1、Designation: D 3711 95 (Reapproved 2005)An American National StandardStandard Test Method forDeposition Tendencies of Liquids in Thin Films and Vapors1This standard is issued under the fixed designation D 3711; the number immediately following the designation indicates the year oforiginal adoption o
2、r, in the case of revision, the 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.1. Scope1.1 This test method covers the determination of the ten-dency of liquids in thin
3、 films and of vapors to form deposits onmetal surfaces. The test method applies to both petroleum-based and synthetic lubricants, hydraulic fluids, heat-transferfluids, and related materials.21.2 The values stated in SI units are to be regarded as thestandard. In cases where materials, products, or
4、equipment areavailable in inch-pound units only, SI units are omitted.1.3 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 practices and determine the
5、 applica-bility of regulatory limitations prior to use. For specificwarning statements, see Section 7 and Annex A2.2. Referenced Documents2.1 ASTM Standards:3D 216 Method of Test for Distillation of Natural Gasoline4D 323 Test Method for Vapor Pressure of Petroleum Prod-ucts (Reid Method)D 4057 Prac
6、tice for Manual Sampling of Petroleum andPetroleum ProductsD 4177 Practice for Automatic Sampling of Petroleum andPetroleum ProductsE 230 Specification Temperature-Electromotive Force(EMF) Tables for Standardized Thermocouples2.2 ANSI Standard:C 96.1 Temperature Measurement Thermocouples.53. Termino
7、logy3.1 Definitions of Terms Specific to This Standard:3.1.1 deposit tendency, nthe deposition tendency of a thinfilm or vapor is an index of the propensity of a material to formcarbonaceous residues on hot surfaces in contact with theliquid or vapor phase of the sample.4. Summary of Test Method4.1
8、The test specimen is allowed to flow slowly in a thinfilm over a steel test specimen in a constant-temperaturechamber (furnace liner). Circulation of the sample from thesump to the heated surface and back to the sump is accom-plished by means of a peristaltic pump. After the prescribedtest period, t
9、he steel test specimen is removed from theapparatus and evaluated. The masses of deposits remainingafter washing with pentane, after washing with chloroform, andafter wiping with a paper tissue are reported.4.2 An optional procedure (see Annex A1) provides amethod for the determination of the tenden
10、cy of sample vaporsto form deposits on heated surfaces. A second test specimen isplaced in the vapor space over a thin flowing film of the liquidin a constant-temperature chamber (furnace liner). After circu-lation of the test liquid for a specified time the deposits on thetest specimen exposed to t
11、he liquid and the vapor phases aremeasured in the manner described in 4.1.5. Significance and Use5.1 The test method shall measure the deposit formationtendencies of liquids on steel surfaces in air at 101.3 KPa(1-atm) pressure. Other surfaces and other atmospheric mediamay be substituted for steel
12、and air at 1 atm provided that thesubstitution is noted in the test report.6. Apparatus6.1 Tube Furnace, with heating chamber 305 mm (12 in.)long by 35 mm (138 in.) in diameter6,7(see Fig. 1).6.2 Furnace Liner (constant-temperature chamber)SeeFig. 2.1This test method is under the jurisdiction of AST
13、M Committee D02 onPetroleum Products and Lubricants and is the direct responsibility of SubcommitteeD02.11 on Engineering Sciences of High Performance Fluids and Solids.Current edition approved June 1, 2005. Published September 2005. Originallyapproved in 1978. Last previous edition approved in 2000
14、 as D 371195(2000)e1.2United States Patent 2,669,865. Joseph Cole and John Krawetz.3For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary pa
15、ge onthe ASTM website.4Withdrawn.5Available from American National Standards Institute (ANSI), 25 W. 43rd St.,4th Floor, New York, NY 10036.6The sole source of supply of the apparatus known to the committee at this timeis the Type FD303A combustion furnace, Hoskins Manufacturing Co., Detroit, MI4823
16、2.7If you are aware of alternative suppliers, please provide this information toASTM International Headquarters. Your comments will receive careful consider-ation at a meeting of the responsible technical committee,1which you may attend.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C7
17、00, West Conshohocken, PA 19428-2959, United States.6.3 Temperature Controller.7,86.4 Potentiometer, direct-temperature readout.7,96.5 Thermocouples, for temperature control and read-out inaccordance with ANSI C 96.1 (see Specification E 230).6.6 Pump, peristaltic or kinetic clamp type capable ofdel
18、ivering 50 6 5 mL of sample per hour.7,106.7 Tubing7,11for use with pump.6.8 Steel Test SpecimensSee Fig. 3.6.9 Analytical Balance capable of measuring mass of testspecimen to the nearest 0.1 mg.7. Reagents and Materials7.1 Chloroform (WarningCan be fatal if swallowed.Harmful if inhaled. May produce
19、 toxic vapors if burned. SeeA2.1.) technical grade.7.2 Chromic Acid Cleaning Solution (WarningCausessevere burns. A recognized carcinogen. Strong oxidizer, con-tact with organic material can cause fire. Hygroscopic. See2.2.)7.3 Mild Steel Shim Stock, 0.051 mm (0.002 in.) thick.8The sole source of su
20、pply of the apparatus known to the committee at this timeis a Model 520 Solid State Controller, Barber Colman Co., Rockford, IL.9The sole source of supply of the apparatus known to the committee at this timeis a Model 400A digital temperature indicator, Doric Scientific, San Diego, CA.10Any peristal
21、tic pump capable of delivering the sample at the prescribed rate issatisfactory. Any tubing compatible with the sample may be used. It is recognizedthat, due to viscosity and compatibility phenomena, no single pump and tubingcombination will be acceptable for use with all samples.11The sole source o
22、f supply of the apparatus known to the committee at this timeis Kimwipes, Type 900M, Kimberly Clark Corp., Neenah, WI, have been foundsatisfactory.in. mm12 304.816 406.4AInlet end cap HSample outlet tubeBSample delivery tube ISample sumpCGas atmosphere outlet JPeristaltic pumpDMetal test piece for t
23、hin liquid films KInsulated terminals of furnace heater elementEFurnace liner (with standard taper male end joints) LTube furnaceFOutlet end cap TC1Control thermocouple for furnace controllerGGas atmosphere inlet TC2Thermocouple for test temperature read outFIG. 1 Tube Furnace1316 in. = 30.1 mmDMeta
24、l test piece for thin liquid filmsEFurnace liner (with standard tape male end joints)MLongitudinal aligning rodsFIG. 2 Furnace LinerD 3711 95 (2005)27.4 Pentane (WarningExtremely flammable. Harmful ifinhaled. Vapors can cause flash fire. See A2.3.) commercialgrade, conforming to the following requir
25、ements:Distillation (Method D 216):Initial boiling point 306.5 K (92F)Dry point 313.8 K (105F)Olefins noneIsopentane, max, % 20n-Pentane, min, % 80Reid vapor pressure 117 kPa (17 psi)(Test Method D 323), max8. Sampling8.1 The sample of test liquid shall be uncontaminated andrepresentative of the bul
26、k liquid as specified in Practice D 4057or Test Method D 4177.9. Test Specimens9.1 One-hundred millilitres of a liquid test specimen arerequired for a single determination of the thin film depositforming tendency.10. Procedure10.1 Prepare a test specimen in accordance with the follow-ing procedure:1
27、0.1.1 Buff both sides of a piece of mild steel shim stockwith jewelers rouge on a cloth wheel. The direction ofpolishing should be the same as that of the intended liquid flow.10.1.2 Clean the shim stock thoroughly by washing withpentane and chloroform. Allow the specimen to dry at roomtemperature.1
28、0.1.3 Cut a test specimen of the proper size from thepolished stock (see Fig. 3).10.1.4 Weigh the test specimen to the nearest 0.1 mg.10.1.4.1 In order to clean the shim stock effectively it isnecessary to wipe it vigorously with a paper tissue saturatedwith chloroform.10.2 Clean the glass parts of
29、the test apparatus by washingwith hot chloroform. Tenacious deposits may be removed withchromic acid cleaning solution. Rinse thoroughly with waterand dry the parts completely.10.3 Insert the clean, dry test specimen in the furnace linerand place the liner in the furnace. Place the end caps on theli
30、ner. Install new tubing in the system. Fill the sump with 100mL of the sample to be tested.10.4 Before connecting the pump outlet tube to the inputhead of the furnace liner determine that the sample flow rate is50 6 5 mL/h. If the flow rate is not within the stated limitsadjust the rate accordingly
31、until it is correct.10.5 Turn on the furnace and allow it to reach temperatureequilibrium at the desired test temperature. Start the samplepump at the same time.10.5.1 A test temperature of 533 K has been found to beuseful for the evaluation of the thin film deposit formingcharacteristics of automot
32、ive crankcase oils and similar mate-rials of petroleum origin. Synthetic materials and highlyrefined petroleum fluids may be tested at higher temperatures ifdesired.10.6 Allow the sample to circulate from the sump, over thetest specimen and back to the sump for 5 h after the furnace hasreached tempe
33、rature equilibrium.10.7 After 5 h turn off the pump and remove the testspecimen from the furnace liner. Carefully rinse the testspecimen with three successive rinses of pentane to removeadhering sample. Dry at room temperature and weigh to thenearest 0.1 mg. Then rinse the test specimen carefully wi
34、ththree successive rinses of chloroform. Dry at room temperatureand weigh to the nearest 0.1 mg. Wipe the test specimenvigorously in the longitudinal direction with a piece of labo-ratory tissue to remove loose deposits. Weigh the test specimento the nearest 0.1 mg.10.7.1 Test periods longer or shor
35、ter than 5 h may be usedprovided that their use is noted in the report of test results.10.7.2 Rinse the test specimen by immersion in the solvents.A spray of solvent from a wash bottle shall not be used, sinceit may cause the loss of loosely adhering deposits. Take care toavoid undue flexing of the
36、exposed test specimen as this canalso cause the loss of some of the deposit.11. Calculations11.1 Gross deposit, mg,dG5 1000 MG2 MO! (1)where:MG= mass of liquid film test specimen plus deposit afterrinse with pentane, gMO= mass of liquid film test specimens before test afterrinse with pentane and chl
37、oroform, gdG= gross deposit from liquid film, mg11.2 Chloroform-insoluble deposit, mg,dC5 1000 MC2 MO! (2)where:dC= chloroform insoluble deposit from liquid film, mgMC= mass of liquid film test specimens plus deposit afterrinse with pentane and chloroform, g11.3 Residual deposit, mg,dR5 1000 MR2 MO!
38、 (3)where:dR= residual deposit from liquid film, mgMR= mass of liquid film test specimen plus deposit afterrinse with pentane and chloroform and after abrasionwith paper tissue to remove loose deposits, gin. mm118 28.59 228.6FIG. 3 Metal Test Piece Thin Film Liquid ContactD 3711 95 (2005)312. Report
39、12.1 Report the following information:12.1.1 Temperature of test, K,12.1.2 Test duration, h, if different from the specified time,12.1.3 Composition of test panel, if different from thespecified composition,13. Precision and Bias13.1 Because of the complex nature of this test method fordeposition te
40、ndencies of liquids in thin films and vapors, thereis not a sufficient number of volunteers to permit a cooperativelaboratory program for determining the precision and bias. Ifthe necessary volunteers can be obtained, a program will beundertaken at a later date.14. Keywords14.1 deposition tendency;
41、deposits; thin films; vaporsANNEXES(Mandatory Information)A1. TEST METHOD FOR DETERMINATION OF VAPOR PHASE DEPOSITION TENDENCIESA1.1 ScopeThis annex covers the determination of thetendency of the vapors produced by the heating of lubricants,hydraulic fluids, heat-transfer fluids, and related materia
42、ls toform deposits on metal surfaces. It is intended that the test shallmeasure the deposit formation tendencies of vapors on steelsurfaces in air at 1 atm pressure. However, other surfaces andother atmospheric media may be substituted for steel and air atone atmosphere provided that the substitutio
43、n is noted in thetest report.A1.2 Summary of Test MethodThe sample is allowed toflow slowly in a thin film over a steel test specimen in aconstant-temperature chamber. Circulation of the sample fromthe sump to the heated surface and back to the sump isaccomplished by means of a peristaltic pump. A s
44、econd testspecimen is located in the vapor space over the thin liquidsample film. After the prescribed test period the test specimenin the vapor space is removed from the apparatus and evalu-ated. The mass of deposits remaining after washing withpentane, after washing with chloroform, and after wipi
45、ng witha paper tissue are reported. The deposits formed by the liquidfilm may also be evaluated by the procedure described in 10.7.A1.3 Symbols:M8O= mass of vapor space test specimen before test afterrinse with pentane and chloroform, g.M8F= mass of vapor space test specimen plus deposit afterrinse
46、with pentane, g.M8C= mass of vapor space test specimen plus deposit afterrinse with pentane and chloroform, g.M8R= mass of vapor space test specimen plus deposit afterrinse with pentane and chloroform and after abra-sion with paper tissue to remove loose deposits, g.d8G= gross deposit from vapor pha
47、se, mg.d8C= chloroform insoluble deposit from vapor phase, mg.d8R= residual deposit from vapor phase, mg.A1.4 Test SpecimenOne-hundred millilitres of a liquidtest specimen are required for a single determination of thevapor phase (and thin film) deposit forming tendency.A1.5 ApparatusThe apparatus u
48、sed for this test is thesame as that described in Section 6 except that an additionalvapor space test specimen (see Fig. A1.1 and Fig. A1.2)isused.A1.6 MaterialsThe materials used for this test are thesame as those described in Section 7.A1.7 Procedure:A1.7.1 Prepare the vapor space and liquid film
49、test speci-mens in accordance with the procedures described in 8.1 andFig. A1.2. Weigh the vapor space test specimen to the nearest0.1 mg.A1.7.1.1 If it is desired to determine the vapor phase andthin film deposition tendencies of the sample simultaneously,treat the liquid film test specimen in accordance with theprocedures outlined in Sections 8 and 10.A1.7.2 Clean the apparatus as described in 10.2 and insertthe clean dry vapor phase and liquid film test specimen in thefurnace liner. Assemble apparatus and adjust flow rates inaccordance with 10.
