1、Designation: D1603 12Standard 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 MethodsE691 Practice for Conducting an Interlaboratory Study toDetermine the Precision of a Test Method2.2 ISO Standard:ISO 6964-1986(E) Polyolefin Pipes and FittingsDetermination of Carbon Black by Calcinati
8、on andPyrolysisTest Method and Basic Specification33. Terminology3.1 DefinitionsFor definitions 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 contro
9、l, technical service, and re-search purposes; and is required by various material specifica-tions 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 le
10、ast 20 cm (7.9 in.) long suitablefor use with the tubing described in 5.2.5.2 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
11、is fitted with groundjoints and mating connectors.5.4 Glass Tubing, approximately 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 cm(3.15 by 0.75 by 0.51 in.). Glazed porcelain, quartz high-sil
12、icaglass, or platinum is suitable.NOTE 2A loose-fitting cover for the combustion boat is optional. If1This 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
13、May 1, 2012. Published June 2012. Originallyapproved in 1958. Last previous edition approved in 2011 as D1603 - 11. DOI:10.1520/D1603-12.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume i
14、nformation, 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, o
15、r equivalent 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.used, it shall be considered a part of the boat a
16、nd 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 rates of1 to 10 L/min.5.8 Traps, three glass traps with removable groun
17、d-glassconnected heads and 10-mm (0.39-in.) diameter inner andconnecting tubes.NOTE 3Only 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 D
18、rying TubeAU-shaped drying tube, having an insidediameter of 20 mm (0.79 in.) or larger, 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 combus
19、tion boat to red heat.NOTE 4When an electric furnace is used, position it in a well-ventilated 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/
20、minthrough the microwave oven is recommended.5.13 BalanceAn analytical balance having a sensitivity 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.
21、6.2 Desiccant, such as anhydrous calcium chloride (CaCl2).6.3 Nitrogen, prepurified, having 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 t
22、hrough a glass trap insertedahead of the drying tube (see Fig. 1), filled approximately onethird 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,
23、 of clean copper tinsel, foil,or wire 7.5 to 10 cm (3 to 4 in.) long into the combustion 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 ma
24、y be taken as a guide for determiningwhen the plug should be renewed.6.3.3 Passage of the 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 p
25、rocedures described is eliminated ifgas having an oxygen content of less than 0.002 % (20 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
26、.Soiled articles must be washed and printed articles are wipedclean with a suitable solvent.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
27、 long asthe temperature, purge time, and flow rate requirements are met.FIG. 1 Assembly of ApparatusD1603 1228.1 Assemble the 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 carbondioxide. Alter
28、natively, the entire apparatus may be placed in afume hood and the two traps following the 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 furna
29、ce; then transfer the boat to the desiccatorand allow it to cool over fresh desiccant for 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 0.00
30、01 g (w2).8.4 Heat the furnace to a constant temperature of 600C(1112F).8.5 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 tube
31、positioned so the boat will be at the proper temperature 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 t
32、hermo-couple so that the weld is in proximity to the 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 (93
33、2 to 1292F), although a heating time as long as 30 minis 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, 450C(842F) in another 10 min, and 500C (9
34、32F) after a total of 30 min,finally heating at 500C (932F) for an 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.8.6 Move
35、the tube or furnace so that the boat is no longer inthe heated zone 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
36、 that the boat does not become contaminated from anydeposits on the walls of the tube. Then 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 shal
37、l be placed in a muffle furnace for approxi-mately 10 min to oxidize 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
38、(w4).8.8 Two determinations are made for each sample.9. Calculation9.1 Calculate 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).
39、10. Report10.1 Report the following information:10.1.1 Complete identification of material 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
40、 determinations calculated as de-scribed in Section 9, and10.1.4 The average of the determinations reported in 10.1.3.10.1.5 Date.11. Precision and Bias511.1 The precision of this test method is based on aninterlaboratory study of this test method conducted in 2011.Five laboratories tested three dif
41、ferent olefin plastic materials.Every “test result” represents the average of two determina-tions. Each laboratory reported three replicate test results foreach material. Except for the limited number of participatinglaboratories, Practice E691 was followed for the design andanalysis of the data.11.
42、1.1 Repeatability limit (r)Two test results obtainedwithin one laboratory shall be judged not equivalent if theydiffer by more than the r value for that material; r is the intervalrepresenting the critical difference between two test results forthe same material, obtained by the same operator using
43、thesame equipment on the same day in the same laboratory.11.1.1.1 Repeatability limits are listed in Table 1.11.1.2 Reproducibility limit (R)Two test results shall bejudged not equivalent if they differ by more than the R valuefor that material; R is the interval representing the criticaldifference
44、between two test results for the same material,obtained by different operators using different equipment indifferent laboratories.11.1.2.1 Reproducibility limits are listed in Table 1.5Supporting data have been filed at ASTM International Headquarters and maybe obtained by requesting Research Report
45、 RR:D20-1256.TABLE 1 Carbon Black Content (%)Material AverageARepeatabilityStandardDeviationReproducibilityStandardDeviationRepeatabilityLimitReproducibilityLimitxsrsRrRMaterial A 1.74 0.03 0.18 0.09 0.50Material B 5.27 0.08 0.16 0.21 0.45Material C 0.79 0.01 0.07 0.03 0.20AThe average of the labora
46、tories calculated averages.D1603 12311.2 The terms repeatability limit and reproducibility limitare used as specified in Practice E177.11.3 Any judgment in accordance with statements 11.1.1and 11.1.2 would normally have an approximate 95 % prob-ability of being correct, however the precision statist
47、ics ob-tained in this ILS must not be treated as exact mathematicalquantities which are applicable to all circumstances and uses.The limited number of laboratories reporting replicate resultsguarantees that there will be times when differences greaterthan predicted by the ILS results will arise, som
48、etimes withconsiderably greater or smaller frequency than the 95 %probability limit would imply. Consider the repeatability limitand the reproducibility limit as general guides, and the asso-ciated probability of 95 % as only a rough indicator of whatcan be expected.11.4 BiasAt the time of the study
49、, there was no acceptedreference material suitable for determining the bias for this testmethod, therefore no statement on bias is being made.11.5 The precision statement was determined through sta-tistical examination of 45 results, from five laboratories, onthree different olefin plastic materials described as:Material A: LLDPE PolyethyleneMaterial B: LLDPE PolyethyleneMaterial C: HDPE Polyethylene12. Keywords12.1 carbon black; content; gravimetric; plastics;polyolefinsSUMMARY OF CHANGESCommittee D20 has identified the location of selected c
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