1、Designation: D 6419 00 (Reapproved 2005)Standard Test Method forVolatile Content of Sheet-Fed and Coldset Web OffsetPrinting Inks1This standard is issued under the fixed designation D 6419; the number immediately following the designation indicates the year oforiginal adoption or, in the case of rev
2、ision, 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 This test method describes a procedure for determina-tion of the weight percent volatile content o
3、f sheet-fed andcoldset web offset printing inks. Test specimens are heated at110 6 1C for 60 min.NOTE 1Coldset web offset printing is often (also) referred to asnon-heatset web offset printing.1.2 This test method is also applicable to sheet-fed andcoldset web offset printing ink vehicles.NOTE 2Vehi
4、cle is the liquid portion of the printing ink.Any substancethat is dissolved in the liquid portion of the ink is a part of the vehicle.1.3 This test method is not applicable to ultra-violet (UV) orelectron beam cured materials, which must be cured byexposure to UV light or an electron beam as part o
5、f the test forvolatile content.1.4 This test method is based on Test Method D 2369,inwhich the allowable ranges are 60.1g for specimen weight and65C for oven temperature. Interlaboratory studies haveshown that specimen weight and oven temperature must bothbe more tightly controlled in order to impro
6、ve the precision oftest results for sheet-fed and coldset web-offset inks. Such inkstypically contain a wide range of high-boiling hydrocarbonsand often have a volatile content below 25 %.1.5 The values stated in SI units are to be regarded as thestandard. The values given in parentheses are for inf
7、ormationonly.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 determine the applica-bility of regulatory limitations prior to use. F
8、or a specifichazard statement see 7.5.1.2. Referenced Documents2.1 ASTM Standards:2D 2369 Test Method for Volatile Content of CoatingsD 362 Specification for Industrial Grade TolueneE 145 Specification for Gravity-Convection and Forced-Ventilation OvensE 691 Practice for Conducting an Interlaborator
9、y Study toDetermine the Precision of a Test Method2.2 Other Standards:EPA Reference Method 24 - Determination of VolatileMatter Content, Water Content, Density, Volume Solids,and Weight Solids of Surface Coatings33. Summary of Test Method3.1 A specimen size of 0.300 6 0.001 g is weighed into analumi
10、num foil dish, dispersed in 3 mL of toluene, and heated inan oven at 110 6 1C for 60 min. The percent volatile iscalculated from the loss in weight.4. Significance and Use4.1 This test method is the procedure of choice for deter-mining volatile content of sheet-fed and coldset web offsetinks. This i
11、nformation is useful to the ink manufacturer anduser and to environmental interests as part of the determinationof the mass of volatile organic compounds emitted from theink.NOTE 3Since these inks do not contain water or any materialscurrently classified by US EPA as negligibly photochemically react
12、ive(exempt solvents), volatile organic compound content is the same asvolatile content. The volatile organic compounds in these inks are highboiling hydrocarbon oils which are, according to US EPAguidelines, 95 %retained in the printed substrate or oxidized into the ink film. Therefore,1This test me
13、thod is under the jurisdiction of ASTM Committee D01 on Paintand Related Coatings, Materials, and Applications and is the direct responsibility ofSubcommittee D01.56 on Printing Inks.Current edition approved Sept. 1, 2005. Published September 2005. Originallyapproved in 1999. Last previous edition a
14、pproved in 2000 as D 6419 00.2For 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.3Available from U.S. Government
15、Printing Office Superintendent of Documents,732 N. Capitol St., NW, Mail Stop: SDE, Washington, DC 20401 or Brezinski, J. J.,ed., Determination of Volatile Organic Compound (VOC) Content in Paints, Inks,and Related Coating Products, MNL 4, ASTM, 1993.1Copyright ASTM International, 100 Barr Harbor Dr
16、ive, PO Box C700, West Conshohocken, PA 19428-2959, United States.the mass of volatile organic compound emitted from the ink would becalculated as only 5 % of the volatile organic compound content of the inkas derived from the results of this test method.5. Apparatus5.1 Aluminum Foil Dishes, 58 mm i
17、n diameter by 18 mmhigh with a smooth (planar) bottom surface. Precondition thedishes for 30 min. in an oven at 110 6 1C and store in adesiccator prior to use. Use tongs or rubber gloves or both, tohandle the dishes.5.2 Desiccator, equipped with a general purpose desiccantsuch as anhydrous calcium s
18、ulfate.5.3 Forced Draft Oven, Type IIA or Type IIB as specified inSpecification E 145.NOTE 4Be sure the shelves are level.5.4 Ink Knives or Taper Knives, suitable for transferring thesmall specimen from the original sample container to thealuminum dish.5.5 Paper Clips, bent for use as stirrers. Prec
19、ondition thebent paper clips along with the aluminum foil dishes, asdescribed in 5.1.5.6 Analytical Balance, capable of weighing to 0.0001 g.5.7 Stopwatch, capable of reading to 1s.6. Reagents6.1 Toluene, technical grade, in accordance with Specifica-tion D 362.7. Procedure7.1 Weigh a preconditioned
20、 foil dish that has been equippedwith a preconditioned bent paper clip to 0.0001g and record asW1. Similarly weigh a duplicate.7.2 Mix the sample by hand using an ink knife (taper knife)prior to extracting the exact specimens to be used in the test.7.3 Weigh a 0.300 g 6 0.001 g specimen directly int
21、o eachof the weighed dishes. Record the specimen weight to 0.0001gas S.NOTE 5Due to the relatively high viscosity and low volatility ofsheet-fed and coldset web offset inks, this may best be achieved using inkknives (taper knives). The quickest way to achieve this specimen size andprecision is to sl
22、ightly overweigh and then remove tiny amounts using thetip of a clean ink knife.7.4 To each dish add 1 mL of toluene and stir, using the bentpaper clip, into the ink specimen. Then add a further 2 mL oftoluene (for a total of 3 mL) and repeat the stirring to achievea homogeneous dispersion.7.5 Heat
23、the aluminum foil dishes containing the dispersedspecimens in the forced draft oven (5.3) for exactly 60 min. at110 6 1C. The bent paper clips should remain in the dishesthroughout the test. Position the dishes as near to the center ofthe oven as possible. Use the stopwatch to time the 60-minoven ex
24、posure.7.5.1 Warning: In addition to other precautions, provideadequate ventilation, consistent with accepted laboratory prac-tice, to prevent solvent vapors from accumulating to a danger-ous level.7.6 Remove the dishes from the oven, place immediately ina desiccator, cool to ambient temperature, an
25、d weigh to0.0001g. Record weight as W2.8. Calculation8.1 For each specimen, calculate the weight percent volatilematter V, in the sheet-fed or coldset web offset ink as follows:V 5W11 S! W2S3 100 (1)where:W1= weight of dish plus paper clip,W2= weight of dish plus paper clip, plus specimen afterheati
26、ng, andS = specimen weight prior to heating.Average the duplicate determinations and report the averageas the weight percent volatile matter.9. Precision and Bias9.1 PrecisionTwo separate interlaboratory studies of thistest method were conducted. In the first, operators in 10laboratories tested in t
27、riplicate 5 coldset web offset black inkswhose volatile content ranged from 3 to 39 %. In the second,operators in 9 laboratories tested in triplicate 5 sheet-fed offsetinks whose volatile content ranged from 7 to 23 %. The testresults were analyzed in accordance with Practice E 691.Inthesame interla
28、boratory studies, the full range of temperature andsample sizes permitted by Test Method D 2369 was alsostudied. The precision, characterized by repeatability (Sr, r)and reproducibility (SR, R) was much better for the test methoddescribe herein. Repeatability was improved by a factor of 4.2for the w
29、eb offset inks and 3.1 for the sheet-fed inks.Reproducibility was improved by a factor of 1.3 for the coldsetinks and by a factor of 1.6 for the sheet-fed inks. Based on thestatistical analysis of the results, the following criteria shouldbe used for judging the acceptability of results at the 95 %c
30、onfidence level:9.1.1 RepeatabilityTwo results, each the mean of dupli-cate determinations, obtained by the same operator should beconsidered suspect if they differ by more than 13 % relative forcoldset web offset inks and by more than 7 % relative forsheet-fed offset inks.9.1.2 ReproducibilityTwo r
31、esults, each the mean of dupli-cate determinations, obtained by operators in different labora-tories should be considered suspect if they differ by more than54 % relative for coldset web offset inks and by more than 16% relative for sheet-fed offset inks.9.2 BiasBias cannot be determined as there ar
32、e no stan-dard materials.10. Keywords10.1 coldset web offset inks; coldset web offset ink vehicles;non-heatset web offset inks; non-heatset web offset vehicles;printing inks; printing ink vehicles; sheet-fed offset inks;sheet-fed offset ink vehicles; VOC in inks; volatile determina-tion; volatilesD
33、6419 00 (2005)2ASTM 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 the riskof infringement of s
34、uch 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 of this standard or for add
35、itional 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 shouldmake your views known to t
36、he 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).D 6419 00 (2005)3
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