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

SIGNIFICANCE AND USE
The gel (fisheye) in PVC resins is generally recognized as a hard particle of resin which will not fuse when the plastic mass is subjected to set conditions of hot processing. The number of unfused particles present is related to the conditions used. The presence of an excess of such particles is detrimental to many applications.
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 is no known ISO equivalent to this standard.

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ASTM D3596-09 - Standard Practice for Determination of Gels (Fisheyes) In General-Purpose Poly(Vinyl Chloride) (PVC) Resins
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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: D3596 − 09
StandardPractice for
Determination of Gels (Fisheyes) In General-Purpose
1
Poly(Vinyl Chloride) (PVC) Resins
This standard is issued under the fixed designation D3596; 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* 5. Significance and Use
1.1 This practice provides a quantitative measure of the gels
5.1 The gel (fisheye) in PVC resins is generally recognized
remaining in a flexible vinyl compound processed from
as a hard particle of resin which will not fuse when the plastic
general-purpose poly(vinyl chloride) (PVC) resins under a
mass is subjected to set conditions of hot processing. The
prescribed set of working conditions. number of unfused particles present is related to the conditions
used.The presence of an excess of such particles is detrimental
1.2 The values stated in SI units are to be regarded as the
to many applications.
standard. The values in parentheses are for information only.
1.3 This standard does not purport to address all of the
6. Apparatus
safety problems, if any, associated with its use. It is the
6.1 Laboratory Mixer, with stainless steel mixing bowl.
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica-
6.2 Two-Roll Mill, 152.4 by 304.8 mm (6 by 12 in.), 263.5
bility of regulatory limitations prior to use.
mm (10.5 in.) between guides, differential speed ratio 1.40 6
0.04, fast roll speed 34 6 2 rpm, with an adjustable tempera-
NOTE 1—There is no known ISO equivalent to this standard.
ture range of 120–205°C (250–400°F).
2. Referenced Documents
NOTE 2—If the mill available does not meet these criteria, the
2
2.1 ASTM Standards:
specifications of the mill used should be included in the report.
D883 Terminology Relating to Plastics
6.3 Surface Pyrometer
D1600 Terminology forAbbreviatedTerms Relating to Plas-
tics 6.4 Balance, 0.1-g sensitivity.
6.5 Hydraulic Press having platens at least 203 by 203 mm
3. Terminology
(8 by 8 in.), rated at a minimum of 140 MPa (20 000 psi) ram
3.1 General—Definitions are in accordance with Terminol-
pressure on a 100-mm (4-in.) ram, which may be heated to 163
ogy D883 and abbreviations with Terminology D1600, unless
6 3°C (325 6 5°F) on the pressing surfaces and equipped with
otherwise indicated.
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/zinc
6.7 Cotton Gloves.
stabilizer, stearic acid, carbon black, and a plasticizer in a
6.8 Mill Knife.
laboratory mixer. The dry blend is milled on a two-roll
laboratory mill.
6.9 Plates or Mold, two 203 by 203-mm (8 by 8-in.)
chrome-platedferroplates,orachrome-platedmoldwitha152
4.2 The milled sheet is press-polished and the gels counted
by 152 by 6.4-mm (6 by 6 by 0.25-in.) cavity.
using a bottom-lighted viewing box and a magnifying com-
parator.
6.10 Backing Plates, two 203 by 203 by 6.4 mm (8 by 8 by
0.250 in.).
1
This practice is under the jurisdiction ofASTM Committee D20 on Plastics and
6.11 BrassShims, four, 0.51 by 13 by 203 mm (0.020 by 0.5
is the direct responsibility of Subcommittee D20.15 on Thermoplastic Materials.
by 8.0 in.).
Current edition approved Feb. 1, 2009. Published February 2009. Originally
approved in 1977. Last previous edition approved in 2001 as D3596 – 92(2001).
6.12 Magnifying Comparator, equipped with a transparent
DOI: 10.1520/D3596-09.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or reticule (scale) showing circles from 0.03 to 1.27 mm (0.001 to
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
0.050 in.) in diameter.
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. 6.13 Bottom-Lighted Viewing Box.
*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
1

---------------------- Page: 1 ----------------------
D3596 − 09
7. Materials 8.3.1 Placethesectioncutfromthemilledsheetbetweenthe
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 Plasticizer
backing plates and insert in a press at 163 6 3°C (325 6 5°F).
7.2.1 Plasticizer Type—The plasticizer selected shall repre-
Preheat for 0.5 min with the press closed at zero pressure. A
sent the plasticizer type commonly used with the resin being
chrome-plated mold can be used instead of the plates.
tested. Less solvating plasticizer
...

This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
Designation:D3596–92 (Reapproved 2001) Designation: D 3596 – 09
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 (´) indicates an editorial change since the last revision or reapproval.
1. 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.
NOTE1—There are no ISO standards covering the primary subject of this practice. 1—There is no known ISO equivalent to this standard.
2. Referenced Documents
2
2.1 ASTM Standards:
D 883 Terminology Relating to Plastics
2
D1249Specification for Octyl Ortho-Phthalate Ester Plasticizers Terminology Relating to Plastics
D 1600 Terminology for Abbreviated Terms Relating to Plastics
3. Terminology
3.1 General—Definitions are in accordance with Terminology D 883 and abbreviations with Terminology D 1600, unless
otherwise indicated.
4. Summary of Practice
4.1Asample of PVC resin is mixed with calcium stearate and di-2-ethylhexyl phthalate plasticizer (DOP) in a laboratory mixer.
After mixing, the dry blend is milled on a two-roll laboratory mill; carbon black dispersion is added during the milling.
4.1 A sample of PVC resin is mixed with calcium/zinc stabilizer, stearic acid, carbon black, and a plasticizer in a laboratory
mixer. The dry blend is milled on a two-roll laboratory mill.
4.2 The milled sheet is press-polished and the gels counted using a bottom-lighted viewing box and a magnifying comparator.
5. Significance and Use
5.1 The gel (fisheye) in PVC resins is generally recognized as a hard particle of resin which will not fuse when the plastic mass
is subjected to set conditions of hot processing. The number of unfused particles present is related to the conditions used. The
presence of an excess of such particles is detrimental to many applications.
6. Apparatus
6.1 Laboratory Mixer, with stainless steel mixing bowl.
6.2 Two-Roll Mill, 152.4 by 304.8 mm (6 by 12 in.), 263.55263.5 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 roll with an adjustable temperature range of 154 6 3°C (310 6
5°F). 120–205°C (250–400°F).
NOTE 2—If the mill available does not meet these criteria, the specifications of the mill used should be included in the report.
1
This practice is under the jurisdiction of ASTM Committee D20 on Plastics and is the direct responsibility of Subcommittee D20.15 on Thermoplastic Materials .
Current edition approved October 15, 1992. Published December 1992. Originally published as D3596–77. Last previous edition D3596–88.
Current edition approved Feb. 1, 2009. Published February 2009. Originally approved in 1977. Last previous edition approved in 2001 as D 3596 – 92(2001).
2
For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at service@astm.org. For AnnualBookofASTM Standards
, Vol 08.01.volume information, refer to the standard’s Document Summary page on the ASTM website.
*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.
1

---------------------- Page: 1 ----------------------
D3596–09
6.3 Surface Pyrometercalibrated in the range of 154°C (310°F) and a leaf pyrometer calibrated in the range of 163°C (325°F).
6.4 Balance, 0.1-g sensitivity.
6.5 Hydraulic Press having platens at least 203 by 203 mm (8 by 8 in.), rated at a minimum of 140 MPa (20 000 psi) ram
pressure on a 100-mm (4-in.) ram, which may be heated to 163 6 3°C (325 6 5°F) on the pressing surfaces and equipped with
cooling water.
6.6 Timer, capable of being read in seconds.
6.7 Cotton Gloves.
6.8 Mill Knife.
...

This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
Designation:D3596–92 (Reapproved 2001) Designation: D 3596 – 09
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 (´) indicates an editorial change since the last revision or reapproval.
1. 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.
NOTE1—There are no ISO standards covering the primary subject of this practice. 1—There is no known ISO equivalent to this standard.
2. Referenced Documents
2
2.1 ASTM Standards:
D 883 Terminology Relating to Plastics
2
D1249Specification for Octyl Ortho-Phthalate Ester Plasticizers Terminology Relating to Plastics
D 1600 Terminology for Abbreviated Terms Relating to Plastics
3. Terminology
3.1 General—Definitions are in accordance with Terminology D 883 and abbreviations with Terminology D 1600, unless
otherwise indicated.
4. Summary of Practice
4.1Asample of PVC resin is mixed with calcium stearate and di-2-ethylhexyl phthalate plasticizer (DOP) in a laboratory mixer.
After mixing, the dry blend is milled on a two-roll laboratory mill; carbon black dispersion is added during the milling.
4.1 A sample of PVC resin is mixed with calcium/zinc stabilizer, stearic acid, carbon black, and a plasticizer in a laboratory
mixer. The dry blend is milled on a two-roll laboratory mill.
4.2 The milled sheet is press-polished and the gels counted using a bottom-lighted viewing box and a magnifying comparator.
5. Significance and Use
5.1 The gel (fisheye) in PVC resins is generally recognized as a hard particle of resin which will not fuse when the plastic mass
is subjected to set conditions of hot processing. The number of unfused particles present is related to the conditions used. The
presence of an excess of such particles is detrimental to many applications.
6. Apparatus
6.1 Laboratory Mixer, with stainless steel mixing bowl.
6.2 Two-Roll Mill, 152.4 by 304.8 mm (6 by 12 in.), 263.55263.5 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 roll with an adjustable temperature range of 154 6 3°C (310 6
5°F). 120–205°C (250–400°F).
NOTE 2—If the mill available does not meet these criteria, the specifications of the mill used should be included in the report.
1
This practice is under the jurisdiction of ASTM Committee D20 on Plastics and is the direct responsibility of Subcommittee D20.15 on Thermoplastic Materials.
Current edition approved October 15, 1992. Published December 1992. Originally published as D3596–77. Last previous edition D3596–88.
Current edition approved Feb. 1, 2009. Published February 2009. Originally approved in 1977. Last previous edition approved in 2001 as D 3596 – 92(2001).
2
For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at service@astm.org. For AnnualBookofASTM Standards
, Vol 08.01.volume information, refer to the standard’s Document Summary page on the ASTM website.
*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.
1

---------------------- Page: 1 ----------------------
D3596–09
6.3 Surface Pyrometercalibrated in the range of 154°C (310°F) and a leaf pyrometer calibrated in the range of 163°C (325°F).
6.4 Balance, 0.1-g sensitivity.
6.5 Hydraulic Press having platens at least 203 by 203 mm (8 by 8 in.), rated at a minimum of 140 MPa (20 000 psi) ram
pressure on a 100-mm (4-in.) ram, which may be heated to 163 6 3°C (325 6 5°F) on the pressing surfaces and equipped with
cooling water.
6.6 Timer, capable of being read in seconds.
6.7 Cotton Gloves.
6.8 Mill Knife.
6
...

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