1、Designation: D 1208 96 (Reapproved 2007)Standard Test Methods forCommon Properties of Certain Pigments1This standard is issued under the fixed designation D 1208; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last rev
2、ision. 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 procedures for dete
3、rminingcertain properties of pigments. The procedures appear in thefollowing order:Dry Pigments SectionsLoss on Ignition and Ash 4Matter Soluble in Water 5Hydrogen Ion Concentration (pHValue)6Alkalinity or Acidity by Titration 7 and 8Water Content (Distillation Method) 9 and 10Pigment Pastes in OilW
4、ater Content (Distillation Method) 9 and 10Pigment Content of Paste in Oil 11Total Volatile Matter in Paste in Oil 121.2 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.3 This standard does not purport to address all of thesaf
5、ety concerns, if any, associated with its use. 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.2. Referenced Documents2.1 ASTM Standards:2D95 Test Method for Water in Pe
6、troleum Products andBituminous Materials by DistillationD 280 Test Methods for Hygroscopic Moisture (and OtherMatter Volatile Under the Test Conditions) in PigmentsD 1135 Test Methods for Chemical Analysis of Blue Pig-mentsE70 Test Method for pH of Aqueous Solutions With theGlass Electrode3. Signifi
7、cance and Use3.1 This collection of test methods is used by pigmentproducers and paint manufacturers for process control, forproduct acceptance, and for research and development.LOSS ON IGNITION AND ASH4. Procedure4.1 Dry about5gofthesample at 105 6 2C for 2 h.Transfer about1gofthedried pigment, wei
8、ghed to 0.1 mg, toa previously ignited, weighed porcelain crucible, and ignite at900 to 1000C for 20 min. Cool in a desiccator and weigh. Heatagain for 10 min at 900 to 1000C to check the loss in weight.4.2 CalculationCalculate the percent of loss on ignition,L, and of ash, A, as follows:L 5LwS13 10
9、0 (1)SA 5WaS13 100Dwhere:Lw= loss in weight on ignition, g,A = ash, %,Wa= weight of ash, g, andS1= specimen weight, g.MATTER SOLUBLE IN WATER5. Procedure (Note 1)5.1 Weigh about 10 g of the sample to 1 mg, and place in a400-mL beaker. Add 100 mL of water (Note 2), boil for 5 mincool, and transfer qu
10、antitatively to a 250-mL volumetric flask.Dilute with water to 250 mL, mix, and allow to settle. Filter thesupernatant liquid through a dry paper (Note 3) and discard thefirst 25 mL. Evaporate 100 mL of the clear filtrate to drynessin a weighed flatbottom dish, preferably in an oven at 105 62C. Cool
11、 and weigh.NOTE 1This test method is not suitable for use with iron bluepigment. Use the conductivity method given in Test Methods D 1135.NOTE 2If the pigment is found to be strongly water-repellent, wet thesample with a small amount of alcohol or carry out a preliminary washingwith chloroform.NOTE
12、3Water-dispersible pigments must be filtered with a suitablefilter pad or the method may not be applicable.1These 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
13、 Specifications.Current edition approved June 1, 2007. Published June 2007. Originallyapproved in 1952. Last previous edition approved in 2002 as D 1208 96 (2002)e1.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Bo
14、ok 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.5.2 CalculationCalculate the percent of matter soluble inwater, M, as follows:M 5
15、R13 2.5S23 100 (2)where:R1= residue weight, g, andS2= specimen weight, g.HYDROGEN ION CONCENTRATION (pH VALUE)6. Procedure6.1 Determine hydrogen ion concentration in accordancewith either of the following methods:6.1.1 Electrometric Method (Preferred Procedure)Weighabout5gofthesample to 10 mg, place
16、 in a 150-mL beaker,and add 50 g of warm distilled water, freshly boiled to removecarbon dioxide. Mix well by means of a glass rod and cool to25C. Measure the pH of the mixture in accordance with TestMethod E70.6.1.2 Colorimetric MethodWeigh about 10 g of thesample to the nearest 10 mg, place in a 2
17、50-mL glass-stopperedErlenmeyer flask, and add 150 g of warm distilled water,freshly boiled to remove carbon dioxide. Stopper the flask andshake vigorously for about 1 min. Cool to 25C. Let stand 1 hto allow the pigment to settle. Decant the clear liquid anddetermine its pH at once by means of a sui
18、table indicator, usinga block comparator or similar colorimetric method.NOTE 4Ablock comparator or equivalent device is necessary in orderto compensate for the color of the extract.6.2 ReportIn reporting test results, state the particularmethod used.ALKALINITY OR ACIDITY BY TITRATION7. Reagents7.1 M
19、ethyl Orange Indicator SolutionDissolve 1 g ofmethyl orange in 1 L of reagent water.7.2 Sodium Hydroxide, Standard Solution (0.02 N).7.3 Sulfuric Acid, Standard Solution (0.02 N).8. Procedure8.1 Shake 20 g of the dry pigment with 200 mL of distilledwater for 5 min, let settle, and filter through a d
20、ry filter paperinto a dry beaker, discarding the first 10 mL of the filtrate.Transfer 100 mL of the clear filtrate to a flask, add 3 drops ofmethyl orange indicator solution, and titrate to the end pointwith 0.02 N sulfuric acid (H2SO4), if alkaline, or 0.02 Nsodium hydroxide (NaOH) solution, if aci
21、d.8.2 CalculationCalculate the acidity or alkalinity, ex-pressed as milligrams of NaOH equivalent to1gofthesample,as follows (1 mL of 0.020 N NaOH solution is equivalent to 0.8mg of NaOH):Alkalinity or acidity 5 mL of NaOH or H2SO43 0.8 (3)WATER CONTENT9. Apparatus9.1 Distillation ApparatusA water d
22、istillation apparatusconsisting of a 250-mL roundbottom flask, a straight-tubereflux condenser, and a graduated receiving trap similar to Fig.1 of Test Method D95.9.2 Heat Source consisting of a gas burner and oil bath, oran electric heater of the enclosed element type.10. Procedure (Note 5 and Note
23、 6)10.1 Place 50 g of the sample in the flask and add 100 mLof toluene or of petroleum solvent having a boiling pointbetween 110 and 120C. Mix well. Add more solvent, ifnecessary, to cover the pigment.10.2 Rinse the inner tube of the condenser with a littletoluene or petroleum solvent just before st
24、arting the distilla-tion, so as to wet the inner surface completely. Distill at amoderate rate until the volume of condensed water no longerincreases (about 3 h). If any water is lodged in the condensertube at the end of the test, wash it down with solvent or witha brush wetted with solvent.10.3 Cal
25、culationCalculate the weight percent of water,W, as follows (assuming that 1 mL of water weighs 1 g):W 5Wc503 100 (4)where Wc= water collected, mL.NOTE 5This test method is not suitable for pigments that releasecombined water under the conditions of the test.NOTE 6Test methods especially adapted for
26、 the determination ofmoisture in iron blue pigments are given in Test Methods D 1135.NOTE 7Test Methods designed for the determination of free water (asopposed to water of crystallization) in dry pigments are given in TestMethods D 280.PIGMENT CONTENT OF PASTE IN OIL11. Procedure11.1 Select a portio
27、n of the well-mixed sample that is free ofskins. Weigh to 10 mg, about 15 g of the sample in a weighed60-mL centrifuge tube. Add about 30 mL of petroleum ether,mix thoroughly with a glass rod, and wash the rod with morepetroleum ether (Note 8). Centrifuge at a moderate speed untilwell settled. Decan
28、t the clear supernatant liquid, and repeat theextraction twice with 40 mL of petroleum ether and once with40 mL of ethyl ether. After decanting the ether, set the tube ontop of a warm oven for 10 min and then in an oven at 105 62C for 2 h. Cool and weigh.NOTE 8Other solvents or solvent mixtures may
29、be used, provided thatthey leave no residue on evaporation.11.2 CalculationCalculate the percent pigment content,P, as follows:P 5R2S33 100 (5)where:R2= residue weight in centrifuge tube, g andS3= specimen weight, g.TOTAL VOLATILE MATTER IN PASTE IN OIL12. Procedure12.1 Weigh to 1 mg a flatbottom di
30、sh about 80 mm indiameter containing a piece of stiff wire 100 mm long. LeaveD 1208 96 (2007)2the wire in the dish throughout the test. Place about4gofthesample, weighed to 1 mg in the dish. Spread the specimen overthe bottom by means of the wire and heat for 212 h in an ovenat 105 6 2C. If a skin f
31、orms, break it up at intervals during theheating by means of the wire. Cool the dish and contents in adesiccator and weigh. Heat again for 30 min to check the lossin weight.12.2 CalculationCalculate the percent volatile matter inthe sample, V, as follows:V 5LS43 100 (6)where:L = loss in weight on he
32、ating, g, andS4= specimen weight, g.PRECISION AND BIAS13. Precision and Bias13.1 Precision data are not available at this time. When theyare available the appropriate statements will be added.13.2 BiasNo bias has been determined for this testmethod.14. Keywords14.1 analytical; ash; common products;
33、loss on ignition;pigments; volatile water; water content; water solubility phASTM 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 validi
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36、t 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, 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).D 1208 96 (2007)3
