1、Designation: D5165 12Standard Practice forLaboratory Preparation of Gelled Vehicles Using a ResinKettle1This standard is issued under the fixed designation D5165; 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 () indicates an editorial change since the last revision or reapproval.1. Scope*1.1 This practice covers a laboratory procedure for thegelation of a resin solution, ink varnish, or vehicle using a resinkettle.
3、1.2 Guidance in preparing gelled vehicle samples suitablefor use in laboratory sample quantity oil-based printing inks isprovided.1.3 The procedure outlined is not intended as a means ofrating or evaluating resin or vehicle gelability, and is applicableonly if the solutions, varnishes, or vehicles p
4、roduced are of arheology that is measurable by conventional ink and varnishindustry viscometers or rheometers.1.4 The values stated in SI units of measurement are to beregarded as the standard. The values given in parentheses arefor information only.1.5 This standard does not purport to address all
5、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 applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D154 Guide for Testing
6、 VarnishesD1545 Test Method for Viscosity of Transparent Liquids byBubble Time MethodD1725 Practice for Preparing Resin Solutions for ViscosityMeasurement by Bubble Time MethodD4040 Test Method for Rheological Properties of PastePrinting and Vehicles by the Falling-Rod ViscometerE1 Specification for
7、 ASTM Liquid-in-Glass Thermometers3. Terminology3.1 Definitions:3.1.1 gel or gelled vehicleany resin solution, or a morecomplex blend of resins and alkyds that has been cooked tobuild molecular weight or reacted with a gelling or crosslinkingagent (for example, organo-aluminum compounds) and exhib-i
8、ts a pseudoplastic rheology.3.1.2 pregel or pregel vehiclethe resin solution or vehiclecomponents comprising the vehicle prior to the addition ofgelling agent and viscosity adjusting solvent.3.1.2.1 DiscussionThe terms “vehicle” and “varnish” arecommonly used interchangeably. Some vehicle and varnis
9、hchemists, however, may consider a varnish to be a vehicle thatundergoes a chemical reaction during a cooking cycle.3.1.3 gel seed, na non-homogeneous, gelatinous particlein a gel vehicle, often the result of poor mixing or localizedover-reaction during gelation.4. Summary of Practice4.1 Prepare a p
10、regel vehicle by dissolving all vehicle orvarnish components, or both, in a heated 1-L, resin kettle withinert gas blanket.4.2 Add gellant solution into the pregel vehicle. Mix usingthe suggested stirring rate at the prescribed reaction tempera-ture for 1 h.4.3 Remove the resin kettle from heat, eva
11、luate, adjust ifnecessary, and re-evaluate.5. Significance and Use5.1 This practice provides a means of preparing gel vehiclesin laboratory equipment that most closely resembles produc-tion reactors. It can be used to predict the performance of gelvehicle components (resins, gellants, alkyds, etc.)
12、in the usersequipment.5.2 An ample amount of gel vehicle can be prepared for usein preparing inks for press testing.6. Apparatus (see Fig. 1)6.1 Balance or Scale, accurate to 0.1 g.6.2 Resin Kettle, 1-L with 5-neck kettle head.6.3 Electric Stirrer, equipped with speed control.6.4 Glass Stirring Rod.
13、1This practice is under the jurisdiction of ASTM Committee D01 on Paint andRelated Coatings, Materials, and Applications and is the direct responsibility ofSubcommittee D01.37 on Ink Vehicles.Current edition approved Nov. 1, 2012. Published December 2012. Originallyapproved in 1993. Last previous ed
14、ition approved in 2004 as D5165 93 (2004)which was withdrawn June 2010 and reinstated in November 2012. DOI: 10.1520/D516512.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information,
15、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 C700, West Conshohocken, PA 19428-2959, United States.6.5 Paddle, 6.4 cm (2.5 in.) in width.6.6 Heating Mantl
16、e, to fit 1-L resin kettle.6.7 Electronic Temperature Control Device.6.8 Thermometer, capable of reading, 0 to 250C andconforming to Specification E1. Alternately, temperature mea-suring devices such as liquid-in-glass thermometers, thermis-tors, thermocouples, or platinum resistance thermometers th
17、atprovide equivalent or better accuracy and precision, that coverthe temperature range specified, may be used.6.9 Inert Gas Blanket Source, (for example, nitrogen, car-bon dioxide).6.10 Auxiliary Equipment, (that is, stopper, Y tube, con-denser, bubbler, etc.).6.11 Insulated Gloves.7. Reagents and M
18、aterials7.1 Nonvolatile materials will include resins, alkyds,gellants, etc., consistent with those used in the manufacture oflithographic ink vehicles (for example, aromatic hydrocarbonresins, modified rosin ester resins, long oil linseed isophthalicalkyds, and aluminum compounds).7.2 Solvents used
19、 in this procedure will be those most oftenused in the manufacture of lithographic ink vehicles, forexample, hydrocarbon petroleum distillate C12C16.8. Procedure8.1 Weigh oil, solvent, and alkyd components for a 500-gsample into resin kettle. Do not add resin and gellant compo-nents at this time.8.2
20、 Separately prepare a gellant solution to be added afterresin dissolution. Dilute gellant to between 30 and 50 % gellantwith the major vehicle solvent.8.3 Start mixer; be sure that all materials are mixing.8.4 Start heating the mixture to 160C, (or the definedreaction temperature) at full power, und
21、er inert gas blanket andrefluxing. Record time.8.5 Slowly add the resin component.8.6 At 150C, reduce to approximately34 power andcontinue heating to 160C.8.7 When the temperature reaches 160C, check that allsystems components have been dissolved into a homogeneoussolution. If yes, record the time a
22、nd the r/min of the stirrer (ifpossible). If not, allow system to mix until all components aredissolved.8.8 After a homogeneous vehicle is obtained, reduce thesolution temperature to 135C.8.9 Add the desired quantity of gellant solution to the pregelvehicle and mix thoroughly.8.10 Raise reaction tem
23、perature to 160C (or defined reac-tion temperature), stirring at 380 to 420 r/min (if able todetermine stirring speed), and record time.NOTE 1Different gellants have different activation temperatures, anddifferent resins have different reactivity.Adjust temperature accordingly tocomplete reaction wh
24、ile preventing gel seeding.8.10.1 Hold at 160C, or other reaction temperature, for 1 h,with constant stirring.8.11 After 1 h, or the prescribed reaction cycle, discontinueheating.8.12 Allow kettle to cool to a safe handling temperature.8.13 Collect test sample from the kettle and evaluate.8.14 Based
25、 on the results of the evaluation, make adjust-ments as necessary to the gel varnish before discharging (forexample, adding resin, adding gellant, adding solvent). Repeatsteps from above to achieve desired test results.8.15 Once gel vehicle passes test requirements, transfer intoa 1-qt can or other
26、container.9. Evaluation9.1 Sample should be tested immediately after preparation,and after 24 h, to determine the effects of post gelation.9.2 Guide D154 outlines many methods applicable to thetesting of varnishes. It is an excellent guide for those lookingfor specific areas of evaluation.9.3 Lightl
27、y gelled resin solutions and vehicles can be testedfor changes in viscosity by using either Test Methods D1545 orD1725. These test methods both use Gardner bubble tubes todetermine the viscosity of liquids.9.4 Another test method for testing gelled ink vehicles isTest Method D4040. This test method
28、utilizes a falling-rodviscometer and can be used to determine the non-Newtoniannature of vehicles. The test method gives poor precision,however. Other viscometers used for determining the rheologyof gelled vehicles include: variable shear rate viscometers, andcone and plate viscometers.FIG. 1 Gel Ve
29、hicle Preparation ApparatusD5165 12210. Report10.1 Report the following information on vehicle prepara-tion:10.1.1 Sample identification,10.1.2 Test run,10.1.3 Starting time of heat-up,10.1.4 Initial stirring rate in r/min,10.1.5 Time when vehicle temperature reaches 160C, ordefined reaction tempera
30、ture,10.1.6 Time at which all pregel material is dissolved,10.1.7 Time at which cooling cycle is initiated,10.1.8 Time at which pregel vehicle reached 120C orbelow,10.1.9 Time when gellant solution is added to pregel ve-hicle,10.1.10 Time when heat up cycle toward 160C has begun,10.1.11 Length of ti
31、me that the reaction is held at 160C orthe optimum reaction temperature, and10.1.12 Time and temperature when gel vehicle is pouredfor storage.10.2 A report on gel vehicles properties should contain:10.2.1 Sample identification,10.2.2 Test run identification, and10.2.3 Results of the analyses made.
32、In the case of fallingrod viscometer determinations the following data could beobtained using Test Method D4040:10.2.3.1 Apparent viscosity at 2500/s at 25C,10.2.3.2 Pseudo-Bingham Yield value at 25C,10.2.3.3 Shortness ratio (yield value/apparent viscosity),and10.2.3.4 Slope (non-Newtonian parameter
33、) as defined inTest Method D4040.11. Keywords11.1 falling rod viscometer; gel; gelability; gelled varnish;gelled vehicle; non-Newtonian fluid; pregel; pregel varnish;pregel vehicle; slope; yield value shortness ratioSUMMARY OF CHANGESCommittee D01.37 has identified the location of selected changes t
34、o this standard since the last issue (D5165 93 (2004) that may impact the use of this standard. (Approved November 1, 2012.)(1) Terminology added definition for “gel seed.”(2) Procedure clarified optimum order of addition. Addedcommentary/caution regarding gel reactivity and the potentialto generate
35、 gel seeds during the reaction.ASTM 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 validity of any such patent rights, and the riskof i
36、nfringement of such rights, are entirely their own responsibility.This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years andif not revised, either reapproved or withdrawn. Your comments are invited either for revision of this sta
37、ndard or for additional standardsand should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of theresponsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you shouldmake your
38、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). Permission rights to photocopy the standard may also be secured from the ASTM website (www.astm.org/COPYRIGHT/).D5165 123
