1、Designation: D1417 10Standard Test Methods forRubber LaticesSynthetic1This standard is issued under the fixed designation D1417; 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 ind
2、icates 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 syntheticrubber latices ABR, BR, CR, IIR, IR, NBR, NCR, NIR, PBR,PSBR, SBR, SCR, SIR, synthetic rubber latices havi
3、ng 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 (re
4、sidual 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 D1418.1.2 The valu
5、es 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-bility of
6、 regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D1076 Specification for RubberConcentrated, AmmoniaPreserved, Creamed, and Centrifuged Natural LatexD1331 Test Methods for Surface and Interfacial Tension ofSolutions of Surface-Active Agents3D1416 Test Methods for Rubbe
7、r from Synthetic Sources-Chemical Analysis3D1418 Practice for Rubber and Rubber LaticesNomenclatureD1646 Test Methods for RubberViscosity, Stress Relax-ation, and Pre-Vulcanization Characteristics (Mooney Vis-cometer)D3182 Practice for RubberMaterials, Equipment, andProcedures for Mixing Standard Co
8、mpounds and Prepar-ing Standard Vulcanized SheetsD3314 Test Method for RubberChemical Analysis forPolystyrene Blocks In SBR (Styrene-Butadiene Rubber)and Styrene-Reinforced LaticesD4483 Practice for Evaluating Precision for Test MethodStandards in the Rubber and Carbon Black ManufacturingIndustriesD
9、6204 Test Method for RubberMeasurement of Unvul-canized Rheological Properties Using Rotorless ShearRheometersE70 Test Method for pH of Aqueous Solutions With theGlass ElectrodeE200 Practice for Preparation, Standardization, and Storageof Standard and Reagent Solutions for Chemical Analysis3. Sampli
10、ng3.1 Rubber latex tends to cream on standing. Once stratifi-cation has occurred, the latex must be thoroughly agitated to1These test methods are under the jurisdiction of ASTM Committee D11 onRubber and are the direct responsibility of Subcommittee D11.23 on SyntheticRubbers.Current edition approve
11、d March 1, 2010. Published April 2010. Originallyapproved in 1956. Last previous edition approved in 2003 as D1417 03a. DOI:10.1520/D1417-10.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volu
12、me information, refer to the standards Document Summary page onthe ASTM website.3Withdrawn. The last approved version of this historical standard is referencedon www.astm.org.TABLE 1 Drying Time for Determination of Total Solids in Latex(Drying Aid, 1 cm3of distilled water.)Type of Latex Drying Time
13、, 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 451Copyright ASTM International, 100
14、Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.obtain a homogeneous blend as a representative sub-sample.The procedure required differs with the type of container andfacilities available.3.2 Sub-Sampling from Tank Cars:3.2.1 If stratification has occurred, take separ
15、ate samplesabout 75 mm (3 in.) from the top surface and about 75 mmfrom the bottom of the tank. If results from 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 fr
16、om Drums:3.3.1 BlendingThe latex shall be blended by one of thefollowing test methods:3.3.1.1 Test Method AIf the 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
17、and repeat the rolling operationfor an additional 10 min. If the drum contains less than 2 % airspace, transfer 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 t
18、ype, remove the end head and thoroughly stirthe contents, preferably by means of a perforated steel diskplunger. 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
19、 cream. Excessive stirring and unnec-essary exposure of the latex to air must be avoided. A suitabletype of stirrer 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 d
20、istant about one quarter the height of thelatex from the bottom of the drum. The stirrer shall be operatedat a minimum 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 creatin
21、g a vortex. The part of the equipment immersedin the latex must contain no copper or brass.3.3.2 Removal of Sub-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
22、reaches the bottom ofthe container. Then close the upper end of the tube and transferthe contents to a clean, dry 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
23、 by remote control. Copperor brass must not be used in any part of its construction.3.3.3 Sample:3.3.3.1 Where sub-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 an
24、d thoroughly blended by stirringor shaking immediately before the final sample is taken.4. Total Solids4.1 Apparatus: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 dispo
25、sable aluminum liner for the metal ointment box maybe used.4.2 Procedure:4.2.1 Method AAccurately weigh a clean, 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 f
26、or 15min. Remove the aluminum foil dish from the oven and let coolin a desiccator. Reweigh the aluminum foil dish. 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
27、.1 %.4.2.2 Method BThe percent solids is determined by mea-suring gravimetrically the solids remaining after volatilizingoff 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. 1A
28、1 pansFisher #01-913-356Fiber paperFisher #01-913-318Place a glass fiber filter circle on an aluminum pan. Open 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
29、 button. Raise the lid and place about 3.0 g of latex in acircle on the filter paper. Again close the lid. Wait 10 s, thenpress the START button. The instrument will automatically runfor about 4 min then shut off. Read the percent (%) solidsdirectly from the printout paper or from the display screen
30、.Report the value to the nearest 0.1 %.4.2.3 Method CTotal solids is determined using a CEMmicrowave oven. This unit can yield accurate results in a fewminutes. For detailed operating instructions, please refer to theoperators manual.4.2.3.1 Equipment:(1) Moisture/Solid Analyzer (microwave oven).(2)
31、 Glass fiber sample pads.(3) 5 mL Disposable Pipet.4.2.3.2 ProcedurePut the pads on the balance. Tare theweight of the pads.Apply the latex sample to the pads by usingthe pipet. Spread the latex in a zig-zag pattern. Use between 1.0to 5.0 g of latex. Keep sample application as uniform aspossible to
32、maximize reproducibility. Press “Start” button andread the percent solids from the display. Record the result toone decimal place.NOTE 3An alternative method for the determination of total solids insynthetic rubber latex is described in Specification D1076.5. Volatile Unsaturates (Residual Styrene)5
33、.1 ScopeThis test method measures the residual styreneof SBR synthetic rubber latices. It is not applicable to othersynthetic rubber latices.D1417 1025.2 Apparatus:5.2.1 Iodine flasks having capacities of 250 cm3each, anddistillation apparatus with ground-glass joints.5.2.2 25-cm3pipet.5.2.3 50-cm3b
34、uret.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) and 10.0 g of potassium bromide (KBr) in water anddilute to 1000 cm3. Standardize with 0.1 N sod
35、ium thiosulfate(Na2S2O3) solution in the presence of an excess (about 3 g) ofpotassium iodide (KI) and sulfuric acid (H2SO4), (18 %).5.3.3 Sulfuric Acid Solution (18 %).5.3.4 Potassium Iodide Solution (10 %).5.3.5 Standard Sodium Thiosulfate Solution (0.1 N).5.3.6 Starch Indicator Solution.5.4 Proce
36、dure: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 synthetic methanol containing 100 ppm of p-tertiarybutyl catechol. Be sure to add the materials in the follo
37、wingorder: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 mixture. Collect the first25 cm3of distillate in a 250-cm3iodine flask, rinse thecondenser with 20 cm3of methano
38、l 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. Rapidly add 15 cm3of 18 % H2SO4solution, stopper the flask, shake it, and adddistilled water to the funnel lips as
39、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 the addition.Make the additions by drawing the standard solution from theburet into the funnel lip and lifting
40、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 bromide-bromate addi-tion, add 10 cm3of 10 % KI solution to the funnel lip, and liftthe stopper to allow the solu
41、tion 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 starch indicator solution andcontinue the titration with sodium thiosulfate solution until thesolution is clear
42、.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:Volatile unsaturates residual styrene!,%5 $D 3 E! 2 F 3 G!# 3 0.0521 3 100/M% 2 H (2)where:D = cubic centimetr
43、es 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 thiosulfate solution,H = blank determination, %, andM = mass of latex used, g.6. pH Value6.1 ApparatusAny pH e
44、lectrometer and a glass electrode-calomel cell assembly may be used as described in TestMethod E70. A flowing calomel electrode has been foundparticularly suited for this use. The glass electrode shall be ofthe type applicable for a pH range of from 2 to 14.6.2 Standard SolutionUse a standard soluti
45、on 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 properly standardized at frequent inter-vals with a standard solution (see 6.2), and that the electrodesare clean.
46、 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 distilled water. Report the pH value forthe latex at a temperature of 25 6 2C.7. Surface Tension7.1 The surfac
47、e 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 with solids as received with littleloss in accuracy.7.2 ApparatusUse a du Nouy tensiometer, carefully cali-brat
48、ed as described in Test Methods D1331.7.3 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 20 mm (0.7 to 0.8 in.) high(Note 4). The surface of the latex must be free of air bubbles,and the surface tensio
49、n 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 tensiometer 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 contact with the ring. Submerge the ringbeneath the s
