1、Designation: D 3716 99 (Reapproved 2008)Standard Test Methods forUse of Emulsion Polymers in Floor Polishes1This standard is issued under the fixed designation D 3716; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of las
2、t revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon (e) indicates an editorial change since the last revision or reapproval.1. Scope1.1 These test methods cover test procedures for emulsionpolymers that are used in water-based floor polishes. The term“emul
3、sion polymers” is used primarily to denote those mate-rials produced by regular emulsion polymerization techniques,but may be extended to those polymers that are subsequentlyemulsified or dispersed after polymerization. Unless otherwisenoted, the tests may be used for any polymer or copolymersystems
4、. 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 thesafety concerns, if any, associated with its use. It is theresponsi
5、bility of the user of this standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2E1 Specification for ASTM Liquid-in-Glass ThermometersE70 Test Method for pH of Aqueous Solutio
6、ns With theGlass ElectrodeE 100 Specification for ASTM Hydrometers3. Significance and Use3.1 The purpose of this test is not to fully identify andcharacterize a polymer, but to identify a variety of basicparameters needed to predetermine the usefulness of thepolymer in formulations as well as for Qu
7、ality Control pur-poses.3.2 Astatement of precision and accuracy is not appropriatein this case.4. Sampling4.1 Outline of Test MethodSince stratification may occurin emulsion polymers, they must be thoroughly agitated toobtain a homogeneous blend as a representative sample. Theprocedure required dif
8、fers with the type of container andfacilities available.4.2 Sampling from Tank CarsTake three samples of atleast 1 pt (473 mL) each, one at the center of the tank, anotherhalf way between the center and the bottom, and the third halfway between the center and the top. Take the top sample first,then
9、the center sample, and the bottom sample last. Use aweighted sampler with a remotely operated, removable top, orother suitable sampling device that will accomplish the sameresults. Determine the applicable specified or characteristicproperties of the samples by the standard procedures ormethods. If
10、there is any evidence that stratification has oc-curred, then thoroughly agitate the contents of the car untilsamples obtained agree within 1 % of total solids.4.3 Sampling from Drums:4.3.1 Blending of ContentsBlend the emulsion polymerby one of the following methods:4.3.1.1 Method AIf the drum is f
11、itted with a bung andcontains 2 % air space, lay it on its side and roll to and frobriskly for not less than 10 min. Then turn the drum upsidedown for about 15 min and repeat the rolling operation for anadditional 10 min. If the drum contains less than 2 % air space,transfer the contents to a larger
12、 vessel and thoroughly stir,preferably by means of a perforated steel disk plunger. Stirringfor about 10 min will normally suffice.1These test methods are under the jurisdiction of ASTM Committee D21 onPolishes and are the direct responsibility of Subcommittee D21.03 on Chemical andPhysical Testing.
13、Current edition approved March 1, 2008. Published April 2008. Originallyapproved in 1978. Last previous edition approved in 2006 as D 3716 99(2006).2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandar
14、ds volume information, refer to the standards Document Summary page onthe ASTM website.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.4.3.1.2 Method BAgitate the contents of the drum bymeans of a suitable motor-driven stirrer for as
15、 long as isnecessary to obtain uniformity. Excessive stirring and unnec-essary exposure of the emulsion polymer to air must beavoided. A suitable type of stirrer consists of a collapsibletwo-bladed stainless steel propeller of 110-mm minimumdiameter, when fully opened, mounted on a stainless steel s
16、haftsufficiently long for the propeller to be distant about onequarter the height of the emulsion polymer from the bottom ofthe drum. Operate stirrer at a minimum speed of 900 rpm. Ifdesired, two propellers may be used on the same shaft, thelower one being near the end of the shaft. The shaft speed
17、shallgive a brisk turnover without creating a vortex. The part of theequipment immersed in the emulsion polymer must contain nocopper or brass.4.3.2 Removal of SampleAfter blending, take the samplewithout delay.Asuitable method is by slowly inserting a clean,dry, glass tube of not more than 15-mm in
18、ternal diameter andopen at both ends, until it reaches the bottom of the container.Then close the upper end of the tube and transfer the contentsto a clean, dry sample bottle. Repeat the operation untilsufficient emulsion polymer has been obtained.4.3.3 Bulk SampleWhere samples are drawn from severa
19、lcontainers, for example 10 % sampling of emulsion polymer indrums, or where samples are taken at different depths, forexample from tanks, combine the samples and thoroughlyblend by stirring or shaking immediately before taking the finalaverage sample.5. Total Solids5.1 ApparatusTared aluminum dishe
20、s with a close-fittingcover, having a diameter of approximately 60 mm and a heightof 15 mm.5.2 ProcedureIf the temperature of the emulsion polymeris above room temperature, allow it to cool to room tempera-ture. Then weigh two samples of approximately 1 g each to thenearest 1.0 mg in tared aluminum
21、weighing dishes. Dry thesamples for2hinaconvection or forced-draft oven at atemperature of 105 + 2, 0.5C. Remove the samples from theoven, cool the container and contents to room temperature in adesiccator, and weigh them to the nearest 0.1 mg. Average thevalues if they are within 0.1 %. If not, mak
22、e additionalduplicate determinations until a pair of duplicate determina-tions agree within 0.1 %.5.3 CalculationCalculate the percent of total solids asfollows:Total solids, % 5weight of dry solidsweight of sample3 100 (1)5.4 ReportSpecify whether the oven used is a convectionor a forced-draft type
23、.6. pH Value6.1 ApparatusAny pH electrometer and a glasselectrodecalomel cell assembly may be used as described inTest Method E70.Aflowing calomel electrode has been foundparticularly suited for the pH range of the latex being tested.6.2 Standard Solution, having a pH of 10, or a standardsolution ha
24、ving a pH approximately the same as that of theemulsion polymer to be tested.6.3 ProcedureBefore making a determination, take carethat the instrument is properly standardized at frequent inter-vals with a standard solution (see 6.2) and that the electrodesare clean. Permit the polymer emulsion to co
25、me to equilibriumwith the glass 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 stir-ring and vacuum connections.7.1.3 Viscometer
26、, Brookfield RV or LV Type.7.2 Preparation of SampleAdjust to the desired solidscontent with distilled water. Bring the pH to the desired pointwith ammonia. Take a sufficient volume of sample so that atleast 500 mL of diluted emulsion polymer will be obtained.Strain the diluted emulsion polymer thro
27、ugh the No. 40(425-m) sieve. After straining, again gently stir the emulsionpolymer for approximately 20 s. If the emulsion polymercontains excessive amounts of occluded air, remove the air inthe following manner before proceeding with the determinationof viscosity: Into a three-necked distillation
28、flask equippedwith a stirrer and vacuum connections, pour a sufficient volumeof diluted emulsion polymer so that at least 500 mL ofemulsion polymer will remain after removal of the air. Start theagitator and evacuate the flask to a vacuum of 26 to 28 mm Hg(3.5 to 3.7 kPa), or until the foam rises to
29、 the neck of the flask.Break the vacuum. Evacuate several times in this manner toensure removal of the occluded air. When required, the samemethod may be used on emulsion polymer as received, withoutlaboratory removal of occluded air.7.3 ProcedureWith the strained emulsion polymer at atemperature at
30、 25 6 2C, pour the emulsion polymer into a600-mL beaker. Insert the shielded spindle of the viscometerinto the emulsion polymer until the surface of the emulsionpolymer is within the notch in the shaft of the spindle. Use aspindle and speed that will give medium scale reading.8. Sediment8.1 ScopeThi
31、s test method covers the determination ofthe 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-mLcapacity, large stem,3,4or Goetz PhosphorusTube witha stopper, 100-mL c
32、apacity, small stem.4,58.2.3 Bromophenol Blue Indicator Solution (0.1 %).3The sole source of supply of Fisher catalog no. 5-622 known to the committeeat this time is Fisher Scientific Co., Pittsburgh, PA.4If you are aware of alternative suppliers, please provide this information toASTM Headquarters.
33、Your comments will receive careful consideration at a meetingof the responsible technical committee, which you may attend.5The sole source of supply of Fisher catalog no. 5-624 known to the committeeat this time is Fisher Scientific Co., Pittsburgh, PA.D 3716 99 (2008)28.3 Procedure:8.3.1 Fill a Goe
34、tz Phosphorus Tube (small stem) with 100mL of polymer emulsion inverting the tube to fill the stemcompletely.8.3.2 Place the sample tube in the centrifuge and place atube filled with 100 mL of water on the opposite side forinstrument balance.8.3.3 Spin for 30 min at 1750 rpm.8.3.4 Alternative Method
35、Dilute the polymer emulsion50/50 with water; then centrifuge for 30 min.8.4 Calculations:8.4.1 Undiluted SamplesRead the sediment level in thetube stem and express directly as percent sediment content.8.4.2 Diluted SamplesRead the sediment level in the tubestem and multiply by the dilution factor (5
36、0/50 = 2,25/75 = 4,etc.); express the result as percent sediment content.9. Storage Stability9.1 Scope:9.1.1 This test method is intended to indicate storagestability of emulsion polymers.9.1.2 Storage for 30 days at 125F (52C), while not aguarantee of one years stability at room temperature, isbeli
37、eved to be a more reliable indicator of storage stability thansimilar tests of shorter duration.9.2 Apparatus:9.2.1 Glass Bottles, 120-mL, round, narrow-mouth, ap-proximately 120 mm high and 45 mm in diameter withpolyethylene-lined screw caps.9.2.2 Oven, capable of maintaining the temperature of the
38、emulsion samples at 125 6 2F (52C).9.3 Samples:9.3.1 The sample shall be thoroughly representative of thematerial in question and the portion used for the test shall bethoroughly representative of the sample itself.9.3.2 Test samples shall be prepared in duplicate for eachmaterial in question.9.4 Pr
39、ocedure:9.4.1 Transfer 100 mL of polymer emulsion to a clean, drytest bottle and hand tighten the screw cap.9.4.2 Place the test set or series inverted in a drying ovencapable of maintaining the temperature of the emulsions at 1256 2F (52C).9.4.3 Observe the samples daily for the first 14 days andtw
40、ice weekly (that is, Monday and Thursday) for the remainderof the 30-day storage period. Samples should be examined asrapidly as possible with a minimum of agitation and returned tothe oven. Do not loosen cap.9.4.4 At the time of each observation, record the followingon a suitable data sheet:9.4.4.1
41、 Date,9.4.4.2 Number of days in test, and9.4.4.3 Condition of the emulsion using the following sym-bols:OK = no signs of instabilitySV = slightly viscousV = viscousCr = creamedG = gelledSep = other types of liquid phase separationSediment = sedimentation of solid matter10. Freeze-thaw Stability10.1
42、Scope:10.1.1 This test method is intended to indicate the freeze-thaw stability of emulsion polymers used for floor polishes.10.1.2 Storage under repeated freeze-thaw conditions is notnecessarily indicative of the freeze-thaw stability of an emul-sion polymer. Materials stable under these conditions
43、 mayexhibit instability to prolonged freezing, and this test method isintended to cover both eventualities. Thus, the three-cycle testis meant to be equivalent to repeated freeze-thaw cycles andthe longer-term single-cycle test is meant to be equivalent toprolonged freezing.10.2 Apparatus:10.2.1 Gla
44、ss Screw Cap Bottle, 120-mL, approximately 38mm in outside diameter, 150 mm high with a 24/400 finish asspecified by the Glass Container Manufacturers Institute usinga polyethylene-lined screw cap (used in ASTM oven stabilitytests).10.2.2 Freeze Chest, capable of maintaining the temperatureof emulsi
45、on samples at 106 2C.10.3 Procedure:10.3.1 Transfer 100 mL of the emulsion polymer to each offour dry clean test bottles and hand-tighten the screw cap.10.3.2 Place the test set or series in a freeze chest capable ofmaintaining 10 6 2C.10.3.3 Allow two of the samples to remain in the chest for18 h;
46、remove and allow to thaw and remain at room tempera-ture for 6 h before evaluating. Repeat for two additional cyclesor a total of three cycles.10.3.4 Allow two of the samples to remain in the chest for72 h; remove and allow to thaw and remain at room tempera-ture for 6 h before making observation. R
47、epeat for twoadditional cycles.NOTE 1It should be noted that emulsion polymers, after freezing, maynot perform adequately in floor polishes even though above tests aresatisfied.10.3.5 Observations should be made on the condition of thethawed sample, before and after shaking, after each cycle,noting
48、particularly any increase in particle size, coagulation,separation, or change in viscosity.11. Specific Gravity11.1 ScopeThis method describes a procedure for thedetermination by means of glass hydrometer of the specificgravity of an emulsion polymer.11.2 Definition:11.2.1 specific gravitythe ratio
49、of weight of a givenvolume of material to the weight of an equal volume of water.In this method the temperature for determination is 60F(15C).11.3 Apparatus:D 3716 99 (2008)311.3.1 Hydrometers, glass, graduated in Specific Gravity60/60F, conforming to Specification E 100. For liquids lighterthan water, use 98H-62. For liquids heavier than water, use111H to 120H-62.11.3.2 Thermometers, having a range from 5 to + 215F(21 to + 104C) and conforming to the requirements forThermometer 12 F as prescribed in Specification E1.11.3.3 Hydrom
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