1、Designation: D 480 88 (Reapproved 2008)Standard Test Methods forSampling and Testing of Flaked Aluminum Powders andPastes1This standard is issued under the fixed designation D 480; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, th
2、e 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.This standard has been approved for use by agencies of the Department of Defense.1. Scope1.1 These test methods cover pr
3、ocedures for sampling,qualitative analysis, and physical testing of flaked aluminumpowders and pastes (leafing and nonleafing) for coatings.1.2 These test methods apply equally to leafing and non-leafing flaked aluminum powders and pastes except wherenoted to the contrary.1.3 The values stated in SI
4、 units are to be regarded as thestandard. 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 use. It is theresponsibility of the user of this standard to establish appro-priate safety and health
5、 practices and determine the applica-bility of regulatory limitations prior to use. For a specifichazard statement, see 7.3.1.2. Referenced Documents2.1 ASTM Standards:2D 185 Test Methods for Coarse Particles in PigmentsD 235 Specification for Mineral Spirits (Petroleum Spirits)(Hydrocarbon Dry Clea
6、ning Solvent)D 329 Specification for AcetoneD 962 Specification for Aluminum Powder and Paste Pig-ments for PaintsD 3980 Practice for Interlaboratory Testing of Paint andRelated Materials3E11 Specification for Wire Cloth and Sieves for TestingPurposesE34 Test Methods for Chemical Analysis of Aluminu
7、m andAluminum-Base AlloysE 607 Test Method for Atomic Emission SpectrometricAnalysis Aluminum Alloys by the Point to Plane Tech-nique Nitrogen AtmosphereE 691 Practice for Conducting an Interlaboratory Study toDetermine the Precision of a Test Method3. Significance and Use3.1 Flaked aluminum pigment
8、s are produced in a variety offorms. These test methods allow the user to determine theapplicability of a given product to this use.4. Sampling4.1 Sampling is subject to mutual agreement between theseller and the purchaser. Place each sample in a clean, drymetal or glass container which shall be nea
9、rly filled, then closewith a tight cover, seal, mark, and send to the laboratory fortesting.4.2 When requested, duplicate samples may be taken fromthe same container and delivered to the seller, and the inspectormay take a third set of samples to hold for test in case ofdisagreement.5. Qualitative A
10、nalysis5.1 Significance and UseThis test method determines ifthere are chemical impurities, other than fatty and oily matter,as specified in Specification D 962, to ensure the absence offillers or extender pigments.5.2 Procedure:5.2.1 Total ImpuritiesDetermine the total impurities byweight in accord
11、ance with Test Methods E34and E 607 or byatomic absorption.5.2.2 Total AluminumDetermine the total aluminum byweight difference with elemental impurities in accordance with5.2.1.6. Leafing Properties6.1 The leafing test conditions specified are selected arbi-trarily, and even though the numerical le
12、afing value obtainedby this test method appears to be low, the pigment may give1These test methods are under the jurisdiction of ASTM Committee D01 onPaint and Related Coatings, Materials, and Applications and are the directresponsibility of Subcommittee D01.31 on Pigment Specifications.Current edit
13、ion approved July 1, 2008. Published July 2008. Originally approvedin 1938. Last previous edition approved in 2003 as D 480 88 (2003).2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume info
14、rmation, refer to the standards Document Summary page onthe ASTM website.3Withdrawn.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.substantially perfect leafing under the conditions of practicalapplication in a paint.6.2 Significanc
15、e and UseThis leafing test method hasbeen established to determine the percent of leafed aluminumflakes at the surface of a simulated paint formula to ensure abright metallic luster. Minimum leafing characteristics mustconform to Specification D 962.6.3 Apparatus:6.3.1 Leafing Spatula, nonmagnetic,
16、stainless steel spatulahaving the following dimensions:Length of blade min, in. (mm) 5.5 (139.7)Width of blade, in. (mm) 0.540 6 0.002 (13.72 6 0.05)Thickness of blade, in. (mm):10 mm from tip 0.013 6 0.003 (0.33 6 0.08)100 mm from tip 0.038 6 0.004 (0.97 6 0.10)Shape of tip rounded or straightThe s
17、urface of the spatula shall be polished with 3/0 emeryor silicon carbide metallographic paper wet with mineralspirits; polishing shall be repeated for 1-min intervals until aconsistent minimum leafing result is obtained in a typicalleafing test.6.3.2 Test Tube, 152 mm (6 in.) in length by 19.0 mm (0
18、.75in.) in diameter.6.3.3 Glass Cylinder, 203 mm (8 in.) in length and 38.1 to50.8 mm (1.5 to 2.0 in.) in inside diameter. A stopper shall beused and the spatula shall be attached to the stopper so as tohang vertically in the cylinder with the tip about 25 mm (1 in.)from the bottom.6.4 Reagents:6.4.
19、1 Coumarone-Idene ResinThe form commerciallyknown as “chipped” and having the following properties:Softening point, C 109 to 117Specific gravity 1.12 to 1.16Acid value, max 0.5Cloud point, C, max 76.4.2 Petroleum SpiritsConforming to SpecificationD 235 and having the following additional properties:
20、Specific gravity at 16C (60F) 0.800 to 0.810Surface tension at 21C (70F), 24.5N/m, minKauri butanol value 42 to 44Aniline point, C (F) 40 to 45 (105 to 115)6.5 Preparation of Leaf-Testing VehiclePrepare solutionby dissolving 30.0 g of resin, in the form of small chips, in 100mL of petroleum spirits,
21、 while heating gently at about 60C(140F). The specific gravity of the solution shall be between0.877 and 0.881 at 16C (60F). Allow the solution to settleand retain the clear portion for use.6.6 AliquotUnless otherwise specified, the aliquot weightshall be as follows:Classification ASTM Designation C
22、lassAliquotWeight, gFlaked aluminum powder D 962, Type 1 A 1.0B1.0C2Aluminum paste D 962, Type 2 A 1.5B1.5C306.7 ProcedurePerform the test at a room temperature of25 6 2C. Place approximately 5 mL of the leaf-testing vehiclein the glass cylinder and cover with a watch glass. Transfer25.0 6 1.0 mL of
23、 the vehicle to a clean container. Weigh therequired aliquot of aluminum powder or paste to the nearest0.01 g and transfer to a small dish. Add about 2.5 mL of the25-mLquantity of vehicle and mix to a stiff paste with a spatulaor small stiff brush. Add approximately 5 mL more of thevehicle and stir
24、to a smooth mixture, then add the remainder ofthe vehicle and continue stirring to obtain complete dispersion.Transfer the mixture to the test tube to give a depth of about110 mm when the specified spatula is immersed. Avoidformation of bubbles. Dip the spatula to the bottom of themixture and rotate
25、 it gently through an arc of about 90 for 10s. Withdraw the spatula at a uniform rate of about 50 mm (2in.)/s. The spatula should not touch the wall of the test tubeabove the liquid level. Immediately suspend the spatula verti-cally in the glass cylinder with leafing liquid in it and allow toremain
26、for 3 min. Measure the height of immersion and theheight of complete leafing on both sides of the spatula,measuring to the bottom of the meniscus in each case. Cleanthe spatula by rinsing it in petroleum spirits and wipe dry witha clean cloth. Stir (do not shake) the mixture in the test tubeand repe
27、at the determination.6.8 CalculationCalculate the leafing value L as follows:L 5 A/B 3 100 5 A 3 100/Bwhere:A = height of complete leafing, in. (mm), andB = height of immersion, in. (mm).7. Coarse Particles7.1 This section provides two test methods for determiningthe percent residue retained on a si
28、eve by wet-screeningtechniques.7.2 Significance and UseThese procedures determine thepercent of coarse particles present in aluminum pigments toensure a smooth appearance, as required in SpecificationD 962.7.3 Procedure A:7.3.1 Aluminum PowderFill two “straight wall” contain-ers not less than 305 mm
29、 (12 in.) in diameter to a depth of notless than 102 mm (4 in.) with petroleum spirits, and fill a thirdsimilar container to a depth of not less than 76 mm (3 in.) withacetone. The petroleum spirits used for the test shall conformto Specification D 235, and the acetone shall conform toSpecification
30、D 329.Weigh5gofthealiquot, transfer to a250-mL beaker, and add in small portions a total of about 150mL of petroleum spirits, mixing thoroughly to a uniformconsistency after each addition. Clamp a standard sieve 203mm (8 in.) in diameter conforming to Specification E11, justabove the level of the pe
31、troleum spirits in the first containerand pour the specimen on the sieve, using a 45-m (No. 325)sieve for Classes A, B, and C powder and in addition a 150-m(No. 100) sieve for Class C powder. Rinse the beaker with clearpetroleum spirits and transfer the rinsings to the sieve. Holdingthe sieve at a s
32、light angle to prevent air lock, shake it backwardand forward working the sieve alternately just under and justabove the level of the liquid with rotation, avoiding spillagefrom the screen, at a rate of approximately 60 to 100 cpm. It isimportant that the material be thoroughly sieved in eachcontain
33、er. After the bulk of the aliquot has passed through theD 480 88 (2008)2sieve (usually about 2 min) repeat the procedure in the secondcontainer for about 2 min. When it is evident that practicallynone of the residue on the sieve is passing through it, repeat theprocedure in the acetone container for
34、 about 2 to 3 min untilnothing more passes through the sieve. Rinse the sides of thesieve with a small stream of acetone, and collect the residue atone side of the sieve. Transfer the residue to a dried andweighed aluminum cup or small evaporating dish with a smallstream of acetone, using not less t
35、han 15 to 25 mL. Place thealuminum cup or dish in an oven, evaporate to dryness at 105to 100C, and continue heating at this temperature for 15 min.(WarningDo not close the door of the oven while evapo-rating the acetone, as there is danger of explosion or flash ofacetone vapor.)7.3.2 Aluminum PasteD
36、etermine the percent of coarseparticles in accordance with the procedure described in 7.3.1using a 45-m (No. 325) sieve for Classes A, B, and C pasteand in addition a 150-m (No. 100) sieve for Class C paste.7.3.3 CalculationCalculate the weight percent of theresidue retained on the sieve R from the
37、increase in weight asfollows:R 5 A/W! 3 CF 3 100where:A = weight of dried residue, g,CF = correction factor (1.0 for NIST sieves), andW = aliquot weight, g.NOTE 1A correction factor shall be applied in the case of sieves usedin the test that have not been certified by the National Institute ofStanda
38、rds and Technology. Sieves having a correction factor above 1.2 orbelow 0.8 should not be used. The correction factor may be calculated asfollows: Determine the coarse particles of an aliquot on a master sievecertified by the National Institute of Standards and Technology followingthe procedure desc
39、ribed in 7.3.1. Sieve the same aliquot on the unknownsieve by the same procedure. Calculate the correction factor, CF,asfollows:CF 5 X/Ywhere:X = weight of residue on the NIST sieve, g, andY = weight of residue on the unknown screen, g.7.4 Procedure BTest in accordance with Test MethodsD 185 to dete
40、rmine conformance of flaked aluminum powdersand pastes to Specification D 235.8. Easily Extracted Fatty and Oily Matter8.1 Easily extracted fatty and oily matter is determined bythe following arbitrary test method. Details of the test proce-dure shall be strictly followed.8.2 Significance and UseThi
41、s test method determines thepercent of easily extracted fatty and oily matter in aluminumpigments in accordance with Specification D 962.8.3 Procedure:8.3.1 Aluminum PowderWeigh accurately (to within 0.01g) approximately2gofthealiquot. Transfer to a 200-mLvolumetric flask and add about 50 mL of redi
42、stilled acetoneconforming to Specification D 329. Heat the mixture to boilingwhile occasionally agitating. Cool, fill to the 200-mL markwith acetone, and mix. Allow the mixture to settle. Draw offapproximately one half of the supernatant liquid and filterthrough dry paper. Discard the first 10 mL of
43、 the filtrate.Transfer 100 mL of the clear filtrate to a weighed dish.Evaporate the acetone at a temperature not above 75C. Heatthe dish for 15 min in an oven at 105 to 110C. Cool and weighthe amount of fatty oily matter.8.3.2 Aluminum PasteDetermine the percent of easilyextracted fatty and oily mat
44、ter in aluminum paste in accordancewith the procedure described in 8.3.1.8.4 CalculationCalculate the weight percent of fatty andoily matter F as follows:F 5 2 3 A/W!# 3 100where:A = weight of residue in 100 mL of acetone, g, andW = weight of aliquot, g.9. Nonvolatile Matter9.1 Determine the percent
45、 of nonvolatile matter in alumi-num paste consisting of aluminum, fatty acids, additives, andtheir inter-reaction products.9.2 Significance and UseThis test method determines thecombined percent of aluminum and other nonvolatile matter,such as fatty acids and their inter-reaction products, in alumi-
46、num pigments and their conformance with Specification D 962.9.3 ProcedureAluminum Paste and PowderWeigh intoan evaporating dish5gofpaste or powder to within 0.01 g.Evaporate in an oven at a temperature of 105 to 110C for 3 h.Cool to room temperature and weigh.9.4 CalculationCalculate the weight perc
47、ent of nonvola-tile matter NV as follows:NV 5 A/W 3 100where:A = weight of residue, g, andW = weight of aliquot, g.10. Precision and Bias10.1 Precision and BiasDetermine in accordance withPractices D 3980 and E 691.11. Keywords11.1 aluminum powders and pastes; flaked powders; leafingpropertiesD 480
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