1、Designation: D1603 11Standard Test Method forCarbon Black Content in Olefin Plastics1This standard is issued under the fixed designation D1603; 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
2、parentheses indicates the year of last reapproval. Asuperscript epsilon () 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 co
3、ntent 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 method
4、 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 pare
5、ntheses are given for informationonly.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 li
6、mitations prior to use.NOTE 1This standard and ISO 6964-1986(E) address the same sub-ject matter, but differ in technical content.2. Referenced Documents2.1 ASTM Standards:2D883 Terminology Relating to PlasticsD4218 Test Method for Determination of Carbon BlackContent in Polyethylene Compounds By th
7、e Muffle-Furnace TechniqueE177 Practice for Use of the Terms Precision and Bias inASTM Test Methods2.2 ISO Standard:ISO 6964-1986(E) Polyolefin Pipes and FittingsDetermination of Carbon Black by Calcination andPyrolysisTest Method and Basic Specification33. Terminology3.1 DefinitionsFor definitions
8、of technical terms pertain-ing to plastics used in this specification, see TerminologyD883.4. Significance and Use4.1 The information provided by this test method is usefulfor manufacturing quality control, technical service, and re-search purposes; and is required by various material specifica-tion
9、s and for the calculation of optical absorptivity.4.2 Test Method D4218 is available for determining thecarbon black content of polyethylene compounds if so desired.5. Apparatus5.1 Electric Furnace, at least 20 cm (7.9 in.) long suitablefor use with the tubing described in 5.2.5.2 High Temperature G
10、lass 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, approximately 10 mm (0.39 in
11、.) indiameter, of sufficient amount, and matching rubber or plastictubing for connections.5.5 Combustion Boat, approximately 8 by 1.9 by 1.3 cm(3.15 by 0.75 by 0.51 in.). Glazed porcelain, quartz high-silicaglass, or platinum is suitable.NOTE 2A loose-fitting cover for the combustion boat is optiona
12、l. Ifused, it shall be considered a part of the boat and handled and weighedwith it.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 Sept. 1, 2011. Pu
13、blished September 2011. Originallyapproved in 1958. Last previous edition approved in 2006 as D1603 - 06. DOI:10.1520/D1603-11.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information
14、, refer to the standards Document Summary page onthe ASTM website.3ISO/IEC Selected Standards 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 equivale
15、nt glass tubing has been found satisfactoryfor this purpose.1*A Summary of Changes section appears at the end of this standard.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.5.6 Iron-Constantan Thermocouple, and a potentiometer ormil
16、livoltmeter suitable for determining temperatures in therange 300 to 700C (572 to 1292F).5.7 Flow Meter, suitable for measuring gas flow at rates of1 to 10 L/min.5.8 Traps, three glass traps with removable ground-glassconnected heads and 10-mm (0.39-in.) diameter inner andconnecting tubes.NOTE 3Only
17、 one trap is 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,
18、fitted with ground 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-venti
19、lated hood. When 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 s
20、ensitivity of0.0001 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, havi
21、ng oxygen content 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 o
22、nethird full 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
23、tubeahead of the 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
24、 nitrogen through 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
25、 ppm) isused.6.4 Trichloroethylene, technical grade (Note 5).7. Sampling and Test Specs7.1 The test specimens can be in a variety of forms which fitin the combustion boat but must satisfy the requirements of 8.3.Soiled articles must be washed and printed articles are wipedclean with a suitable solve
26、nt.8. 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 requirements are met.8.1 Assemble the
27、apparatus as shown in Fig. 1. Both coldtraps following the combustion tube shall contain trichloroeth-ylene, but only the first need be cooled with solid carbonFIG. 1 Assembly of ApparatusD1603 112dioxide. Alternatively, the entire apparatus may be placed in afume hood and the two traps following th
28、e combustion tubeomitted. Fill the drying tube with anhydrous CaCl2or othersuitable desiccant. Hold between loose plugs of glass wool.8.2 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 for
29、 not less than 30min.8.3 Remove the boat from the desiccator and weigh it tonearest 0.0001 g (w1). Immediately place 1.0 6 0.1 g of theethylene plastic under test in the boat and quickly weigh to thenearest 0.0001 g (w2).8.4 Heat the furnace to a constant temperature of 600C(1112F).8.5 With the comb
30、ustion 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 temperature whenin the furnace. Close the in
31、let 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 boat. Insert thecopper plug, if this
32、 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 minis desirable at the lower temperatu
33、re. 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, 450C(842F) in another 10 min, and 500C (932F) after a total of 30 min,finally heating at 500C (932F) for an additional 15 min.NOTE
34、 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.8.6 Move the tube or furnace so that the boat is no longer inthe heated zone of the furnace and al
35、low 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 the walls of the tube. Th
36、en quickly reweigh theboat and its contents to the nearest 0.0001 g (w3).8.7 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 oxidize the carbon black. Th
37、is 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).8.8 Two determinations are made for each sample.9. Calculation9.1 Calculate the carb
38、on 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).10. Report10.1 Report the following information:10.1.1 Complete identification of material
39、 tested, includingtype, source, manufacturers code number, form, previoushistory, etc.10.1.2 If applicable, the specific location of the specimen, ifsignificant, for example, from articles.10.1.3 The individual determinations calculated as de-scribed in Section 9, and10.1.4 The average of the determ
40、inations reported in 10.1.3.10.1.5 Date.11. Precision and Bias511.1 The interlaboratory precision, exclusive of samplingerror, was determined by an interlaboratory study with sevenlaboratories to be 60.156 % (3S) as defined in Practice E177,over the range 2.5 to 3.0 % carbon black, and 60.309 % (3S)
41、over the range 35 to 55 % carbon black.12. Keywords12.1 carbon black; content; gravimetric; plastics;polyolefins5Supporting data have been filed at ASTM International Headquarters and maybe obtained by requesting Research Report RR:D20-1027.D1603 113SUMMARY OF CHANGESCommittee D20 has identified the
42、 location of selected changes to this standard since the last issue, D1603 - 06,that may impact the use of this standard. (September 1, 2011)(1) Revised ISO statement in Note 1.(2) Added Test Method D4218 as a referenced document.(3) Revised Significance and Use (Section 4) to align with TestMethod
43、D4218.(4) Added Section 7: Sampling and Test Specimens.(5) Clarified the number of determinations in 8.8.(6) Revised Report (Section 10) to align with Test MethodD4218 and clarifications made to 8.8.(7) Revised Keywords (Section 12) to include the wordcontent.ASTM International takes no position res
44、pecting 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 rights, are entirely their own responsibility.This
45、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 standardsand should be addressed to ASTM Intern
46、ational 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 Committee on Standards, at the address shown be
47、low.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). Permission rights to photocopy the standard may also be secured from the ASTM website (www.astm.org/COPYRIGHT/).D1603 114
