ASTM D3716-99(2006)
(Test Method)Standard Test Methods for Use of Emulsion Polymers in Floor Polishes
Standard Test Methods for Use of Emulsion Polymers in Floor Polishes
SIGNIFICANCE AND USE
The purpose of this test is not to fully identify and characterize a polymer, but to identify a variety of basic parameters needed to predetermine the usefulness of the polymer in formulations as well as for Quality Control purposes.
A statement of precision and accuracy is not appropriate in this case.
SCOPE
1.1 These test methods cover test procedures for emulsion polymers that are used in water-based floor polishes. The term "emulsion polymers" is used primarily to denote those materials produced by regular emulsion polymerization techniques, but may be extended to those polymers that are subsequently emulsified or dispersed after polymerization. Unless otherwise noted, the tests may be used for any polymer or copolymer systems. The methods appear in the following order:SectionSamplingTotal SolidspH ValueApparent ViscositySedimentStorage StabilityFreeze-thaw StabilitySpecific Gravity
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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Designation:D3716–99(Reapproved2006)
Standard Test Methods for
Use of Emulsion Polymers in Floor Polishes
This standard is issued under the fixed designation D3716; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (e) indicates an editorial change since the last revision or reapproval.
1. Scope 3. Significance and Use
1.1 These test methods cover test procedures for emulsion 3.1 The purpose of this test is not to fully identify and
polymers that are used in water-based floor polishes. The term characterize a polymer, but to identify a variety of basic
“emulsion polymers” is used primarily to denote those mate- parameters needed to predetermine the usefulness of the
rials produced by regular emulsion polymerization techniques, polymer in formulations as well as for Quality Control pur-
but may be extended to those polymers that are subsequently poses.
emulsified or dispersed after polymerization. Unless otherwise 3.2 Astatementofprecisionandaccuracyisnotappropriate
noted, the tests may be used for any polymer or copolymer in this case.
systems. The methods appear in the following order:
4. Sampling
Section
4.1 Outline of Test Method—Since stratification may occur
Sampling 4
in emulsion polymers, they must be thoroughly agitated to
Total Solids 5
obtain a homogeneous blend as a representative sample. The
pH Value 6
Apparent Viscosity 7
procedure required differs with the type of container and
Sediment 8
facilities available.
Storage Stability 9
4.2 Sampling from Tank Cars—Take three samples of at
Freeze-thaw Stability 10
Specific Gravity 11
least 1 pt (473 mL) each, one at the center of the tank, another
half way between the center and the bottom, and the third half
1.2 This standard does not purport to address all of the
way between the center and the top. Take the top sample first,
safety concerns, if any, associated with its use. It is the
then the center sample, and the bottom sample last. Use a
responsibility of the user of this standard to establish appro-
weighted sampler with a remotely operated, removable top, or
priate safety and health practices and determine the applica-
other suitable sampling device that will accomplish the same
bility of regulatory limitations prior to use.
results. Determine the applicable specified or characteristic
2. Referenced Documents
properties of the samples by the standard procedures or
methods. If there is any evidence that stratification has oc-
2.1 ASTM Standards:
curred, then thoroughly agitate the contents of the car until
E1 Specification forASTM Liquid-in-GlassThermometers
samples obtained agree within 1% of total solids.
E70 Test Method for pH of Aqueous Solutions With the
4.3 Sampling from Drums:
Glass Electrode
4.3.1 Blending of Contents—Blend the emulsion polymer
E100 Specification for ASTM Hydrometers
by one of the following methods:
4.3.1.1 Method A—If the drum is fitted with a bung and
These test methods are under the jurisdiction of ASTM Committee D21 on
contains 2% air space, lay it on its side and roll to and fro
Polishes, and are the direct responsibility of Subcommittee D21.03 on Chemical
briskly for not less than 10 min. Then turn the drum upside
and Physical Testing.
down for about 15 min and repeat the rolling operation for an
Current edition approved June 1, 2006. Published June 2006. Originally
approved in 1978. Last previous edition approved in 1999 as D3716–99. additional10min.Ifthedrumcontainslessthan2%airspace,
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
transfer the contents to a larger vessel and thoroughly stir,
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
preferablybymeansofaperforatedsteeldiskplunger.Stirring
Standards volume information, refer to the standard’s Document Summary page on
for about 10 min will normally suffice.
the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D3716–99 (2006)
4.3.1.2 Method B—Agitate the contents of the drum by 6.2 Standard Solution, having a pH of 10, or a standard
means of a suitable motor-driven stirrer for as long as is solution having a pH approximately the same as that of the
emulsion polymer to be tested.
necessary to obtain uniformity. Excessive stirring and unnec-
essary exposure of the emulsion polymer to air must be 6.3 Procedure—Before making a determination, take care
that the instrument is properly standardized at frequent inter-
avoided. A suitable type of stirrer consists of a collapsible
vals with a standard solution (see 6.2) and that the electrodes
two-bladed stainless steel propeller of 110-mm minimum
areclean.Permitthepolymeremulsiontocometoequilibrium
diameter,whenfullyopened,mountedonastainlesssteelshaft
with the glass electrode before taking the final reading.
sufficiently long for the propeller to be distant about one
6.4 Report—ReportthepHvalueforthepolymeremulsion.
quarter the height of the emulsion polymer from the bottom of
the drum. Operate stirrer at a minimum speed of 900 rpm. If
7. Apparent Viscosity
desired, two propellers may be used on the same shaft, the
7.1 Apparatus:
loweronebeingneartheendoftheshaft.Theshaftspeedshall
7.1.1 Sieve, U.S. No. 40 (425-µm).
give a brisk turnover without creating a vortex.The part of the
7.1.2 Distillation Flask, Three-Necked, equipped with stir-
equipment immersed in the emulsion polymer must contain no
ring and vacuum connections.
copper or brass.
7.1.3 Viscometer, Brookfield RV or LV Type.
4.3.2 Removal of Sample—After blending, take the sample
7.2 Preparation of Sample—Adjust to the desired solids
withoutdelay.Asuitablemethodisbyslowlyinsertingaclean,
content with distilled water. Bring the pH to the desired point
dry, glass tube of not more than 15-mm internal diameter and
with ammonia. Take a sufficient volume of sample so that at
open at both ends, until it reaches the bottom of the container.
least 500 mL of diluted emulsion polymer will be obtained.
Then close the upper end of the tube and transfer the contents
Strain the diluted emulsion polymer through the No. 40
to a clean, dry sample bottle. Repeat the operation until
(425-µm) sieve.After straining, again gently stir the emulsion
sufficient emulsion polymer has been obtained.
polymer for approximately 20 s. If the emulsion polymer
4.3.3 Bulk Sample—Where samples are drawn from several
contains excessive amounts of occluded air, remove the air in
containers,forexample10%samplingofemulsionpolymerin
thefollowingmannerbeforeproceedingwiththedetermination
drums, or where samples are taken at different depths, for
of viscosity: Into a three-necked distillation flask equipped
example from tanks, combine the samples and thoroughly
withastirrerandvacuumconnections,pourasufficientvolume
blendbystirringorshakingimmediatelybeforetakingthefinal
of diluted emulsion polymer so that at least 500 mL of
average sample.
emulsionpolymerwillremainafterremovaloftheair.Startthe
agitatorandevacuatetheflasktoavacuumof26to28mmHg
5. Total Solids
(3.5to3.7kPa),oruntilthefoamrisestotheneckoftheflask.
Break the vacuum. Evacuate several times in this manner to
5.1 Apparatus—Tared aluminum dishes with a close-fitting
ensure removal of the occluded air. When required, the same
cover,havingadiameterofapproximately60mmandaheight
methodmaybeusedonemulsionpolymerasreceived,without
of 15 mm.
laboratory removal of occluded air.
5.2 Procedure—If the temperature of the emulsion polymer
7.3 Procedure—With the strained emulsion polymer at a
is above room temperature, allow it to cool to room tempera-
temperature at 25 6 2°C, pour the emulsion polymer into a
ture.Thenweightwosamplesofapproximately1geachtothe
600-mL beaker. Insert the shielded spindle of the viscometer
nearest 1.0 mg in tared aluminum weighing dishes. Dry the
into the emulsion polymer until the surface of the emulsion
samples for2hina convection or forced-draft oven at a
polymer is within the notch in the shaft of the spindle. Use a
temperatureof105+2,−0.5°C.Removethesamplesfromthe
spindle and speed that will give medium scale reading.
oven, cool the container and contents to room temperature in a
desiccator, and weigh them to the nearest 0.1 mg.Average the
8. Sediment
values if they are within 0.1%. If not, make additional
8.1 Scope—This test method covers the determination of
duplicate determinations until a pair of duplicate determina-
the percent sediment content of emulsion polymers.
tions agree within 0.1%.
8.2 Apparatus and Material:
5.3 Calculation—Calculate the percent of total solids as
8.2.1 International Oil Testing Centrifuge, Model DE.
follows:
8.2.2 Centrifuge Tubes (Graduated)—Goetz Pear-Shaped,
,
weightofdrysolids
100-mLcapacity,largestem, orGoetzPhosphorusTubewith
Totalsolids,% 5 3100 (1)
4,5
weightofsample
a stopper, 100-mL capacity, small stem.
8.2.3 Bromophenol Blue Indicator Solution (0.1 %).
5.4 Report—Specify whether the oven used is a convection
or a forced-draft type.
The sole source of supply of Fisher catalog no. 5-622 known to the committee
6. pH Value
at this time is Fisher Scientific Co., Pittsburgh, PA.
If you are aware of alternative suppliers, please provide this information to
6.1 Apparatus—Any pH electrometer and a glass
ASTMHeadquarters.Yourcommentswillreceivecarefulconsiderationatameeting
electrode—calomel cell assembly may be used as described in
of the responsible technical committee, which you may attend.
TestMethodE70.Aflowingcalomelelectrodehasbeenfound
The sole source of supply of Fisher catalog no. 5-624 known to the committee
particularly suited for the pH range of the latex being tested. at this time is Fisher Scientific Co., Pittsburgh, PA.
D3716–99 (2006)
8.3 Procedure:
V = viscous
8.3.1 Fill a Goetz Phosphorus Tube (small stem) with 100
Cr = creamed
mL of polymer emulsion inverting the tube to fill the stem
G = gelled
completely. Sep = other types of liquid phase separation
Sediment = sedimentation of solid matter
8.3.2 Place the sample tube in the centrifuge and place a
tube filled with 100 mL of water on the opposite side for
10. Freeze-thaw Stability
instrument balance.
8.3.3 Spin for 30 min at 1750 rpm.
10.1 Scope:
8.3.4 Alternative Method—Dilute the polymer emulsion
10.1.1 This test method is intended to indicate the freeze-
50/50 with water; then centrifuge for 30 min.
thaw stabili
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