ASTM D3596-92

Standard Practice for Determination of Gels (Fisheyes) In General-Purpose Poly(Vinyl Chloride) (PVC) Resins (Withdrawn 2001)

SCOPE
1.1 This practice provides a quantitative measure of the gels remaining in a flexible vinyl compound processed from general-purpose poly(vinyl chloride) (PVC) resins under a prescribed set of working conditions.
1.2 The values stated in SI units are to be regarded as the standard. The values in parentheses are for information only.  
1.3 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.
Note 1—There are no ISO standards covering the primary subject of this practice.

General Information

• Status: Historical
• Publication Date: 14-Oct-1992
• Withdrawal Date: 09-Oct-2001
• ICS: 83.080.10 - Thermosetting materials
• Technical Committee: D20 - Plastics
• Drafting Committee: D20.15 - Thermoplastic Materials

Relations

• Replaced By: ASTM D3596-92(2001) - Standard Practice for Determination of Gels (Fisheyes) In General-Purpose Poly(Vinyl Chloride) (PVC) Resins
• Effective Date: 15-Oct-1992

Standards Content (Sample)

Designation: D 3596 – 92 An American National Standard
AMERICAN SOCIETY FOR TESTING AND MATERIALS
100 Barr Harbor Dr., West Conshohocken, PA 19428
Reprinted from the Annual Book of ASTM Standards. Copyright ASTM
Standard Practice for
Determination of Gels (Fisheyes) In General-Purpose
1
Poly(Vinyl Chloride) (PVC) Resins
This standard is issued under the fixed designation D 3596; 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 using a bottom-lighted viewing box and a magnifying com-
parator.
1.1 This practice provides a quantitative measure of the gels
remaining in a flexible vinyl compound processed from
5. Significance and Use
general-purpose poly(vinyl chloride) (PVC) resins under a
5.1 The gel (fisheye) in PVC resins is generally recognized
prescribed set of working conditions.
as a hard particle of resin which will not fuse when the plastic
1.2 The values stated in SI units are to be regarded as the
mass is subjected to set conditions of hot processing. The
standard. The values in parentheses are for information only.
number of unfused particles present is related to the conditions
1.3 This standard does not purport to address all of the
used. The presence of an excess of such particles is detrimental
safety problems, if any, associated with its use. It is the
to many applications.
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica-
6. Apparatus
bility of regulatory limitations prior to use.
3
6.1 Laboratory Mixer, with stainless steel mixing bowl.
NOTE 1—There are no ISO standards covering the primary subject of
6.2 Two-Roll Mill, 152.4 by 304.8 mm (6 by 12 in.), 263.55
this practice.
mm (10.5 in.) between guides, differential speed ratio 1.40 6
0.04, fast roll speed 34 6 2 rpm, suitably heated to maintain
2. Referenced Documents
roll temperature of 154 6 3°C (310 6 5°F).
2.1 ASTM Standards:
2
NOTE 2—If the mill available does not meet these criteria, the specifi-
D 883 Terminology Relating to Plastics
cations of the mill used should be included in the report.
D 1249 Specification for Octyl Ortho-Phthalate Ester Plas-
2
ticizers 6.3 Surface Pyrometer calibrated in the range of 154°C
D 1600 Terminology for Abbreviated Terms Relating to
(310°F) and a leaf pyrometer calibrated in the range of 163°C
2
Plastics (325°F).
6.4 Balance, 0.1-g sensitivity.
3. Terminology
6.5 Hydraulic Press having platens at least 203 by 203 mm
3.1 General—Definitions are in accordance with Terminol-
(8 by 8 in.), rated at a minimum of 140 MPa (20 000 psi) ram
ogy D 883 and abbreviations with Terminology D 1600, unless
pressure on a 100-mm (4-in.) ram, which may be heated to 163
otherwise indicated.
6 3°C (325 6 5°F) on the pressing surfaces and equipped with
cooling water.
4. Summary of Practice
6.6 Timer, capable of being read in seconds.
4.1 A sample of PVC resin is mixed with calcium stearate
6.7 Cotton Gloves.
and di-2-ethylhexyl phthalate plasticizer (DOP) in a laboratory
6.8 Mill Knife.
mixer. After mixing, the dry blend is milled on a two-roll
6.9 Plates or Mold, two 203 by 203-mm (8 by 8-in.)
laboratory mill; carbon black dispersion is added during the
chrome-plated ferro plates, or a chrome-plated mold with a 152
milling.
by 152 by 6.4-mm (6 by 6 by 0.25-in.) cavity.
4.2 The milled sheet is press-polished and the gels counted
6.10 Backing Plates, two 203 by 203 by 6.4 mm (8 by 8 by
0.250 in.).
6.11 Brass Shims, four, 0.51 by 13 by 203 mm (0.020 by 0.5
by 8.0 in.).
1
This practice is under the jurisdiction of ASTM Committee D-20 on Plastics
and is the direct responsibility of Subcommittee D20.15 on Thermoplastic Materi-
als.
Current edition approved Oct. 15, 1992. Published December 1992. Originally
published as D 3596 – 77. Last previous edition D 3596 – 88.
2 3
Annual Book of ASTM Standards, Vol 08.01. The Hobart Model N-50 is satisfactory.
1

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D 3596
4
roll and produce a 9.5-mm (0.375-in.) diameter (pencil size) rolling bank.
6.12 Magnifying Comparator, equipped with a transparent
Use a clean-up batch to determine the correct amount. Report the weight
reticule (scale) showing circles from 0.03 to 1.27 mm (0.001 to
of dry blend used.
0.050 in.) in diameter.
5
8.3 Cut a 152 by 152-mm (6 by 6-in.) section from the
6.13 Bottom-Lighted Viewing Box.
milled stock.
7. Materials
8.3.1 Place the section cut from the milled sheet between the
two chrome-plated ferro plates, chrome side to the specimen,
7.1 PVC Resin.
then put the chrome ferro plates and the specimen between the
7.2 DOP, Specification D 1249, Type 1.
6
backing plates and insert in a press at 163 6 3°C (325 6 5°F).
7.3 Calcium Stearate.
7
Preheat for 0.5 min with the press closed at z
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