1、Designation: D 480 88 (Reapproved 2003)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 (e) 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 p
3、rocedures 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 S
4、I 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 healt
5、h 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:D 185 Test Methods for Coarse Particles in Pigments,Pastes, and Paints2D 235 Specification for Mineral Spirits (Petroleum Spirits)(
6、Hydrocarbon Drycleaning Solvent)3D 329 Specification for Acetone3D 962 Specification for Aluminum Powder and Paste Pig-ments for Paints2D 3980 Practice for Interlaboratory Testing of Paint andRelated Materials4E11 Specification for Wire-Cloth Sieves for Testing Pur-poses5E34 Test Methods for Chemica
7、l Analysis of Aluminum andAluminum Alloys6E 607 Test Method for Optical Emission SpectrometricAnalysis of Aluminum and Aluminum Alloys by thePoint-to-Plane Technique, Nitrogen Atmosphere7E 691 Practice for Conducting an Interlaboratory Study toDetermine the Precision of a Test Method83. Significance
8、 and Use3.1 Flaked aluminum pigments 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
9、 glass container which shall be nearly 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 c
10、ase ofdisagreement.5. Qualitative Analysis5.1 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
11、total impurities byweight in accordance with Test Methods E 34 and 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-trar
12、ily, and even though the numerical leafing 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 o
13、n Pigment Specifications.Current edition approved Oct. 1, 2003. Published October 2003. Originallyapproved in 1938. Last previous edition approved in 1988 as D 480 88 (1999).2Annual Book of ASTM Standards, Vol 06.03.3Annual Book of ASTM Standards, Vol 06.04.4Annual Book of ASTM Standards, Vol 06.01.
14、5Annual Book of ASTM Standards, Vol 14.02.6Annual Book of ASTM Standards, Vol 03.05.7Annual Book of ASTM Standards, Vol 03.06.8Annual Book of ASTM Standards, Vol 14.02.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.substantially per
15、fect leafing under the conditions of practicalapplication in a paint.6.2 Significance 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 m
16、ustconform to Specification D 962.6.3 Apparatus:6.3.1 Leafing Spatula, nonmagnetic, 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
17、.08)100 mm from tip 0.038 6 0.004 (0.97 6 0.10)Shape of tip rounded or straightThe surface 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 obtai
18、ned in a typicalleafing test.6.3.2 Test Tube, 152 mm (6 in.) in length by 19.0 mm (0.75in.) 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 vertical
19、ly in the cylinder with the tip about 25 mm (1 in.)from the bottom.6.4 Reagents:6.4.1 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 Spi
20、ritsConforming to SpecificationD 235 and having the following additional properties: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 di
21、ssolving 30.0 g of resin, in the form of small chips, in 100mL of petroleum spirits, 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 otherwis
22、e specified, the aliquot weightshall be as follows:Classification ASTM Designation ClassAliquotWeight, 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
23、 vehiclein the glass cylinder and cover with a watch glass. Transfer25.0 61.0 mL of 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
24、 a spatulaor small stiff brush. Add approximately 5 mL more of thevehicle and stir 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
25、. Avoidformation of bubbles. Dip the spatula to the bottom of themixture and rotate 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 spat
26、ula verti-cally in the glass cylinder with leafing liquid in it and allow toremain 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 w
27、ipe dry witha clean cloth. Stir (do not shake) the mixture in the test tubeand repeat 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 se
28、ction provides two test methods for determiningthe percent residue retained on a sieve 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 Procedu
29、re A:7.3.1 Aluminum PowderFill two “straight wall” contain-ers not less than 305 mm (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
30、shall conformto Specification D 235, and the acetone shall conform toSpecification 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
31、 (8 in.) in diameter conforming to Specification E11, justabove the level of the petroleum 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 cle
32、arpetroleum spirits and transfer the rinsings to the sieve. Holdingthe sieve at a slight 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
33、60 to 100 cpm. It isimportant that the material be thoroughly sieved in eachcontainer. After the bulk of the aliquot has passed through theD 480 88 (2003)2sieve (usually about 2 min) repeat the procedure in the secondcontainer for about 2 min. When it is evident that practicallynone of the residue o
34、n the sieve is passing through it, repeat theprocedure in the acetone container for 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 alu
35、minum cup or small evaporating dish with a smallstream of acetone, using not less than 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 aceto
36、ne, as there is danger of explosion or flash ofacetone vapor.)7.3.2 Aluminum PasteDetermine 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 Calc
37、ulationCalculate the weight percent of theresidue retained on the sieve R from the 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 sie
38、ves usedin the test that have not been certified by the National Institute ofStandards 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 sievecertifie
39、d by the National Institute of Standards and Technology followingthe procedure described 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
40、 unknown screen, g.7.4 Procedure BTest in accordance with Test MethodsD 185 to determine 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. De
41、tails of the test proce-dure shall be strictly followed.8.2 Significance and UseThis 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) approximat
42、ely2gofthealiquot. Transfer to a 200-mLvolumetric flask and add about 50 mL of redistilled 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 hal
43、f of the supernatant liquid and filterthrough dry paper. Discard the first 10 mL of 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 mat
44、ter.8.3.2 Aluminum PasteDetermine the percent of easilyextracted fatty and oily matter 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 ace
45、tone, g, andW = weight of aliquot, g.9. Nonvolatile Matter9.1 Determine the percent 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
46、nonvolatile matter,such as fatty acids and their inter-reaction products, in alumi-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
47、for 3 h.Cool to room temperature and weigh.9.4 CalculationCalculate the weight percent 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
48、. Keywords11.1 aluminum powders and pastes; flaked powders; leafingpropertiesD 480 88 (2003)3ASTM 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 determinati
49、on 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 be reviewed every five years andif not revised, either reapproved or withdrawn. Your comments are invited either for 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 t
