1、Designation: D1417 10D1417 16Standard 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 parenth
2、eses 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 synthetic rubber laticesABR, BR, CR, IIR, IR, NBR, NCR, NIR, PBR, PSBR,SBR, SCR, SIR, synthetic rubber lati
3、ces having substitute carboxylic acid (COOH) groups on the polymer chain (X), and syntheticrubber latices that are reinforced (Y). Exceptions to the above are noted in the individual test procedures. The test methods includeprocedures for sampling, and for determining total solids, volatile unsatura
4、tes (residual styrene), pH value, surface tension,viscosity, coagulum, bound styrene, Mooney viscosity, mechanical stability, polystyrene reinforcement in contained polymer, andresidual acrylonitrile content.NOTE 1The nomenclature used in these test methods is in accordance with Practice D1418.1.2 T
5、he values stated in SI units are to be regarded as standard.1.3 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibilityof the user of this standard to establish appropriate safety and health practices and determine the applicabi
6、lity of regulatorylimitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D1076 Specification for RubberConcentrated, Ammonia Preserved, Creamed, and Centrifuged Natural LatexD1331 Test Methods for Surface and Interfacial Tension of Solutions of Paints, Solvents, Solutions of Surface-Act
7、ive Agents,and Related MaterialsD1416 Test Methods for Rubber from Synthetic SourcesChemical Analysis (Withdrawn 1996)3D1418 Practice for Rubber and Rubber LaticesNomenclatureD1646 Test Methods for RubberViscosity, Stress Relaxation, and Pre-Vulcanization Characteristics (Mooney Viscometer)D3182 Pra
8、ctice for RubberMaterials, Equipment, and Procedures for Mixing Standard Compounds and Preparing StandardVulcanized SheetsD3314 Test Method for RubberChemical Analysis for Polystyrene Blocks In SBR (Styrene-Butadiene Rubber) andStyrene-Reinforced LaticesD4483 Practice for Evaluating Precision for Te
9、st Method Standards in the Rubber and Carbon Black Manufacturing IndustriesD6204 Test Method for RubberMeasurement of Unvulcanized Rheological Properties Using Rotorless Shear RheometersE70 Test Method for pH of Aqueous Solutions With the Glass ElectrodeE200 Practice for Preparation, Standardization
10、, and Storage of Standard and Reagent Solutions for Chemical AnalysisE1970 Practice for Statistical Treatment of Thermoanalytical DataE2975 Test Method for Calibration of Concentric Cylinder Rotational Viscometers3. Sampling3.1 Rubber latex tends to cream on standing. Once stratification has occurre
11、d, the latex must be thoroughly agitated to obtaina homogeneous blend as a representative sub-sample. The procedure required differs with the type of container and facilitiesavailable.3.2 Sub-Sampling from Tank Cars:1 These test methods are under the jurisdiction of ASTM Committee D11 on Rubber and
12、are the direct responsibility of Subcommittee D11.23 on Synthetic Rubbers.Current edition approved March 1, 2010June 1, 2016. Published April 2010June 2016. Originally approved in 1956. Last previous edition approved in 20032010 asD1417 03a.D1417 10. DOI: 10.1520/D1417-10.10.1520/D1417-16.2 For refe
13、rencedASTM standards, 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.3 The last approved version of this historical standard is referenced o
14、n www.astm.org.This document is not an ASTM standard and is intended only to provide the user of an ASTM 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 co
15、nsult prior editions as appropriate. In all cases only the current versionof the standard as published by ASTM is to be considered the official document.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States13.2.1 If stratification has occur
16、red, take separate samples about 75 mm (3 in.) from the top surface and about 75 mm from thebottom of the tank. If results from the top and bottom samples do not agree within 1 % total solids, the contents of the car shallbe thoroughly agitated until samples obtained do agree within this tolerance.3
17、.3 Sub-Sampling from Drums:3.3.1 BlendingThe latex shall be blended by one of the following test methods:3.3.1.1 Test Method AIf the drum is fitted with a bung and contains at least 2 % air space, lay it on its side and roll back andforth briskly for not less than 10 min. Then turn the drum upside d
18、own 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 vessel and thoroughly stir,preferably by means of a perforated steel disk plunger. Stirring for about 10 min will normally suffice. If the dr
19、um is of theopen-head type, remove the end head and thoroughly stir the contents, preferably by means of a perforated steel disk plunger.Stirring for about 10 min will normally suffice.3.3.1.2 Test Method BAgitate the contents of the drum by means of a suitable motor-driven stirrer for as long as is
20、 necessaryto disperse the cream. Excessive stirring and unnecessary exposure of the latex to air must be avoided. A suitable type of stirrerconsists of a collapsible two-bladed stainless steel propeller of 11 cm minimum diameter, when fully opened, mounted on astainless steel shaft sufficiently long
21、 for the propeller to be distant about one quarter the height of the latex from the bottom of thedrum. The stirrer shall be operated at a minimum speed of 900 r/min. If desired, two propellers may be used on the same shaft,the lower one being near the end of the shaft. The shaft speed shall give a b
22、risk turnover without creating a vortex. The part ofthe equipment immersed in the latex must contain no copper or brass.3.3.2 Removal of Sub-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 an
23、d open at both ends until it reaches the bottom of the container. Thenclose the upper end of the tube and transfer the contents to a clean, dry sample bottle. Repeat the operation until sufficient latexhas been obtained.NOTE 2Alternatively, a specially constructed metal sampling tube may be used, th
24、e bottom of which can be closed by remote control. Copper or brassmust not be used in any part of its construction.3.3.3 Sample:3.3.3.1 Where sub-samples are drawn from several containers, for example, 10 % sampling of latex in drums, or where takenat different depths, for example from tanks, the su
25、b-samples shall be combined and thoroughly blended by stirring or shakingimmediately before the final sample is taken.4. Total Solids4.1 Apparatus:4.1.1 Tared, covered, all-metal ointment boxes, having a capacity of approximately 50 to 60 cm3, a minimum diameter of 38mm (1.5 in.), and a maximum heig
26、ht of 23 mm (0.9 in.). The disposable aluminum liner for the metal ointment box may be used.4.2 Procedure:TABLE 1 Drying Time for Determination of Total Solids in Latex(Drying Aid, 1 cm3 of distilled water.)Type of Latex Drying Time, minSBR 2000 45SBR 2001 45SBR 2002 45SBR 2003 45BR 2004 45SBR 2005
27、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 45D1417 1624.2.1 Method AAccurately weigh a clean, dry aluminum foil dish. Record the weight. Measure 2 m
28、L of sample and put in thealuminum foil dish. Reweigh the dish and record the weight. Put the aluminum foil dish in a 170C oven; heat for 15 min. Removethe aluminum foil dish from the oven and let cool in a desiccator. Reweigh the aluminum foil dish. Record the weight. Calculations:A = weight of dis
29、h empty; B = weight of dish + sample; C = weight of dish + residue;C2A!100!B2A! 5%Total Solids (1)Report the total solids to the nearest 0.1 %.4.2.2 Method BThe percent solids is determined by measuring gravimetrically the solids remaining after volatilizing off theliquid portion.4.2.2.1 Instrument
30、ConditionsThe following instrument conditions 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 the lid of the IR-100 and center the pan (with fil
31、ter) between the fourprongs of the“ X”-shaped holder. Close the lid and press the START button. When display reads “tare pan,” press the TARE button.Raise the lid and place about 3.0 g of latex in a circle on the filter paper. Again close the lid. Wait 10 s, then press the STARTbutton. The instrumen
32、t will automatically run for about 4 min then shut off. Read the percent (%) solids directly from the printoutpaper or from the display screen. Report the value to the nearest 0.1 %.4.2.3 Method CTotal solids is determined using a CEM microwave oven. This unit can yield accurate results in a few min
33、utes.For detailed operating instructions, please refer to the operators manual.4.2.3.1 Equipment:(1) Moisture/Solid Analyzer (microwave oven).(2) Glass fiber sample pads.(3) 5 mL Disposable Pipet.4.2.3.2 ProcedurePut the pads on the balance. Tare the weight of the pads. Apply the latex sample to the
34、 pads by using thepipet. Spread the latex in a zig-zag pattern. Use between 1.0 to 5.0 g of latex. Keep sample application as uniform as possible tomaximize reproducibility. Press “Start” button and read the percent solids from the display. Record the result to one decimal place.NOTE 3An alternative
35、 method for the determination of total solids in synthetic rubber latex is described in Specification D1076.5. Volatile Unsaturates (Residual Styrene)5.1 ScopeThis test method measures the residual styrene of SBR synthetic rubber latices. It is not applicable to other syntheticrubber latices.5.2 App
36、aratus:5.2.1 Iodine flasks having capacities of 250 cm3 each, and distillation apparatus with ground-glass joints.5.2.2 25-cm3 pipet.5.2.3 50-cm3 buret.5.3 Reagents:5.3.1 Synthetic Methanol, containing 100 ppm of p-tertiary butyl catechol.5.3.2 Standard Potassium Bromide-Potassium Bromate Solution (
37、0.1 N)Dissolve 2.784 g of potassium bromate (KBrO3) and10.0 g of potassium bromide (KBr) in water and dilute to 1000 cm3. Standardize with 0.1 N sodium thiosulfate (Na2S2O3) solutionin the presence of an excess (about 3 g) of potassium iodide (KI) and sulfuric acid (H2SO4), (18 %).5.3.3 Sulfuric Aci
38、d 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 Procedure:5.4.1 Weigh approximately 25 g of the latex to the nearest 0.1 g in a tared, covered, 250-cm3 iodine flask. Remove the coverand add 25 cm3 of dist
39、illed water to the iodine flask. Add 25 cm3 of synthetic methanol containing 100 ppm of p-tertiary butylcatechol. Be sure to add the materials in the following order:1. Latex.2. Distilled water.3. Methanol containing p-tertiary butyl catechol.5.4.2 Connect the iodine flask to the distillation appara
40、tus with ground-glass joints and distill the mixture. Collect the first 25cm3 of distillate in a 250-cm3 iodine flask, rinse the condenser with 20 cm3 of methanol containing 100 ppm of p-tertiary butylcatechol, and add the rinsings to the recovery flask.D1417 1635.4.3 From a buret add 20 cm3 of 0.1
41、N standard KBr-KBrO3 solution. Cool the solution to 30 C. Rapidly add 15 cm3 of 18 %H2SO4 solution, stopper the flask, shake it, and add distilled water to the funnel lips as a vapor seal. Allow the bottle to stand for60 s. If no yellow color remains, add successive 10-cm3 portions of the bromide-br
42、omate solution until a slight yellow colorpersists for 60 s after the addition. Make the additions by drawing the standard solution from the buret into the funnel lip and liftingthe stopper so that the solution enters the flask around the stopper. Wash the funnel lip with distilled water in the same
43、 mannerand seal with water.After 60 s has elapsed since the final bromide-bromate addition, add 10 cm3 of 10 % KI solution to the funnellip, and lift the stopper to allow the solution to enter the flask around the stopper. Shake the bottle and contents and titrate theliberated iodine with 0.1 N stan
44、dard sodium thiosulfate solution to a faint yellow color.Add 1 cm3 of starch indicator solution andcontinue the titration with sodium thiosulfate solution until the solution is clear.5.4.3.1 For a blank determination, repeat the procedure using distilled water instead of latex.5.5 CalculationCalcula
45、te the percentage of volatile unsaturates (residual styrene) as follows:Volatile unsaturates residual styrene!,% (2)5$D 3E! 2F 3G!# 30.05213100/M% 2Hwhere:D = cubic centimetres of standard bromide-bromate solution used,E = normality of the bromide-bromate solution,F = cubic centimetres of standard t
46、hiosulfate solution used for the titration,G = normality of the thiosulfate 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 inTest Method E70.A flowing calomel electrode
47、 has been found particularly suited for this use. The glass electrode shall be of the type applicable fora pH range of from 2 to 14.6.2 Standard SolutionUse a standard solution having a pH of 10 or a standard solution having a pH approximately the sameas that of the latex to be tested.6.3 ProcedureB
48、efore 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 latex to come to equilibrium with the glass electrodebefore taking the final reading. After the pH determination
49、has been made, clean the electrodes thoroughly and immerse them indistilled water. Report the pH value for the latex at a temperature of 25 6 2C.7. Surface Tension7.1 The surface tension of styrene-butadiene rubber latex shall be determined on the total solids of 40 6 1 %. If the viscosityis below 200 mPas (200 cP) on No. 1 spindle at 20 r/min, the latex can be tested with solids as received with little loss in accuracy.7.2 ApparatusUse a du Nouy tensiometer, carefully calibrated as described in Test Methods D1331.7.3 ProcedureStra
