ASTM D3596-13
(Practice)Standard Practice for Determination of Gels (Fisheyes) In General-Purpose Poly(Vinyl Chloride) (PVC) Resins
Standard Practice for Determination of Gels (Fisheyes) In General-Purpose Poly(Vinyl Chloride) (PVC) Resins
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.
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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Designation: D3596 − 13
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 has the capacity for
ogy D883 and abbreviations with Terminology D1600, unless
heating to 163 6 3°C (325 6 5°F) on the pressing surfaces and
otherwise indicated.
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/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 Nov. 1, 2013. Published November 2013. Originally
approved in 1977. Last previous edition approved in 2009 as D3596 – 09. DOI:
6.12 Magnifying Comparator (optional), equipped with a
10.1520/D3596-13.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or transparent reticule (scale) showing circles from 0.03 to 1.27
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
mm (0.001 to 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 − 13
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 s
...
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 − 09 D3596 − 13
Standard Practice 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*
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.
2. Referenced Documents
2
2.1 ASTM Standards:
D883 Terminology Relating to Plastics
D1600 Terminology for Abbreviated Terms Relating to Plastics
3. Terminology
3.1 General—Definitions are in accordance with Terminology D883 and abbreviations with Terminology D1600, unless
otherwise indicated.
4. Summary of Practice
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.), 263.5 mm (10.5 in.) between guides, differential speed ratio 1.40 6 0.04,
fast roll speed 34 6 2 rpm, with an adjustable temperature range of 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.
6.3 Surface Pyrometer
6.4 Balance, 0.1-g sensitivity.
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 Feb. 1, 2009Nov. 1, 2013. Published February 2009November 2013. Originally approved in 1977. Last previous edition approved in 20012009
as D3596 – 92D3596 – 09.(2001). DOI: 10.1520/D3596-09.10.1520/D3596-13.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Standards
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 − 13
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 has the capacity for heating 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.
6.9 Plates or Mold, two 203 by 203-mm (8 by 8-in.) chrome-plated ferro plates, or a chrome-plated mold with a 152 by 152
by 6.4-mm (6 by 6 by 0.25-in.) cavity.
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.).
6.12 Magnifying Comparator, Comparator (optional), equipped with a transparent reticule (scale) showing circles from 0.03 to
1.27 mm (0.001 to 0.050 in.) in diameter.
6.13 Bottom-Lighted Viewing Box.
7. Materials
7.1 PVC Resin
7.2 Plasticizer
7.2.1 Plasticizer Type—The plasticizer selected shall represent the plasticizer type commonly used with the re
...
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