1、Designation: D 4713 92 (Reapproved 2007)Standard Test Methods forNonvolatile Content of Heatset and Liquid Printing InkSystems1This standard is issued under the fixed designation D 4713; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revisi
2、on, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon (e) indicates an editorial change since the last revision or reapproval.1. Scope1.1 These test methods cover the determination of weightcontent of nonvolatile matter in two types of pri
3、nting inks.1.2 Test MethodAis applicable to heatset-type printing inksand resin solutions; solvents in such systems typically haveinitial boiling points in the range from 240 to 275C (470 to535F) and vapor pressures less than 0.2 mm Hg.1.3 Test Method B is applicable to liquid-type printing inksand
4、vehicles based on aqueous or organic solvents that evapo-rate readily at ordinary room temperatures.NOTE 1Test Method A (for heatset systems) specifies a specimen filmthickness that is much thinner than those produced by related testmethods; one exception is Test Method B in Test Methods D 1259, whi
5、chis recommended as a referee test.NOTE 2Test Method B (for liquid ink systems) is similar to TestMethod D 2369 except that a solvent is not required for spreading the testspecimen.1.4 The values stated in SI units are to be regarded as thestandard. The values given in parentheses are for informatio
6、nonly.1.5 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 determine the applica-bility of regulatory limitations prior to use.2. Refere
7、nced Documents2.1 ASTM Standards:2D 1259 Test Methods for Nonvolatile Content of ResinSolutionsD 2369 Test Method for Volatile Content of CoatingsE1 Specification for ASTM Liquid-in-Glass ThermometersE 145 Specification for Gravity-Convection and Forced-Ventilation OvensE 691 Practice for Conducting
8、 an Interlaboratory Study toDetermine the Precision of a Test Method3. Summary of Test Methods3.1 Test Method AHeatset Systems. A 0.15-g specimen ismechanically spread in a 57-mm weighing dish to a nominalthickness of 80 6 10 g/m2and heated in a forced ventilationoven at 110C for 3 h.3.2 Test Method
9、 BLiquid Ink Systems.A0.5-g specimen isdispensed into a 57-mm weighing dish by means of a dispos-able syringe, mechanically spread out, and heated in an oven at110C for 1 h.4. Significance and Use4.1 Nonvolatile content of printing inks is useful for speci-fication acceptance between the producer an
10、d the user.4.2 In order to obtain accurate results for heatset systemswithin the specified 3-h heating time, the specimen filmthickness must be less than 100 g/m2, and the oven must haveforced ventilation. Thickness of the specimen film is lesscritical for liquid ink systems.5. Apparatus5.1 Balance,
11、 accurate to 1 mg.5.2 Oven, forced-ventilation type conforming to Type IIB inSpecification E 145 and maintained at 110 6 2C.5.3 Thermometer, bulb-type, capable of reading 110 6 2C,such as Thermometer 88C prescribed in Specification E1.5.4 Weighing Dish, such as an aluminum foil dish 57 mmwide, the l
12、id of a 1-lb ink can 94 mm wide, or otherflat-bottomed container. The bottom of the container must nothave a trough or depression into which the test material mightcollect.5.5 Spatula, or small ink knife.5.6 Spreading Device, one per weighing dish, of heat-stablematerial, such as a glass stirring ro
13、d or thick L-shaped wire.5.7 Forceps,5.8 Desiccator,5.9 Syringe3(for liquid ink systems only), single-use 2 to5-mL capacity without needle, or other weighing device listedin the Apparatus section of Test Methods D 1259.1These test methods are under the jurisdiction of ASTM Committee D01 onPaint and
14、Related Coatings, Materials, and Applications and are the directresponsibility of Subcommittee D01.56 on Printing Inks.Current edition approved June 1, 2007. Published June 2007. Originallyapproved in 1987. Last previous edition approved in 2002 as D 4713 92 (2002).2For referenced ASTM standards, vi
15、sit 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.3Available from any scientific supply house.1Copyright ASTM International, 100 Barr Harbor Driv
16、e, PO Box C700, West Conshohocken, PA 19428-2959, United States.6. Reagents6.1 Toluene, technical grade.7. Preparations of Equipment and Sample7.1 Check the levelness of shelving in the oven; adjust, ifnecessary. Lay the thermometer on shelf with the bulb at theplace where the samples will be placed
17、. Adjust oven controlsuntil thermometer reads 110 6 2C. If air flow is adjustable, setcontrol dampers at 50 %.7.2 Wear disposable gloves prior to handling weighing dish,spreading device, or syringe in order to minimize contamina-tion by moisture from hands.7.3 Measure diameter of bottom of weighing
18、dish in milli-metres. For example, a catalogue listing of 57 mm refers to thetop diameter, whereas the bottom diameter may be only 50mm. The bottom diameter must be used in the calculations ofweight per unit area in 9.1.7.4 Mark weighing dishes with a suitable notation. Rinsewith toluene and heat in
19、 oven at 110C for12 h.7.5 Thoroughly mix ink in container to ensure that thesample is uniform. Close can after removing specimen. Resealwhen finished.8. Procedure8.1 Test Method AHeatset Systems:8.1.1 For each specimen, tare to the nearest milligram twoweighing dishes each with a spreading device. R
20、etain spread-ing device throughout the test.8.1.2 Transfer a representative portion of the sample to thetip of a spatula and dab about 0.15 6 0.02 g around the bottomof each 57-mm dish, or 0.43 6 0.02 g if a 94-mm can lid isused. Quickly reweigh and calculate the weight per unit area inaccordance wi
21、th 9.1. If in excess of 100 g/m2, discard andweigh out a new specimen.8.1.3 With spreader, smooth out the specimen into a reason-ably uniform film covering the entire bottom of the dish. Highviscosity inks may require a few drops of a suitable solvent toaid in spreading out the film.8.1.4 Place the
22、dishes in the forced draft oven at 110C for3 h. Remove dishes from oven, cool in desiccator, and reweigh.8.2 Test Method BLiquid Ink Systems:8.2.1 Tare weighing dishes as in 8.1.1. Transfer 2 to 4 mL ofrepresentative sample to syringe and weigh. Dispense a 0.5 60.1 g specimen from the syringe to a 5
23、7-mm dish, or 1.5 6 0.1g to a 94-mm can lid. Immediately spread out as in 8.1.2.Reweigh syringe.8.2.2 Repeat 8.2.1 with second dish.8.2.3 Place dishes in forced draft oven at 110C for 1 h.Remove dishes from oven, cool in desiccator, and reweigh.9. Calculation9.1 Calculate initial weight/area of each
24、 specimen:S/A 5 S 3 106/3.14 R2, g/m2(1)where:S = initial specimen weight, g,A = area, andR = radius of dish bottom, = diameter/2 mm.NOTE 3For a dish with a 50-mm bottom diameter, weight/area = 510S. For a can lid with a 94-mm bottom diameter, weight/area = 145 S.9.2 Calculate content of nonvolatile
25、 matter as follows:NVM,%5 W/S! 3 100 (2)where:W = specimen weight after heating, g.9.3 Optional:The percent of volatile matter may be calculated by differ-ence as follows:VM,%5 100 2 NVM %. (3)10. Report10.1 Report NVM to the nearest 0.1 % as the mean ofreplicate determinations.10.2 Optional: Report
26、 VM to the nearest 0.1 %.10.3 Report the mean weight per unit area of the initialspecimens to the nearest gram per square metre.11. Precision and Bias11.1 Precision:11.1.1 Test Method AHeatset Systems. An interlaboratory4study was conducted in which one operator in each of fivelaboratories tested in
27、 duplicate on each of two days four heatsetprinting inks, of which two were low NVM (about 50 %) andtwo were high NVM (about 60 %). The round-robin data wereanalyzed according to Practice E 691. There were no outliers.The within-laboratory pooled standard deviation was found tobe 0.44 % absolute at
28、12 degrees of freedom, and the between-laboratories pooled standard deviation was 2.0 % absolute at16 degrees of freedom. Based on these standard deviations, thefollowing criteria should be used for judging the acceptabilityof results at the 95 % confidence level:11.1.1.1 RepeatabilityTwo results, e
29、ach the mean of tworuns obtained by one operator, should be considered suspect ifthey differ by more than 1.2 % absolute.11.1.1.2 ReproducibilityTwo results, each the mean oftwo runs obtained by operators in different laboratories, shouldbe considered suspect if they differ by more than 5.7 %absolut
30、e.11.1.2 Test Method BLiquid Ink Systems. See Precisionsection of Test Method D 2369.11.2 BiasIn the interlaboratory study of heatset inksdescribed in 11.1, the mean values for NVM agreed with thecalculated values within 1 % absolute.12. Keywords12.1 heatset-type printing inks; liquid printing ink;
31、nonvola-tile matter content; ovens; printing inks; resin solutions;solvents; vehicles4Supporting data are available from ASTM International Headquarters. RequestRR: D01 1053.D 4713 92 (2007)2ASTM International takes no position respecting the validity of any patent rights asserted in connection with
32、 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 to revision at any time by the responsible techni
33、cal 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. Your comments will receive careful consideratio
34、n 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 copyrighted by ASTM International, 100 Barr Harb
35、or 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).D 4713 92 (2007)3
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