ASTM D3716-14(2020)
(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
3.1 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.
3.2 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
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 concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use.
1.3 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
General Information
Relations
Standards Content (Sample)
This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
Designation: D3716 − 14 (Reapproved 2020)
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 E100Specification for ASTM Hydrometers
1.1 These test methods cover test procedures for emulsion
3. Significance and Use
polymers that are used in water-based floor polishes. The term
“emulsion polymers” is used primarily to denote those mate-
3.1 The purpose of this test is not to fully identify and
rials produced by regular emulsion polymerization techniques,
characterize a polymer, but to identify a variety of basic
but may be extended to those polymers that are subsequently
parameters needed to predetermine the usefulness of the
emulsified or dispersed after polymerization. Unless otherwise
polymer in formulations as well as for Quality Control pur-
noted, the tests may be used for any polymer or copolymer
poses.
systems. The methods appear in the following order:
3.2 Astatementofprecisionandaccuracyisnotappropriate
Section
in this case.
Sampling 4
Total Solids 5
4. Sampling
pH Value 6
Apparent Viscosity 7
4.1 Outline of Test Method—Since stratification may occur
Sediment 8
in emulsion polymers, they must be thoroughly agitated to
Storage Stability 9
obtain a homogeneous blend as a representative sample. The
Freeze-thaw Stability 10
Specific Gravity 11
procedure required differs with the type of container and
1.2 This standard does not purport to address all of the facilities available.
safety concerns, if any, associated with its use. It is the
4.2 Sampling from Tank Cars—Take three samples of at
responsibility of the user of this standard to establish appro-
least 1 pt (473 mL) each, one at the center of the tank, another
priate safety, health, and environmental practices and deter-
half way between the center and the bottom, and the third half
mine the applicability of regulatory limitations prior to use.
way between the center and the top. Take the top sample first,
1.3 This international standard was developed in accor-
then the center sample, and the bottom sample last. Use a
dance with internationally recognized principles on standard-
weighted sampler with a remotely operated, removable top, or
ization established in the Decision on Principles for the
other suitable sampling device that will accomplish the same
Development of International Standards, Guides and Recom-
results. Determine the applicable specified or characteristic
mendations issued by the World Trade Organization Technical
properties of the samples by the standard procedures or
Barriers to Trade (TBT) Committee.
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
contains 2% air space, lay it on its side and roll to and fro
These test methods are under the jurisdiction of ASTM Committee D21 on briskly for not less than 10 min. Then turn the drum upside
PolishesandarethedirectresponsibilityofSubcommitteeD21.03onChemicaland
down for about 15 min and repeat the rolling operation for an
Physical Testing.
additional10min.Ifthedrumcontainslessthan2%airspace,
Current edition approved Oct. 1, 2020. Published October 2020. Originally
transfer the contents to a larger vessel and thoroughly stir,
approved in 1978. Last previous edition approved in 2014 as D3716–14. DOI:
10.1520/D3716-14R20.
preferablybymeansofaperforatedsteeldiskplunger.Stirring
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
for about 10 min will normally suffice.
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
4.3.1.2 Method B—Agitate the contents of the drum by
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. means of a suitable motor-driven stirrer for as long as is
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D3716 − 14 (2020)
necessary to obtain uniformity. Excessive stirring and unnec- 6.3 Procedure—Before making a determination, take care
essary exposure of the emulsion polymer to air must be 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—Report the pH value for the polymer emulsion.
quarter the height of the emulsion polymer from the bottom of
the drum. Operate stirrer at a minimum speed of 900 r/min. 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, Rotational—The essential instrumentation
4.3.2 Removal of Sample—After blending, take the sample
required providing the minimum rotational viscometer analyti-
withoutdelay.Asuitablemethodisbyslowlyinsertingaclean,
cal capabilities for this test method include:
dry, glass tube of not more than 15-mm internal diameter and
7.1.3.1 Drive Motor, to apply a unidirectional rotational
open at both ends, until it reaches the bottom of the container.
displacement to the specimen of 0.5 revolutions per minute
Then close the upper end of the tube and transfer the contents
(r/min) to 60 r/min constant to within 61%.
to a clean, dry sample bottle. Repeat the operation until
7.1.3.2 Force Sensor, to measure the torque developed by
sufficient emulsion polymer has been obtained.
the specimen to within 61 % full scale.
4.3.3 Bulk Sample—Where samples are drawn from several
7.1.3.3 Coupling Shaft, or other means to transmit the
containers,forexample10%samplingofemulsionpolymerin
rotational displacement from the motor to the specimen.
drums, or where samples are taken at different depths, for
7.1.3.4 Geometry, Spindle, Tool or Rotational Element, to
example from tanks, combine the samples and thoroughly
fix the specimen between the drive shaft and a stationary
blendbystirringorshakingimmediatelybeforetakingthefinal
position.
average sample.
NOTE 1—Each geometry typically covers a range of 1.5 decades of
5. Total Solids
viscosity. The geometry is selected so that the measured viscosity is
between 10 and 90 % of the range of the geometry.
5.1 Apparatus—Tared aluminum dishes with a close-fitting
7.1.3.5 Guard, to protect the geometry from mechanical
cover,havingadiameterofapproximately60mmandaheight
damage.
of 15 mm.
7.1.3.6 Temperature Sensor, to provide an indication of the
5.2 Procedure—If the temperature of the emulsion polymer
specimentemperatureoverthetemperaturerangefrom15°Cto
is above room temperature, allow it to cool to room tempera-
30°C measurable to within 60.1°C.
ture.Thenweightwosamplesofapproximately1geachtothe
7.1.3.7 Data Collection Device, to provide a means of
nearest 1.0 mg in tared aluminum weighing dishes. Dry the
acquiring, storing, and displaying measured or calculated
samples for2hina convection or forced-draft oven at a
signals, or both. The minimum output signals required for
temperatureof105+2,−0.5°C.Removethesamplesfromthe
rotationalviscometryaretorque,rotationalspeed,temperature,
oven, cool the container and contents to room temperature in a
and time.
desiccator, and weigh them to the nearest 0.1 mg.Average the
7.1.3.8 Stand, to support, level and adjust the height of the
values if they are within 0.1%. If not, make additional
drive motor, shaft and geometry.
duplicate determinations until a pair of duplicate determina-
7.1.3.9 Specimen Container, with a capacity of 600 mL to
tions agree within 0.1%.
contain the test specimen during testing.
5.3 Calculation—Calculate the percent of total solids as
NOTE 2—A 600-mL labortory beaker has been found suitable for this
follows:
service.
weightofdrysolids
7.1.3.10 Auxiliary instrumentation considered necessary or
Totalsolids, % 5 3100 (1)
weightofsample
useful in conducting this test method includes:
5.4 Report—Specify whether the oven used is a convection
(1) Data analysis capability to provide viscosity, stress,
or a forced-draft type.
shear rate or other useful parameters derived from measured
signals.
6. pH Value
(2) Level to indicate the vertical plumb of the drive motor,
6.1 Apparatus—Any pH electrometer and a glass shaft and geometry.
electrode—calomel cell assembly may be used as described in
7.2 Preparation of Sample—Adjust to the desired solids
Test Method E70.Aflowing calomel electrode has been found
content with distilled water. Bring the pH to the desired point
particularly suited for the pH range of the latex being tested.
with ammonia. Take a sufficient volume of sample so that at
6.2 Standard Solution, having a pH of 10, or a standard least 500 mL of diluted emulsion polymer will be obtained.
solution having a pH approximately the same as that of the Strain the diluted emulsion polymer through the No. 40
emulsion polymer to be tested. (425-µm) sieve.After straining, again gently stir the emulsion
D3716 − 14 (2020)
polymer for approximately 20 s. If the emulsion polymer 8.3.2 Place the sample tube in the centrifuge and place a
contains excessive amounts of occluded air, remove the air in tube filled with 100 mL of water on the opposite side for
thefollowingmannerbeforeproceedingwiththedetermination instrument balance.
of viscosity: Into a three-necked distillation flask equipped 8.3.3 Spin for 30 min at 1750 r/min.
withastirrerandvacuumconnections,pourasufficientvolume 8.3.4 Alternative Method—Dilute the polymer emulsion
of diluted emulsion polymer so that at least 500 mL of 50/50 with water; then centrifuge for 30 min.
emulsionpolymerwillremainafterremovaloftheair.Startthe
8.4 Calculations:
agitatorandevacuatetheflasktoavacuumof26to28mmHg
8.4.1 Undiluted Samples—Read the sediment level in the
(3.5to3.7kPa),oruntilthefoamrisestotheneckoftheflask.
tube stem and express directly as percent sediment content.
Break the vacuum. Evacuate several times in this manner to
8.4.2 Diluted Samples—Read the sediment level in the tube
ensure removal of the occluded air. When required, the same
stem and multiply by the dilution factor (50/50=2,25⁄75=4,
methodmaybeusedonemulsionpolymerasreceived,without
etc.); express the result as percent sediment content.
laboratory removal of occluded air.
7.3 Procedure: 9. Storage Stability
7.3.1 Ensure that the strained emulsion polymer is at a
9.1 Scope:
temperature at 25 6 2°C.
9.1.1 This test method is intended to indicate storage
7.3.2 Pour the emulsion polymer into the container.
stability of emulsion polymers.
7.3.3 Inserttheguardedgeometryoftheviscometerintothe
9.1.2 Storage for 30 days at 125°F (52°C), while not a
emulsion polymer until the surface of the emulsion polymer is
guarantee of one year’s stability at room temperature, is
within the measurement indicator on the shaft.
believedtobeamorereliableindicatorofstoragestabilitythan
7.3.4 Initiate the rotation of the geometry at the lowest
similar tests of shorter duration.
speed available for 1 min.
9.2 Apparatus:
7.3.5 Increase the geometry speed to that required to pro-
9.2.1 Glass Bottles, 120-mL, round, narrow-mouth, ap-
duce a reading nearest the midpoint of the scale.
proximately 120 mm high and 45 mm in diameter with
7.3.6 Stop the rotation of the geometry and wait for 1 min.
polyethylene-lined screw caps.
7.3.7 Restart the rotational of the geometry and allow at
9.2.2 Oven, capable of maintaining the temperature of the
least 5 revolutions of the geometry.
emulsion samples at 125 6 2°F (52°C).
NOTE 3—For routine measurement of quality control samples where a
9.3 Samples:
specific viscosity range is to be expected and rotational geometry and
speed settings are pre-defined through method validation, steps 7.3.4
9.3.1 The sample shall be thoroughly representative of the
through 7.3.6 can be skipped.
material in question and the portion used for the test shall be
7.3.8 Measure and report the observed viscosity, the rota- thoroughly representative of the sample itself.
tional speed and the geometry type used. 9.3.2 Test samples shall be prepared in duplicate for each
7.3.9 Stop the rotation of the geometry. Elevate the geom- material in question.
etry out of the test specimen. Clean the geometry with a
9.4 Procedure:
suitable solvent. Safely dispose of the test specimen.
9.4.1 Transfer 100 mL of polymer emulsion to a clean, dry
test bottle and hand tighten the screw cap.
8. Sediment
9.4.2 Place the test set or series inverted in a drying oven
8.1 Scope—Thistestmethodcoversthedeterminationofthe
capableofmaintainingthetemperatureoftheemulsionsat125
percent sediment content of emulsion polymers.
6 2°F (52°C).
9.4.3 Observe the samples daily for the first 14 days and
8.2 Apparatus and Material:
twiceweekly(thatis,MondayandThursday)fortheremainder
8.2.1 International Oil Testing Centrifuge, Model DE.
of the 30-day storage period. Samples should be examined as
8.2.2 Centrifuge Tubes (Graduated)—Goetz Pear-Shaped,
3,4
rapidlyaspossiblewithaminimumofagitationandreturnedto
100-mLcapacity,largestem, orGoetzPhosphorusTubewith
4,5
the oven. Do not loosen cap.
a stopper, 100-mL capacity, small stem.
9.4.4 At the time of each observation, record the following
8.2.3 Bromophenol Blue Indicator Solution (0.1 %).
on a suitable data sheet:
8.3 Procedure:
9.4.4.1 Date,
8.3.1 Fill a Goetz Phosphorus Tube (small stem) with 100
9.4.4.2 Number of days in test, and
mL of polymer emulsion inverting the
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