1、Designation: D6801 07 (Reapproved 2015)Standard Test Method forMeasuring Maximum Spontaneous Heating Temperature ofArt and Other Materials1This standard is issued under the fixed designation D6801; the number immediately following the designation indicates the year oforiginal adoption or, in the cas
2、e of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1. Scope1.1 This test method covers a small-scale laboratory proce-dure to determine the self heating t
3、endency of oil-basedmaterials by exposure to elevated temperatures in air in acontrolled semi-adiabatic system.1.2 This test method has been developed to address anurgent need to identify oil-based materials that may requirelabeling for spontaneous heating tendency. Studies based onthis test method
4、may allow the development of a practice toidentify such oil-based materials.1.3 The values stated in SI units are to be regarded asstandard. The values given in parentheses are for informationonly.1.4 This standard does not purport to address all of thesafety concerns, if any, associated with its us
5、e. It is theresponsibility of the user of this standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use. For safety concernsspecific to disposal of solvent-soaked rags, see Appendix X1.2. Referenced Documents2.1 ASTM Stand
6、ards:2E633 Guide for Use of Thermocouples in Creep and Stress-Rupture Testing to 1800F (1000C) in AirE771 Test Method for Spontaneous Heating Tendency ofMaterials (Withdrawn 2001)33. Terminology3.1 Definitions:3.1.1 maximum spontaneous heating temperature,nmaximum temperature reached during spontane
7、ous heatingunder the specified test conditions.3.1.2 oil-based materials, nseed and nut oils or materialsthat contain such oils.3.1.3 spontaneous heating, nexothermic reaction of amaterial due to slow or incomplete reaction that results in atemperature rise above that of its surroundings (see TestMe
8、thod E771); also called self heating.3.2 Symbols:3.2.1 TDdifference between maximum spontaneous heat-ing temperature and control temperature.3.2.2 TSmaximum spontaneous heating temperature.3.2.3 TCcontrol temperature or maximum spontaneoustemperature measured over 1 h immediately preceding thebeginn
9、ing of an experiment.4. Summary of Test Method4.1 A non-woven paper cloth is covered uniformly in 9.0mL of test material mixed with 0.25 mL of 6 to 10 %manganese drier. This covered pad is then put in a smallstainless steel holder with air holes in the sides. This holder isplaced in a larger chamber
10、, which is opened to the air from thetop and heated until peak temperature is reached. The maxi-mum spontaneous heating temperature inside the soaked papercloth is recorded with a K thermocouple and maximumtemperature recorder with the base temperature adjusted to 706 2C.5. Significance and Use5.1 T
11、his test method provides a means of accelerating thetendency of a material toward spontaneous heating that mayeventually lead to a fire. It is applicable to liquids and pastes.5.2 The spontaneous heating behavior of an oil-based ma-terial is affected by such factors as the availability of oxygen,the
12、 amount of driers present, the degree of polymerization ofoils, the surface area of the cellulose material, measures toprevent heat dissipation, and the amount of oil in contact withcellulose material. The degree of spontaneous heating bearslittle relationship to the type of cellulose material to wh
13、ich anoil-based material comes in contact or whether or not oil1This test method is under the jurisdiction of ASTM Committee D01 on Paintand Related Coatings, Materials, and Applications and is the direct responsibility ofSubcommittee D01.57 on Artist Paints and Related Materials.Current edition app
14、roved Dec. 1, 2015. Published December 2015. Originallyapproved in 2000. Last previous edition approved in 2007 as D6801 07. DOI:10.1520/D6801-07R15.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStanda
15、rds volume information, refer to the standards Document Summary page onthe ASTM website.3The last approved version of this historical standard is referenced onwww.astm.org.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States1soaked materia
16、ls are first air dried. Small amounts ofcontaminants, such as oil paint, quartz dust, dirt or drier (forexample, materials that might be found on a dirty, oil-soakedrag), can act as catalysts for this reaction.46. Apparatus6.1 Constant Temperature Water Bathset so that the baseinternal temperature o
17、f the test materials is 70 6 2C, see Fig.1.6.2 K Thermocouple, as described in Guide E633.6.3 Maximum Temperature Recorder, which records maxi-mum spontaneous heating temperature during a specifiedinterval and is accurate to at least 60.3C and calibratedagainst NIST traceable standards.6.4 Stainless
18、 Steel Chamber for Water BathSee Fig. 1 fordimensions.6.5 Stainless Steel Holder (for paper cloth)Ten equallyspaced 3-mm (18-in.) holes are drilled at 13 mm (12 in.) abovethe base. The holder is made with 2 mm (116 in.) stainless steelsheeting to form an open-topped box having a size of 70 mm(234 in
19、.) wide by 80 mm (318 in.) high by 30 mm (128 in.) thick(see Fig. 1). Close seams with spot welding.7. Materials7.1 Non-woven Paper Cloth in rolls, 6.5 to 7.5 g/sheet.Sheet size is 20 by 30 cm (8 by 12 in.) and sheet density is 0.12gm/cm3.7.2 Manganese Drier (manganese naphthenate-2-ethylhexanoate,
20、6 % Mn by weight) or manganese octanoate,10 % Mn by weight.8. Procedure8.1 Fill water bath with water and adjust the heat until thecenter of a dry test cloth is at 70 6 2C.8.2 Mix the liquid or paste material thoroughly with 0.25mL the test materials weight of 6 to 10 % manganese drier.8.3 Pipette l
21、iquids or use a spatula to spread pastes evenlyover the surface of the non-woven paper cloth folded in14 thsand fold the soaked cloth in116 ths.8.4 Put the folded, soaked cloth in the stainless steel holderwith the thermocouple placed centrally within the folded cloth(see Fig. 1).8.5 After placing t
22、he cloth in the water bath chamber,partially open the lid (11 mm (716 in.) to allow some airflowwithout loss of heat.8.6 Record maximum spontaneous heating temperature witha K thermocouple and maximum temperature recorder untilpeak temperature is reached (usually 1.5 to 2 hours).8.7 Record whether o
23、r not smoke is given off 15 min afterpeak temperature is reached and the degree blackening notedwhen the test cloth is unfolded with the following scale:0 no charring+ minimum charring+ extensive charring+ extensive charring plussmoke4Supporting data have been filed at ASTM International Headquarter
24、s and maybe obtained by requesting Research Report RR:D01-1115. ContactASTM CustomerService at serviceastm.org.FIG. 1 Spontaneous Combustion ApparatusD6801 07 (2015)28.8 WarningThis apparatus should not be left unattendedduring the course of a test.9. Calculation and Interpretation9.1 Calculate the
25、temperature difference (TD) between themaximum spontaneous heating temperature (TS) and controltemperature, TC, as follows:TD5 TS2 TC(1)9.2 The greater the temperature difference (TD), the greaterthe risk of spontaneous combustion associated with spontane-ous heating.10. Report10.1 Report the follow
26、ing information:10.1.1 Type of oil or material tested,10.1.2 Maximum spontaneous heating temperature, and10.1.3 Temperature difference (TD) between control and testruns.10.1.4 Degree of combustion.11. Precision and Bias411.1 Precision:11.1.1 RepeatabilityThe within laboratory standard devia-tion and
27、 95 % repeatability limits for testing a liquid materialare reported in Table 1.11.1.2 ReproducibilityThe between-laboratory standarddeviations and 95 % reproducibility limits for testing threevegetable-based mediums and a paint are reported in Table 2.511.1.3 BiasA low voltage to the maximum temper
28、aturerecorder results in erroneously high maximum spontaneousheating temperature readings. To prevent bias, ensure that thebattery meets manufacturers specifications for voltage beforeeach run or use a constant voltage source. Between laboratoryvariability increases for non-homogenous materials (alk
29、ydmedium, Table 2). Non-homogenous samples must be homog-enized prior to testing.12. Keywords12.1 art materials; autocombustion; autoignition; flamma-bility; ignition; spontaneous heating; vegetable oils5Supporting data have been filed at ASTM International Headquarters and maybe obtained by request
30、ing Research Report RR:D01-1138. ContactASTM CustomerService at serviceastm.org.FIG. 1 Spontaneous Combustion Apparatus (continued)TABLE 1 Within Laboratory Variability in Determination ofMaximum Spontaneous Heating Temperature Using a RefinedLinseed Oil/Manganese Drier Mix with Non-Woven Paper Clot
31、h(8 df)4,5Control (C)TCMaximum (C)TSDifference (C)TDMean value 70.0 247 177Repeatability standarddeviation1.4 6 6Repeatability 95 %confidence limits70.03.9 24712 17712D6801 07 (2015)3APPENDIX(Nonmandatory Information)X1. DISPOSAL OF OIL OR SOLVENT-SOAKED RAGSX1.1 For oils materials that present a ri
32、sk of spontaneouscombustion, special disposal procedures are necessary todecrease risk. Hanging contaminated rags out to “dry” isineffective at decreasing risk.4In order to prevent unexpectedfires, store water-damped contaminated rags in a metal con-tainer with an air-tight top. Alternately, washing
33、 such rags willremove contaminating materials and eliminate risk.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 su
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38、ive, Danvers, MA 01923, Tel: (978) 646-2600; http:/ 2 Between Laboratory Variability in Determination ofMaximum Spontaneous Heating Temperature Difference (TD)4Linseed oil#1Linseed oil#2AlkydMediumAlkydPaintMean value (C) 132.9 137.7 8.5 19.4Degrees of freedom 2 2 2 2Repeatability standarddeviation4.2 3.6 2.2 5.4Repeatability 95 % limits 8.4 7.2 4.4 10.8Reproducibility standarddeviation11.3 16.1 8.8 6.3Reproducibility 95 %limits22.6 32.2 17.6 12.3D6801 07 (2015)4