1、Designation: D4713 12Standard Test Methods forNonvolatile Content of Heatset and Liquid Printing InkSystems1This standard is issued under the fixed designation D4713; 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.1. Scope*1.1 These test methods cover the determination of weightcontent of nonvolatile matter in two types of printing inks.1.2 Test
3、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 vehicles based on aq
4、ueous 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 D1259, whichis recommended as a
5、 referee test.NOTE 2Test Method B (for liquid ink systems) is similar to TestMethod D2369 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 informationonly.1.5 This standar
6、d 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. Referenced Documents2.1 ASTM
7、 Standards:2D1259 Test Methods for Nonvolatile Content of ResinSolutionsD2369 Test Method for Volatile Content of CoatingsE1 Specification for ASTM Liquid-in-Glass ThermometersE145 Specification for Gravity-Convection and Forced-Ventilation OvensE691 Practice for Conducting an Interlaboratory Study
8、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 BLiquid Ink Systems. A0.5
9、-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 and the user.4.2 In order t
10、o 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, accurate to 1 mg.5.2 Ove
11、n, forced-ventilation type conforming to Type IIB inSpecification E145 and maintained at 110 6 2C.5.3 Thermometer, capable of reading 110 6 2C and con-forming to Specification E1. Alternately, temperature measur-ing devices such as liquid-in-glass thermometers, thermistors,thermocouples, or platinum
12、 resistance thermometers that pro-vide equivalent or better accuracy and precision, that cover thetemperature range specified, may be used.5.4 Weighing Dish, such as an aluminum foil dish 57 mmwide, the lid of a 1-lb ink can 94 mm wide, or otherflat-bottomed container. The bottom of the container mu
13、st nothave a trough or depression into which the test material mightcollect.5.5 Spatula, or small ink knife.1These test methods are under the jurisdiction of ASTM Committee D01 onPaint and Related Coatings, Materials, and Applications and are the directresponsibility of Subcommittee D01.56 on Printi
14、ng Inks.Current edition approved Nov. 1, 2012. Published November 2012. Originallyapproved in 1987. Last previous edition approved in 2007 as D4713 92 (2007).DOI: 10.1520/D4713-12.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org
15、. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.*A Summary of Changes section appears at the end of this standardCopyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States15.
16、6 Spreading Device, one per weighing dish, of heat-stablematerial, such as a glass stirring rod 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 Me
17、thods D1259.6. 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 or temperature measuringdevice on shelf with the bulb or sensor at the place where thesamples will be placed. Adjust ov
18、en controls until a tempera-ture reading of 110 6 2C is obtained. If air flow is adjustable,set control 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
19、 weighing 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 a
20、nd heat in 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
21、 device. Retain 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 inacc
22、ordance with 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
23、Place the 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 syri
24、nge to a 57-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/ar
25、ea of each specimen:S/A 5 S 3106/3.14 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 no
26、nvolatile matter as follows:NVM,%5 W/S! 3100 (2)where:W = specimen weight after heating, g.9.3 Optional: The percent of volatile matter may be calcu-lated by difference 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 Optiona
27、l: Report 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
28、tested in 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 E691. There were no outliers.The within-laboratory pooled standard deviation was found tobe 0.44 % abso
29、lute at 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 re
30、sults, each 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
31、%absolute.3Available from any scientific supply house.4Supporting data have been filed at ASTM International Headquarters and maybe obtained by requesting Research Report RR:D01-1053.D4713 12211.1.2 Test Method BLiquid Ink Systems. See Precisionsection of Test Method D2369.11.2 BiasIn the interlabor
32、atory 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; nonvola-tile matter content; ovens; printing inks; resin solutions;solvents; vehiclesSUMMARY OF CHANGESCommitte
33、e D01 has identified the location of selected changes to this standard since the last issue (D4713 92 (2007) that may impact the use of this standard. (Approved November 1, 2012.)(1) Changed thermometer reference in the method to allow aselection of temperature measuring devices in Sections 5.3 and7
34、.1.(2) Added a Summary of Changes section.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 t
35、he riskof infringement 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
36、of this standard 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 shoul
37、dmake your 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/).D4713 123
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