ASTM D3716-99(2008)
(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:
Section Sampling4 Total Solids5 pH Value6 Apparent Viscosity7 Sediment8 Storage Stability9 Freeze-thaw Stability10 Specific Gravity11
1.2 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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Standards Content (Sample)
NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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Designation: D3716 − 99 (Reapproved2008)
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 (´) indicates an editorial change since the last revision or reapproval.
1. Scope parameters needed to predetermine the usefulness of the
polymer in formulations as well as for Quality Control pur-
1.1 These test methods cover test procedures for emulsion
poses.
polymers that are used in water-based floor polishes. The term
“emulsion polymers” is used primarily to denote those mate- 3.2 Astatementofprecisionandaccuracyisnotappropriate
rials produced by regular emulsion polymerization techniques, in this case.
but may be extended to those polymers that are subsequently
4. Sampling
emulsified or dispersed after polymerization. Unless otherwise
noted, the tests may be used for any polymer or copolymer
4.1 Outline of Test Method—Since stratification may occur
systems. The methods appear in the following order:
in emulsion polymers, they must be thoroughly agitated to
Section
obtain a homogeneous blend as a representative sample. The
procedure required differs with the type of container and
Sampling 4
facilities available.
Total Solids 5
pH Value 6
4.2 Sampling from Tank Cars—Take three samples of at
Apparent Viscosity 7
least 1 pt (473 mL) each, one at the center of the tank, another
Sediment 8
Storage Stability 9
half way between the center and the bottom, and the third half
Freeze-thaw Stability 10
way between the center and the top. Take the top sample first,
Specific Gravity 11
then the center sample, and the bottom sample last. Use a
1.2 This standard does not purport to address all of the
weighted sampler with a remotely operated, removable top, or
safety concerns, if any, associated with its use. It is the
other suitable sampling device that will accomplish the same
responsibility of the user of this standard to establish appro-
results. Determine the applicable specified or characteristic
priate safety and health practices and determine the applica-
properties of the samples by the standard procedures or
bility of regulatory limitations prior to use.
methods. If there is any evidence that stratification has
occurred, then thoroughly agitate the contents of the car until
2. Referenced Documents
samples obtained agree within 1% of total solids.
2.1 ASTM Standards:
4.3 Sampling from Drums:
E1Specification for ASTM Liquid-in-Glass Thermometers
4.3.1 Blending of Contents—Blend the emulsion polymer
E70Test Method for pH of Aqueous Solutions With the
by one of the following methods:
Glass Electrode
4.3.1.1 Method A—If the drum is fitted with a bung and
E100Specification for ASTM Hydrometers
contains 2% air space, lay it on its side and roll to and fro
briskly for not less than 10 min. Then turn the drum upside
3. Significance and Use
down for about 15 min and repeat the rolling operation for an
3.1 The purpose of this test is not to fully identify and
additional10min.Ifthedrumcontainslessthan2%airspace,
characterize a polymer, but to identify a variety of basic
transfer the contents to a larger vessel and thoroughly stir,
preferablybymeansofaperforatedsteeldiskplunger.Stirring
for about 10 min will normally suffice.
These test methods are under the jurisdiction of ASTM Committee D21 on
4.3.1.2 Method B—Agitate the contents of the drum by
PolishesandarethedirectresponsibilityofSubcommitteeD21.03onChemicaland
means of a suitable motor-driven stirrer for as long as is
Physical Testing.
necessary to obtain uniformity. Excessive stirring and unnec-
Current edition approved March 1, 2008. Published April 2008. Originally
essary exposure of the emulsion polymer to air must be
approved in 1978. Last previous edition approved in 2006 as D3716–99(2006).
DOI: 10.1520/D3716-99R08.
avoided. A suitable type of stirrer consists of a collapsible
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
two-bladed stainless steel propeller of 110-mm minimum
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
diameter,whenfullyopened,mountedonastainlesssteelshaft
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. sufficiently long for the propeller to be distant about one
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D3716 − 99 (2008)
quarter the height of the emulsion polymer from the bottom of 6.4 Report—Report the pH value for the polymer emulsion.
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
loweronebeingneartheendoftheshaft.Theshaftspeedshall
7.1 Apparatus:
give a brisk turnover without creating a vortex.The part of the
7.1.1 Sieve, U.S. No. 40 (425-µm).
equipment immersed in the emulsion polymer must contain no
7.1.2 Distillation Flask, Three-Necked, equipped with stir-
copper or brass.
ring and vacuum connections.
4.3.2 Removal of Sample—After blending, take the sample
7.1.3 Viscometer, Brookfield RV or LV Type.
withoutdelay.Asuitablemethodisbyslowlyinsertingaclean,
7.2 Preparation of Sample—Adjust to the desired solids
dry, glass tube of not more than 15-mm internal diameter and
content with distilled water. Bring the pH to the desired point
open at both ends, until it reaches the bottom of the container.
with ammonia. Take a sufficient volume of sample so that at
Then close the upper end of the tube and transfer the contents
least 500 mL of diluted emulsion polymer will be obtained.
to a clean, dry sample bottle. Repeat the operation until
Strain the diluted emulsion polymer through the No. 40
sufficient emulsion polymer has been obtained.
(425-µm) sieve.After straining, again gently stir the emulsion
4.3.3 Bulk Sample—Where samples are drawn from several
polymer for approximately 20 s. If the emulsion polymer
containers,forexample10%samplingofemulsionpolymerin
contains excessive amounts of occluded air, remove the air in
drums, or where samples are taken at different depths, for
thefollowingmannerbeforeproceedingwiththedetermination
example from tanks, combine the samples and thoroughly
of viscosity: Into a three-necked distillation flask equipped
blendbystirringorshakingimmediatelybeforetakingthefinal
withastirrerandvacuumconnections,pourasufficientvolume
average sample.
of diluted emulsion polymer so that at least 500 mL of
emulsionpolymerwillremainafterremovaloftheair.Startthe
5. Total Solids
agitatorandevacuatetheflasktoavacuumof26to28mmHg
5.1 Apparatus—Tared aluminum dishes with a close-fitting
(3.5to3.7kPa),oruntilthefoamrisestotheneckoftheflask.
cover,havingadiameterofapproximately60mmandaheight Break the vacuum. Evacuate several times in this manner to
of 15 mm.
ensure removal of the occluded air. When required, the same
methodmaybeusedonemulsionpolymerasreceived,without
5.2 Procedure—If the temperature of the emulsion polymer
laboratory removal of occluded air.
is above room temperature, allow it to cool to room tempera-
ture.Thenweightwosamplesofapproximately1geachtothe 7.3 Procedure—With the strained emulsion polymer at a
nearest 1.0 mg in tared aluminum weighing dishes. Dry the
temperature at 25 6 2°C, pour the emulsion polymer into a
samples for2hina convection or forced-draft oven at a 600-mL beaker. Insert the shielded spindle of the viscometer
temperatureof105+2,−0.5°C.Removethesamplesfromthe
into the emulsion polymer until the surface of the emulsion
oven, cool the container and contents to room temperature in a polymer is within the notch in the shaft of the spindle. Use a
desiccator, and weigh them to the nearest 0.1 mg.Average the
spindle and speed that will give medium scale reading.
values if they are within 0.1%. If not, make additional
8. Sediment
duplicate determinations until a pair of duplicate determina-
tions agree within 0.1%.
8.1 Scope—Thistestmethodcoversthedeterminationofthe
percent sediment content of emulsion polymers.
5.3 Calculation—Calculate the percent of total solids as
follows:
8.2 Apparatus and Material:
8.2.1 International Oil Testing Centrifuge, Model DE.
weightofdrysolids
Totalsolids, % 5 3100 (1)
8.2.2 Centrifuge Tubes (Graduated)—Goetz Pear-Shaped,
weightofsample
3,4
100-mLcapacity,largestem, orGoetzPhosphorusTubewith
5.4 Report—Specify whether the oven used is a convection
4,5
a stopper, 100-mL capacity, small stem.
or a forced-draft type.
8.2.3 Bromophenol Blue Indicator Solution (0.1 %).
8.3 Procedure:
6. pH Value
8.3.1 Fill a Goetz Phosphorus Tube (small stem) with 100
6.1 Apparatus—Any pH electrometer and a glass
mL of polymer emulsion inverting the tube to fill the stem
electrode—calomel cell assembly may be used as described in
completely.
Test Method E70.Aflowing calomel electrode has been found
8.3.2 Place the sample tube in the centrifuge and place a
particularly suited for the pH range of the latex being tested.
tube filled with 100 mL of water on the opposite side for
6.2 Standard Solution, having a pH of 10, or a standard
instrument balance.
solution having a pH approximately the same as that of the
emulsion polymer to be tested.
The sole source of supply of Fisher catalog no. 5-622 known to the committee
6.3 Procedure—Before making a determination, take care
at this time is Fisher Scientific Co., Pittsburgh, PA.
If you are aware of alternative suppliers, please provide this information to
that the instrument is properly standardized at frequent inter-
ASTMHeadquarters.Yourcommentswillreceivecarefulconsiderationatameeting
vals with a standard solution (see 6.2) and that the electrodes
of the responsible technical committee, which you may attend.
areclean.Permitthepolymeremulsiontocometoequilibrium
The sole source of supply of Fisher catalog no. 5-624 known to the committee
with the glass electrode before taking the final reading. at this time is Fisher Scientific Co., Pittsburgh, PA.
D3716 − 99 (2008)
8.3.3 Spin for 30 min at 1750 rpm. 10.1.1 This test method is intended to indicate the freeze-
8.3.4 Alternative Method—Dilute the polymer emulsion thaw stability of emulsion polymers used for floor polishes.
50/50 with water; then centrifuge for 30 min.
10.1.2 Storage under repeated freeze-thaw conditions is not
necessarily indicative of the freeze-thaw stability of an emul-
8.4 Calculations:
sion polym
...
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