1、Designation: D5958 99 (Reapproved 2012)1Standard Practices forPreparation of Oil-Based Ink Resin Solutions1This standard is issued under the fixed designation D5958; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last
2、revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1NOTEThermometer references and Footnote 5 were editorially corrected in November 2012.1. Scope*1.1 These practices describe laboratory
3、 procedures for pre-paring an oil-based ink resin solution in a high-boiling solventusing four pieces of lab equipment; (1) a hot oil bath (Sections4 to 11),(2) a stirrer/hot plate (Sections 12 to 16),(3) an industrial blender (Sections 17 to 22), and(4) a hot air gun (Sections 23 to 27).ASTM Subcom
4、mittee D01.37 recommends using the hot oilbath procedure (Practice D5597) where possible.1.2 These practices use laboratory equipment generallyavailable in a normal, well-equipped laboratory.1.3 One or several of these practices allows for rapid resinsolution preparation (under 30 min, typical), can
5、 regulate themaximum temperature, can be done under an inert atmosphere,and can prevent the random solvent loss during preparation.1.4 These procedures are for use with ink resins intendedmainly for oil-based offset and letterpress inks. The type ofresins are typically, but not limited to C9aromatic
6、 hydrocarbonresins, modified dicyclopentadiene resins, rosin pentaerythritolor glycerine esters, phenolic modified rosin esters, maleicanhydride modified rosin esters, and naturally occurring resinssuch as gilsonite.1.5 The typical high boiling solvents to be used include C12to C16petroleum distilla
7、tes, 2,2,4 trimethyl 1,3-pentanedioldi-isobutyrate,2alkali refined linseed oil, tridecyl alcohol, orcombinations of the above.1.6 To avoid fire or injury, or both, to the operator, thesepractices should not be used with low flash point solvents suchas toluene or xylene. The minimum flash point of th
8、e solventsused should be 60C (140F) as determined by Test MethodD56.(WarningUsers of this practice should be aware thatthe flash point of many solvents used for this test (as defined inTest Methods D56 and D1310) is exceeded in the heating cycleof this test method. Take safety precautions since ther
9、e is thepotential for vapor ignition. Do the methods outlined in ashielded exhaust hood, where there is access to a fire extin-guisher if needed.)1.7 The values stated in SI units are to be regarded asstandard. The values given in parentheses are for informationonly.1.8 This standard does not purpor
10、t 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 applica-bility of regulatory limitations prior to use. For specific hazardstatement see 25.11.2. Refer
11、enced Documents2.1 ASTM Standards:3D56 Test Method for Flash Point by Tag Closed Cup TesterD1310 Test Method for Flash Point and Fire Point of Liquidsby Tag Open-Cup ApparatusD1725 Practice for Preparing Resin Solutions for ViscosityMeasurement by Bubble Time MethodD5062 Test Method for Resin Soluti
12、on Dilutability byVolumetric/Gravimetric DeterminationD5597 Practice for Preparation of Oil-Based Ink ResinSolutions Using a Hot Oil Bath (Withdrawn 1999)4E1 Specification for ASTM Liquid-in-Glass ThermometersE230 Specification and Temperature-Electromotive Force(EMF) Tables for Standardized Thermoc
13、ouples3. Terminology3.1 Definitions of Terms Specific to This Standard:1These practices are under the jurisdiction of ASTM Committee D01 on Paintand Related Coatings, Materials, and Applications and are the direct responsibilityof Subcommittee D01.37 on Ink Vehicles.Current edition approved Nov. 1,
14、2012. Published November 2012. Originallyapproved in 1996. Last previous edition approved in 2011 as D5958 99 (2011).DOI: 10.1520/D5958-99R12E01.2The sole source of supply of the plasticizer TXIB known to the committee atthis time is Eastman Chemical Company, / Texas E. M. Division, P.O. Box 7444,Lo
15、ngview, TX 75607-7444. If you are aware of alternative suppliers, please providethis information to ASTM International Headquarters. Your comments will receivecareful consideration at a meeting of the responsible technical committee,1whichyou may attend.3For referenced ASTM standards, visit the ASTM
16、 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.4The last approved version of this historical standard is referenced onwww.astm.org.*A Summary of Changes s
17、ection appears at the end of this standardCopyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States13.1.1 cold cut, ndispersion of resin into solvent using highshear dispersion without external heating.3.1.2 compatibility, nresin and solvent mi
18、xture forms aclear, homogeneous, and stable solution.3.1.3 dissolution, nthe point at which all resin completelydissolves in the solvent.3.1.4 incompatibility, nresin and solvent mixture is notcompatible, an opaque or two-phase mixture results.3.1.5 oil bath, nnon-volatile, silicone fluid contained
19、in alarge heat resistant crystallizing dish heated by a temperaturecontrolled stirrer hot-plate.3.1.6 solution, nresin and solvent form a clear,compatible, and homogeneous mixture.3.1.6.1 DiscussionIndustrial practice may use the term“solution” loosely to describe what may actually be a clear“disper
20、sion.” For the sake of simplification, the terms solutionand dispersion have been used interchangeably in this practice.HOT OIL BATH4. Summary of Hot Oil Bath Practice4.1 Place the required amount of resin and solvent in a250-mL Erlenmeyer flask.4.2 A hot oil bath is heated to the required dissoluti
21、ontemperature (150 to 200C, typically about 180C or slightlyhigher for high softening point or poorly solvated resins).4.3 The Erlenmeyer flask containing the mixture of resinand solvent is placed into the hot oil bath with inert gas purgeand a cold water condenser.4.4 Allow the mixture to mix at th
22、e desired temperatureuntil all of the resin is completely dissolved.4.5 Remove the flask from the hot oil bath and allow it tocool while still under an inert atmosphere for 10 to 15 min.Save the sample for future testing.5. Significance and Use5.1 These practices provide means of preparing small qua
23、n-tities of resin solution (in some procedures in an inert gasatmosphere using uniform, controlled heating).5.2 This practice provides quick ways to prepare a resinsolution for quality control testing during the manufacture ofresin solutions and vehicles. Samples can usually be preparedin approximat
24、ely 30 to 45 minutes or less.5.3 These practices can be used to prepare commonlyspecified ink test solutions such as 33.3 % resin in alkalirefined linseed oil, and 50 % resin in heat-set ink solvent (thatis, C12to C16hydrocarbon petroleum distillate with initialboiling point (IBP) about 470F).6. App
25、aratus6.1 Balance, capable of weighing to 60.01 g accuracy.6.2 Sieve, 16-mesh.6.3 Thermometer, capable of reading 0 to 250C and con-forming to Specification E1. Alternately, temperature measur-ing devices such as liquid-in-glass thermometers, thermistors,thermocouples, or platinum resistance thermom
26、eters that pro-vide equivalent or better accuracy and precision, that cover thetemperature range specified, may be used.6.4 Heat Resistant Crystallizing Dish, 150 by 75 mm insize.6.5 Stirrer/Hot Plate, with a range of 38 to 371C.6.6 Condenser, with ground glass joints.6.7 Erlenmeyer Flask, 250-mL wi
27、th 24/40 joint top and sidearm.6.8 Silicone Oil.6.9 Auxiliary Equipment, (that is, a 76-mm stir bar, lab jack,lab stand, flask clamp, glass bubbler filled with mineral oil,inert gas source, etc.).6.10 Assembly of Hot Oil Bath Set-UpPlace a stirrer/hotplate in an aluminum tray on a lab jack. Put the
28、crystallizationdish filled approximately23 with silicone oil on top of the hotplate. Arrange the condenser above the center of the bath.Clamp the Erlenmeyer flask containing the solution ingredientson to the condenser. Adjust the flow of nitrogen to flow downthe condenser into the Erlenmeyer flask.
29、Lower the flask intothe oil bath.7. Reagents7.1 Solvents used in this procedure will be those most oftenused in the manufacture of lithographic ink vehicles, forexample, hydrocarbon petroleum distillate C12to C16andvegetable oils.8. Reagents and Materials8.1 Nonvolatile Resins, (for example, hydroca
30、rbon resins,rosin ester resins).8.2 Solvents, used in this procedure will be those most oftenused in the manufacture of lithographic ink vehicles, forexample, alkali refined linseed oil (ARLO), hydrocarbonpetroleum distillate C12to C16.8.3 The resins and solvents agreed upon between producerand user
31、.8.4 Standard Ink Oils.59. Procedure9.1 Set the hot oil bath to heat at the specified temperature.Set the temperature, if possible, at 10C above the softeningpoint of the resin, but below the initial boiling point of thesolvent. (180C is a common starting temperature for manyhigh-melting-point ink r
32、esins.)9.2 Crush large size pieces of resin sample and pass thecrushed resin through a 16-mesh sieve.9.3 Weigh to the nearest 0.02 g, an appropriate amount ofthe screened resin into a 250-mL Erlenmeyer flask to meet the5The use of ink industry recognized standard test oils (petroleum distillates) is
33、recommended for evaluating resins. The test oils are closely controlled from lot tolot to ensure consistent data. Sources and ordering information are available atwww.napim.org/testmethods/standardstest.aspx.D5958 99 (2012)12concentration requirements for preparation of a 30 to 100-gsample. Typicall
34、y 100 g of solution is prepared.9.3.1 Examples of common ink resin solutions are asfollows:Solution No. 1 Percent Solution No. 2 Percentresin 33.3 resin 50alkali refined linseed oil 66.7 470F IBP ink oil 50100.0 1009.3.2 High-viscosity, high-molecular weight, (“structured”or “self-gelling”) resins m
35、ay require a stronger solvent system.Possible resin solutions for use with these resins are as follows:Solution No. 3 Percentresin 45TXIB230243C (470F) IBP ink oil 25100.0Solution No. 4 Percentresin 50TXIB 50100.09.4 Weigh concentration of solvent needed to the nearest 0.1g.9.5 Place flask containin
36、g resin mixture into ground glassfitting on water-cooled condenser, secure flask with clamp, jackup hot oil bath under flask until the bottom of the flask is closeenough to the bottom of the bath (but not touching the bottom)for the stir bar to mix efficiently. Maintain inert gas flow overthe resin-
37、solvent mixture at approximately 1 bubble per 5 sthrough the outlet mineral oil bubbler. If lab jack not available,lower flask manually.9.6 Allow the mixture to continue mixing until all resin isdissolved.9.7 Check to see that all resin is dissolved.9.8 After all the resin is in solution, and if the
38、 solution isclear, lower the hot oil bath and allow the solution to coolunder the inert gas atmosphere.10. Evaluation10.1 During solution preparation, observe the dissolution ofresin and, if desired, record the time and temperature at whichdissolution occurred or the maximum temperature at which the
39、mixture was heated if the resin did not dissolve.10.2 Upon cooling, samples can be tested for viscosityfollowing Test Method D1725, dilutability following TestMethod D5062, color, etc.11. Report11.1 Report on solution preparation the following informa-tion:11.1.1 Dissolution time and temperature,11.
40、1.2 Solution clarity,11.1.3 Failure of resin dissolution, if necessary, and11.1.4 Maximum temperature at which resin failed to dis-solve.STIRRERHOT PLATE12. Summary of Stirrer/Hot Plate Practice12.1 Small samples of ink resin and aliphatic ink oil or inkresin and alkali-refined linseed oil (ARLO) ar
41、e cut intodispersion in an Erlenmeyer flask to a specific temperature, ata specified rate, with stirring.12.2 The resulting fluid dispersion can be used to measureparameters such as viscosity and aliphatic solubility or com-patibility of a printing ink resin.13. Apparatus13.1 Erlenmeyer Flask, 125-m
42、L, fitting the following de-scription: a height of 114 mL, an outside base diameter of 67mL, and an opening of 27 mL.13.2 Magnetic Stirring Bar, polytetrafluoroethylene-coated,and 25 mm in length.13.3 Thermometer, capable of reading 0 to 250C andconforming to Specification E1. Alternately, temperatu
43、re mea-suring devices such as liquid-in-glass thermometers,thermistors, thermocouples, or platinum resistance thermom-eters that provide equivalent or better accuracy and precision,that cover the temperature range specified, may be used.13.4 Cork Stopper, high quality, designed to fit the flaskused.
44、 This cork is then bored out appropriately to receive thethermometer in 13.3 in a snug fashion. The hole should bedrilled at an angle of approximately 25 so the tip of thethermometer comes to rest at the inside edge of the flask. Placea small groove on the side of the cork to prevent pressurebuild-u
45、p.13.5 Hot Plate Stirrer, capable of a surface temperature of300C.13.6 Stop Watch.14. Calibration and Standardization14.1 The setting of the hot plate surface temperature mustbe calibrated by making a blank run in the following manner.14.2 Determine the total mass of the intended solutiondescribed i
46、n 12.1 (Note: the mass should be between 30 and 45g). Weigh into the 125-mL Erlenmeyer flask a quantity ofARLO equal to the intended solution mass described in 12.2.Next, add the stirring bar and affix the thermometer/corkassembly described in 13.4 to the Erlenmeyer flask.14.3 Turn on the hot plate
47、temperature controller to a settingthat will give a surface temperature of approximately 300C.Allow the hot plate 10 min to heat up and equilibrate.14.4 Set the flask on the preheated hot plate stirrer and beginstirring.14.5 Start the stop watch.14.6 Measure the time required for the ARLO to reach a
48、temperature of 215C.14.7 The hot plate surface temperature is correct when theARLO heats from room temperature to 215C in 11 min 615s. On a hot plate, this is usually at a setting between 5 and 6 onthe temperature-controller dial.D5958 99 (2012)1315. Procedure15.1 Crush large size pieces of resin sa
49、mple and pass thecrushed resin through a 16-mesh sieve.15.2 Weigh to 60.02 g into the Erlenmeyer flask, the inkresin and solvent at the ratio agreed upon between producerand user. Typical resin solutions are noted in 9.3.1. The totalmass of ink resin solids and solvent should be between 30 and45 g.15.3 Carefully place the stirring bar into the flask to avoidsplashing the solvent.NOTE 1It is not recommended that the stirring bar be added to thetared flask while on an electronic balance. The magnetic field associatedwith the stirring bar can affect
