1、Designation: D 1603 06Standard Test Method forCarbon Black Content in Olefin Plastics1This standard is issued under the fixed designation D 1603; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revision. A number i
2、n parentheses indicates the year of last reapproval. Asuperscript epsilon (e) indicates an editorial change since the last revision or reapproval.This standard has been approved for use by agencies of the Department of Defense.1. Scope*1.1 This test method covers the determination of the carbonblack
3、 content in polyethylene, polypropylene, and polybuty-lene plastics. Its use with acrylic or other polar monomermodifications which might affect the accuracy is not recom-mended. Determinations of carbon black content are madegravimetrically after pyrolysis of the sample under nitrogen.This test met
4、hod is not applicable to compositions that containnonvolatile pigments or fillers other than carbon black.1.1.1 This test method is not applicable to materials con-taining brominated flame retardant additives at the end.1.2 The values stated in SI units are to be regarded asstandard. The values in b
5、rackets are given for information only.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 regulatory l
6、imitations prior to use.NOTE 1This test method is similar to ISO 6964-1986(E) in title only.The technical content is significantly different.2. Referenced Documents2.1 ASTM Standards:2D 883 Terminology Relating to PlasticsE 177 Practice for Use of the Terms Precision and Bias inASTM Test Methods2.2
7、ISO Standard:ISO 6964-1986(E) Polyolefin Pipes and FittingsDetermination of Carbon Black by Calcination andPyrolysisTest Method and Basic Specification33. Terminology3.1 DefinitionsFor definitions of technical terms pertain-ing to plastics used in this specification, see TerminologyD 883.4. Signific
8、ance and Use4.1 The information provided by this test method is usefulfor control purposes and is required by various materialspecifications and for the calculation of optical absorptivity.5. Apparatus5.1 Electric Furnace, at least 20 cm 7.9 in. long suitablefor use with the tubing described in 5.2.
9、5.2 High Temperature Glass Combustion Tube,4of appro-priate diameter and approximately twice as long as the furnacedescribed in 5.1.5.3 StoppersTwo rubber or neoprene stoppers, to fit thetube described in 5.2, unless the tube is fitted with groundjoints and mating connectors.5.4 Glass Tubing, approx
10、imately 10 mm 0.39 in. indiameter, of sufficient amount, and matching rubber or plastictubing for connections.5.5 Combustion Boat, approximately 8 by 1.9 by 1.3 cm3.15 by 0.75 by 0.51 in. Glazed porcelain, quartz high-silicaglass, or platinum is suitable.NOTE 2A loose-fitting cover for the combustio
11、n boat is optional. Ifused, it shall be considered a part of the boat and handled and weighedwith it.5.6 Iron-Constantan Thermocouple, and a potentiometer ormillivoltmeter suitable for determining temperatures in therange 300 to 700C 572 to 1292F.5.7 Flow Meter, suitable for measuring gas flow at ra
12、tes of1 to 10 L/min.1This test method is under the jurisdiction of ASTM Committee D20 on Plasticsand is the direct responsibility of Subcommittee D20.70 on Analytical Methods(Section D20.70.01).Current edition approved March 15, 2006. Published March 2006. Originallyapproved in 1958. Last previous e
13、dition approved in 2001 as D 1603 - 01.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3ISO/IEC Selected Stan
14、dards for Testing Plastics, Second Edition, published byASTM. Also available from American National Standards Institute (ANSI), 25 W.43rd St., 4th Floor, New York, NY 10036.4Borosilicate, high-silica, or equivalent glass tubing has been found satisfactoryfor this purpose.1*A Summary of Changes secti
15、on appears at the end of this standard.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.5.8 Traps, three glass traps with removable ground-glassconnected heads and 10-mm 0.39-in. diameter inner andconnecting tubes.NOTE 3Only one trap i
16、s required if the entire apparatus train is placedin a fume hood. None is required if in addition, nitrogen of sufficientpurity is used and produced by the alternative means provided in Section6.5.9 Drying TubeAU-shaped drying tube, having an insidediameter of 20 mm 0.79 in. or larger, fitted with g
17、round glassor neoprene stoppers.5.10 Glass Wool.5.11 Desiccator, with desiccant.5.12 Bunsen Burner or Muffle FurnaceElectricresistance-heated or microwave-heated furnace capable ofheating the combustion boat to red heat.NOTE 4When an electric furnace is used, position it in a well-ventilated hood. W
18、hen a microwave furnace is used, position it within oradjacent to a hood and the exhaust tube vented into the hood to prevent thebreathing of byproducts of any combustion.An air flow rate of 2.8 m3/minthrough the microwave oven is recommended.5.13 BalanceAn analytical balance having a sensitivity of
19、0.0001 g.6. Reagents and Materials6.1 Carbon Dioxide, Solid (Dry Ice).NOTE 5The solid carbon dioxide and the trichloroethylene are notrequired if the entire apparatus train is placed in a fume hood.6.2 Desiccant, such as anhydrous calcium chloride (CaCl2).6.3 Nitrogen, prepurified, having oxygen con
20、tent below0.01 %. As a safeguard against accidental leakage, contamina-tion, or inadequate purity, the gas shall be further purified byone of the following procedures:6.3.1 Passage of the nitrogen through a glass trap insertedahead of the drying tube (see Fig. 1), filled approximately onethird full
21、of potassium hydroxide - pyrogallol solution made tocontain5gofpyrogallol and 50 g of KOH in 100 mL of water.Technical grade, or better, reagents are satisfactory.6.3.2 Insertion of a plug, or roll, of clean copper tinsel, foil,or wire 7.5 to 10 cm 3 to 4 in. long into the combustion tubeahead of th
22、e sample (see Fig. 1) so that it is completely withinthe heated region of the furnace. Take care to prevent chan-neling of the nitrogen through the plug. The extent of black-ening of the copper may be taken as a guide for determiningwhen the plug should be renewed.6.3.3 Passage of the nitrogen throu
23、gh a combustion tubefilled to a length of 15 cm 6 in. or greater with clean coppertinsel, foil, or wire, and maintained in a furnace at a tempera-ture around 500C 932F.6.3.4 The need for the procedures described is eliminated ifgas having an oxygen content of less than 0.002 % (20 ppm) isused.6.4 Tr
24、ichloroethylene, technical grade (Note 5).7. ProcedureNOTE 6The procedure below assumes that the combustion tube canbe easily removed from the furnace. If this is not the case, alternatemethods of inserting and removing sample boats are acceptable as long asthe temperature, purge time, and flow rate
25、 requirements are met.7.1 Assemble the apparatus as shown in Fig. 1. Both coldtraps following the combustion tube shall contain trichloroet-hylene, but only the first need be cooled with solid carbondioxide. Alternatively, the entire apparatus may be placed in afume hood and the two traps following
26、the combustion tubeomitted. Fill the drying tube with anhydrous CaCl2or othersuitable desiccant. Hold between loose plugs of glass wool.7.2 Heat a clean combustion boat to red heat in a bunsenflame or muffle furnace; then transfer the boat to the desiccatorand allow it to cool over fresh desiccant f
27、or not less than 30min.7.3 Remove the boat from the desiccator and weigh it tonearest 0.0001 g (w1). Immediately place 1.0 6 0.1 g of theFIG. 1 Assembly of ApparatusD1603062ethylene plastic under test in the boat and quickly weigh to thenearest 0.0001 g (w2).7.4 Heat the furnace to a constant temper
28、ature of 600C1112F.7.5 With the combustion tube removed from the furnace,adjust the rate of nitrogen flow through the tube to 1.7 6 0.3L/min. Open the inlet end of the combustion tube, quicklyplace the combustion boat with the sample into the tubepositioned so the boat will be at the proper temperat
29、ure whenin the furnace. Close the inlet to the tube and allow the nitrogento flow for a minimum of 5 min to purge oxygen from thesystem prior to placing the tube in the furnace. If the furnace iscontrolled by an external thermocouple, adjust the thermo-couple so that the weld is in proximity to the
30、boat. Insert thecopper plug, if this is used (see 6.3.2). Quickly place the tubeinto the furnace, close the furnace, and allow heating toproceed for at least 15 min.NOTE 7The exact temperature of heating is not critical in the range500 to 700C 932 to 1292F, although a heating time as long as 30 mini
31、s desirable at the lower temperature. If desired, the sample may be put inthe furnace at 300C 572F or less and the temperature of the furnacethen programmed for sample heating to 350C 662F in 10 min, 450C842F in another 10 min, and 500C 932F after a total of 30 min,finally heating at 500C 932F for a
32、n additional 15 min.NOTE 8If the combustion tube and furnace are of adequate size,several sample boats may be tested simultaneously if they are positionedin the furnace within the area which meets the temperature requirements.7.6 Move the tube or furnace so that the boat is no longer inthe heated zo
33、ne of the furnace and allow 5 min for cooling,while maintaining the flow of nitrogen. Remove the copperplug, if present, and the boat through the inlet end of the tubeand allow it to cool in the desiccator for at least 30 min. Takecare that the boat does not become contaminated from anydeposits on t
34、he walls of the tube. Then quickly reweigh theboat and its contents to the nearest 0.0001 g (w3).7.7 If carbon black measurements are to be made at valuesless than 1 %, then the sample boat with the residue of the tubefurnace burn shall be placed in a muffle furnace for approxi-mately 10 min to oxid
35、ize the carbon black. This is to correct forthe presence of residual inorganic matter in the sample. Afterheating, cool the sample boat in a desiccator until it is at roomtemperature. Weigh the boat plus contents to the nearest 0.0001g(w4).7.8 Make all determinations in duplicate.8. Calculation8.1 C
36、alculate the carbon black content as follows:Carbon black, % 5Wr2 Wo!Ws3 100(1)where:Wr= w3-w1= mass of residue (g) after burning in nitro-gen,Wo= w4-w1= mass of residue (g) afterburning in air, andWs= w2-w1= mass of sample(g).9. Report9.1 Report the following information:9.1.1 Identity of the sampl
37、e,9.1.2 The individual values calculated as described in Sec-tion 8, and9.1.3 The average of the values reported in 9.1.2.10. Precision and Bias510.1 The interlaboratory precision, exclusive of samplingerror, was determined by an interlaboratory study with sevenlaboratories to be 60.156 % (3S) as de
38、fined in Practice E 177,over the range 2.5 to 3.0 % carbon black, and 60.309 % (3S)over the range 35 to 55 % carbon black.11. Keywords11.1 carbon black; gravimetric; plastics; polyolefins5Supporting data for this test method is available from ASTM Headquarters.Request RR: D20-1027.D1603063SUMMARY OF
39、 CHANGESCommittee D20 has identified the location of selected changes to this standard since the last issue,D 1603 - 01, that may impact the use of this standard. (March 15, 2006)(1) Revised title, 1.1, 4.1, 5.12, and 7.2.(2) Deleted supplier footnote for 5.7.(3) Added Note 4.(4) Deleted 5.14 for We
40、ights.ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentionedin this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the riskof infringement of such right
41、s, are entirely their own responsibility.This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years andif not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional s
42、tandardsand should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of theresponsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you shouldmake your views known to the ASTM C
43、ommittee on Standards, at the address shown below.This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the aboveaddress or at 610-832-9585 (phone), 610-832-9555 (fax), or serviceastm.org (e-mail); or through the ASTM website(www.astm.org).D1603064
