1、Designation: D5040 90 (Reapproved 2016)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 U.S. Department of Defense.1. Scope1.1 These test methods cover procedures used in determin-in
3、g the 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-
4、volatilecontent 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
5、in SI 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 h
6、ealth 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 Nitrate (With-drawn 2011)3D907 Terminology of AdhesivesD2415 Test Method for Ash in Co
7、al Tar and Pitch3. Terminology3.1 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 a
8、ll carbona-ceous material 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 t
9、he sample.6. Apparatus6.1 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
10、tray.6.4 Analytical Balance, 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-l
11、ation (600 6 25C (1112 6 45F).7. Reagents7.1 Nitric Acid (HNO3), concentrated, sp gr 1.42.8. Test Specimens8.1 For each test, use 5 to6gofmaterial.1These test methods are under the jurisdiction of ASTM Committee D14 onAdhesives and are the direct responsibility of Subcommittee D14.10 on WorkingPrope
12、rties.Current edition approved May 1, 2016. Published May 2016. Originallyapproved in 1990. Last previous edition approved in 2011 as D5040 90 (2011).DOI: 10.1520/D5040-90R16.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For
13、 Annual Book of ASTMStandards 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. Un
14、ited States18.2 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 0.5-g test specimen in anignited and tared crucible and evaporate to dryness on a steambath. Cool in a desicc
15、ator and weigh accurately. Heat thecrucible and its contents in a muffle furnace, gradually heatingthe furnace 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 re
16、ached. Check weight by cooling indesiccator and weighing to constant weight.9.2 Test Method B:9.2.1 Place 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
17、 to subsequent drying operation.9.2.2 Dry the test specimen in the oven at 100 to 105C (212to 221F) for 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 ste
18、am bath until initial vigorous reactionceases. Repeat addition of 25 mL nitric acid and heating on thesteam 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 elec
19、tric hotplate, or under an infrared lamp, orin a cold furnace while raising the temperature slowly toprevent 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
20、constant weight.NOTE 2The nitric acid treatment in Test Method B increases oxidationof organic material at relatively low temperatures while burning off onlythe residual carbon in the muffle furnace. Rubbery residues heated in amuffle furnace can produce a viscous foam which may expand andoverflow o
21、r spatter due to gaseous decomposition while heating, causingloss of sample.9.2.3 Warning: All operations 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 t
22、he total weight of the specimen as follows:CA,%5 W1/W23100where:W1= weight of ash, andW2= weight of test specimen.10.2 Test Method B:10.2.1 Calculate non-volatile content, CN, in the specimenas follows:CN,%5 w/W 3100where:w = weight of specimen after oven heating, andW = original weight of sample.10
23、.2.2 Calculate ash content of the non-volatile content, AN,based on the weight of the non-volatile content in the sampleas follows:AN,%5 W1/w 3100where: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 ca
24、lculated as specified in 10.1.11. Report11.1 Report the following information:11.1.1 Pertinent contractual 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-volatilecont
25、ent,11.1.4 The temperature and the length of time the specimenwas in the muffle furnace, and11.1.5 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
26、 more than 0.01 %.12.1.2 Duplicate determinations by two sets of laboratoriesshould not differ by more than 0.03 %.13. Keywords13.1 adhesive; ash contentD5040 90 (2016)2ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentionedin
27、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 standard is subject to revision at any time by the responsible technical committee and must
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29、esponsible 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 below.This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700,
30、 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 Copyright Clearance Center, 222Rosewood Drive, Danvers, MA 01923, Tel: (978) 646-2600; http:/ 90 (2016)3
