1、Designation: D3716 99 (Reapproved 2008)D3716 14Standard Test Methods forUse of Emulsion Polymers in Floor Polishes1This standard is issued under the fixed designation D3716; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year
2、of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1. Scope1.1 These test methods cover test procedures for emulsion polymers that are used in water-based floor polishes. The ter
3、m“emulsion polymers” is used primarily to denote those materials produced by regular emulsion polymerization techniques, but maybe extended to those polymers that are subsequently emulsified or dispersed after polymerization. Unless otherwise noted, the testsmay be used for any polymer or copolymer
4、systems. The methods appear in the following order:SectionSampling 4Total Solids 5pH Value 6Apparent Viscosity 7Sediment 8Storage Stability 9Freeze-thaw Stability 10Specific Gravity 111.2 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the
5、 responsibilityof the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatorylimitations prior to use.2. Referenced Documents2.1 ASTM Standards:2E1 Specification for ASTM Liquid-in-Glass ThermometersE70 Test Method for pH of Aqueous So
6、lutions With the Glass ElectrodeE100 Specification for ASTM Hydrometers3. Significance and Use3.1 The purpose of this test is not to fully identify and characterize a polymer, but to identify a variety of basic parametersneeded to predetermine the usefulness of the polymer in formulations as well as
7、 for Quality Control purposes.3.2 A statement of precision and accuracy is not appropriate in this case.4. Sampling4.1 Outline of Test MethodSince stratification may occur in emulsion polymers, they must be thoroughly agitated to obtaina homogeneous blend as a representative sample. The procedure re
8、quired differs with the type of container and facilities available.4.2 Sampling from Tank CarsTake three samples of at least 1 pt (473 mL) each, one at the center of the tank, another halfway between the center and the bottom, and the third half way between the center and the top. Take the top sampl
9、e first, then thecenter sample, and the bottom sample last. Use a weighted sampler with a remotely operated, removable top, or other suitablesampling device that will accomplish the same results. Determine the applicable specified or characteristic properties of thesamples by the standard procedures
10、 or methods. If there is any evidence that stratification has occurred, then thoroughly agitatethe contents of the car until samples obtained agree within 1 % of total solids.1 These test methods are under the jurisdiction of ASTM Committee D21 on Polishes and are the direct responsibility of Subcom
11、mittee D21.03 on Chemical and PhysicalTesting.Current edition approved March 1, 2008Sept. 1, 2014. Published April 2008October 2014. Originally approved in 1978. Last previous edition approved in 20062008 asD3716 99(2006).(2008). DOI: 10.1520/D3716-99R08.10.1520/D3716-14.2 For referencedASTM standar
12、ds, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standardsvolume information, refer to the standards Document Summary page on the ASTM website.This document is not an ASTM standard and is intended only to provide the user of an ASTM
13、 standard an indication of what changes have been made to the previous version. Becauseit 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 versionof the standard as published b
14、y ASTM is to be considered the official document.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States14.3 Sampling from Drums:4.3.1 Blending of ContentsBlend the emulsion polymer by one of the following methods:4.3.1.1 Method AIf the drum
15、is fitted with a bung and contains 2 % air space, lay it on its side and roll to and fro briskly fornot less than 10 min. Then turn the drum upside down for about 15 min and repeat the rolling operation for an additional 10 min.If the drum contains less than 2 % air space, transfer the contents to a
16、 larger vessel and thoroughly stir, preferably by means ofa perforated steel disk plunger. Stirring for about 10 min will normally suffice.4.3.1.2 Method BAgitate the contents of the drum by means of a suitable motor-driven stirrer for as long as is necessary toobtain uniformity. Excessive stirring
17、and unnecessary exposure of the emulsion polymer to air must be avoided. A suitable typeof stirrer consists of a collapsible two-bladed stainless steel propeller of 110-mm minimum diameter, when fully opened, mountedon a stainless steel shaft sufficiently long for the propeller to be distant about o
18、ne quarter the height of the emulsion polymer fromthe bottom of the drum. Operate stirrer at a minimum speed of 900 rpm.r/min. If desired, two propellers may be used on the sameshaft, the lower one being near the end of the shaft. The shaft speed shall give a brisk turnover without creating a vortex
19、 The partof the equipment immersed in the emulsion polymer must contain no copper or brass.4.3.2 Removal of SampleAfter blending, take the sample without delay.Asuitable method is by slowly inserting a clean, dry,glass tube of not more than 15-mm internal diameter and open at both ends, until it re
20、aches the bottom of the container. Then closethe upper end of the tube and transfer the contents to a clean, dry sample bottle. Repeat the operation until sufficient emulsionpolymer has been obtained.4.3.3 Bulk SampleWhere samples are drawn from several containers, for example 10 % sampling of emuls
21、ion polymer indrums, or where samples are taken at different depths, for example from tanks, combine the samples and thoroughly blend bystirring or shaking immediately before taking the final average sample.5. Total Solids5.1 ApparatusTared aluminum dishes with a close-fitting cover, having a diamet
22、er of approximately 60 mm and a height of15 mm.5.2 ProcedureIf the temperature of the emulsion polymer is above room temperature, allow it to cool to room temperature.Then weigh two samples of approximately 1 g each to the nearest 1.0 mg in tared aluminum weighing dishes. Dry the samplesfor 2 h in a
23、 convection or forced-draft oven at a temperature of 105 + 2, 0.5C. Remove the samples from the oven, cool thecontainer and contents to room temperature in a desiccator, and weigh them to the nearest 0.1 mg. Average the values if they arewithin 0.1 %. If not, make additional duplicate determinations
24、 until a pair of duplicate determinations agree within 0.1 %.5.3 CalculationCalculate the percent of total solids as follows:Total solids,%5weight of dry solidsweight of sample 3100 (1)5.4 ReportSpecify whether the oven used is a convection or a forced-draft type.6. pH Value6.1 ApparatusAny pH elect
25、rometer and a glass electrodecalomel cell assembly may be used as described in Test MethodE70. A flowing calomel electrode has been found particularly suited for the pH range of the latex being tested.6.2 Standard Solution, having a pH of 10, or a standard solution having a pH approximately the same
26、 as that of the emulsionpolymer to be tested.6.3 ProcedureBefore making a determination, take care that the instrument is properly standardized at frequent intervals witha standard solution (see 6.2) and that the electrodes are clean. Permit the polymer emulsion to come to equilibrium with the glass
27、electrode before taking the final reading.6.4 ReportReport the pH value for the polymer emulsion.7. Apparent Viscosity7.1 Apparatus:7.1.1 Sieve, U.S. No. 40 (425-m).7.1.2 Distillation Flask, Three-Necked, equipped with stirring and vacuum connections.7.1.3 Viscometer, RotationalBrookfield RV or LV T
28、ype.The essential instrumentation required providing the minimumrotational viscometer analytical capabilities for this test method include:7.1.3.1 Drive Motor, to apply a unidirectional rotational displacement to the specimen of 0.5 revolutions per minute (r/min) to60 r/min constant to within 61 %.7
29、1.3.2 Force Sensor, to measure the torque developed by the specimen to within 61 % full scale.7.1.3.3 Coupling Shaft, or other means to transmit the rotational displacement from the motor to the specimen.7.1.3.4 Geometry, Spindle, Tool or Rotational Element, to fix the specimen between the drive sh
30、aft and a stationary position.D3716 142NOTE 1Each geometry typically covers a range of 1.5 decades of viscosity. The geometry is selected so that the measured viscosity is between 10and 90 % of the range of the geometry.7.1.3.5 Guard, to protect the geometry from mechanical damage.7.1.3.6 Temperatur
31、e Sensor, to provide an indication of the specimen temperature over the temperature range from 15C to 30Cmeasurable to within 60.1C.7.1.3.7 Data Collection Device, to provide a means of acquiring, storing, and displaying measured or calculated signals, or both.The minimum output signals required for
32、 rotational viscometry are torque, rotational speed, temperature, and time.7.1.3.8 Stand, to support, level and adjust the height of the drive motor, shaft and geometry.7.1.3.9 Specimen Container, with a capacity of 600 mL to contain the test specimen during testing.NOTE 2A 600-mL labortory beaker h
33、as been found suitable for this service.7.1.3.10 Auxiliary instrumentation considered necessary or useful in conducting this test method includes:(1) Data analysis capability to provide viscosity, stress, shear rate or other useful parameters derived from measured signals.(2) Level to indicate the v
34、ertical plumb of the drive motor, shaft and geometry.7.2 Preparation of SampleAdjust to the desired solids content with distilled water. Bring the pH to the desired point withammonia. Take a sufficient volume of sample so that at least 500 mL of diluted emulsion polymer will be obtained. Strain thed
35、iluted emulsion polymer through the No. 40 (425-m) sieve. After straining, again gently stir the emulsion polymer forapproximately 20 s. If the emulsion polymer contains excessive amounts of occluded air, remove the air in the following mannerbefore proceeding with the determination of viscosity: In
36、to a three-necked distillation flask equipped with a stirrer and vacuumconnections, pour a sufficient volume of diluted emulsion polymer so that at least 500 mL of emulsion polymer will remain afterremoval of the air. Start the agitator and evacuate the flask to a vacuum of 26 to 28 mm Hg (3.5 to 3.
37、7 kPa), or until the foamrises to the neck of the flask. Break the vacuum. Evacuate several times in this manner to ensure removal of the occluded air. Whenrequired, the same method may be used on emulsion polymer as received, without laboratory removal of occluded air.7.3 ProcedureProcedure: With t
38、he strained emulsion polymer at a temperature at 25 6 2C, pour the emulsion polymer intoa 600-mLbeaker. Insert the shielded spindle of the viscometer into the emulsion polymer until the surface of the emulsion polymeris within the notch in the shaft of the spindle. Use a spindle and speed that will
39、give medium scale reading.7.3.1 Ensure that the strained emulsion polymer is at a temperature at 25 6 2C.7.3.2 Pour the emulsion polymer into the container.7.3.3 Insert the guarded geometry of the viscometer into the emulsion polymer until the surface of the emulsion polymer iswithin the measurement
40、 indicator on the shaft.7.3.4 Initiate the rotation of the geometry at the lowest speed available for 1 min.7.3.5 Increase the geometry speed to that required to produce a reading nearest the midpoint of the scale.7.3.6 Stop the rotation of the geometry and wait for 1 min.7.3.7 Restart the rotationa
41、l of the geometry and allow at least 5 revolutions of the geometry.NOTE 3For routine measurement of quality control samples where a specific viscosity range is to be expected and rotational geometry and speedsettings are pre-defined through method validation, steps 7.3.4 through 7.3.6 can be skipped
42、7.3.8 Measure and report the observed viscosity, the rotational speed and the geometry type used.7.3.9 Stop the rotation of the geometry. Elevate the geometry out of the test specimen. Clean the geometry with a suitablesolvent. Safely dispose of the test specimen.8. Sediment8.1 ScopeThis test metho
43、d covers the determination of the percent sediment content of emulsion polymers.8.2 Apparatus and Material:8.2.1 International Oil Testing Centrifuge, Model DE.8.2.2 Centrifuge Tubes (Graduated)Goetz Pear-Shaped, 100-mL capacity, large stem,3,4 or Goetz Phosphorus Tube with astopper, 100-mL capacity
44、 small stem.4,58.2.3 Bromophenol Blue Indicator Solution (0.1 %).8.3 Procedure:8.3.1 Fill a Goetz PhosphorusTube (small stem) with 100 mLof polymer emulsion inverting the tube to fill the stem completely.8.3.2 Place the sample tube in the centrifuge and place a tube filled with 100 mL of water on t
45、he opposite side for instrumentbalance.8.3.3 Spin for 30 min at 1750 rpm.r/min.3 The sole source of supply of Fisher catalog no. 5-622 known to the committee at this time is Fisher Scientific Co., Pittsburgh, PA.4 If you are aware of alternative suppliers, please provide this information to ASTM Hea
46、dquarters. Your comments will receive careful consideration at a meeting of theresponsible technical committee, which you may attend.5 The sole source of supply of Fisher catalog no. 5-624 known to the committee at this time is Fisher Scientific Co., Pittsburgh, PA.D3716 1438.3.4 Alternative MethodD
47、ilute the polymer emulsion 50/50 with water; then centrifuge for 30 min.8.4 Calculations:8.4.1 Undiluted SamplesRead the sediment level in the tube stem and express directly as percent sediment content.8.4.2 Diluted SamplesRead the sediment level in the tube stem and multiply by the dilution factor
48、50/50 = 2,2575 = 4, etc.);express the result as percent sediment content.9. Storage Stability9.1 Scope:9.1.1 This test method is intended to indicate storage stability of emulsion polymers.9.1.2 Storage for 30 days at 125F (52C), while not a guarantee of one years stability at room temperature, is
49、believed to bea more reliable indicator of storage stability than similar tests of shorter duration.9.2 Apparatus:9.2.1 Glass Bottles, 120-mL, round, narrow-mouth, approximately 120 mm high and 45 mm in diameter with polyethylene-lined screw caps.9.2.2 Oven, capable of maintaining the temperature of the emulsion samples at 125 6 2F (52C).9.3 Samples:9.3.1 The sample shall be thoroughly representative of the material in question and the portion used for the test shall bethoroughly representative of the sample itself.9.3.2 Test samples sha
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