ay Designation: D 5774-95 Standard Test Methods for . Rubber From Synthetic Sources—Chemical Analysis of Extractables* ‘Thi san ctl une the Sno designation D S77; the sumer idly Bowing 0 dergntion inde the yar of. ‘iia kyon oi th cae fein, the year of fat ein. Aber pets ints fhe year of lit approval A 1. Seope 1.1 These test methods for chemical analysis of extractables from synthetic rubbers are intended for general use on solid ‘uncompounded styrene-butadiene copolymers commonly re- ferred to as SBR. Analysis of olher synthetic rubbers is also possible with some ofthese test methods, The test methods and the sections in which they are covered are as follows: Total Extroctabes on Sree ass 219 so 2025 or ae ‘Nore 1_-The nomenclature wel in thse test methods is ia accordance with Practise D 1418 12 This standard does not purport to address all of the safety concems, if any, associated with its use. It is the responsibility 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 Documents 21 ASTM Standards: D297 Test Methods for Rubber Products Analysis? D 1418 Practice for Rubber and Rubber Latie ‘Nomenclature? 1D 4483 Practice for Determining Precision for Test Method Standards in the Rubber and Carbon Black Industries? Chemical Reagents 3.1 Purity of Reagents Reagent grade chemicals shall be used in all tests. Unless otherwise indicated, itis intended that all reagens conform othe specifications of the Committee on “Analytical Reagents ofthe American Chemical Society, where such specifications are available.’ Other grades may be used, "Thirteen he juicion ASTM Commits D1 on Rubber sd the dat rponsiy of Subcom DI. o4 Chemie Aya ‘Creat ton apo Spt. 10, 195. Publis November 19, inal Book of ASTM Standard, Nl 8.0 2Rengnt Chemiain dmericn Chemea Sockey Specmons: Aman Cerin Seciey, Washington,DC. For ugpetins on he esing of ages wot ltd by the Amen Chomial Sect, se daar Sanden for Laboratry Chandos, DH L2, Fool Doe U.K ad the ted Stes Pharmacypta (ar National Formulary, US Mgreaceta Cevenio, Ine. (USPC) Roel, {)lodats an eal change sae the st revision o apm provided iti first ascertained thatthe reagent is of sufficiently high purity to permit its use without decreasing the accuracy of the determination. ‘TOTAL EXTRACTABLES 4, Summary of Test Method 4.1 Thin, narrow strips of the dried rubber are extracted three times with 100 em? of hot solvent for 10, 20, and 40-min periods, respectively. The extracted rubber is then extracted for § min in 100 cm of hot acetone to thoroughly remove the extraction solvent and aid drying of the rubber, The extracted rubber is then dried to constant mass, The difference in mass between the original sample and the extracted sample is the total extractable. 5. Significance and Use 5.1 This procedure is intended to determine the total ex- tractable materials in rubber. It will give the combined amount of rosin and fatty acids, soaps, extender oils, defoamer tars, antioxidants, and other tuncombined organic constituents that are extractable in the solvent used. The rubber hydrocarbon can be estimated by subtracting the sum of the total extract, the total ash, the volatile matter, and carbon black content (for carbon black masterbateh) from 100. 6. Apparatus (641 Wide-Mouth Flask, 400 to 500 cx? 6.2 Hot Plate and Reftuc Condenser. [Nore 2-Estrtetion apparatus in Fig. 1 of Test Methods D297 may sed, but without the exttction siphon op, 63 Filter Paper and Wire Gauze or Asbestos Mat. 64 Weighing Dish or Watch Glass. 65 Vacium Oven, capable of maintaining a temperature of 105°C and a pressure of 3.0 kPa (23 mm Hg) or k 7. Reagents 7. Solvents TAL BTA Ethanol-Toluene-Azeotrope) Prepare by mix- ing 70 volumes of ethyl alcohol and 30 volumes of toluene, refluxing the mixture for 4 h over calcium oxide and distilling. ‘iseard the first and last portions, keeping only that distillate ‘cofning over within a range of 1°C. Distilling may be omitted if absolute grain alcohol or anhydrous, formula 3A alcohol used.Qh 5774 2 HATM (Hydrous Isopropanol-Toluene Mixture) _repare by mixing 75 volumes of anhydrous isopropanol with 25 volumes of toluene and then mixing 92 volumes of this solution with 8 volumes of water. 713 Acetone, 8. Preparai 81 Dry the sample in accordance with the procedure described in 8.1.1 oF 81.2. 8.1.1. Weigh a piece of rubber (atleast 450 g) to the nearest O11 g. Pass the rubber repeatedly through a laboratory mill, with the rolls ofthe mill maintained at 100 + °C (212 = 9°F) and the distance botween the rolls at 0.25 = 0.05 mm (0,010 = 6.002 in.), as determined by a lead slug. Do mot allow the rubber to band, and take eare to prevent any loss of sample. At the end of 4 min, weigh the rubber tothe nearest 0.1 g, Pass the rubber through the mil for an additional 2 min, and reweigh it the weights atthe end of the 4 and 6-min periods are within 6.1 g, calculate the-volatile matter; ifnot, continue passing the sample thtough the mill for 2-min periods until the weight remains constant within 0.1 8.1.2 Sheet out the rubber (at least 250 g) on a laboratory rill, with the distance betwen the ros set at 0.28 * 0.05 mm (0.010 * 0.002 in), as determined by a lead slug, and the temperature of the Fell being no greater than 32°C: (90°F), Weigh the enlire sheet to the nearest O.1 g. Place in a forced-circulation oven set at 100 * S°C (212 = 9°F) so that both surfaces of the sheet are exposed to the draft. Allow the rubber to remain in the oven until the mass is constant to within 0.1 g, Usually 1 his sullicent for eubbers containing no more than 1.0% moisture 8.2 Sheet the dry polymer to a thickness of 0.5 mm (0.020 in.) oF less. Cut approximately 6 g ofthe dried, sheeted sample info strips not wider than 10 mm or Tenger than $0 mm. ion of Sample Nort 3 To ensure complete extraction ofthe ribb,the sickness of | the sheet must ot exced the prescribed maximum. © or rubber typos that dsing exration tnd 19 msss oF stick tgsthor (that is, low viscosity uber and aluny-eaagulte rubber) and freer {yp containing mata that are other dlc o slow 10 ext, {he deed shod may be ppared for extecion by one of the fllowing mmathods to capac and provide compete extaction: borsory press with ft hese platens, press 15 10 1.7 10 Semen (3.5 to 3.7m) diameter ciate of ving openings of apptoximatsy 0.177 mm 5.2 mil wite damater) or of polyester monofilament ssteen ‘loth that has boen previously exacted uth he solvent boing used, Remove any excess rab tht extends hoyond the cg of he sreo0 Accuately weigh the propated rubber and screen. Aller the tes is ‘omplcted, the wubber ean be burn elf within mle furnace snd the + inlese soe screen can be res (@) Cu S 6 g ofthe shot into squstes approximately 38 by 38 mm (ES by 15 in) and weigh between two 30 mm (2 in) squares of polypropylene seen that previously ns boon extras in the salve Ping we “A sual see spate monaflanttsewen cla syle PES212HC, 14120 mesh Alb from Cars Far Sap S581 Mose, Houston, TX nurs. > A ible cen with 0.84 mm sare opengs ed 025 me dancer wie an i press rm Southern Fran apt Madi Co, PO Box 2, Aug, GA, ‘de th dxgaston of 24 by 24 ek, Vs uns pels, 1 ni arte ‘cen polypropylene cen. gh 6 g of the dried rubber strips 9.2 \Add 100 em? bf the chosen solvent (ETA or 1-ITM) to the extraction flask, and add each strip of the weighed polymer separately to the flask, swirling the flask after each addition so that eaeh strip is thoroughly wetted with solvent 0 avoid sticking. To prevent the sample from sticking to the flask, a filter paper may be placed inthe bottom of the flask and a wire ‘gauze or asbestos mat may be placed on the het plate under the ask. Sample preparation, as described in Note 3 (a) or (b) also ‘may be used, ifonly the total exiratables are to be determined, 9.3 Reflux the contents of the flask on the hot plate for at Jeast 10 mip (1 h max), Decant the solvent, rinse the rubber with 20 cm? of fresh solvent, and add 100 em of fresh solvent to the flask 9.4 Reflux the contents of the flask on the hot plate for at Yeast 20 min (1h max). Again decant the solvent, rinse the ‘rubber with 20 em? of fresh solvent, and add 100 em? of fresh solvent to the flask. 9.5 Reflux the contents of the flask on the hot plate for at feast 40 min (1 h max), Again devant the solvent, and then add 100 em of acetone to the flask, 9.6 Reflux again for $ min to remove the extraction solvent from the rubber. Decant and diseard the aectone solution 9.7 ‘Transfer the extracted rubber to a tared weighing dish, Place the dish in a vacuum oven and dry for 1 hat 10S = 3°C ‘and a pressure not greater than 3.0 kPa (23 mm Hg). Reweigh the dried rubber. 10, Caleutation 10.1 Calculate the percentage of total extractables as fol- lows: “Tota eae, % » [L004 ~ By} o where: A= mass of the original dry sample, g, and B= muss of the extracted dried sample, ¢ 11, Precision and Bias © 1.1 The precision results for these test methods were originally derived from an interlaboratory test program (ITP) conducted prior to the adoption of Practice [4483 as the reference precision standard for Committee D-1 test methods and therefore was not conducted according to the guidelines set forth in Practice D 4483. Ilowever, the results of that ITP have been translated into Practice D'4483 precision expression format and are given in this soction. See Practice 1 4483 for terminology and other statistical ealeulation details. 11.2 The precision results in this precision and bias section give an estimate of the precision of the test method with the ‘materials used in the particular TTP as deseribed in 1.3. The precision parameters should not he used for acceptance oF rejection testing of any group of materials without documentation that they are applicable to those materials and the specific testing protocols of the test method * Sepponing sar slabs fom ASTM Headutran, Roget RR: DII-b 5774 + The Type 1 precision is based on a program that -aployed three materials (ubbers), With tests on each of two ays by eight laboratories. A test result is the average of Wo eterminations. The precision data are given in Table 1 11.4 Bias isthe dillerence between an average test value and the reference (true) test property value. Reference values do hot exist for this test method; therefore, bias cannot be evaluated ORGANIC ACID 12, Summary of Test Method 12. Thin marrow strips of the dried rubber prepared as described in 8.1 and 8.2 are accurately weighed to Secure about 6 g. The polymer strips are extracted twice in hot extraction solvent, The solvent extacis and rinsings are combined in a 250-cm’ volumetric flask and made up to volume with fresh solvent. A 100-cm’ portion ofthe extract solution is titrated to the first eolor change with 0.1 M NaOH solution, using the chosen indicator. The tiation and sample mass are used to calculate the organic acid 13, Significance and Use 13.1 This procedure is intended to determine the organic acid remaining in a synthetic rubber. There are Wvo test methods: B for alum-coagulated polymers, and A forall others. While these procedures were developed for emulsion SBR, they may be applicable to other emulsion polymers, Organic acid in the polymer may affect cure rate of compounded stock, 14. Apparatus 14.1 Bpical Laboratory Apparatus. 15, Reagents 15.1 Solvents: 15.1.1 Ethanol Toluene-Azeotrope (ETA See 7.1.1. Not applicable when testing alum-coagulsted polymers. 15.1.2 Alternative Extraction Solvent—Ilydrous Isopropanol-Toluene Mixture (H-ITM) See 7.1.2. U-TTM is applicable to all polymers, and especially the alum-coagulated polymers. 15.2 Indicator Solutions: = 152.1 Meta-Creso! Purple Indicator Solution (0.1%), in ‘thyl alcohol or in water. Neutralize each 0.1 g of indicator in the solution with 26.2 em! of 001 M NaOH solution before diluting to volume, Store the indicator solution in a brown TABLE 1 Type 1 Precision for Total Extractablos Wawa Non SOR Noe 200s 01? ost 108 om 129 No 324s 082 0232 072 O488 13041 Noa ars oia2 oa om 02 O82 206 rerage 2409 04M O5t4 092 05% os1 29 75, = epelaily sandra evan, MESSE UN 7 repetaitymmaasuromere units, (9 ropes (ana) pron, ‘Se = rears standard devaton, n messrement unt, R= eproaucbityh messirement uns, 26 (f= rprosucuy (lave) poem bottle out of contact with fluorescent lighis, which will eause the solution to deteriorate 18.22 Thymol Blue Indicator Solution (0.2 %)—Dissolve 0.06 g of indicator in 6.45 em’ of 0.02 M aqueous NaOH and dilute to 50 cm? with distilled water. (Recommended for use with H-ITM extracts) 15.3 Sodium Hydroxide Standard Solution (0.1 M)— Prepare and standardize a 0.10 M solution of sodium hydroxide (a01. 16, Preparation of Sample 16.1 Prepare a sample in accordance with 8.1 and 8.2. 17. Procedures 171 est Method A Non-Alum-Coagulated Polymers 17-1 Weigh a6 spesimen of the died rubber strips to the rarest 1 mg. 17.1.2 Add 100 em of the chosen solvent (15.1) 10 the extraction flask and add each stip of the separately to the flask. Suiel the flask after each addition so that cach strip is thoroughly wetted with solvent to avoid sticking. To prevent the sample fiom sticking tothe Mask, a filter paper may be placed in the bottom ofthe flask, and a wire gauze or asbestos mat may be pled on the ot plate under the flask. Sample preparation, as deseribed in Note 4(0), also may bo used 17:13 Reflux the contents ofthe Nask on the hot plate for a least 10 min (I'b, max). Decant the solvent into a 250-cm° volumetric flask, rinse the sample with 20 em? of fresh solvent, ‘adding the rinsing tothe ask, Add 100 em’ of fresh solvent to the extraction flask 17.14 Reflux the contents ofthe fask onthe hot plate for at teast 20 min (Ib, max). Again devant the solvent inte the Volumetric ask and rinse the sample with 20 em’ of fresh solver, adding the ritsing to the flask. Cool the extract Soltion to room temperature and add enough fresh solvent to bring the volume to 250 em". Mix the solution thoroughly. 17.1.5 With a pipet, measure two 100-em" portions of the extract solution into 250-em’ Erlenmeyer flasks. Save one 100-cm’ portion for dhe soap determination (Sections 20-26) 17.1.6 To a one 100-em? portion of the extract solution, add six drops ofthe ehosen indicator solution. Titra the solution with 0.1 M NaOH solution to the first eolor change, Run a blank titration using 100 em? of fresh extraction solvent that has been treated in the sume manner as the sample solution and using the same type and amount of indicator, Deduct the ‘volume of NaOH solution required forthe blank from that used for the sample titration, 172 Test Method B—Alum-Congulated Polymers: 172.1 Accurately weigh a -g sample of the dried rubber strips 17.2.2 Add 100 em? of the TEITM solvent (9.1.2) to the extraction flask, (ITM should be used for alum-coagulated polymers.) Add each strip of the weighed sample that has been prepared in accordance with Note 3 to the flask. To prevent the sample from sticking to the flask, filter paper may be placed in the bottom of the flask anda wire gauze or asbestos mat may bbe placed on the hot plate under the flask 1723 Reflux the contents ofthe Nask on the hotplate for at~- Gh D574 40 min (1h, max), Decant the solvent into a 250-cm? columetrie flask, Rinse the sample with 20 em? of fresh Solvent, adding the rinsing to the Mask.Add 100 em" of fresh solvent to the extraction flask. 17.24 Rellux the contents of the flask on the hotplate for at least 20 min (1h, max). Again decant the solvent into the volumetric flask and rinse the sample with 20 em’ of fresh solvent, adding the rinsing to the Mask. Cool the extract Solution to room temperature and add enough fresh solvent to boring the volume to 250 em’. Mix the solution thoroughly. 172.5 Add 100 em? of fresh solvent tothe extraction flask; Reflux the contents ofthe flask on the hot plate for at least 15 min (1b, max). Decant the solvent into a 250-em* Erleameyer flask and rinse the sample with 20 em! of fresh solvent, adding the rinsing to the flask, Save this extract solution as Supplement Extraction No. 1 17.2.6 Add 100 em? of fresh solvent tothe extraction flask Reflux the contents ofthe flask on the hot plate for at least 15 ‘min (1 h, max), Decant the solvent into a 250-em? Erlenmeyer tesk andl inse the sample with 20 em’ of fresh solvent, adding the rinsing to the flask. Save this extract solution as Supplement Extraction No. 2. 172.7 With a pipet, measure a 100-m? portion of the extract solution as deseribed in 17.24 into a 250-cm* Exlenmeyer flask. 17.28 ‘Tothe 100-em' portion of the extract solution and the supplement extractions (ftal amount), add six drops of the Chosen indicator solytion. Titrate the three solutions individually with 0.1 M)NaOH solution to the first color ‘change. Runa blank titration sing 100 em’ of fresh extraction Solvent that has been treated in the sume manner asthe sample Solution and using the same type and amount of indicator. Deduct the volume of NaOH solution required for the blank from that used for each of the sample titrations. Now 4 Ifthe poscsnt ae in the No. supplement st tos than 0.1% calculated on the onginal sample mass, un a adional supplement extraction as desenibsd in 1726. 18, Calculation 18.1 Test Method A—Caleulate the percentage of organic acid as follows: WS PRK KL O28)A eo Ores where: Jy Volume of NaOH solution used for titration (corrected for blank), em’, K = molanity of standard NaOH solution, L determined; it y 5 1 values: 284 for ss 15 for $0 + SO mixture 4 mass of original dry sample, z 18.2 Test Method B Calculate the percentage of organic acid as follows: KXLK02S o where JF = volume of NAOH solution used for titration of 100- portion of 250-cm' solution (corrected for blank), em, molarity of standard NaOH solution, equivalent mass of organic acid determined: if ‘unknown, use the Following typical values: 284 for stearic acid, 346 for rosin aeid, 315 for $0 + 50 mixture of stearic and rosin acids, mass of original dry sample, 8, Volume of NaOH! solution used for titration of entire volume of Supplement Extraction No. 1 (corrected for blank), em’, and Y= volume of NaOH solution used for titration of entire volume of Supplement Extraction No. 2 (corrected for blank), em. 19, Precision and Bias ® 19.1 This procision and bias section has been prepared in ordance with Practice I 4483, Refer to Practice D 4483 for terminology and other statistical caleulation details 19.2 ‘The precision resulis in this precision ane bias section sive an estimate of the precision of this test method with the materials (rubbers) used inthe particular interlaboratory program as described in 19.3, The precision parameters should pt be used for aeveplance or rejection testing of any group of ‘materials without documentation that they are applicable to those particular materials and the specific testing protocols that include this test method. 193 A Type | (interlaboratory) precision was evaluated. Both repeatability and reprodueibility are short term; a period of a few days separates replicate test results, A test result is the average value, a3 specified by ths test method, obtained on two tleiermination(s) of measurement(s). Four different materials ‘wore used in the interlaboratory program: these were tested in cight laboratories on two different days. 19.4 The results of the precision calculations for repeatability and reproducibility are given in Table 2 in fsconding order of material average or level For each of the ‘materials evaluated 19.5 The precision of this test method may be expressed in the format of the following statements whieh use an lappropriate value of 7 R, (7), oF (R), to be used in decisions about test results, The appropriate value is that value of ror R fssociated with a mean level in Table 2 closest to the mean evel under consideration at any given time for any giver ‘material in routine testing operations TABLE 2 Type 1 Precision for Organic Acid—Test Methods A and ot Geape NT Tabraoaes Between Labores tel eR Toe aa Omer orm 400080 ORS 7H NSS Ss oeest O16 33 OMS O41 BS NSE G58 Soaae cae 37 oat ose 88 N53 99 oor ote 4002 _osts_ 103 7s, = repent anci dvato, hr measoreren uns 1 captain meas unk, {oS tapout (oistve) perce. o. teprotcty sandare savin, n reaseranent us, = reproduc, 9 measurorert unis and (ro mero (lne) percent atonalMh D 5774 : ~ See 26,6 through 26.9 for repeatability statements as -xpressed in Table 2 : SOAP 20, Summary of Test Method 20.1 One of the 100m’ portions of solvent extract remaining from the organic acid test deseribed in 17.1.5 is, titrated with 0.05 Af TCI, using the chosen indicator to the ist ‘color change. From the weight of the original sample strips and the titrations, the percentage of soap is calculated 21. Significance and Use 21.1 This procedure is intended 10 determine the organic soap in an emulsion polymer. That soap is a by-product of the temilsion process; it may affect the cure rate of compounded stock. While this procedure was originally developed for ‘emulsion SBR, it may be applicable to other polymers. 22. Reagents 2.1 Hydrochloric Acid, Standard (0.05 M). 2 Indicator Solutions: 1 Meta Cresol Purple Indicator Solution (0.1 %). Ses 152.1 2.2.2 Bromophenol Blue Indicator Sohuion (0.1%), in «thy! aleohol. Bromothymol Blue Indicator Sotution (0.1%), in ethyl alcohol. 2.2.4 Tiymol Blue Indicator Solution. See (recommended for use with ILITM extracts), 15.2.2 23, Preparation of Sample 23.1 Prepare the sample in accordance with 8.1 and 8.2 and determine the percentage soap on a portion of the solvent ‘extract remaining from the test for organic acid (17.1.5). 24, Procedure 24.1 Add six drops of the chosen indicator solution to the 100 cm of extract solution saved from the organic acid test (Q7.1.5). Titrate the solution with 0.05 A/1ICLto the first color ‘change. Runa blank titration, using 100 em’ of fresh extraction ‘solvent that has been treated in the same manner as the sample (17.12 10 17.15), and using the same amount of indicator (Note §). Deduct the volume of HCI used for the blank from that used for the sample. Now 5 of the analyst. Whichever indicator solution gives the clearest, most Aisemible end-point for the ype sample being esta should be used “Thymol Blue has been recommended for use with TLITM exits 25. Calculation 25.1 Calculate the percentage of soap as follows: Sap, 6 = (MANX P 028A ® where M-= volume of standard HCI used for tration (corre = for blank), em’, N= molarity of standard HCl, P equivalent weight. of scant: ifunknown, use the following typical valuee 306 for sodium steara 322 for potassium stearate, 368 for sodium rosinate, 384 for potassium rosie, 337 for $0-+ $0 mixture of soulum stearate and sodium rosnate, 383 for $0 1 50 mixture of potassium stearate and potas eosinate, 343 for 50-450. mixture of sodium; Searle and Potassium rosinale‘or potassium Steaaté sind sodium rosinate, and *y 8 SF A = mas of original dey sample, g 26, Precision and Bias © 7 26.1 This precision and bias section ins been prepared in’ ‘accordance with Practice D 4483. Refer to Practice D 4483 for terminology and other statistical ealeulation details. : 262 ‘The precision results in this precision and biaé section | ive an estimate of the precision of this test method with the materials (cubbers) used in the particular interlaboratory program as deseribed in 26.3. The precision parameters should not be used for acceptance or rejection testing of any group of ‘materials without documentation that they are applicable to those particular materials and the specific testing protocols that include this test method. 263 A Type 1 (interlaboratory) precision was evaluated, Both repeatability and reproducibility are short term, a period ‘of a few days separates replicate test results. A test resull is the average value, as specified by this test method, obtained on two ‘determination(s) or measurements). Four different materials (rubbers) were used in the interlaboratory program; these were tested in eight laboratories on two different days. 264 The results of the precision calculations for repeatability and reproducibility are given in Table 3, in ascending order of material average or level, for each of the ‘materials evaluated. 26.5 The precision of this test method may be expressed in the format of the following statements which use an appropriate value of rR, (r), oF (R), to be used in decisions about test results. The appropriate value is that value of ror R associated with a mean Jevel in Table 3 closest to the mean level under consideration at any given time for any given ‘material in routine testing operations. 26.6 Repeatability —The repeatability, , ofthis test method has been established as the appropriate value tabulated in Table 3. Two single test results oblained under normal test method procedures that differ by more than this tabulated r (for any ‘TABLE 3 Type 1 Precision for Soap Betwoon taboos away Rego __ Wi Casio Une Sr Se RR Nes OGM Gong 0a] SAT ooNe oar -900 Nod 8018 90086 0188 220 OosIS casey G00 Nas 9019 Soom oozes 1090 008% Goeza 400 Nes 0036 00007 027s 75300625 0177 _ 4900 7s, ~ repasabiy, sansa devise, in es5uFTer wis 7 repel. moasureen unt, (9 = repoaatiy, ola) pon 5, = epeductiy, slanard dev, measurement uns = reproduc In messuemor uns, Sra (fe) repost, tate parent.Qh p s774 + level) must be considered as derived from different or ‘nonidentical sample populations. 267 Reproducibility—The reproducibility, R, of this test ‘method has been established as the appropriate value tabulated in Table 3. Two single test results obtained in two different laboratories under normal test method procedures tht differ by ‘more than the tabulated R (for any given level) must be ‘considered to have come {rom different or nonidentical sample populations. 26.8 Repeatability and reproducibility expressed asa percent of the mean level, (r) and (R), have equivalent application statements as in 26.6 and 26.7 for r and R. For the (7) and (R) statements, the difference in the two single test resulls is expressed as a percent ofthe arithmetic mean of the to test results, As is usual with the analysis of materials that are present in low concentrations, the relative repeatability and reprodueibility are high. 26.9 Bias—In- test method terminology, bias is the difference between an average test value and the reference (oF true) test property value. Reference values do not exist for this test method since the value (of the test property) is exclusively defined by the test method. Bias, therefore, cannot be determined, oO. Test Method A 27. Summary of Test Method 27.1 The Total Extractables of the dried rubber is determined in accordance with Sections 4 through 11. The eil content ofthe sample is estimated by subtracting from the Total Extractables a correction value that is the total of the major extractable constituents ofthe particular type being tested other than the oil. The difference is an estimate ofthe eil content, 28. Significance und Use 28.1 This test method covers the estimation of oil content of cilextended polymers and carbon black masterbatches, It intended for use in checking the uniformity of shipments, While this method was developed for emulsion SBR, it may be applicable to other polymers and earhon black masterbatches, 29. Apparatus 20.1 See Section 6. 30, Reagents 31. Preparation of Sample 31M See 33. Caleulation 33.1 Calculate the percentage of oil as follows: Oikconteat.% = (10014 — id] C+D) ner: ‘mass of the original dry sample, g, ‘mass of extracted sample, g, ‘organic acid, % soap, %, antioxidanVantiozonant, %. If antioxidanvantiozonant cannot be determined, the following value may be calculated: 4 1 B ie D D= Us) x 100 © where: ‘nominal antioxidant added to rubber, phr, and ‘masterbatch recipe, in parts = 100+ phr of oil + phr of ‘carbon black. 34. Precision 34.1. Repeatability Duplicate results by the same operator should not be considered suspect unless they differ by more than 0.28 %. Nore 6—Altbough the ropentobility and wspoduciility of this tet mathod ate good, the accuracy deponds onthe aearaey ofthe analysis of {ci Soup, and antioxidant antozonan 34.2 Reproducibility Results submitted by each of wo laboratories should not be considered suspect unless the (Wo results differ by more than 0.34 % (Note 6). 343 The precision of the H-ITM test method is being uated, Test Method B (Quick) 35. Summary of Test Method 35.1 The Total Extractables of the rubber are determined by extracting a 1-g sample in the chosen solvent and then in acetone and drying the extracted rubber. The oil content is estimated by subtracting from the total extract a correction value that isan average of the major extractable constituents of the particular type being tested other than the il. This difference is an estimate of the oil content. 36, Significance and Use 36.1 Test Method B is an altemative quick test method for estimating the oil content of oil-oxtended SBR type polymers (oil masterbatches) and oil-black masterbatches of SBR polymers. This test method is intended for use as a quick test ‘method for determining the total extract of a rubber simple for estimation of oil content where other constituents of the sample may be determined or where their normal average values are this method was developed for emulsion SBR, it plicable to other polymers and carbon black smasterhatches. 37. Apparatus 37.1 See 6.1 through 6.4. 37.2 Convection Oven, 130 + 3°C (266 + S°F). 38. Reagents 38.1 See Section 7. 39, Preparation of Sample 39.1 Prepare the sample in accordance with the probb 5774. -abed in Section 8. 40, Procedure 40.1 Accurately weigh a L-g sample of the dried strips. 40.2 Add 150 cm? of the chosen solvent to the 400 em? extract flask and add each strip of the weighed sample separately to the flask. Swirl the flask after each addition s0 that each strip is thoroughly. wetted with solvent to avoid sticking 40.3. Reflux the sample at least 10 min (1, max) on the hot plate, Decant and discard the solvent and rinse the sample with 10 em’ of fresh solvent. Decant and discard the rinse solvent 40.4 Add 150 em’ of acetone to the flask and reflux for 15 ‘min on the hot plate. Decant and diseard the acetone. 40.5 Transfer the extracted sample toa tared weighing dish Day the sample for 15 min or o constant mass in 8 conv drying oven at 130 + 3°C (266 = S*F), 41. Calculation 41.1 See Seotion 33, 42, Procision 42.1 Precision of this test method his not been determined. 43, Keywords 43.1 extractables; oil; erganie acid; soap ‘To Amaran Soc Testing and Male takes ro positon respecting the ayo any pater assed coneston ith any ten mented i Os standard Uses of 9s Sandal ae expressly advsed Bat eerialn of ak ay Sic) Date es, and raking such MHS, ae celia oh rapes ‘Tn sana is suet oreson at any tie by the response lechncal commits and must be evewed eve We ears and Ite! roised eter aareroved or winan Yer comments are Miedo ese o hs sandr rasan anaes ‘td shad be sucesso 0 AST Heacurs. You conmearts i fcav crf contest a 9 ooing oe fospane Tecra! cormilen ich yo may aon. Fy fel at your contents have mt rca 3 athena YOU SROUE Ma YU ‘ows noun tn ASTM Commitos en Standards, 100 Bar Harbor Dv, Wes! Conshovokan, PA T9428,