Ally Designation: D 2765 —01 sutt Standard Test Methods for Determination of Gel Content and Swell Ratio of Crosslinked Ethylene Plastics* “Tie smd is ued unde the fed designation D2 ial aoption 8 the number edit flloning he desipmaion inden the year of eee of ein the yar of st revision. Amber in premees dete Be yea of nt eal A ‘pct pin (fainter an etal change sae the la evn or epoa 1. Scope 1.1 The gel content (insoluble fraction) produced in ethyl- ene plasties by erasslinking can be determined by extracting. with solvents such as degahydronaphthatene or xylenes. Such extraction test methods are described herein. They are appli- cable to crosslinked ethylene plastics of all densities, including “hose containing filles, and all provide corrections for the inert fillers present in some of those compounds. 1.2 Test Method A, which permits most complete extraction in least time, is to be used for referee tess, but two alternative nonreferee Test Methods B and C are also described. The first ‘of these differs from the referee test method only in sample” preparation; that is, it requires use of shavings taken at selected points in eable insulation, for example, rather than the ground ‘sample required by the referee test method. Because the shaved particles ate larger, less total surface per sample is exposed to the extractant, So this test method ordinatly yields extraction values about | to 2% lower than the referee method, The second of the altemative test methods requires that a specimen in one piece be extracted in xylenes at @ constant temperature of 110°C. At this temperature and with a one-piece specimen, even less extraction oceurs (from 3 to 9 % tess than the referee test method) but swell ratio (a measure of the degree of crosslinking in the gel phase) can be determined. 13 Extraction tests can be made on articles of any shape. They have been particularly useful for electrical insulations since specimens may be selected from those portions of the ‘ngulation most susceptible to insuflicient crosslinking. 1.4 The values stated in St units are to be regarded as the standard, The inel-pound units in parentheses are for informa tion only. [Nore {180 1UIAT i similar to this tex, but isnot equivalent, 15 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard 10 establish appro priate safety and health practices and determine the applica- "These tent mete are ener the junedition af ASTI Commitee D20 on ‘iar nd ae diet repent of Sabeonmiee 02015 on Themoplase Matis ‘Cure eon aproved June 10,2001, Published August 2001 Origa published as D27ES G8, Last previous edition D 2765 95 bili of regulatory limitations prior 10 wse. Specific precau- tionary statements are given in Seetions 6, 10, and 25. 2, Referenced Documents 2A ASTH Standards: D297 Test Methods for Rubber Products—Chemical Analysis* D618 Practice for Conditioning Plastics and Electrical Insulating Materials for Testing’ D883 Terininology Relating to Plastics’ 1D 1603 Test Method for Carbon Black in Olefin Plates? D 1998 Specification for Polyethylene Upright Storage Tank? 1D 3351 Test Method for Gel Count of Plastic Filmt E691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method" 3. Terminology 3.1. Defnitions of Terms Specific to This Standard: 3.l.1_ gel content—the percentage by mass of polymer insoluble in a specified solvent afer extraction under the specified conditions. 3.1.2 soluble—capable of being loosened or dissolved, sus ceptible of being dissolved in or as if ina fluid. (See Webster's Ninth New Collegiate Dictionary, 1988.) 3.1.3 swell ratio—the ratio of the gel volume in the swollen state to its volunie in the unswollen state 3.2 ‘Terms as shown in Terminology D 883 are applicable to this test method, 4. Summary of Test Methods 4.1 Specimens of the crosslinked ethylene plastic are ‘weighed and then immersed in the extracting solvent at the temperature specified by the procedure selected and for the time designated by that procedure. After extraction, the speci- ‘mens are removed, dried, and reweighed as directed. The amount of material extracted is calculated and, if desired, swell ratio also may be determined by the means described in altemative Test Method C. * Anml Book of ASTM Standods O09. > faa Book of 487M Sunda el 06.1 * dame Book of ASTM Sanders el 080, 2 Lana Book of ASTM Standards Nol 1402. Copyright by ASTM Int (al rights reserved [Reproduction authorized per License Agreement with (Book Supply Bureau}: Wed Nox 10 06:02:35 EST 20082 Significance and Use vimnprtdt prapetes oT crosslinked cilylene plas ties xarg.with the gel content-Hencerdetetiiinaiion of the gel content provides a means of both contclling the process and rating the quality of finished products 5. Extraction tests permit verification af the prop content of any given crosslinked ethylene plastic and they also hermit comparison between aliferent crosslinked etliylene plastics, including those containing fillers, provided that, for the latter, the following conditions are met: 52.1 The Biller isnot soluble in ether decahydeonaphha- lene of xylenes at the extaetion texperature $2.2 The amount of filler present in the compound either is ‘known or can be determined. 5.2.3 Sufficient crosslinking has been achieved to prevent rigration of filler during the extraction. Usually it has been found that, at extaction levels up to 50%, the extractant remains clear and fre of fle. '53 Since some oxidative degradation of the material can foceur at the reflux tomperature of the extractants, a suitable antioxidant is added to the extractant to inhibit such deprada- tion. 5.4 Before proceeding with this test method, reference, Any st specimen preparation, conditioning, dimensions, oF testing parameters, ar a combination thereof, covered in the materials specification shall take precedence over those men- tioned in this test method. If there are no material specifies tions, then the defaul conditions apply. 6. Precautions 6.1 This test method measures a much larger three — dimensional polymer network than that measured by Test ‘Method D 3351 and should not be confused with it. 6.2 Ithas been reported that crosslinked ultra-high molecu- lar weight polyethylene fails to completely dissolve in this, procedure at times. 7. Conditioning 7.1 Conditioning—Condition the test specimens at 23 = 2°C (73.4 = 36°F) for not less than 40 h prior to test in accordance with Procedure A of Practice D 618, for those tests ‘where conditioning is required. In cases of disagreement, the tolerance shall be + 1°C (+1.8°F), 7.2 Test Conditions—Prepare samples in the standard labo- ratory atmosphere of 23. 2°C (73.4 * 36°F), unless ‘otherwise specified in the test methods. In eases of disagree- ‘ment, the tolerance shall be =1°C (1.8°F), TEST METHOD A (REFEREE TEST METHOD) 8 Apparatus 8.1 The extraction apparatus shall be of the followi general type, as illustrated in Fig. 1 8.1.1 Round-Borrom Flask, with large-mouth ground cr cork joint. For one or two determinations at one time, a 500-mL flask is appropriate, For several determinations at ene time, but not exceeding six. 2 2000-ml. flask is suitable Copyright by ASTM Int (all ights reserved: should be made to the specification ofthe material being tested. 2 weve fp 0 2705 8.1.2 Heating Mantle to fit the Mask and with safficient heating capacity to boil decahydronaphthalene (boiling point 190 to 193°C) or xylenes (boiling point 138 to 141°C) 8.1.3 Reffur Condenser with ground-glass oF cork joint to fit into fask, 8.14 Ring Stand and Appropriate Clamps. 8.2. Grinding Equipment, suitable for reducing the sample to 2 fineness between 30 and GO mesh, A bench-top laboratory ‘mill” is satisfactory, although any procedure which will pro- duce a sample of the required fineness without generating ‘excessive heat may be used R21 U.S. Nu, 30 and US. No. 60 Sieves, 82.2 US. No. 120 Stainless Steel Wire Cloth. 8.3 Vacuum Oven, with vacuum source capable of creating, a vacuum of at least 710 mm (28 in.) Hg and equipped with a thermometer capable of measuring 150°C. 84 Analytical Balance, capable of weighing to 0.001 g, ore 218 slighty higher 2m) a degree of accuracy is desired (about 1 10 odifed Soxhlet Extractor; Kentes Catalog, No. $86100-0023. Size C, Kontes Gass Co, Vineland, NI or eqivalemt may be employed ‘wherein the specimen is held in en extraction thimble. The extraction ‘thimble, with exa-coarse Fined glass disk sealed in; Kontes 586500, (023, 45-mm body diameter, 130-mm height ot equivalent (height must subsequently be cu o 75 mm). The fried disk i exta-ceare with used ‘ge: Kontes 95200-4925, dsm direter or sqvalnt. Glass wool 13 te 1 sm thick (1 to Yan placed on the Bot othe exeation thimble ‘te support one gram 30-60 mesh ground sample which s covered with 13 to 19 mm thick layer of glass wont, fied glare disk and sll glass ‘eight The extaction thimble ascmbly ese up the SS pin oF "he humble previa ct of, theater stele the mii Sox, 9. Reagents 9.1 Decahydronaphthatene, anhydrous, boiling point 189 to wire, 9.2 Xvlenes, ACS reagent grade, boiling point 138 to 141°C. 9.3 2,2 -meihylene-bis (4-methyl-6-tertiary butyl phenol). 10. Safety Precautions 10.1 Xylenes and decahydronaphthalene are toxie and flam- mable solvents and as such should be handled carefully. Use only in a ventilated hood. Check the effectiveness of the hood before starting the tests. Do not inhale the vapors. Excessive inhalation of the vapors may cause dizziness or headache, or both, In the event of excessive inhalation, seek fresh clean at. 11, Test Specimens LLL Atleast two specimens cach containing 0.300 = 0.015 1g of ground polymer weighed to the nearest 0.001 g shall be tested. 11.2 The test samples shall be ground to a fineness that will, ppass through a 30-mesh sieve. Shake this sieved material over, 12 60-mesh sieve and reject any material that passes through, ‘Aes Cting Mil Interdit Mods, oegivlent Catalog No 68.338, salle fom Fister Seeatife Co, 711 Fortes Ave, Preburph PA 15219, Rt ‘een fan een forthe pumone Astin, able fom Ce ued he Wad ae ya 256, ha een found snsfacan fr hs pacpse Che Indes Poymer Adve Deparine Reproduction authorized per License Agreement with (Book Supply Bureau); Wed Nov 10 06:02:35 EST 2004‘A taenescavon ag and tow wre atacrad wo age —Refurcandenste (CRing sland core, [Eachound 08 oF crx ot Fence ate “Deeanyronapnnatene o syene Heating mante (Lazo mesh ire cape containing to scien FIG. 4 Extraction Apparatus 11.3 Test specimens originating from insulation eut from wire should be homogeneous and consist of an equal mixture ‘of samples representative of insulation nearest to the conductor and samples representative of insulation nearest the outer periphery of the construction unless specific portions of the insulation are being examined for insufficient crosslinking, 12. Procedure 12.1 Prepare a specimen holder by cutting a picce of 120-mesh stainless steel cloth measuring approximately 80 by 40 mm G by 14 in), Fold this to formn a square measuring approximately 40 mun (IY: in), Poll two sides of this square closed by folding the cloth atthe edges about 6 to 7 mm (Yin) anal ntapling those folds, fn that wanes, # peatch open atthe top is ebtained. Weigh this paueh CH), 12.2 Place approximately 0.3 g of the ground and screened sample in the weighed pouch. Weigh the pouch and specimen (182), Fold over the open side of the pouch and staple the edge to form a cage, Weigh the cage and sample (173). 123 Fill a round-bottom flask as described in 8.1.1 with enough solvent to immerse the 120-mesh cage and sample ‘completely. Three hundred fity grams in a 500-mL. flask or 1000 g in a 2000-ml flask is sufficient. Dissolve 1% of Copyright by ASTM ltt (llrightsreserved), 3 antioxidant in the decahydronaphthalene or xylenes to inhibit further crosslinking of the specimen, 124 Boil the decahydronaphthalene or xylenes vigorously ‘enough to ensure good agitation of the solution. Twenty to 40 rops/min from the condenser, while using 1000 g pf solvent, isa satisfactory boiling rate. Suspend the cage and specimen in the solvent so that the bottom edge of the cage is almost touching the bottom of the flask. A small wire, attached to the cage and extending through the reflux condenser ean be used for suspending the cage, Extract the specimen for 6 hin ilceahyalro aphthalene or for 12 h in xylenes. Ni 2 Since most af the extaction eccoHs within fe tha the specified vine, the perl of extntion sy We eben for cond tee {otc hanes expenwee. Mh se, i’ of eAQar ttn feported Fr veftce text exactions kW Bes spied by thi teat tho 125 Afer extraction, place the eage and specimen imme- diately in a vacuum oven prcheated to 150°C. Dry the specimen to constant weight under atleast 710 mm (28 in.) Hg, vacuum, Cool and weigh (174). If the compound absorbs ‘moisture, cool the specimen in a desiccator before weighing. Nore 41 has been seponed that dvi time sometimes can be Reproduction authorized per License Agreement with (Book Supply Bureau): Wed Nov 10 06:02:35 EST 2004‘alt materaly shortened if the min and then and sap are coole for fre placed either on 2 suspended seen of lintfice absorbent material to remove excess solvent before being pur int the vacuums dr sing oven 12.6 If extraction tests are regularly made, the apparatus may be left assembled and the extracting solvent (containing inhibitor as directed) may be reused until it darkens. However, if there is any doubt about the values obtained with reused ‘extractant, the test should be repeated with fresh extractant [Nove S—If the modified Soxhlet apparatus ie used, the complete thimble assembly containing 1g of sample is weighed tthe nearest 120,000! before extaction and after vacuum drying, 13. Calculation 13.1 Calculate the solvent extraction in percent as follows: [Extract % = (weight lst during extraction) (sueight of orginal specimen ~ weight of fille) 0 = 10, — ean, ~ Hy ~ Fa = Wi} x 100 = [0 = Wands — Fy, = HFN] x 100 where: W, = weight of the pouch (sealed on three sides, one side open}, W, = weight of the specimen and the pouch (sealed on three sides, one side open), W, = weight of the specimen and the cage, after being stapled shut, We ‘weight of the specimen and the cage after extraction and drying r netiot of filler (eich must be insoluble in deeay= dronapinhalene or xylene) inthe polyethylene com- pound, and gel content = 100 ~ percent extrac. Nore 6—If the faction of filler in the material is not known, the tet smetiods deserved in Tet Method D 1603 or in Test Methods D 297, may be used to termine filler conten. 14, Report 14.1 Repos the following information: 14.1.1 Complete identification of the compound, 14.12 Density of the polyethylene in the compound (usu- ally as idemtfied by its supplier), 14.13 Weight percent of polyethylene in the compound (usually as identified by its supplier, although it may be determined by the test methods identified in Note 6), 14.14 Percent extract; the value for each specimen and the average for the sample, 14.1.5 Solvent usei sample preparation, and 14.1.6 Any unusual or abnormal behavior observed during the test time of extraction, and any pertinent ‘TEST METHOD B (NONREFEREE TEST METHOD) 15. Scope 15.1 This modification of the referee test method was developed particularly for wire and eable insulations and differs from the referce test method only in specimen prepara- tion, Copyright by ASTM Intl (all ighs reserved 2765 1 ng this a native test method, it should be recognized that the values obtained may be lower than those ‘obtained by referce Test Method A for the reason given in 1.2. 16. Test Specimens 16.1 Using 2 wood plane, shave @ strip approximately 0.4 mm (0.015 in) thick parallel to the axis of the insulated conductor The test strip used for extraction should be taken next to the conductor only when strand shielding tapes or ‘compounds are not employed. In high-voltage cable employing, strand shielding tapes or compounds, the strip should be shaved as closely as possible along the shielded surface, being, careful not to include any of the semiconducting compound (see Fig. 2). 16.2 A section approximately 6 mm (4 in.) wide, depend ing on cable size, is cut longitudinally through the center + portion of the strip obtained as described in 15.1. The outer + sections ofthis strip are discarded, thus leaving only 2 sample of the material elosest to the conductor or shielded surface. ‘This sample then is cut or diced into pieces measuring «approximately 6 by 6 mm (¥4 by % in.) for extraction. 163 The dimensions given in 16.2 are for cable sizes 1/0 AWG and larger. For Size 2 AWG and smaller, the dimensions should be proportionately less. 17. Procedure 17.1 Place approximately 0.3 g of the diced sample, pre- pared as described in Scction 16, in a previously weighed pouch (IF) and then reweigds (1), Clase the pouch by foliing, over the open side aid stapling it to form a cage. Weigh this ‘cage and the sumple again (1¥’,)(see Section 12 of Test Method A. 17.2 Conduct the extraction as described in Section 12, using decahydronaphthalene as the extractant 17.3 After extraction, dry the specimen and reweigh also as described in Section 12, 18. Calculation 48.1 Calculate solvent extraction in percent as described én Section 13 of the referce test method, ‘ALShaved sigs to be cated. (CoAvan most susoptin 1 ute tossing, DoCretsnd pat aon. E—Specmen ft seven erties (ade aon, FIG. 2 Enlarged Cross-Sectional View of High-Voltage Cable ‘Showing Sample Location 4 Reproduction authorized per License Agreement with (Book Supply Bureau); Wed Nov 10 06:02:35 EST 2004pv 276 19, Report 19.41 See Section 14 but include ientitication of the alter native test method used (Test Method B), ‘TEST METHOD C (NONREFEREE TEST METHOD) 20. Scope : 20,1. Degece of exosslinkiny swell js determined by measuring the ind extraction occurring in a solvent that attaches that portion of the polymer which is not crosslinked. Both mea~ surements are obiained in one test. The degree of erosstinking. is not expressed as a percent of total erosslinkability or simile expression, but is judged from swell ratio and percent extra bbased on experience with the particular polymer-solvent sy tem under consideration. 20.2 This test method js applicable to crosslinked ethylene plastics of any density and including those containing fillers, provided thatthe fillers are insoluble in the extractant. 20.3 In using this altemative test method. it should be fecognized that the extraction values obtained will be lower than those obtained by either Test Method A or Test Method B for the reasons given in 1.2. However, this test method permits swell ratio to be determined. 21, Summary of Test Method 2.1 Specimens of the crosslinked polymer are weighed, immersed in hot xylene for 24 h, removed, weighed in the swollen state, and dried and reweighed. The swell ratio and percent extract are calculated from these weight measurements. 22. Significance and Use 22.1 This test method provides useful measurements when the temperature of the solvent in which the polymer is immersed is above the crystalline melting point of the polymer and below the temperature at which chemical degradation begins (o occur. Xylene, which thermodynamicaly is a good solvent for polyethylene, depresses the melting point of poly- ethylene (in accordance with Flory's theory of diluent forces) about 30°C. In the presence of xylene, polyethylene in the sensity range from 0.910 to 0.925 glem? (Jow density) has a ‘melting point less than 80°C, and polyethylene in the density range from 0.941 10 0.965 gem? (high density) has a melting point less than 110°C. Thus, tests on both types of polyethylene can be made at 110°C, 222 The percent extract is a measure of the amount of polymer that is soluble or is not entrapped in the main gel Phase, or both, at the end of the immersion period, Provided tit no ehemical degradation aceurs, the greater the degree of crosslinking the lower the amount of extract (lower percent extrac) 22.3 Swell ratio is a relative measure of erossinking in the sain gel phase, Provided that no ebemieal degradation occurs, the lower the swell ratio the greater the crosslinking and the lower the molecular weight between erasstinks. 23, Apparatus 23.1 Oil Bath at 110°C, agitated to ensure temperature uniformity 23.2 Wide-Mouth Glass Jars, 8-02, with screw caps. Copyright by ASTM Int all rights reserved DAY Anulsical Halanee, aveunate ws 0.00 234 Forceps, long, 280mm (10) 23.5 Cussing Devices 10 cut specimens from sample. 23.6 Tacuum Oven at 100°C, with pump and cold tap, 23.7 Flasks, 100-mL, 24/40 joint Desiccator, containing drying agent. 280 Mahi: Morales, Mean. and Geta BAA Pipes, 100 mt, or Mantle Tap: Dispenser capable of dispensing, 100 mL of liquid 24, Reagents and Materials 2A Nplenes, LEC. 24.2. Oil, sable at 110°C, 243 Acetone, tectinical grade. 244 Dry lee. ACS senpent ic, boiling point 138 10 25, Safety Precautions 25.1 Xylenes are toxic and flammable and as such should be handled carefully, Use only in a ventilated hood. Check the effectiveness of the hood before starting the tests. Do not inhale the vapors. Excessive inhalation of the vapors may cause dizziness or headache, or both. In case of excessive inhalation, seek fresh clean air. 26, Test Specimens 26.1. At least two specimens each containing 0.500 * 0.020 g of polymer shall be weighed to the nearest 0.001 g. 26.2 The test specimens shall be cut with sharp tools from the sample and all edges shall be smooth and clean. The surface-to-volume ratio shall be kept as small as reasonably possible, 26.3 ‘Test specimens consisting of insulation cut from wire shall be slit longitudinally. If necessary, they may be cut inte ‘vo or three pieces crosswise so that they ean be completely, submerged in the solvent 27. Procedure 27.1 Place the weighed test specimen in an 8-0z jar; add 100 = 0.1 mL of xylenes with the automatic pipet; make sure the + test specimen is completely immersed in the solvent (Note 7); serew the eap on the jar finger tight. Nore 7The solvent must cover the swollen st specimen at the conclision ofthe immersion peed to obiain eliable fess Tests shall be Sicatded and repeated wil fica test specimen if specimens ate not cosered wath sate! al the eens of the extinct Hep, 27.2 Place the jat iw the wil bath so that the fevel of the oil is ator slightly above the level of the solvent in the jar. The temperature ofthe oil bath must be 110°C and the bath must be at that temperate within 0.5°C no ess than Ys hater the jar is placed therein. IF necessary place a weight on the clamp it to hold it in place 27.3. Maintain the oil bath atthe proper temperature within 205°C for 24 h, with agitation, Nore &—The immersion pried specified seems to be adequate to reach an approximate equilibrium state fr swell easements Increasing this pesiod to 72h had na siificant effects on the results However longer immersion period des slighilyfneteare the wales for perent extrac, Reproduction authorized per License Agreement with (Book Supply Bureaul: Wed Nov 10 06:02:35 EST 2004lp 0 2765 274 Remove the jar after 24h in the hot oil bath and transfer the swollen test specimen with the forceps without delay to a clean, dry tared weighing bottle (Note 9). Handle the swollen test specimen gently and carefully. Blow the surfaces (Note 10). Stopper the weighing bottle, [None 9—The sie ofthe swollen test specimen dstates the sizeof the weighing bolle to be used. ‘Nore 1—Extreme care must be used in handling the wollen test specimen to obtain tliable results, The tst specimen should not be squeezed with the forceps. The transfer ofthe test specimen should be ‘made quickly. The surfaces should nt be subjected to exces Blowing (too Tong or more than once on each sie) otherwise more than the surface xylene wil be removed “Test specimens that beak up during the immersion period (usually very low degrees of crosslinking canbe eaught ona 60-mesh o finer stsinless steel sreen,tansfered to 2 weighing boule, and treated inthe specified ‘manner Results obtained from such specimens ate of imited valve. the fystem is unfilled, the swell rato wil bein eror because i i impossible {a eliminate the surface xylene, but the pereent entrst will be correct ial the gel pales were elleted. Ifthe system is led, both the swell rats! and the percent extact wil be ertoneous becsuse of loss of Bille 27.5 Place the weighing bottle in the desiccator, allow to cool fo room temperature, and weigh to the nearest 0.001 g. 27.6 Place the opened weighing bottle with the swollen test specimen in the vacuum oven at 100°C. Apply vacuum slowly. * Cool cold trap with dry ice and acetone to catch and condense ‘xylene vapor. Heat in vacuum until xylene is all removed. as determined by repeated weighing. Formulations containing low-density polyethylene usually require 24 h and those containing high-density polyethylene require 16 h to reach ‘weight equilibrium, 28. Caleulation (See Note 11 for Derivation) 28.1 Calculate the swell ratio as follows: Swell ratio= (Hg — RAUF, VK * 1 @ 282 Calculate the percent extract as follows: Bua Lo, ~ mega} 10 o polymer factor (Ihe ratio of the weight of the polymer in the formulation to the total weight of the formulation) W, = original polymer weight (the amount of polymer in the specimen being tested) WW, = weight of specimen being tested Ww, = OW, 19, = weigh of exract (amount of polymer extracted from the specimen in the test) ‘weight of swollen gel after the immersion period weight of dried gel W, ~ Wy, weight of xylene in swollen gel weight of insoluble polymer in swollen gel We We density of polymer at the immersion temperature volume of polymer in gel OW, = WD, = Wy /D, Weiei of slfent nel ee : ‘volume of solvent in get 6 Copyright by ASTM Int (ll ight reserved, rs OW, K wy, = WD, ratio of density of polymer to that ofthe solvent at the immersion temperature, This ratio is approxi mately 1.07 for low-density polyethylene at 80°C and 1.17 for high-density polyethylene at 110°C 28.3 High swell ratios indicate a low degree of crosslinking. that is, a high molecular weight between crosslinks. Low swell ratios indicate 2 more tightly’ bound structure, Low values of percent extract indicate a high degree of crosslinking, Nowe -=Der sation of calculations Sweat etylune ef poymer in ge + wokene of abserbed lene volume of pomerin gl Vane 09 + WK, 2M otinai ib) S(OUDWEIN) = 1 Ko, 17) Stings wi Wa Swi weit olenrarvonnialpelymes weigh)» 100 (ivi ~300= fv, = WH 7 100 =vd,= Wein» 100 29, Report 29.1. Report the following information: 29.1.1 Complete identification of the compound, 29.12 Density of the polyethylene polymer in the com- pound (usally as identified by is supplies), 20.1.3 Weight percent of polyethylene in the compound (osually as identified by its. supplier, although it may be determined by the methods identified in Note 6), 29.1.4 Swell ratio; the value for each specimen and the average forthe sample, 29.1.5 Percent extract; the val for each specimen andthe average forthe sample, 29.1.6 Identification ofthe method used, that is, Method C, 20.1.7 Any deviations from ths test method and the reasons for such deviations, and 29.1.8 Any unusual or abnormal behavior observed during the test 30. Precision and Bias * 30.1 Test Method A—Table 1 is based on a round robin conducted in 1967 involving six materials tested by three laboratories. For each material, all the samples were prepared at one source, but the individual specimens were prepared at the laboratories that tested them. Each test result was the result, of one individual determination. Each laboratory obtained thrce test results for each material, 302 Test Method B—Table 1 is based on a round robin conducted in 1967 involving six materials tested by one laboratory. For cach material, all the samples were prepared at ‘one source, but the individual specimens were prepated at the laboratory that tested them. Each test result was the result of fone individual determination. Each laboratory obsained three test results for each material, 303 Test Method C—Teble 1 is based on a round robin conducted in 1967 i wing six materials tested by three laboratories. For each material, all the samples were prepared at one source, bat the indivichtal specimens were prepared at * Sapp dr te uae oy ASTIN Mende Request RR DBD, Reproduction authorized per License Agreement with (Book Supply Bureau); Wed Nov 10 06:02:35 EST 2008lh 0 2765 my ebstained Nout Se~ with ertocy stand destin ofthe average Hhvee test rests for cult ater Sie etweenlaboratones standard deviation Of 38S Soy 12-—Ceution: The folowing explanations of and ROM Ir =280 50 30.43) ace onli mo 240 5k dd wo present « meaning ay of eansideing the approximate precision of thie tex method, The test data i Table should 3 M5 98D 180 N48 448 THe principles of 301-3043 would then be valid for such dt, $m our aie gee 304 Concept ofr and R—If S, and 5, have been caleuated oe from a large enough body of data, and for ext results that were Tawar maeigmnBCED arama | erages medansiother functions) for testing. {Wo spec "ONGSo" oto coo oo ou mens 2 wer 0057 = 000016000 30.4.1. Repeatabilin:, (Comparing two test results for the 3am 93g G09 92H 8m me material obtained by the same operator using. the rame $ (at Gars_ Bente, con. equipment on the same day) the two test results should be £ 291 o288 290 O703 0 judged not equivalent if they differ by more than the r value for Test Weed 6 Pecen Eac that materia Mate mecage STS it 30.4.2 Reductil, R{Comparing wo test results for 2 West 13s. Saas 383. Garo” the same material, obtained by diferent operators using difer- 3 ety BltaG4EB Gale 8360 Gn equpment on deren dys) the two fest els shuld be 4 Hk gate to YBBR + dpe nat equivalent if they difer by more than the valve aoa ore tae 280 at for that material, Tout Watoa € val Ra 3043 Any judgment in accordance with 30.4.1 oF 30.42 vatas —Areage SCENES yg would have an approximate 95 % (095) probability of being "Mee ote ast ome tn ae 3 or wba eee 30.5 There are no recognized standards by which to esti- {ther tse Zee Ota F57——_mate bias ofthis teat method $0 otis tae ode tose aoe an 31. Keywords 31.1 crosslinked ethylene plastics; gel content; insoluble the laboratory that ested them, Each test result was the result faction: swell ratio, SUMMARY OF CHANGES. Committee D20 has identified the location of selected changes to this test method since the lat issue that may impact the use of this procedure. D215 - 95: (5) Cortected an evvor in the Precision and Bins statement as (J) 180 statement was changed. pet Research Report @) Changed xylene to xylenes where appropriate. (6) General editorial changes were made throughout the {G) Updated equipment catalog numbers in Note 2 Stondard. (4 Removed humility requirement as per 14976. [ASTM njomatonal ahs no postion espactng the vac of ay patent his asserted in connerton wih ny tem menoned ‘nos sancara Users of ths standard ar express ade at eatamnnation the vy ony cuan patent i, 2nd We Mek ‘intingement of uch its ae ene tae ow respon. Ti stancar ie sujoctio reson a any tne Byte response tach conmtae and mut be reviewed ary oe years and Linatrevses, either eaperovedor wianm Your tomenets ae ved er forrson of sands fr aaa tandards ‘2d should bo aclassed i ASTM Iarnatonal Heaceuaters. You cnwnents nl eceve crea consieroon a3 Mee ote ‘esponaiie tinal commie, wii you may atond. you eel tat youreammenis have no eceied a far Rea you MOVE ‘make yout views now fo the ASTM Commitee on Stndas, ate ads shown below Tis standart cope ty ASTM ieratana, 100 Bar Harte Cre, PO Box C700, West Constr, PR $9420 2050, ned Sites. Incl rapnnts site or male copes) of Urs standoré may be eblined by covtatng ASTI at fhe above ses or a Gr0az20285 (par), Ee Es Fa 7 sere onimOy femal or MNRh he AST webale 7 Copyright by ASTM Int (all rights reserved: Reproduction authorized per License Agreement with (Book Supply Bureau); Wed Nov 10 06:02:35 EST 2008