave oven.
Subcommittee D01.37 on Ink Vehicles.
Current edition approved Dec. 10, 1997. Published June 1998. Originally
published as D 5166 – 91. Last previous edition D 5166 – 91.
2 5
Annual Book of ASTM Standards, Vol 06.03. Any common microwave oven, available at most appliance stores, can be used.
Annual Book of ASTM Standards, Vol 06.02. A 750–watt oven with a built–in turntable is preferred. Ovens with lower power will
Annual Book of ASTM Standards, Vol 14.03. require adjustments in the test cycle.
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NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
D5166–97
TABLE 1 Microwave Gelability Test, Weights and Concentrations
6.5 Glass Dish, 15.2 cm in diameter.
for 50-g Samples
6.6 Balance or Scale, capable of weighing to 60.1 g
Weight Gellant
accuracy.
A
Gellant Actual Gellant Solution, g
A
6.7 Ink Knife or Rigid Spatula. Weight Ink Oil, g
Solution, % Concentration, % (at 33.3 %
6.8 Rheology Testing Apparatus, at the discretion of the Gellant in Ink Oil)
user.
0 0.00 0.0 5.0
1 0.33 0.5 4.5
2 0.67 1.0 4.0
7. Reagents and Materials
3 1.00 1.5 3.5
7.1 Nonvolatile materials including resins, alkyds, gellants, 4 1.33 2.0 3.0
5 1.67 2.5 2.5
etc., consistent with those used in the manufacture of litho-
6 2.00 3.0 2.0
graphic ink vehicles, for example, aromatic hydrocarbon res-
7 2.33 3.5 1.5
8 2.67 4.0 1.0
ins, modified rosin ester resins, long oil linseed isophthalic
9 3.00 4.5 0.5
alkyds, and aluminum compounds.
10 3.33 5.0 0.0
7.2 Solvents typically used in the manufacture of litho-
A
Weight added to 45-g pregel sample.
graphic ink vehicles, for example, hydrocarbon petroleum
distillate with carbon numbers in the range of C12 to C16 and
initial boiling point above 150°C.
8.4 Place the five sample bottles, without tops, into the
15.2-cm glass dish and place on the carousel in the microwave
8. Procedure
oven.
8.1 Place 45 g (or the calculated weight) of previously
8.5 Turn on the carousel and ensure that it is turning before
prepared pregel veh
...