ASTM D3716-99
(Test Method)Standard Test Methods for Use of Emulsion Polymers in Floor Polishes
Standard Test Methods for Use of Emulsion Polymers in Floor Polishes
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 Sampling 4 Total solids 5 pH value 6 Apparent viscosity 7 Sediment 8 Storage stability 9 Freeze-thaw stability 10 Specific gravity 11
1.2 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.
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Designation:D3716–99
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 3.2 Astatementofprecisionandaccuracyisnotappropriate
in this case.
1.1 These test methods cover test procedures for emulsion
polymers that are used in water-based floor polishes. The term
4. Sampling
“emulsion polymers” is used primarily to denote those mate-
4.1 Outline of Test Method—Since stratification may occur
rials produced by regular emulsion polymerization techniques,
in emulsion polymers, they must be thoroughly agitated to
but may be extended to those polymers that are subsequently
obtain a homogeneous blend as a representative sample. The
emulsified or dispersed after polymerization. Unless otherwise
procedure required differs with the type of container and
noted, the tests may be used for any polymer or copolymer
facilities available.
systems. The methods appear in the following order:
4.2 Sampling from Tank Cars—Take three samples of at
Section
least 1 pt (473 mL) each, one at the center of the tank, another
Sampling 4
half way between the center and the bottom, and the third half
Total Solids 5
way between the center and the top. Take the top sample first,
pH Value 6
then the center sample, and the bottom sample last. Use a
Apparent Viscosity 7
Sediment 8
weighted sampler with a remotely operated, removable top, or
Storage Stability 9
other suitable sampling device that will accomplish the same
Freeze-thaw Stability 10
results. Determine the applicable specified or characteristic
Specific Gravity 11
properties of the samples by the standard procedures or
1.2 This standard does not purport to address all of the
methods. If there is any evidence that stratification has oc-
safety concerns, if any, associated with its use. It is the
curred, then thoroughly agitate the contents of the car until
responsibility of the user of this standard to establish appro-
samples obtained agree within 1% of total solids.
priate safety and health practices and determine the applica-
4.3 Sampling from Drums:
bility of regulatory limitations prior to use.
4.3.1 Blending of Contents—Blend the emulsion polymer
by one of the following methods:
2. Referenced Documents
4.3.1.1 Method A—If the drum is fitted with a bung and
2.1 ASTM Standards:
contains 2% air space, lay it on its side and roll to and fro
E1 Specification for ASTM Thermometers
briskly for not less than 10 min. Then turn the drum upside
E70 Test Method for pH of Aqueous Solutions with the
down for about 15 min and repeat the rolling operation for an
Glass Electrode
additional10min.Ifthedrumcontainslessthan2%airspace,
E100 Specification for ASTM Hydrometers
transfer the contents to a larger vessel and thoroughly stir,
preferablybymeansofaperforatedsteeldiskplunger.Stirring
3. Significance and Use
for about 10 min will normally suffice.
3.1 The purpose of this test is not to fully identify and
4.3.1.2 Method B—Agitate the contents of the drum by
characterize a polymer, but to identify a variety of basic
means of a suitable motor-driven stirrer for as long as is
parameters needed to predetermine the usefulness of the
necessary to obtain uniformity. Excessive stirring and unnec-
polymer in formulations as well as for Quality Control pur-
essary exposure of the emulsion polymer to air must be
poses.
avoided. A suitable type of stirrer consists of a collapsible
two-bladed stainless steel propeller of 110-mm minimum
diameter,whenfullyopened,mountedonastainlesssteelshaft
These test methods are under the jurisdiction of ASTM Committee D-21 on
Polishes, and are the direct responsibility of Subcommittee D21.03 on Chemical
sufficiently long for the propeller to be distant about one
and Physical Testing.
quarter the height of the emulsion polymer from the bottom of
Current edition approved Sept. 10, 1999. Published November 1999. Originally
e1
the drum. Operate stirrer at a minimum speed of 900 rpm. If
published as D3716–78. Last previous edition D3716–83(1993) .
Annual Book of ASTM Standards, Vol 14.03. desired, two propellers may be used on the same shaft, the
Annual Book of ASTM Standards, Vol 15.05.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D3716
loweronebeingneartheendoftheshaft.Theshaftspeedshall 7.1.2 Distillation Flask, Three-Necked, equipped with stir-
give a brisk turnover without creating a vortex.The part of the ring and vacuum connections.
equipment immersed in the emulsion polymer must contain no 7.1.3 Viscometer, Brookfield RV or LV Type.
copper or brass. 7.2 Preparation of Sample—Adjust to the desired solids
4.3.2 Removal of Sample—After blending, take the sample content with distilled water. Bring the pH to the desired point
withoutdelay.Asuitablemethodisbyslowlyinsertingaclean, with ammonia. Take a sufficient volume of sample so that at
dry, glass tube of not more than 15-mm internal diameter and least 500 mL of diluted emulsion polymer will be obtained.
open at both ends, until it reaches the bottom of the container. Strain the diluted emulsion polymer through the No. 40
Then close the upper end of the tube and transfer the contents (425-µm) sieve.After straining, again gently stir the emulsion
to a clean, dry sample bottle. Repeat the operation until polymer for approximately 20 s. If the emulsion polymer
sufficient emulsion polymer has been obtained. contains excessive amounts of occluded air, remove the air in
4.3.3 Bulk Sample—Where samples are drawn from several thefollowingmannerbeforeproceedingwiththedetermination
containers,forexample10%samplingofemulsionpolymerin of viscosity: Into a three-necked distillation flask equipped
drums, or where samples are taken at different depths, for withastirrerandvacuumconnections,pourasufficientvolume
example from tanks, combine the samples and thoroughly of diluted emulsion polymer so that at least 500 mL of
blendbystirringorshakingimmediatelybeforetakingthefinal emulsionpolymerwillremainafterremovaloftheair.Startthe
average sample. agitatorandevacuatetheflasktoavacuumof26to28mmHg
(3.5to3.7kPa),oruntilthefoamrisestotheneckoftheflask.
5. Total Solids
Break the vacuum. Evacuate several times in this manner to
ensure removal of the occluded air. When required, the same
5.1 Apparatus—Tared aluminum dishes with a close-fitting
methodmaybeusedonemulsionpolymerasreceived,without
cover,havingadiameterofapproximately60mmandaheight
laboratory removal of occluded air.
of 15 mm.
7.3 Procedure—With the strained emulsion polymer at a
5.2 Procedure—If the temperature of the emulsion polymer
temperature at 25 6 2°C, pour the emulsion polymer into a
is above room temperature, allow it to cool to room tempera-
600-mL beaker. Insert the shielded spindle of the viscometer
ture.Thenweightwosamplesofapproximately1geachtothe
into the emulsion polymer until the surface of the emulsion
nearest 1.0 mg in tared aluminum weighing dishes. Dry the
polymer is within the notch in the shaft of the spindle. Use a
samples for2hina convection or forced-draft oven at a
spindle and speed that will give medium scale reading.
temperatureof105+2,−0.5°C.Removethesamplesfromthe
oven, cool the container and contents to room temperature in a
8. Sediment
desiccator, and weigh them to the nearest 0.1 mg.Average the
8.1 Scope—This test method covers the determination of
values if they are within 0.1%. If not, make additional
duplicate determinations until a pair of duplicate determina- the percent sediment content of emulsion polymers.
8.2 Apparatus and Material:
tions agree within 0.1%.
5.3 Calculation—Calculate the percent of total solids as 8.2.1 International Oil Testing Centrifuge, Model DE.
8.2.2 Centrifuge Tubes (Graduated)—Goetz Pear-Shaped,
follows:
4,5
100-mLcapacity,largestem, orGoetzPhosphorusTubewith
weightofdrysolids
,
Totalsolids,% 5 3100 (1)
a stopper, 100-mL capacity, small stem.
weightofsample
8.2.3 Bromophenol Blue Indicator Solution (0.1 %).
5.4 Report—Specify whether the oven used is a convection
8.3 Procedure:
or a forced-draft type.
8.3.1 Fill a Goetz Phosphorus Tube (small stem) with 100
mL of polymer emulsion inverting the tube to fill the stem
6. pH Value
completely.
6.1 Apparatus—Any pH electrometer and a glass
8.3.2 Place the sample tube in the centrifuge and place a
electrode—calomel cell assembly may be used as described in
tube filled with 100 mL of water on the opposite side for
TestMethodE70.Aflowingcalomelelectrodehasbeenfound
instrument balance.
particularly suited for the pH range of the latex being tested.
8.3.3 Spin for 30 min at 1750 rpm.
6.2 Standard Solution, having a pH of 10, or a standard
8.3.4 Alternative Method—Dilute the polymer emulsion
solution having a pH approximately the same as that of the
50/50 with water; then centrifuge for 30 min.
emulsion polymer to be tested.
8.4 Calculations:
6.3 Procedure—Before making a determination, take care
8.4.1 Undiluted Samples—Read the sediment level in the
that the instrument is properly standardized at frequent inter-
tube stem and express directly as percent sediment content.
vals with a standard solution (see 6.2) and that the electrodes
areclean.Permitthepolymeremulsiontocometoequilibrium
with the glass electrode before taking the final reading.
The sole source of supply of Fisher catalog no. 5-622 known to the committee
6.4 Report—ReportthepHvalueforthepolymeremulsion.
at this time is Fisher Scientific Co., Pittsburgh, PA.
If you are aware of alternative suppliers, please provide this information to
ASTMHeadquarters.Yourcommentswillreceivecarefulconsiderationatameeting
7. Apparent Viscosity
of the responsible technical committee, which you may attend.
7.1 Apparatus:
The sole source of supply of Fisher catalog no. 5-624 known to the committee
7.1.1 Sieve, U.S. No. 40 (425-µm). at this time is Fisher Scientific Co., Pittsburgh, PA.
D3716
8.4.2 Diluted Samples—Read the sediment level in the tube intended to cover both eventualities. Thus, the three-cycle test
stemandmultiplybythedilutionf
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