1、Designation: D5958 99 (Reapproved 2011)Standard 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 r
2、evision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1. Scope1.1 These practices describe laboratory procedures for pre-paring an oil-based ink resin solution in a high-boiling solventusing
3、 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 Subcommittee D01.37 recommends using the hot oilbath procedure (Practice D5597) where possible.
4、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 regulate themaximum temperature, can be done under an inert atmosphere,and can prevent t
5、he 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 hydrocarbonresins, modified dicyclopentadiene resins, rosin pentaerythritolor glycerine
6、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 distillates, 2,2,4 trimethyl 1,3-pentanedioldi-isobutyrate,2alkali refined linseed oil, tridecyl
7、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 the solventsused should be 60C (140F) as determined by Test MethodD56.(WarningUsers of this
8、 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 there is thepotential for vapor ignition. Do the methods outlined in ashielded exhaust hood,
9、where there is access to a fire extin-guisher if needed.)1.7 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.8 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is theresp
10、onsibility 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. Referenced Documents2.1 ASTM Standards:3D56 Test Method for Flash Point by Tag Closed Cup T
11、esterD1310 Test Method for Flash Point and Fire Point ofLiquids by Tag Open-Cup ApparatusD1725 Test Method for Viscosity of Resin SolutionsD5062 Test Method for Resin Solution Dilutability byVolumetric/Gravimetric DeterminationD5597 Practice for Preparation of Oil-Based Ink ResinSolutions Using a Ho
12、t Oil Bath4E1 Specification for ASTM Liquid-in-Glass ThermometersE230 Specification and Temperature-Electromotive Force(EMF) Tables for Standardized Thermocouples3. Terminology3.1 Definitions of Terms Specific to This Standard:3.1.1 cold cut, ndispersion of resin into solvent using highshear dispers
13、ion without external heating.3.1.2 compatibility, nresin and solvent mixture forms aclear, homogeneous, and stable solution.1These practices are under the jurisdiction of ASTM Committee D01 on Paintand Related Coatings, Materials, and Applications and are the direct responsibilityof Subcommittee D01
14、.37 on Ink Vehicles.Current edition approved June 1, 2011. Published June 2011. Originallyapproved in 1996. Last previous edition approved in 2005 as D5958 - 99 (2005)1.DOI: 10.1520/D5958-99R11.2The sole source of supply of the plasticizer TXIB known to the committee atthis time is Eastman Chemical
15、Company, / Texas E. M. Division, P.O. Box 7444,Longview, 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 atte
16、nd.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.4Withdrawn. The last approved version of this historical s
17、tandard is referencedon www.astm.org.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.3.1.3 dissolution, nthe point at which all resin completelydissolves in the solvent.3.1.4 incompatibility, nresin and solvent mixture is notcompatib
18、le, an opaque or two-phase mixture results.3.1.5 oil bath, nnon-volatile, silicone fluid contained in alarge heat resistant crystallizing dish heated by a temperaturecontrolled stirrer hot-plate.3.1.6 solution, nresin and solvent form a clear, compat-ible, and homogeneous mixture.3.1.6.1 DiscussionI
19、ndustrial practice may use the term“solution” loosely to describe what may actually be a clear“dispersion.” For the sack 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
20、 resin and solvent in a250-mL Erlenmeyer flask.4.2 A hot oil bath is heated to the required dissolutiontemperature (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 in
21、to the hot oil bath with inert gas purgeand a cold water condenser.4.4 Allow the mixture to mix at the 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 samp
22、le for future testing.5. Significance and Use5.1 These practices provide means of preparing small quan-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 testin
23、g during the manufacture ofresin solutions and vehicles. Samples can usually be preparedin approximately 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
24、(thatis, C12to C16hydrocarbon petroleum distillate with initialboiling point (IBP) about 470F).6. Apparatus6.1 Balance, capable of weighing to 60.01 g accuracy.6.2 Sieve, 16-mesh.6.3 Thermometer (see Specification E1)orThermocouple(see Specification E230), AP style with a range of 0 to 250C.6.4 Heat
25、 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 with 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 c
26、lamp, glass bubbler filled with mineral oil,inert gas source, etc.).6.10 Assembly of Hot Oil Bath Set-Up Place a stirrer/hotplate in an aluminum tray on a lab jack. Put the crystallizationdish filled approximately23 with silicone oil on top of the hotplate. Arrange the condenser above the center of
27、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. Lower the flask intothe oil bath.7. Reagents7.1 Solvents used in this procedure will be those most oftenused in the manufacture
28、 of lithographic ink vehicles, forexample, hydrocarbon petroleum distillate C12to C16andvegetable oils.8. Reagents and Materials8.1 Nonvolatile Resins, (for example, hydrocarbon resins,rosin ester resins).8.2 Solvents, used in this procedure will be those most oftenused in the manufacture of lithogr
29、aphic ink vehicles, forexample, alkali refined linseed oil (ARLO), hydrocarbonpetroleum distillate C12to C16.8.3 The resins and solvents agreed upon between producerand user.8.4 Standard Ink Oils.59. Procedure9.1 Set the hot oil bath to heat at the specified temperature.Set the temperature, if possi
30、ble, 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 resins.)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
31、.02 g, an appropriate amount ofthe screened resin into a 250-mL Erlenmeyer flask to meet theconcentration requirements for preparation of a 30 to 100-gsample. Typically 100 g of solution is prepared.5Suitable standard ink oils are available from several suppliers. Please contactthe National Associat
32、ion of Printing Ink Manufacturers, Inc., (NAPIM) at 581 MainSt., Woodbridge, NJ 07095; (email: napimnapim.org) for assistance.D5958 99 (2011)29.3.1 Examples of common ink resin solutions are asfollows:Solution No. 1 Percent Solution No. 2 Percentresin 33.3 resin 50alkali refined linseed oil 66.7 470
33、F IBP ink oil 50100.0 1009.3.2 High-viscosity, high-molecular weight, (“structured”or “self-gelling”) resins may 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 Perc
34、entresin 50TXIB 50100.09.4 Weigh concentration of solvent needed to the nearest 0.1g.9.5 Place flask containing 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
35、 bath (but not touching the bottom)for the stir bar to mix efficiently. Maintain inert gas flow overthe resin-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 res
36、in isdissolved.9.7 Check to see that all resin is dissolved.9.8 After all the resin is in solution, and if the 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
37、 desired, record the time and temperature at whichdissolution occurred or the maximum temperature at which themixture 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. Re
38、port11.1 Report on solution preparation the following informa-tion:11.1.1 Dissolution time and temperature,11.1.2 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 Prac
39、tice12.1 Small samples of ink resin and aliphatic ink oil or inkresin and alkali-refined linseed oil (ARLO) are 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 viscosit
40、y and aliphatic solubility or com-patibility of a printing ink resin.13. Apparatus13.1 Erlenmeyer Flask, 125-mL, 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 l
41、ength.13.3 Thermometer, No. 42C, conforming to SpecificationE1, or other accurate temperature measuring device capable ofmeasuring to 220C or greater, in 1C increments.13.4 Cork Stopper, high quality, designed to fit the flaskused. This cork is then bored out appropriately to receive thethermometer
42、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-up.13.5 Hot Plate Stirrer, capable of a surface temperature of300C.13.
43、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 in 12.1 (Note: the mass should be between 30 and 45g). Weigh into the
44、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 temperature controller to a settingthat will give a surface temperatu
45、re 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 atemperature of 215C.14.7 The hot plate surface temperature is correct
46、 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.15. Procedure15.1 Crush large size pieces of resin sample and pass thecrushed resin through a 16-mesh sieve.15.2 Weigh to 60.02 g into the
47、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.D595
48、8 99 (2011)3NOTE 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 weighing accuracies.15.4 Affix the thermometer/cork assembly in the mouth ofthe flask. Adjust the thermometer tip so
49、it is just off the bottomsurface of the flask (1 mm).15.5 Place the flask on the hot plate stirrer that has beenheated 10 min to the calibrated setting derived in Section 14.15.6 Without stirring, let the ink resin-solvent slurry heat to100C.15.7 When the temperature reaches 100C, begin stirringthe mixture. Keep the stir rate slow at first (so that resin ismoving in the solvent but does not splash resin up above thesolvent level). For more efficient dissolution, mixing speed isgradually increased as the resin softens. Avoid over-stirringthat cause
