1、Designation: D5040 90 (Reapproved 2011)Standard Test Methods forAsh Content of Adhesives1This standard is issued under the fixed designation D5040; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revision. A number
2、 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 Department of Defense.1. Scope1.1 These test methods cover procedures used in determin-ing the
3、 ash content of adhesives. This standard is intended as areplacement for Method 4032.1 of Federal Test Method Stan-dard 175B, “Adhesives: Methods of Testing.”1.2 Two test methods are used:1.2.1 Test Method A is used for a starch adhesive or othertype glue, where there is no danger from the non-volat
4、ilecontent forming a rubbery mass when ignited.1.2.2 Test Method B employs nitric acid to avoid thenon-volatile residue being transformed into a viscous foamwhen ignited.1.3 These methods are not applicable to adhesives contain-ing decomposable salts such as zinc chloride.1.4 The values stated in SI
5、 units are to be regarded as thestandard. The values given in parentheses are for informationonly.1.5 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
6、 practices and determine the applica-bility of regulatory limitations prior to use. For a specifichazard statement, see 9.2.3.2. Referenced Documents2.1 ASTM Standards:2D301 Test Methods for Soluble Cellulose NitrateD907 Terminology of AdhesivesD2415 Test Method for Ash in Coal Tar and Pitch3. Termi
7、nology3.1 DefinitionsDefinitions of terms in this standard maybe found in Terminology D907.4. Summary of Test Methods4.1 Ash content of adhesive materials is determined byheating a sample of material to remove all of the volatilecomponents. Complete oxidation and removal of all carbona-ceous materia
8、l may be enhanced by the addition of concen-trated HNO3. The general method of burning the residual ashin a muffle furnace at 600 6 25C (1112 6 45F) for8horuntil constant weight, is used.5. Significance and Use5.1 This test method measures the amount of inorganicmaterial in the sample.6. Apparatus6.
9、1 Crucible, porcelain, silica or platinum with a tightlyfitting lid, having a capacity of 30 to 45 mL.6.2 Evaporating Dish, porcelain, silica, or platinum, with acapacity of 150 mL.6.2.1 Watch Glasses to cover evaporating dishes.6.3 Desiccator, equipped with drying agent and tray.6.4 Analytical Bala
10、nce, sensitive to 1 mg.6.5 Steam Bath.6.6 Drying Oven, with temperature control for maintainingtemperature at 100 to 105C (212 to 221F).6.7 Electric Hotplate.6.8 Muffle Furnace, for igniting crucibles containing testspecimens. Capable of maintaining desired temperature regu-lation (6006 25C (1112 6
11、45F).7. Reagents7.1 Nitric Acid (HNO3), concentrated, sp gr 1.42.8. Test Specimens8.1 For each test, use 5 to6gofmaterial.8.2 The specimen being tested should represent the entirelot of material. Two specimens shall be taken for testing fromeach sample unit.9. Procedure9.1 Test Method APlace a 5.0 6
12、 0.5-g test specimen in anignited and tared crucible and evaporate to dryness on a steambath. Cool in a desiccator and weigh accurately. Heat thecrucible and its contents in a muffle furnace, gradually heating1These test methods are under the jurisdiction of ASTM Committee D14 onAdhesives and are th
13、e direct responsibility of Subcommittee D14.10 on WorkingProperties.Current edition approved April 1, 2011. Published April 2011. Originallyapproved in 1990. Last previous edition approved in 2005 as D5040 90 (2005).DOI: 10.1520/D5040-90R11.2For referenced ASTM standards, visit the ASTM website, www
14、.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.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.the f
15、urnace until the temperature reaches 600 6 25C (1112 645F). With the ignition temperature kept at 600C (1112F),allow the specimen to remain in the muffle furnace for8horuntil constant weight is reached. Check weight by cooling indesiccator and weighing to constant weight.9.2 Test Method B:9.2.1 Plac
16、e 5.0 6 0.5 g test specimen in a tared and igniteddish and evaporate to dryness on a steam bath.NOTE 1It is necessary to evaporate all volatile solvent to avoid firehazard when subjecting material to subsequent drying operation.9.2.2 Dry the test specimen in the oven at 100 to 105C (212to 221F) for
17、5 h, cool in the desiccator, then reweigh to thenearest mg. Add 25 mL nitric acid to the dried material in theevaporating dish, cover with a watch glass to prevent loss byspattering, heat on a steam bath until initial vigorous reactionceases. Repeat addition of 25 mL nitric acid and heating on thest
18、eam bath until no further action occurs. Remove the watchglass and continue heating on the steam bath until all excessnitric acid has been removed. Heat the evaporating dish andcontents on an electric hotplate, or under an infrared lamp, orin a cold furnace while raising the temperature slowly topre
19、vent spattering and until all volatile matter is driven off andthe contents of the dish are charred. Then ignite the evaporatingdish and contents in the muffle furnace at 600 6 25C (1112 645F) to constant weight.NOTE 2The nitric acid treatment in Test Method B increases oxida-tion of organic materia
20、l at relatively low temperatures while burning offonly the residual carbon in the muffle furnace. Rubbery residues heated ina muffle furnace can produce a viscous foam which may expand andoverflow or spatter due to gaseous decomposition while heating, causingloss of sample.9.2.3 Warning: All operati
21、ons involving handling and useof corrosive acids are extremely dangerous. Special careshould be taken when using nitric acid.10. Calculation10.1 Test Method ACalculate the ash content, CA, basedon the total weight of the specimen as follows:CA,%5 W1/W23 100where:W1= weight of ash, andW2= weight of t
22、est specimen.10.2 Test Method B:10.2.1 Calculate non-volatile content, CN, in the specimenas follows:CN,%5 w/W 3 100where:w = weight of specimen after oven heating, andW = original weight of sample.10.2.2 Calculate ash content of the non-volatile content, AN,based on the weight of the non-volatile c
23、ontent in the sampleas follows:AN,%5 W1/w 3 100where:W1= weight of ash, andw = weight of non-volatile content in sample.NOTE 3If required, the ash content of the total weight of the specimenshall be calculated as specified in 10.1.11. Report11.1 Report the following information:11.1.1 Pertinent cont
24、ractual requirements,11.1.2 Whether the test was determined by Test MethodAorB,11.1.3 The percentage of ash and whether it is based on theoriginal weight of the sample or the weight of non-volatilecontent,11.1.4 The temperature and the length of time the specimenwas in the muffle furnace, and11.1.5
25、The weight percent of ash to the nearest 0.01 %.12. Precision and Bias12.1 Use the following criteria to judge the acceptability ofresults:12.1.1 Duplicate values in this test method shall not differby more than 0.01 %.12.1.2 Duplicate determinations by two sets of laboratoriesshould not differ by m
26、ore than 0.03 %.13. Keywords13.1 adhesive; ash contentASTM 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 r
27、ights, and the riskof infringement of such rights, 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 f
28、or revision of this standard or for additional standardsand 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 heari
29、ng you shouldmake your views known to the ASTM Committee 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 m
30、ay 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/).D5040 90 (2011)2
