1、Designation: D 6038 05Standard Test Methods forDetermining the Compatibility of Resin/Solvent Mixtures byPrecipitation Temperature (Cloud Point)1This standard is issued under the fixed designation D 6038; the number immediately following the designation indicates the year oforiginal adoption or, in
2、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. Scope*1.1 These test methods cover the manual and automaticprocedures for testing the compat
3、ibility of lithographic inkresins in high boiling ink solvents by precipitation temperature(cloud point) in a range from 35 to 210C.1.2 The manual procedure in this test method uses labora-tory equipment generally available in a normal, well-equippedlaboratory. The automated procedure uses the Chemo
4、tronicCloudpoint Tester.21.3 This test method is for use with ink resins intendedmainly for oil-based offset and letterpress inks. The type ofresins are typically, but not limited to C9aromatic hydrocarbonresins, modified dicyclopentadiene resins, rosin pentaerythritolor glycerol esters, phenolic mo
5、dified rosin esters, maleicanhydride modified-rosin esters, and naturally occurring resinssuch as gilsonite.1.4 A resin solution or ink vehicle could also be used in thistest instead of the resin.1.5 The typical high boiling solvents to be used are C12toC16petroleum distillates.1.6 To avoid fire or
6、injury, or both, to the operator, this testmethod should not be used with low flash point solvents suchas toluene or xylene. The minimum flash point of the solventsused should be 60C (140F) as determined by Test MethodD56.NOTE 1Users of this test method should be aware that the flash pointof many so
7、lvents used for this test (as defined in Test Methods D56andD 1310) is exceeded in the heating cycle of this test method. Safetyprecautions should be taken since there is the potential for vapor ignition.The method outlined should be done in a shielded exhaust hood, wherethere is access to a fire ex
8、tinguisher if needed.1.7 The values stated in SI units are to be regarded as thestandard. The values given in parentheses are for informationonly.1.8 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 stan
9、dard 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:3D56 Test Method for Flash Point by Tag Closed Cup TesterD 1310 Test Method for Flash Point and Fire Point ofLiquids by Tag Ope
10、n-Cup ApparatusE1 Specification for ASTM Liquid-in-Glass ThermometersE 180 Practice for Determining the Precision of ASTMMethods for Analysis and Testing of Industrial and Spe-cialty ChemicalsE 691 Practice for Conducting an Interlaboratory Study toDetermine the Precision of a Test Method3. Terminol
11、ogy3.1 Definitions:3.1.1 cloud point, n(precipitation temperature) the tem-perature at which a resin/solvent mixture changes from clear toturbid and opaque.3.1.2 compatibility, nresin and solvent mixture forms aclear, homogeneous, and stable solution.3.1.3 incompatibility, nresin and solvent mixture
12、 does notform a uniform solution and may be in two phases or opaque.3.1.4 precipitation, nresin separates from the resin/solvent mixture.1These test methods are under the jurisdiction of ASTM Committee D01 onPaint and Related Coatings, Materials, and Applications and are the directresponsibility of
13、Subcommittee D01.37 on Ink Vehicles.Current edition approved July 1, 2005. Published August 2005. Originallyapproved in 1996. Last previous edition approved in 1996 as D 6038 96.2The sole source of supply of the apparatus is Testprint B. V., Zilverweg 10, POBox 127, 8440 AC Heerenveen, The Netherlan
14、ds. If you are aware of alternativesuppliers, please provide this information to ASTM International Headquarters.Your comments will receive careful consideration at a meeting of the responsibletechnical committee,1which you may attend.3For referenced ASTM standards, visit the ASTM website, www.astm.
15、org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.1*A Summary of Changes section appears at the end of this standard.Copyright ASTM International, 100 Barr Harbor Drive, PO Box
16、 C700, West Conshohocken, PA 19428-2959, United States.3.1.5 solubility, nthe degree of resin compatibility in agiven solution.4. Summary of Test Method4.1 A 10 % by weight mixture of the resin (or ink vehicle)to be tested in the reference solvent (or vice versa) is heated ina test tube and stirred
17、until a clear solution is obtained.4.2 The solution is allowed to cool. The cloud point is thelowest temperature that can be read on a thermometer, posi-tioned at the back wall of the test tube, or in the case of theautomated tester, before the solution reaches the preset turbid-ity level.4.3 If the
18、 solution remains clear at room temperature, thetest tube is cooled (cold water, ice water, or dry ice/acetonebath) until the cloud point can be recorded. (Cooling belowambient temperature can only be done in the manual method.)5. Significance and Use5.1 These test methods provide a means of determi
19、ning thecompatibility of a resin (or vehicle), at low concentrations, ina high boiling ink solvent.5.2 Resin-solvent mixtures that exhibit a high precipitationtemperature are less compatible than those exhibiting a lowprecipitation temperature.5.3 Resin-solvent mixtures that exhibit precipitation te
20、m-peratures at or close to the cloud point of the pure solvent areconsidered infinitely compatible or the resin is infinitelysoluble in that solvent.6. Reagents and Materials6.1 Resins, (for example, modified hydrocarbon, or rosinester resins, or both) or Ink Vehicle.6.2 Solvents, will be those comm
21、only used for makinglithographic ink vehicles, for example, hydrocarbon petroleumdistillate C12to C16as agreed upon by producer and user.NOTE 2The use of ink industry recognized Test Ink Oils are recom-mended for evaluating resins. The Test Ink Oils are controlled from lot tolot to ensure meaningful
22、 data. (Contact NAPIM4for a list of approvedTest Ink Oils).6.3 Calibration Materials, PRIFRAC 2981 stearic acid andHaltermann N-C16 oil5designated for automatic method onlybut can be used for manual method.MANUAL METHOD7. Apparatus7.1 Balance or Scale, weighing to 60.02 g accuracy and aminimum 250 g
23、 capacity.7.2 Heat-Resistant Test Tube, 25mm width by 150mmheight.7.3 Thermometer, AP style, 0 to 250C, conforming toSpecification E1.7.4 Thermometer, -100 to 50C range.7.5 Hot Air Gun6, 260 to 399C, 120 volts, alternatingcurrent (VAC), 60 HZ, 14A.7.6 Auxiliary Equipment, (that is, mixing loop (if d
24、esired),lab stand, and test tube clamp, 500-mL beaker for cooling,etc.).8. Sample Preparation8.1 Pulverize the solid resin to a size no larger than 3 mm2.9. Procedure9.1 Weigh 2.00 6 0.02 g of pulverized crushed resin and18.00 6 0.02 g of the solvent to be tested into the test tube.9.2 Place test tu
25、be in tube with the sample in a tube clampwith the thermometer and mixing loop (optional).9.3 Aim the heat gun at the bottom of the test tube (keepnozzle at least 25.4 mm from tube), and turn on.9.4 Mix resin and solvent slowly as heat rises.NOTE 3To avoid loss of solvent while stirring, do not remo
26、ve thestirring apparatus from the mixture.9.5 WarningCare must be taken in stirring the resin/solvent mixture not to drop the thermometer or stirring loop.This could cause the test tube to break, which could cause aserious fire or accident.9.6 Heat to 200C; hold this temperature for 2 min, and thenr
27、emove the heat source.NOTE 4Low softening point and very compatible resins will dissolveat temperatures well below 200C. The maximum temperature to dissolvesuch resin and solvent mixtures can be much lower than 200C. In suchcases the maximum temperature for the test should be one agreed uponbetween
28、the customer and the supplier.9.7 Check to see that all resin is dissolved.9.8 Start to blow ambient air from the heat gun onto the testtube.9.8.1 If the mixture is not clear after heating for 2 min at200C, continue to heat until dissolution has occurred. Start thecooling procedure at this point.9.8
29、.2 If the mixture is clear except for a very slight presenceof precipitate, continue to end point and note the presence of “slight precipitate.”9.8.3 If the mixture does not become clear or exhibitssignificant precipitation, record it as incompatible.9.9 Observe mixture closely as temperature drops
30、andrecord the approximate rate of cooling, and the temperature atwhich solution becomes so cloudy that the thermometer, whenheld at the back wall of the test tube, can no longer be read (orthe thermometer fluid can no longer be seen). This is observa-tion is defined as the precipitation temperature
31、or cloud point(see Note 5 and Note 6).NOTE 5Cooling water, ice water, or a dry ice/acetone bath and a lowtemperature thermometer may be needed to reach the precipitationtemperature for very soluble resins.4National Association of Printing Ink Manufacturers (NAPIM), 581 Main St.,Woodbridge, NJ 07095,
32、 (napimnapim.org).5Available from Testprint B. V., Zilverweg 10, PO Bos 127, 8440 ACHeerenveen, The Netherlands.6The sole source of supply of the hot air gun, Model HG-501A known to thecommittee at this time is Master Appliance Corp., Racine, WI 53403. If you areaware of alternative suppliers, pleas
33、e provide this information to ASTM Interna-tional Headquarters. Your comments will receive careful consideration at a meetingof the responsible technical committee,1which you may attend.D6038052NOTE 6This test method is recommended for resins and solventmixtures exhibiting a precipitation temperatur
34、e between 50 and 180C at10 % resin solids. If a mixture is out of that range, a change in resinconcentration (for example, 20 % solids) or solvent is recommended.10. Report10.1 A report on precipitation temperature should note thefollowing information:10.1.1 Sample identification number,10.1.2 Test
35、run number,10.1.3 Maximum temperature achieved,10.1.4 Approximate rate of cooling, and10.1.5 Precipitation temperature.11. Precision and Bias11.1 PrecisionAn interlaboratory study of the precipita-tion temperature of two resins was run by seven laboratories.11.1.1 The precision estimates here are ba
36、sed on one analystin each laboratory performing triplicate determinations on eachof two materials.11.1.2 Practice E 180 was used in developing these preci-sion statements.11.2 Repeatability (Within-Laboratory)The standard de-viation of results obtained by the same analyst running thedifferent analys
37、es has been estimated to be 0.8 absolute at 20df at the 60C level and 2.4 absolute at 20 df at the 160Clevel. The 95 % limit for the difference between two suchaverages is 2.1 absolute and 6.7 absolute, respectively.11.3 Reproducibility (Multilaboratory)The standard de-viation of results obtained by
38、 analysts in different laboratorieshas been estimated to be 4.1 absolute at 6 df at the 60C leveland 6.9 absolute at 6 df at the 160C level. The 95 % limit forthe difference between two such averages is 11.5 absolute and19.3 absolute, respectively.11.4 BiasThe procedure in this test method has no bi
39、asbecause the value of the precipitation temperature is defined interms of this test method.AUTOMATED METHOD12. Apparatus12.1 Balance or Scale, weighing to 60.02 g accuracy and aminimum 250 g capacity.12.2 Chemotronic Cloudpoint Tester.212.3 Glass Tube5with external diameter 22 mm, length 20cm.12.4
40、Mortar and Pestle.12.5 Teflon Magnetic Stirring Bar5, length 50 mm, diam-eter 7 mm.12.6 Teflon Tube Holder.513. Materials13.1 PRIFRAC 2981 stearic acid513.2 Haltermann N-C16 oil514. Sample Preparation14.1 Pulverize the solid resin to a size no larger than 3 mm2.15. Instrument Calibration15.1 Place t
41、he test tube with stirring magnet and test tubeholder on the balance.15.2 Weigh 10 6 0.02 g of PRIFRAC 2981 stearic acid5with 10 6 0.02 g of Haltermann N-C 16 oil5into the test tube.15.3 Place the thermocouple assembly on the tube and intothe Chemotronic.15.4 Start the test.15.5 Results should be re
42、peated and the final cloud point forcorrect calibration of the instrument is 58C 6 1. If theinstrument is outside these parameters, consult your manual fortroubleshooting or call the manufacturer.15.6 The manufacturer suggest calibration every two weeks.16. Procedure16.1 Insert the magnetic stirring
43、 bar into the test tube. Placethe test tube in the Teflon tube holder.16.2 Weigh 2.00 6 0.02 g of pulverized crushed resin(using the mortar and pestle) and 18.00 6 0.02 g of the solventto be tested into the test tube.NOTE 7Care should be taken to wash down the dust on the sides ofthe tube with solve
44、nt.16.3 Place the test tube with test sample into theChemotronic Cloudpoint Tester and insert the thermocoupleassembly attached to the instrument.16.4 Start the standard cloud point sequence for both theChemotronic I and II machines. For the Chemotronic I, turn onthe “Motor” button (setting should b
45、e 5). Press the “Reset”button. (The “ sensitivity” setting should be at 5.) Then pressthe “Run” switch to start the test.16.5 For the Chemotronic II, start the standard machineprogram with all default values. Press the start button, and themachine will run automatically.NOTE 8Resins that have not be
46、en tested before may require theoperator to lift the tube right after the instrument establishes a cloud pointvalue. A visual inspection will ensure the resin is totally dissolved.16.6 The instrument will print a record of the cloud pointtemperature.16.7 Remove the test tube from the instrument; dis
47、cardsample, and clean using normal lab cleaning procedures.D603805317. Instrument Sequence17.1 The instrument should have this program installed asthe “STD” program.Chemotronic I Chemotronic IISP 100C 100CSL1 30C/min microprocessor controlledEP1 230C 230CSL2 0 .DL2 2.0 min 2.0 min.SL3 -30C.min. micr
48、oprocessor controlledEP3 80C 80CSL4 -10C microprocessor controlledEP4 30C 30CSL5 0 .DL5 0 .SF 0 .CC 1 .EC 0 .18. Evaluation18.1 The precipitation temperature or cloud point deter-mines the degree of resin compatibility in a particular solvent.The higher the precipitation temperature, generally, the
49、lesscompatible the resin and solvent mix is at ambient temperature.18.2 Resins and solvent mixes exhibiting precipitation tem-peratures well above 25C are not considered highly compat-ible or highly soluble at ambient temperatures.18.3 Resins and solvent mixes exhibiting precipitation tem-peratures below 25C are considered very compatible andsoluble at ambient temperatures.18.4 It should be noted that many resins exhibiting precipi-tation temperatures above 25C at the 10 % resin solids levelform compatible resin solutions at
