1、Designation: D1603 12D1603 14Standard 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 nu
2、mber in 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 U.S. Department of Defense.1. Scope*1.1 This test method covers the determination of the c
3、arbon black content in polyethylene, polypropylene, and polybutyleneplastics. Its use with acrylic or other polar monomer modifications which might affect the accuracy is not recommended.Determinations of carbon black content are made gravimetrically after pyrolysis of the sample under nitrogen. Thi
4、s test methodis not applicable to compositions that contain nonvolatile pigments or fillers other than carbon black.1.1.1 This test method is not applicable to materials containing brominated flame retardant additives at the end.1.2 The values stated in SI units are to be regarded as standard. The v
5、alues in parentheses are given for information only.1.3 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibilityof the user of this standard to establish appropriate safety and health practices and determine the applicability of
6、regulatorylimitations prior to use.NOTE 1This standard and ISO 6964-1986(E) address the same subject matter, but differ in technical content.2. Referenced Documents2.1 ASTM Standards:2D883 Terminology Relating to PlasticsD4218 Test Method for Determination of Carbon Black Content in Polyethylene Com
7、pounds By the Muffle-Furnace TechniqueE177 Practice for Use of the Terms Precision and Bias in ASTM Test MethodsE691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method2.2 ISO Standard:ISO 6964-1986(E) Polyolefin Pipes and FittingsDetermination of Carbon Blac
8、k by Calcination and PyrolysisTest Methodand Basic Specification33. Terminology3.1 DefinitionsFor definitions of technical terms pertaining to plastics used in this specification, see Terminology D883.4. Significance and Use4.1 The information provided by this test method is useful for manufacturing
9、 quality control, technical service, and researchpurposes; and is required by various material specifications and for the calculation of optical absorptivity.4.2 Test Method D4218 is available for determining the carbon black content of polyethylene compounds if so desired.5. Apparatus5.1 Electric F
10、urnace, at least 20 cm (7.9 in.) long suitable for use with the tubing described in 5.2.5.2 High Temperature Glass Combustion Tube,Tube4, of appropriate diameter and approximately twice as long as the furnacedescribed in 5.1.1 This test method is under the jurisdiction of ASTM Committee D20 on Plast
11、ics and is the direct responsibility of Subcommittee D20.70 on Analytical Methods (SectionD20.70.01).Current edition approved May 1, 2012Aug. 1, 2014. Published June 2012August 2014. Originally approved in 1958. Last previous edition approved in 20112012 asD1603 - 11.D1603 - 12. DOI: 10.1520/D1603-1
12、2.10.1520/D1603-14.2 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standardsvolume information, refer to the standards Document Summary page on the ASTM website.3 ISO/IEC Selected Standards for Testing P
13、lastics, Second Edition, published by ASTM. Also available from American National Standards Institute (ANSI), 25 W. 43rdSt., 4th Floor, New York, NY 10036.4 Borosilicate, high-silica, or equivalent glass tubing has been found satisfactory for this purpose.This document is not an ASTM standard and is
14、 intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Becauseit may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the
15、current versionof the standard as published by ASTM is to be considered the official document.*A Summary of Changes section appears at the end of this standardCopyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States15.3 StoppersTwo rubber or n
16、eoprene stoppers, to fit the tube described in 5.2, unless the tube is fitted with ground joints andmating connectors.5.4 Glass Tubing, approximately 10 mm (0.39 in.) in diameter, of sufficient amount, and matching rubber or plastic tubing forconnections.5.5 Combustion Boat, approximately 8 by 1.9 b
17、y 1.3 cm (3.15 by 0.75 by 0.51 in.). Glazed porcelain, quartz high-silica glass,or platinum is suitable.NOTE 2A loose-fitting cover for the combustion boat is optional. If used, it shall be considered a part of the boat and handled and weighed with it.5.6 Iron-Constantan Thermocouple, and a potentio
18、meter or millivoltmeter suitable for determining temperatures in the range300 to 700C (572 to 1292F).5.7 Flow Meter, suitable for measuring gas flow at rates of 1 to 10 L/min.5.8 Traps, three glass traps with removable ground-glass connected heads and 10-mm (0.39-in.) diameter inner and connectingtu
19、bes.NOTE 3Only one trap is required if the entire apparatus train is placed in a fume hood. None is required if in addition, nitrogen of sufficient purityis used and produced by the alternative means provided in Section 6.5.9 Drying TubeA U-shaped drying tube, having an inside diameter of 20 mm (0.7
20、9 in.) or larger, fitted with ground glass orneoprene stoppers.5.10 Glass Wool.5.11 Desiccator, with desiccant.5.12 Bunsen Burner or Muffle FurnaceElectric resistance-heated or microwave-heated furnace capable of heating thecombustion boat to red heat.NOTE 4When an electric furnace is used, position
21、 it in a well-ventilated hood. When a microwave furnace is used, position it within or adjacent toa hood and the exhaust tube vented into the hood to prevent the breathing of byproducts of any combustion. An air flow rate of 2.8 m3/min through themicrowave oven is recommended.5.13 BalanceAn analytic
22、al balance having a sensitivity of 0.0001 g.6. Reagents and Materials6.1 Carbon Dioxide, Solid (Dry Ice).NOTE 5The solid carbon dioxide and the trichloroethylene are not required if the entire apparatus train is placed in a fume hood.6.2 Desiccant, such as anhydrous calcium chloride (CaCl2).6.3 Nitr
23、ogen, prepurified, having oxygen content below 0.01 %. As a safeguard against accidental leakage, contamination, orinadequate purity, the gas shall be further purified by one of the following procedures:6.3.1 Passage of the nitrogen through a glass trap inserted ahead of the drying tube (see Fig. 1)
24、, filled approximately one thirdFIG. 1 Assembly of ApparatusD1603 142full of potassium hydroxide - pyrogallol solution made to contain 5 g of pyrogallol and 50 g of KOH in 100 mLof water. Technicalgrade, or better, reagents are satisfactory.6.3.2 Insertion of a plug, or roll, of clean copper tinsel,
25、 foil, or wire 7.5 to 10 cm (3 to 4 in.) long into the combustion tube aheadof the sample (see Fig. 1) so that it is completely within the heated region of the furnace. Take care to prevent channeling of thenitrogen through the plug. The extent of blackening of the copper may be taken as a guide for
26、 determining when the plug shouldbe renewed.6.3.3 Passage of the nitrogen through a combustion tube filled to a length of 15 cm (6 in.) or greater with clean copper tinsel,foil, or wire, and maintained in a furnace at a temperature around 500C (932F).6.3.4 The need for the procedures described is el
27、iminated if gas having an oxygen content of less than 0.002 % (20 ppm) is used.6.4 Trichloroethylene, technical grade (Note 5).7. Sampling and Test Specs7.1 The test specimens can be in a variety of forms which fit in the combustion boat but must satisfy the requirements of 8.3.Soiled articles must
28、be washed and printed articles are wiped clean with a suitable solvent.8. ProcedureNOTE 6The procedure below assumes that the combustion tube can be easily removed from the furnace. If this is not the case, alternate methods ofinserting and removing sample boats are acceptable as long as the tempera
29、ture, purge time, and flow rate requirements are met.8.1 Assemble the apparatus as shown in Fig. 1. Both cold traps following the combustion tube shall contain trichloroethylene,but only the first need be cooled with solid carbon dioxide. Alternatively, the entire apparatus may be placed in a fume h
30、ood andthe two traps following the combustion tube omitted. Fill the drying tube with anhydrous CaCl2 or other suitable desiccant. Holdbetween loose plugs of glass wool.8.2 Heat a clean combustion boat to red heat in a bunsen flame or muffle furnace; then transfer the boat to the desiccator andallow
31、 it to cool over fresh desiccant for not less than 30 min.8.3 Remove the boat from the desiccator and weigh it to nearest 0.0001 g (w1). Immediately place 1.0 6 0.1 g of the ethyleneplastic under test in the boat and quickly weigh to the nearest 0.0001 g (w2).8.4 Heat the furnace to a constant tempe
32、rature 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 0.30.3 LL/min. min. Open the inlet end of the combustion tube, quickly place the combustion boat with the sample into the tube positionedso the boat will be at the
33、 proper temperature when in the furnace. Close the inlet to the tube and allow the nitrogen to flow fora minimum of 5 min to purge oxygen from the system prior to placing the tube in the furnace. If the furnace is controlled by anexternal thermocouple, adjust the thermocouple so that the weld is in
34、proximity to the boat. Insert the copper plug, if this is used(see 6.3.2). Quickly place the tube into the furnace, close the furnace, and allow heating to proceed for at least 15 min.NOTE 7The exact temperature of heating is not critical in the range 500 to 700C (932 to 1292F), although a heating t
35、ime as long as 30 min isdesirable at the lower temperature. If desired, the sample may be put in the furnace at 300C (572F) or less and the temperature of the furnace thenprogrammed for sample heating to 350C (662F) in 10 min, 450C (842F) in another 10 min, and 500C (932F) after a total of 30 min, f
36、inally heatingat 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 positioned in thefurnace within the area which meets the temperature requirements.8.6 Move the tube or furnace so that th
37、e boat is no longer in the heated zone of the furnace and allow 5 min for cooling, whilemaintaining the flow of nitrogen. Remove the copper plug, if present, and the boat through the inlet end of the tube and allow itto cool in the desiccator for at least 30 min. Take care that the boat does not bec
38、ome contaminated from any deposits on the wallsof the tube. Then quickly reweigh the boat and its contents to the nearest 0.0001 g (w3).8.7 If carbon black measurements are to be made at values less than 1 %, then the sample boat with the residue of the tubefurnace burn shall be placed in a muffle f
39、urnace for approximately 10 min to oxidize the carbon black. This is to correct for thepresence of residual inorganic matter in the sample. After heating, cool the sample boat in a desiccator until it is at roomtemperature. Weigh the boat plus contents to the nearest 0.0001 g 0.0001 g (w4).8.8 Two d
40、eterminations are made for each sample.9. Calculation9.1 Calculate the carbon black content as follows:Carbon black,%5Wr 2Wo!Ws 3100(1)Carbon black,%5Wr 2Wo!Ws3100 (1)D1603 143where:Wr = w3 - w1 = mass of residue (g) after burning in nitrogen,Wo = w4 - w1 = mass of residue (g) afterburning in air, a
41、ndWs = w2 - w1 = mass of sample (g).Wr = w3 w1 = mass of residue (g) after burning in nitrogen,Wo = w4 w1 = mass of residue (g) after burning in air, andWs = w2 w1 = mass of sample (g).10. Report10.1 Report the following information:10.1.1 Complete identification of material tested, including type,
42、source, manufacturers code number, form, previous history,etc.10.1.2 If applicable, the specific location of the specimen, if significant, for example, from articles.10.1.3 The individual determinations calculated as described in Section 9, and10.1.4 The average of the determinations reported in 10.
43、1.3.10.1.5 Date.11. Precision and Bias511.1 The precision of this test method is based on an interlaboratory study of this test method conducted in 2011. Fivelaboratories tested three different olefin plastic materials. Every “test result” represents the average of two determinations. Eachlaboratory
44、 reported three replicate test results for each material. Except for the limited number of participating laboratories,Practice E691 was followed for the design and analysis of the data.11.1.1 Repeatability limit (r)Two test results obtained within one laboratory shall be judged not equivalent if the
45、y differ bymore than the r value for that material; r is the interval representing the critical difference between two test results for the samematerial, obtained by the same operator using the same equipment on the same day in the same laboratory.11.1.1.1 Repeatability limits are listed in Table 1.
46、11.1.2 Reproducibility limit (R)Two test results shall be judged not equivalent if they differ by more than the R value for thatmaterial; R is the interval representing the critical difference between two test results for the same material, obtained by differentoperators using different equipment in
47、 different laboratories.11.1.2.1 Reproducibility limits are listed in Table 1.11.2 The terms repeatability limit and reproducibility limit are used as specified in Practice E177.11.3 Any judgment in accordance with statements 11.1.1 and 11.1.2 would normally have an approximate 95 % probability ofbe
48、ing correct, however the precision statistics obtained in this ILS must not be treated as exact mathematical quantities which areapplicable to all circumstances and uses. The limited number of laboratories reporting replicate results guarantees that there willbe times when differences greater than p
49、redicted by the ILS results will arise, sometimes with considerably greater or smallerfrequency than the 95 % probability limit would imply. Consider the repeatability limit and the reproducibility limit as generalguides, and the associated probability of 95 % as only a rough indicator of what can be expected.11.4 BiasAt the time of the study, there was no accepted reference 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 st
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