ASTM D5062-09(2017) Standard Test Method for Resin Solution Dilutability by Volumetric Gravimetric Determination.pdf

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1、Designation: D5062 09 (Reapproved 2017)Standard Test Method forResin Solution Dilutability by Volumetric/GravimetricDetermination1This standard is issued under the fixed designation D5062; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revi

2、sion, 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. Scope1.1 This test method covers both volumetric and gravimetricdetermination of resin solution dilutability

3、which gives anumerical value for the overall solubility of the resin expressedas percent dilutability.1.2 This test method is applicable only if the test solution isof sufficient clarity to allow accurate visual judgement of theend point and of low enough viscosity for efficient mixing totake place.

4、1.3 This test method is primarily for, but not limited to,resins used in the printing ink industry.1.4 The percent solvent tolerance of a resin can be deter-mined using this test method if the solvent in the resin solutionand the dilution solvent are the same.1.5 The values stated in SI units are to

5、 be regarded asstandard. No other units of measurement are included in thisstandard.1.6 This standard does not purport 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

6、 determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D1725 Practice for Preparing Resin Solutions for ViscosityMeasurement by Bubble Time MethodE1 Specification for ASTM Liquid-in-Glass Thermometers3. Terminology3.1 Definitions of Terms Spec

7、ific to This Standard:3.1.1 resin solution dilutability, nthe maximum amount ofdiluent tolerated to reach a defined degree of turbidity; beyondthis point, resin precipitation will occur.4. Summary of Test Method4.1 Asample of resin solution is weighed into a glass beakerthat is placed over a piece o

8、f 10 point print (standardnewspaper print).4.2 The dilution solvent is added slowly from a buret untilthe newsprint can no longer be read (cloud point) when viewedfrom the top of the beaker.4.3 The solvent dilutability is calculated by weight, orvolume.5. Significance and Use5.1 This test method pro

9、vides a means for resin producersand users as well as solvent and varnish manufacturers to ratevarious types of resins for solubility by assigning a numericaldilutability value. This percent dilutability value can be used todifferentiate resin types for end users and can be utilized as aquality cont

10、rol tool by resin manufacturers.5.2 When running a series of these tests, the same lot orbatch of dilution solvent must be used throughout to ensurereproducible results.6. Apparatus6.1 Glass Beakers, 150-mL (51-mm diameter, 79-mmheight) and 250-mL (65-mm diameter, 90-mm height).6.2 Graduated Buret,

11、50 mL.6.3 Constant Temperature Water Bath at 25C.6.4 Thermometer, 0 to 40C range with subdivisions of0.5C conforming to Specification E1.6.5 Magnetic Stirring Bar and Stirring Plate or StirringRod.6.6 Sheet of Newsprint, with 10-point (Note 1), No. 31old-style type, lower case letters 1.5-mm high wi

12、th normalspacing, upper and lower case with no italicized or bold letters.NOTE 1The term point is derived from the American Point System.72 points=1in.1This test method is under the jurisdiction of ASTM Committee D01 on Paintand Related Coatings, Materials, and Applications and is the direct respons

13、ibility ofSubcommittee D01.37 on Ink Vehicles.Current edition approved Feb. 1, 2017. Published February 2017. Originallyapproved in 1990. Last previous edition approved in 2009 as D5062 09. DOI:10.1520/D5062-09R17.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM C

14、ustomer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United StatesThis international standard was de

15、veloped in accordance with internationally recognized principles on standardization established in the Decision on Principles for theDevelopment of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.17. Reagents and

16、Materials7.1 Resin SolutionA resin solution prepared in such a wayas to provide an accurate percent solids and to have sufficientclarity to allow accurate visual judgment of the cloud point.The solution must also have low enough viscosity at 25C toallow efficient mixing during the addition of the di

17、lutionsolvent.7.2 Dilution SolventThe dilution solvent for this test istypically, but not limited to, a hydrocarbon. The dilutionsolvent should have minimal loss by evaporation at roomtemperature, and be agreed upon between the purchaser and thesupplier.7.3 Standard Ink Oils.8. Procedure8.1 Preparat

18、ion of Resin Solution:8.1.1 The resin solution may be prepared by either heatingthe resin/solvent combination as described in Test MethodD1725, or dispersing using a high-speed mixer such as ablender. Please note results may vary dependent on method ofpreparation.8.1.2 The ratio of resin to solvent

19、in the preparation shouldcorrespond as much as possible to the intended end use of thematerial, but should be chosen to avoid difficulty in effectingsolution at a low enough viscosity for efficient mixing duringdilution.8.1.3 The precision of weighing the resin and solvent shouldensure a maximum dev

20、iation of 61 % in the desired concen-tration. This percent solids must not be altered during resinsolution preparation by solvent loss.8.2 Determine the proper choice of beaker as follows:8.2.1 If no previous dilutability data is available for the testsample, start the test with a 150-mL glass beake

21、r.8.2.2 If previous dilutability data indicates that the testsample is highly soluble, start the test with a 250-mL glassbeaker.8.3 Weigh the beaker with the magnetic stirrer bar or stirringrod. Record this tare weight as W1.8.4 Accurately weigh 10 6 0.1 g of the resin solution intothe beaker. Recor

22、d this sample weight as W2.8.5 Place the beaker in a 25C constant temperature bathuntil the resin solution reaches 25 6 1C as measured with thethermometer specified in 6.4.8.6 Prepare the dilution solvent by bringing it to a tempera-ture of 25 6 1C before adding it to the buret.8.7 Place the beaker

23、over the piece of 10-point print andbegin adding solvent slowly (5 to 6 mL/min) while stirring.Ensure that the sample temperature remains at 25 6 1C,which may require periodic return of the beaker to the waterbath. If the sample has started to form a haze it should not bereturned to the water bath.8

24、.8 Observe the 10-point print from the top of the beakerlooking through the solution.8.9 If the resin solution begins to cloud, add solvent slowlyone drop at a time while continuing to mix. Do not return thesample to the water bath at this point. If more than 100 g isrequired for the solution to beg

25、in to cloud, repeat the testbeginning at 8.4 using a 250-mL glass beaker.8.10 If the resin solution begins to cloud, add solvent slowlyone drop at a time while continuing to mix. Do not return thesample to the water bath at this point. If more than 200 g isrequired, the resin solution can be conside

26、red infinitely solubleunless otherwise specified in an agreement between the pur-chaser and supplier.8.11 The end point is reached when the 10-point printcannot be read looking through the solution from the top of thebeaker.8.12 Record the final weight of the beaker and its contents(W3).8.13 Record

27、the sample temperature at the end point.9. Calculation9.1 Calculate the percent resin solution dilutability, D,asfollows:D 5W32 W11W2!W23100 (1)9.2 Calculate the percent solvent tolerance of the resin, S,(percent resin solids at cloud point) as follows:T 5W23 S/100!#W21W32 W11W2!#3100 (2)where S = r

28、esin in solution, %.10. Report10.1 Report the following information:10.1.1 The identification of the resins and the solvent in thesolution as well as the dilution solvent,10.1.2 The method used to prepare the resin solution,10.1.3 The percent solids of the resin solution, and10.1.4 The percent resin

29、 dilutability value or volume ofsolvent added per weight solution, and operating conditionsincluding air temperature, relative humidity, initial resin solu-tion temperature, final resin solution temperature, initial dilu-tion solvent temperature, and final dilution solvent tempera-ture.11. Precision

30、11.1 An interlaboratory study was conducted in which oneoperator in each of eight laboratories determined the percentdilutability of two common resin solutions and two dilutionsolvents completed in duplicate on two different days. Thepooled within-laboratory standard deviation was found to be3.25 %

31、of the value measured with 12 df. The between-laboratory standard deviation was 7.63 % of the value mea-sured with 28 df. Based on these standard deviations, thefollowing criteria should be used for judging the acceptabilityof results at the 95 % confidence level.11.2 RepeatabilityTwo results, each

32、the mean of duplicatedeterminations, obtained by the same operator should beconsidered suspect if they differ by more than 9.19 % of thevalue measured.D5062 09 (2017)211.3 ReproducibilityTwo results, each the mean of dupli-cate determinations obtained by operators in differentlaboratories, should be

33、 considered suspect if they differ bymore than 23.38 % of the value measured.12. Keywords12.1 dilutability value; percent dilutability; printing inkresins; resins; resin solution cloud point; resin solution di-lutability; solvent toleranceASTM International takes no position respecting the validity

34、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 infringement of such rights, are entirely their own responsibility.This standard is subject t

35、o 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 standard or for additional standardsand should be addressed to ASTM International Headquarters.

36、 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 views known to the ASTM Committee on Standards, at the address shown below.This standard is

37、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 Copyright Clearance Center, 222Rosewood Drive, Danvers, MA 01923, Tel: (978) 646-2600; http:/ 09 (2017)3