1、Designation: D 6038 051Standard 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 () indicates an editorial change since the last revision or reapproval.1NOTEAdded research report footnote to Section 11 editorially in September 2008.1. Scope*1.1 Th
3、ese test methods cover the manual and automaticprocedures for testing the compatibility 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 availa
4、ble in a normal, well-equippedlaboratory. The automated procedure uses the ChemotronicCloudpoint 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, modifie
5、d dicyclopentadiene resins, rosin pentaerythritolor glycerol esters, phenolic modified 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 boi
6、ling solvents to be used are C12toC16petroleum distillates.1.6 To avoid fire or 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 MethodD5
7、6.NOTE 1Users of this test method should be aware that the flash pointof many solvents 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 outli
8、ned should be done in a shielded exhaust hood, wherethere is access to a fire extinguisher 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, i
9、f 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:3D56 Test Method for Flash Point by Tag Closed
10、Cup TesterD 1310 Test Method for Flash Point and Fire Point ofLiquids by Tag Open-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 Conductin
11、g an Interlaboratory Study toDetermine the Precision of a Test Method3. Terminology3.1 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, ho
12、mogeneous, and stable solution.3.1.3 incompatibility, nresin and solvent mixture 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 Re
13、lated Coatings, Materials, and Applications and are the directresponsibility of 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 apparatu
14、s is Testprint B. V., Zilverweg 10, POBox 127, 8440 AC Heerenveen, The Netherlands. 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
15、you may attend.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 page onthe ASTM website.1*A Summary of Changes section appears at the
16、end of this standard.Copyright ASTM International, 100 Barr Harbor Drive, PO Box 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 test
17、ed in the reference solvent (or vice versa) is heated ina test tube and stirred 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 theauto
18、mated tester, before the solution reaches the preset turbid-ity level.4.3 If the 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
19、method.)5. Significance and Use5.1 These test methods provide a means of determining 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 lowpr
20、ecipitation temperature.5.3 Resin-solvent mixtures that exhibit precipitation tem-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
21、, or rosinester resins, or both) or Ink Vehicle.6.2 Solvents, will be those commonly 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 evaluat
22、ing resins. The Test Ink Oils are controlled from lot tolot to ensure meaningful 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
23、. Apparatus7.1 Balance or Scale, weighing to 60.02 g accuracy and aminimum 250 g 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, alternati
24、ngcurrent (VAC), 60 HZ, 14A.7.6 Auxiliary Equipment, (that is, mixing loop (if desired),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 an
25、d18.00 6 0.02 g of the solvent to be tested into the test tube.9.2 Place test tube 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
26、 slowly as heat rises.NOTE 3To avoid loss of solvent while stirring, do not remove 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 aserio
27、us fire or accident.9.6 Heat to 200C; hold this temperature for 2 min, and thenremove 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
28、suchcases the maximum temperature for the test should be one agreed uponbetween 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 h
29、eat until dissolution has occurred. Start thecooling procedure at this point.9.8.2 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 precipitati
30、on, record it as incompatible.9.9 Observe mixture closely as temperature drops 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 lon
31、ger be seen). This is observa-tion is defined as the precipitation temperature 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 Associ
32、ation of Printing Ink Manufacturers (NAPIM), 581 Main St.,Woodbridge, NJ 07095, (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 App
33、liance Corp., Racine, WI 53403. If you areaware of alternative suppliers, please 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.D60380512NOTE 6This test method is
34、recommended for resins and solventmixtures exhibiting a precipitation temperature 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 shoul
35、d note thefollowing information:10.1.1 Sample identification number,10.1.2 Test run number,10.1.3 Maximum temperature achieved,10.1.4 Approximate rate of cooling, and10.1.5 Precipitation temperature.11. Precision and Bias711.1 PrecisionAn interlaboratory study of the precipita-tion temperature of tw
36、o resins was run by seven laboratories.11.1.1 The precision estimates here are based 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 standa
37、rd de-viation of results obtained by the same analyst running thedifferent analyses 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.
38、3 Reproducibility (Multilaboratory)The standard de-viation of results obtained by 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 an
39、d19.3 absolute, respectively.11.4 BiasThe procedure in this test method has no biasbecause 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 C
40、loudpoint Tester.212.3 Glass Tube5with external diameter 22 mm, length 20cm.12.4 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 acid.513.2 Haltermann N-C16 oil.514. Sample Preparation14.1 Pulverize th
41、e solid resin to a size no larger than 3 mm2.15. Instrument Calibration15.1 Place the 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 assembl
42、y on the tube and intothe Chemotronic.15.4 Start the test.15.5 Results should be repeated 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
43、 suggest calibration every two weeks.16. Procedure16.1 Insert the magnetic stirring 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.
44、NOTE 7Care should be taken to wash down the dust on the sides ofthe tube with solvent.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
45、and II machines. For the Chemotronic I, turn onthe “Motor” button (setting should be 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
46、 start button, and themachine will run automatically.NOTE 8Resins that have not been 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 recor
47、d of the cloud pointtemperature.16.7 Remove the test tube from the instrument; discardsample, and clean using normal lab cleaning procedures.7Supporting data have been filed at ASTM International Headquarters and maybe obtained by requesting Research Report RR: D011103.D6038051317. Instrument Sequen
48、ce17.1 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. microprocessor controlledEP3 80C 80CSL4 -10C microprocessor controlledEP4 30C 30CSL5 0 .DL5
49、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 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
