1、Designation: D6038 051D6038 14Standard Test Methods forDetermining the Compatibility of Resin/Solvent Mixtures byPrecipitation Temperature (Cloud Point)1This standard is issued under the fixed designation D6038; the number immediately following the designation indicates the year oforiginal adoption
2、or, in 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.1 NOTEAdded research report footnote to Section 11 editorially in September 2008.1. Scope
3、*1.1 These test methods cover the manual and automatic procedures for testing the compatibility of lithographic ink resins in highboiling ink solvents by precipitation temperature (cloud point) in a range from 35 to 210C.1.2 The manual procedure in this test method uses laboratory equipment generall
4、y available in a normal, well-equippedlaboratory. The automated procedure uses the Chemotronic Cloudpoint Tester. a programmable cloudpoint tester.1.3 This test method is for use with ink resins intended mainly for oil-based offset and letterpress inks. The type of resins aretypically, but not limit
5、ed to C9 aromatic hydrocarbon resins, modified dicyclopentadiene resins, rosin pentaerythritol or glycerolesters, phenolic modified rosin esters, maleic anhydride modified-rosin esters, and naturally occurring resins such as gilsonite.1.4 A resin solution or ink vehicle could also be used in this te
6、st instead of the resin.1.5 The typical high boiling solvents to be used are C12 to C16 petroleum distillates.1.6 To avoid fire or injury, or both, to the operator, this test method should not be used with low flash point solvents such astoluene or xylene. The minimum flash point of the solvents use
7、d should be 60C (140F) as determined by Test Method D56.NOTE 1Users of this test method should be aware that the flash point of many solvents used for this test (as defined in Test Methods D56 and D1310)is exceeded in the heating cycle of this test method. Safety precautions should be taken since th
8、ere is the potential for vapor ignition. The method outlinedshould be done in a shielded exhaust hood, where there is access to a fire extinguisher if needed.1.7 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for informationonly.standard. No oth
9、er units of measurement are included in this standard.1.8 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibilityof the user of this standard to establish appropriate safety and health practices and determine the applicability o
10、f regulatorylimitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D56 Test Method for Flash Point by Tag Closed Cup TesterD1310 Test Method for Flash Point and Fire Point of Liquids by Tag Open-Cup ApparatusE1 Specification for ASTM Liquid-in-Glass ThermometersE180 Practice for Determi
11、ning the Precision of ASTM Methods for Analysis and Testing of Industrial and Specialty Chemicals(Withdrawn 2009)3E691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method3. Terminology3.1 Definitions:1 These test methods are under the jurisdiction of ASTM Com
12、mittee D01 on Paint and Related Coatings, Materials, and Applications and are the direct responsibility ofSubcommittee D01.37 on Ink Vehicles.Current edition approved July 1, 2005Jan. 1, 2014. Published August 2005January 2014. Originally approved in 1996. Last previous edition approved in 19962005
13、asD6038 96.D6038 051. DOI: 10.1520/D6038-05E01.10.1520/D6038-14.2 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standardsvolume information, refer to the standards Document Summary page on the ASTM websi
14、te.3 The last approved version of this historical standard is referenced on www.astm.org.This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Becauseit may not be technically possible
15、to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current versionof the standard as published by ASTM is to be considered the official document.*A Summary of Changes section appears at the end of this standardCopyrigh
16、t ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States13.1.1 cloud point, n(precipitation temperature) the temperature at which a resin/solvent mixture changes from clear to turbidand opaque.3.1.2 compatibility, nresin and solvent mixture forms a cl
17、ear, homogeneous, and stable solution.solution at room temperature.3.1.3 incompatibility, nresin and solvent mixture does not form a uniform solution and may be in two phases or opaque.3.1.4 precipitation, nresin separates from the resin/solvent mixture.3.1.5 solubility, nthe degree of resin compati
18、bility in a given 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 in atest tube and stirred until a clear solution is obtained.4.2 The solution is allowed to cool. The cloud point is the lowe
19、st temperature that can be read on a thermometer, positionedat the back wall of the test tube, or in the case of the automated tester, before the solution reaches the preset turbidity level.4.3 If the solution remains clear at room temperature, the test tube is cooled (cold water, ice water, or dry
20、ice/acetone bath) untilthe cloud point can be recorded. (Cooling below ambient temperature can only be done in the manual method.)5. Significance and Use5.1 These test methods provide a means of determining the compatibility of a resin (or vehicle), at low concentrations, in a highboiling ink solven
21、t.5.2 Resin-solvent mixtures that exhibit a high precipitation temperature are less compatible than those exhibiting a lowprecipitation temperature.5.3 Resin-solvent mixtures that exhibit precipitation temperatures at or close to the cloud point of the pure solvent areconsidered infinitely compatibl
22、e or the resin is infinitely soluble in that solvent.6. Reagents and Materials6.1 Resins, (for example, modified hydrocarbon, or rosin ester resins, or both) or Ink Vehicle.6.2 Solvents, will be those commonly used for making lithographic ink vehicles, for example, hydrocarbon petroleum distillateC1
23、2 to C16 as agreed upon by producer and user.NOTE 2The use of ink industry recognized Test Ink Oils are recommended for evaluating resins. The Test Ink Oils are controlled from lot to lot toensure meaningful data. (Contact NAPIM NAPIM4 for a list of approved Test Ink Oils).6.3 Calibration Materials,
24、 PRIFRAC 2981 stearic acid and Haltermann N-C16 oil oil5 designated for automatic method onlybut can be used for manual method.MANUAL METHOD7. Apparatus7.1 Balance or Scale, weighing to 60.02 g accuracy and a minimum 250 g capacity.7.2 Heat-Resistant Test Tube, 25mm width by 150mm height.7.3 Thermom
25、eter, AP style, 0 to 250C, conforming to Specification 250C range.E1.7.4 Thermometer, -100 to 50C range.7.5 Hot Air Gun Gun6, 260 to 399C, 120 volts, alternating current (VAC), 60 HZ, 14A.7.6 Auxiliary Equipment, (that is, mixing loop (if desired), lab stand, and test tube clamp, 500-mL beaker for c
26、ooling, 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 and 18.00 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 clamp with the therm
27、ometer and mixing loop (optional).4 National Association of Printing Ink Manufacturers (NAPIM), 581 Main St., Woodbridge, NJ 07095, (napimnapim.org).5 Available from Testprint B. V., Zilverweg 10, PO Bos 127, 8440 AC Heerenveen, The Netherlands.6 The sole source of supply of the hot air gun, Model H
28、G-501A known to the committee at this time is Master Appliance Corp., Racine, WI 53403. If you are aware ofalternative suppliers, please provide this information to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of the responsibletechnical committee,1
29、which you may attend.D6038 1429.3 Aim the heat gun at the bottom of the test tube (keep nozzle 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 remove the stirring apparatus from the mixture.9.5 WarningCare
30、must be taken in stirring the resin/solvent mixture not to drop the thermometer or stirring loop. This couldcause the test tube to break, which could cause a serious fire or accident.9.6 Heat to 200C; hold this temperature for 2 min, and then remove the heat source.NOTE 4Low softening point and very
31、 compatible resins will dissolve at temperatures well below 200C. The maximum temperature to dissolve suchresin and solvent mixtures can be much lower than 200C. In such cases the maximum temperature for the test should be one agreed upon between thecustomer and the supplier.9.7 Check to see that al
32、l resin is dissolved.9.8 Start to blow ambient air from the heat gun onto the test tube.9.8.1 If the mixture is not clear after heating for 2 min at 200C, continue to heat until dissolution has occurred. Start the coolingprocedure at this point.9.8.2 If the mixture is clear except for a very slight
33、presence of precipitate, continue to end point and note the presence of “slightprecipitate.”9.8.3 If the mixture does not become clear or exhibits significant precipitation, record it as incompatible.9.9 Observe mixture closely as temperature drops and record the approximate rate of cooling, and the
34、 temperature at whichsolution becomes so cloudy that the thermometer, when held at the back wall of the test tube, can no longer be read (or thethermometer fluid can no longer be seen). This is observation is defined as the precipitation temperature or cloud point (see Note5 and Note 6).NOTE 5Coolin
35、g water, ice water, or a dry ice/acetone bath and a low temperature thermometer may be needed to reach the precipitation temperaturefor very soluble resins.NOTE 6This test method is recommended for resins and solvent mixtures exhibiting a precipitation temperature between 50 and 180C at 10 % resinso
36、lids. If a mixture is out of that range, a change in resin concentration (for example, 20 % solids) or solvent is recommended.10. Report10.1 A report on precipitation temperature should note the following information:10.1.1 Sample identification number,10.1.2 Test run number,10.1.3 Maximum temperatu
37、re achieved,10.1.4 Approximate rate of cooling, and10.1.5 Precipitation temperature.11. Precision and Bias711.1 PrecisionAn interlaboratory study of the precipitation temperature of two resins was run by seven laboratories.11.1.1 The precision estimates here are based on one analyst in each laborato
38、ry performing triplicate determinations on eachof two materials.11.1.2 Practice E180 was used in developing these precision statements.11.2 Repeatability (Within-Laboratory)The standard deviation of results obtained by the same analyst running the differentanalyses has been estimated to be 0.8 absol
39、ute at 20 df at the 60C level and 2.4 absolute at 20 df at the 160C level. The 95 %limit for the difference between two such averages is 2.1 absolute and 6.7 absolute, respectively.11.3 Reproducibility (Multilaboratory)The standard deviation of results obtained by analysts in different laboratories
40、has beenestimated to be 4.1 absolute at 6 df at the 60C level and 6.9 absolute at 6 df at the 160C level. The 95 % limit for the differencebetween two such averages is 11.5 absolute and 19.3 absolute, respectively.11.4 BiasThe procedure in this test method has no bias because the value of the precip
41、itation temperature is defined in termsof this test method.AUTOMATED METHOD12. Apparatus12.1 Balance or Scale, weighing to 60.02 g accuracy and a minimum 250 g capacity.12.2 ChemotronicProgrammable Cloudpoint Tester. Tester.7 Supporting data have been filed at ASTM International Headquarters and may
42、 be obtained by requesting Research Report RR:D01-1103. Contact ASTM CustomerService at serviceastm.org.D6038 14312.3 Glass Tube Tube5with with external diameter 22 mm, length 20 cm.12.4 Mortar and Pestle.12.5 Teflon Magnetic Stirring Bar Bar, 5 length 50 mm, diameter 7 mm.12.6 Teflon Tube Holder. H
43、older.513. Materials13.1 PRIFRAC 2981 stearic acid. acid.513.2 Haltermann N-C16 oil. oil.514. Sample Preparation14.1 Pulverize the solid resin to a size no larger than 3 mm2.15. Instrument Calibration15.1 Place the test tube with stirring magnet and test tube holder on the balance.15.2 Weigh 10 6 0.
44、02 g of PRIFRAC 2981 stearic acid acid5 with 10 6 0.02 g of Haltermann N-C 16 oil 5 into the test tube.15.3 Place the thermocouple assembly on the tube and into the Chemotronic.programmable cloudpoint tester.15.4 Start the test.15.5 Results should be repeated and the final cloud point for correct ca
45、libration of the instrument is 58C 6 1. If the instrumentis outside these parameters, consult your manual for troubleshooting or call the manufacturer.15.6 The manufacturer suggest calibration every two weeks.16. Procedure16.1 Insert the magnetic stirring bar into the test tube. Place the test tube
46、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 solvent to betested into the test tube.NOTE 7Care should be taken to wash down the dust on the sides of the tube with solvent.16.3 Place the test tube with test samp
47、le into the Chemotronic Cloudpoint Testerprogrammable cloudpoint tester and insert thethermocouple assembly attached to the instrument.16.4 Start the standard cloud point sequence for both the Chemotronic I and II machines. For the Chemotronic I, turn on the“Motor” button (setting should be 5). Pres
48、s the “Reset” button. (The “sensitivity” setting should be at 5.) Then press the “Run”switch to start the test.and the machine will run automatically.16.5 For the Chemotronic II, start the standard machine program with all default values. Press the start button, and the machinewill run automatically
49、.NOTE 8Resins that have not been tested before may require the operator to lift the tube right after the instrument establishes a cloud point value.A visual inspection will ensure the resin is totally dissolved.NOTE 8Resins that have not been tested before may require the operator to lift the tube once the test reaches 230C. A visual inspection shouldconfirm that the resin is in solution and that the solution is clear.16.5 The instrument will print a record of the cloud point temperature.16.6 Remove the test tube from the i
