1、Designation: D 1417 03aStandard Test Methods forRubber LaticesSynthetic1This standard is issued under the fixed designation D 1417; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revision. A number in parentheses
2、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 syntheticrubber latices ABR, BR, CR, IIR, IR, NBR, NCR, NIR, PBR,PSBR, SBR, SCR, SIR, synthetic rubber latices
3、having substi-tute carboxylic acid (COOH) groups on the polymer chain (X),and synthetic rubber latices that are reinforced (Y). Exceptionsto the above are noted in the individual test procedures. Thetest methods include procedures for sampling, and for deter-mining total solids, volatile unsaturates
4、 (residual styrene), pHvalue, surface tension, viscosity, coagulum, bound styrene,Mooney viscosity, mechanical stability, polystyrene reinforce-ment in contained polymer, and residual acrylonitrile content.NOTE 1The nomenclature used in these test methods is in accordancewith Practice D 1418.1.2 The
5、 values stated in SI units are to be regarded asstandard.1.3 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibility of the user of this standard to establish appro-priate safety and health practices and determine the applica-bili
6、ty of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D 1076 Specification for RubberConcentrated, AmmoniaPreserved, Creamed, and Centrifuged Natural LatexD 1331 Test Methods for Surface and Interfacial Tension ofSolutions of Surface-Active AgentsD 1416 Test Methods fo
7、r Rubber from Synthetic SourcesChemical AnalysisD 1418 Practice for Rubber and Rubber LaticesNomenclatureD 1646 Test Methods for RubberViscosity, Stress Relax-ation, and Pre-Vulcanization Characteristics (Mooney Vis-cometer)D 3182 Practice for RubberMaterials, Equipment, andProcedures for Mixing Sta
8、ndard Compounds and Prepar-ing Standard Vulcanized SheetsD 3314 Test Method for RubberChemical Analysis forPolystyrene Blocks in SBR (Styrene-Butadiene Rubber)and Styrene-Reinforced LaticesD 4483 Practice for Determining Precision for Test MethodStandards in the Rubber and Carbon Black IndustriesD 6
9、204 Test Methods for RubberMeasurement of Unvul-canized Rheological Properties Using Rotorless ShearRheometersE 70 Test Method for pH of Aqueous Solutions with theGlass ElectrodeE 200 Practice for Preparation, Standardization, and Stor-age of Standard and Reagent Solutions for ChemicalAnalysis3. Sam
10、pling3.1 Rubber latex tends to cream on standing. Once stratifi-cation has occurred, the latex must be thoroughly agitated toobtain a homogeneous blend as a representative sub-sample.The procedure required differs with the type of container andfacilities available.1These test methods are under the j
11、urisdiction of ASTM Committee D11 onRubber and are the direct responsibility of Subcommittee D11.23 on SyntheticRubbers.Current edition approved Nov. 1, 2003. Published December 2003. Originallyapproved in 1956. Last previous edition approved in 2003 as D 1417 03.2For referenced ASTM standards, visi
12、t the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.TABLE 1 Drying Time for Determination of Total Solids in Latex(Drying Aid, 1 cm3of distilled wate
13、r.)Type of Latex Drying Time, minSBR 2000 45SBR 2001 45SBR 2002 45SBR 2003 45BR 2004 45SBR 2005 45SBR 2006 45SBR 2076 45SBR 2100 60SBR 2101 and X765 45SBR 2102 60SBR 2103 60BR 2104 45SBR 2105 45SBR 2106 45SBR 2107 45SBR 2108 45SBR 2109 45SBR 2110 45SBR 2111 45SBR 2112 45SBR 2113 45SBR 2114 451Copyri
14、ght ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.3.2 Sub-Sampling from Tank Cars:3.2.1 If stratification has occurred, take separate samplesabout 75 mm (3 in.) from the top surface and about 75 mmfrom the bottom of the tank. If results from
15、the top and bottomsamples do not agree within 1 % total solids, the contents of thecar shall be thoroughly agitated until samples obtained doagree within this tolerance.3.3 Sub-Sampling from Drums:3.3.1 BlendingThe latex shall be blended by one of thefollowing test methods:3.3.1.1 Test Method AIf th
16、e drum is fitted with a bung andcontains at least 2 % air space, lay it on its side and roll backand forth briskly for not less than 10 min. Then turn the drumupside down for about 15 min and repeat the rolling operationfor an additional 10 min. If the drum contains less than 2 % airspace, transfer
17、the contents to a larger vessel and thoroughlystir, preferably by means of a perforated steel disk plunger.Stirring for about 10 min will normally suffice. If the drum isof the open-head type, remove the end head and thoroughly stirthe contents, preferably by means of a perforated steel diskplunger.
18、 Stirring for about 10 min will normally suffice.3.3.1.2 Test Method BAgitate the contents of the drum bymeans of a suitable motor-driven stirrer for as long as isnecessary to disperse the cream. Excessive stirring and unnec-essary exposure of the latex to air must be avoided. A suitabletype of stir
19、rer consists of a collapsible two-bladed stainlesssteel propeller of 11 cm minimum diameter, when fullyopened, mounted on a stainless steel shaft sufficiently long forthe propeller to be distant about one quarter the height of thelatex from the bottom of the drum. The stirrer shall be operatedat a m
20、inimum speed of 900 r/min. If desired, two propellersmay be used on the same shaft, the lower one being near theend of the shaft. The shaft speed shall give a brisk turnoverwithout creating a vortex. The part of the equipment immersedin the latex must contain no copper or brass.3.3.2 Removal of Sub-
21、SampleAfter blending, take thesample without delay. A suitable method is by slowly insertinga clean, dry, glass tube of not more than 15 mm internaldiameter and open at both ends until it reaches the bottom ofthe container. Then close the upper end of the tube and transferthe contents to a clean, dr
22、y sample bottle. Repeat the operationuntil sufficient latex has been obtained.NOTE 2Alternatively, a specially constructed metal sampling tubemay be used, the bottom of which can be closed by remote control. Copperor brass must not be used in any part of its construction.3.3.3 Sample:3.3.3.1 Where s
23、ub-samples are drawn from several contain-ers, for example, 10 % sampling of latex in drums, or wheretaken at different depths, for example from tanks, the sub-samples shall be combined and thoroughly blended by stirringor shaking immediately before the final sample is taken.4. Total Solids4.1 Appar
24、atus:4.1.1 Tared, covered, all-metal ointment boxes, having acapacity of approximately 50 to 60 cm3, a minimum diameterof 38 mm (1.5 in.), and a maximum height of 23 mm (0.9 in.).The disposable aluminum liner for the metal ointment box maybe used.4.2 Procedure:4.2.1 Method AAccurately weigh a clean,
25、 dry aluminumfoil dish. Record the weight. Measure 2 mL of sample and putin the aluminum foil dish. Reweigh the dish and record theweight. Put the aluminum foil dish in a 170C oven; heat for 15min. Remove the aluminum foil dish from the oven and let coolin a desiccator. Reweigh the aluminum foil dis
26、h. Record theweight. Calculations: A = weight of dish empty; B = weight ofdish + sample; C = weight of dish + residue;CA!100!BA!5 % Total Solids (1)Report the total solids to the nearest 0.1 %.4.2.2 Method BThe percent solids is determined by mea-suring gravimetrically the solids remaining after vol
27、atilizingoff the liquid portion.4.2.2.1 Instrument ConditionsThe following instrumentconditions are based on work done with a Denver IR-100:Oven Temperature145CSlope0.05 %/minProgramNo. 1A1 pansFisher #01-913-356Fiber paperFisher #01-913-318Place a glass fiber filter circle on an aluminum pan. Open
28、thelid of the IR-100 and center the pan (with filter) between thefour prongs of the“ X”-shaped holder. Close the lid and pressthe START button. When display reads “tare pan,” press theTARE button. Raise the lid and place about 3.0 g of latex in acircle on the filter paper. Again close the lid. Wait
29、10 seconds,then press the START button. The instrument will automati-cally run for about 4 min then shut off. Read the percent (%)solids directly from the printout paper or from the displayscreen. Report the value to the nearest 0.1 %.NOTE 3An alternative method for the determination of total solids
30、 insynthetic rubber latex is described in Specification D 1076.5. Volatile Unsaturates (Residual Styrene)5.1 ScopeThis test method measures the residual styreneof SBR synthetic rubber latices. It is not applicable to othersynthetic rubber latices.5.2 Apparatus:5.2.1 Iodine flasks having capacities o
31、f 250 cm3each, anddistillation apparatus with ground-glass joints.5.2.2 25-cm3pipet.5.2.3 50-cm3buret.5.3 Reagents:5.3.1 Synthetic Methanol, containing 100 ppm of p-tertiarybutyl catechol.5.3.2 Standard Potassium Bromide-Potassium Bromate So-lution (0.1 N)Dissolve 2.784 g of potassium bromate(KBrO3)
32、 and 10.0 g of potassium bromide (KBr) in water anddilute to 1000 cm3. Standardize with 0.1 N sodium thiosulfate(Na2S2O3) solution in the presence of an excess (about 3 g) ofpotassium iodide (KI) and sulfuric acid (H2SO4), (18 %).D 1417 03a25.3.3 Sulfuric Acid Solution (18 %).5.3.4 Potassium Iodide
33、Solution (10 %).5.3.5 Standard Sodium Thiosulfate Solution (0.1 N).5.3.6 Starch Indicator Solution.5.4 Procedure:5.4.1 Weigh approximately 25 g of the latex to the nearest0.1 g in a tared, covered, 250-cm3iodine flask. Remove thecover and add 25 cm3of distilled water to the iodine flask. Add25 cm3of
34、 synthetic methanol containing 100 ppm of p-tertiarybutyl catechol. Be sure to add the materials in the followingorder:1. Latex.2. Distilled water.3. Methanol containing p-tertiary butyl catechol.5.4.2 Connect the iodine flask to the distillation apparatuswith ground-glass joints and distill the mix
35、ture. Collect the first25 cm3of distillate in a 250-cm3iodine flask, rinse thecondenser with 20 cm3of methanol containing 100 ppm ofp-tertiary butyl catechol, and add the rinsings to the recoveryflask.5.4.3 From a buret add 20 cm3of 0.1 N standard KBr-KBrO3solution. Cool the solution to 30 C. Rapidl
36、y add 15 cm3of 18 % H2SO4solution, stopper the flask, shake it, and adddistilled water to the funnel lips as a vapor seal. Allow thebottle to stand for 60 s. If no yellow color remains, addsuccessive 10-cm3portions of the bromide-bromate solutionuntil a slight yellow color persists for 60 s after th
37、e addition.Make the additions by drawing the standard solution from theburet into the funnel lip and lifting the stopper so that thesolution enters the flask around the stopper. Wash the funnel lipwith distilled water in the same manner and seal with water.After 60 s has elapsed since the final brom
38、ide-bromate addi-tion, add 10 cm3of 10 % KI solution to the funnel lip, and liftthe stopper to allow the solution to enter the flask around thestopper. Shake the bottle and contents and titrate the liberatediodine with 0.1 N standard sodium thiosulfate solution to afaint yellow color. Add 1 cm3of st
39、arch indicator solution andcontinue the titration with sodium thiosulfate solution until thesolution is clear.5.4.3.1 For a blank determination, repeat the procedureusing distilled water instead of latex.5.5 CalculationCalculate the percentage of volatile unsat-urates (residual styrene) as follows:V
40、olatile unsaturates residual styrene!,%5 $D 3 E! 2 F 3 G!# 3 0.0521 3 100/M% 2 H (2)where:D = cubic centimetres of standard bromide-bromate solu-tion used,E = normality of the bromide-bromate solution,F = cubic centimetres of standard thiosulfate solutionused for the titration,G = normality of the t
41、hiosulfate solution,H = blank determination, %, andM = mass of latex used, g.6. pH Value6.1 ApparatusAny pH electrometer and a glass electrode-calomel cell assembly may be used as described in TestMethod E 70. A flowing calomel electrode has been foundparticularly suited for this use. The glass elec
42、trode shall be ofthe type applicable for a pH range of from 2 to 14.6.2 Standard SolutionUse a standard solution having a pHof 10 or a standard solution having a pH approximately thesame as that of the latex to be tested.6.3 ProcedureBefore making a determination take carethat the instrument is prop
43、erly standardized at frequent inter-vals with a standard solution (see 6.2), and that the electrodesare clean. Permit the latex to come to equilibrium with theglass electrode before taking the final reading. After the pHdetermination has been made, clean the electrodes thoroughlyand immerse them in
44、distilled water. Report the pH value forthe latex at a temperature of 25 6 2C.7. Surface Tension7.1 The surface tension of styrene-butadiene rubber latexshall be determined on the total solids of 40 6 1%.Iftheviscosity is below 200 mPas (200 cP) on No. 1 spindle at 20r/min, the latex can be tested w
45、ith solids as received with littleloss in accuracy.7.2 ApparatusUse a du Nouy tensiometer, carefully cali-brated as described in Test Methods D 1331.7.3 ProcedureStrain approximately 25 cm3of latex, ad-justed to a temperature of 25 6 2C, into a pan 60 to 65 mm(2.4 to 2.6 in.) in diameter and 18 to 2
46、0 mm (0.7 to 0.8 in.) high(Note 4). The surface of the latex must be free of air bubbles,and the surface tension test shall be within 3 to 4 min to avoid“skinning over” of the latex. Clean the tensiometer ring byheating in a bunsen flame. Extreme care must be taken to avoiddistortion as the tensiome
47、ter ring is handled. Place the pan,containing the latex being tested, beneath the ring on theadjustable platform of the instrument. With the instrumentadjusted so that the ring system is in its zero position when thering is dry and the scale reading is zero, raise the platform untilthe latex makes c
48、ontact with the ring. Submerge the ringbeneath the surface of the latex. Now slowly lower theplatform by means of the platform-adjusting screw and in-crease the torsion of the wire simultaneously, proportioningthese two adjustments so that the torsion arm remains exactlyin its zero position. As the
49、film adhering to the ring approachesthe breaking point, proceed more slowly with the adjustmentsto make certain that the moving system is in its zero positionwhen the rupture occurs. The scale reading at which the ringdetaches from the latex represents, after proper correction, thesurface tension of the latex at the given temperature. Recordthe average of three consecutive readings, discounting the firstreading. The ring is cleaned by flaming between readings andall readings shall agree within 0.5 mN/m (0.5 dynes/cm).NOTE 4The pan must be
