1、Designation: D1465 10 (Reapproved 2015) Technical Association of Pulp and Paper IndustrySuggested Method T 652Standard Test Method forBlocking and Picking Points of Petroleum Wax1This standard is issued under the fixed designation D1465; the number immediately following the designation indicates the
2、 year oforiginal adoption or, in the case of revision, 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 the determination of the bl
3、ock-ing point and picking point of petroleum wax.1.2 WARNINGMercury has been designated by manyregulatory agencies as a hazardous material that can causecentral nervous system, kidney and liver damage. Mercury, orits vapor, may be hazardous to health and corrosive tomaterials. Caution should be take
4、n when handling mercury andmercury containing products. See the applicable product Ma-terial Safety Data Sheet (MSDS) for details and EPAswebsitehttp:/www.epa.gov/mercury/faq.htmfor addi-tional information. Users should be aware that selling mercuryand/or mercury containing products into your state
5、or countrymay be prohibited by law.1.3 The values stated in SI units are to be regarded asstandard. The values given in parentheses are provided forinformation only.1.4 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibility of th
6、e 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 Standards:2D87 Test Method for Melting Point of Petroleum Wax(Cooling Curve)D938 Test Method for Congealing Point of P
7、etroleumWaxes, Including PetrolatumD2423 Test Method for Surface Wax on Waxed Paper orPaperboardE1 Specification for ASTM Liquid-in-Glass Thermometers3. Terminology3.1 Definitions:3.1.1 wax blocking pointthe lowest temperature at whichfilm disruption occurs across 50 % of the waxed paper surfacewhen
8、 the test strips are separated.3.1.2 wax picking pointthe temperature at which the firstfilm disruption occurs on the waxed paper when test strips areseparated.4. Summary of Test Method4.1 Paper test specimens are coated with the wax sample,folded with the waxed surfaces together, and placed on ablo
9、cking plate. The plate is heated at one end and cooled at theother end to impose a measured temperature gradient along itslength. After a conditioning period on the plate, the specimensare removed, unfolded, and examined. The points of initial filmdisruption (picking point) and where 50 % of the spe
10、cimenwidth is disrupted (50 % blocking point) are noted. Thetemperatures of corresponding points on the blocking plate arereported as the picking point and blocking point or blockingrange.5. Significance and Use5.1 Blocking of waxed paper, because of the relatively lowtemperatures at which it may oc
11、cur, can be a major problem tothe paper-coating industry. For example, when the waxedsurfaces in a roll of waxed paper stick together, upon separa-tion the surface films are marred and the glossy finish isdestroyed. The wax picking point and the wax blocking pointindicate an approximate temperature
12、range at or above whichwaxed surfaces in contact with each other are likely to causesurface film injury.6. Apparatus6.1 Wax Coating DeviceAny manual- or machine-drivenwaxer that gives uniform coatings of the desired weights to astrip of paper not less than 51 mm (2 in.) wide.6.2 Trimming Board, or o
13、ther device for cutting paper strips.6.3 Paper Scales, sensitive to 0.002 g, or suitable balancefor measuring basis weights of unwaxed and waxed paper.1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products, Liquid Fuels, and Lubricantsand is the direct responsibility
14、ofSubcommittee D02.10.0A on Physical/Chemical Properties. This test method wasprepared jointly by the TechnicalAssociation of the Pulp and Paper Industry and theAmerican Society for Testing and Materials.Current edition approved Oct. 1, 2015. Published December 2015. Originallyapproved in 1957. Last
15、 previous edition approved in 2010 as D1465 10. DOI:10.1520/D1465-10R15.2For 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 AS
16、TM website.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States16.4 Blocking Plate Assembly, consisting of a metal plate305 mm (12 in.) wide, 13 mm to 51 mm (12 in. to 2 in.) thick,and 559 mm to 914 mm (22 in. to 36 in.) long. It is heated
17、 atone end and cooled at the other end to provide a 457 mm to762 mm (18 in. to 30 in.) test section having an averagetemperature gradient of 0.8 C to 2.2 C (1.5 F to 4.0 F) in.The temperature gradient across the width of the plate from thelongitudinal axis to 25 mm (1 in.) from the edge must notexce
18、ed 0.3 C (0.5 F). The temperature at any point should notvary more than 0.3 C (0.5 F). Details of two acceptableblocking plates are given in Fig. 1 and Fig. 2.6.4.1 Eight Foam Rubber Strips, 25 mm to 38 mm (1 in. to112 in.) wide by 6 mm to 13 mm (14 in. to12 in.) thick,extending the length of the te
19、st section on the blocking plate.6.4.2 Eight Sets of Steel Weights, 25 mm by 25 mm (1 in. by1 in.) in cross section made from stock having a density rangefrom 7800 kg m3to 8000 kg m3(0.28 lb in.3to 0.29 lb in.3).The weights may be in single lengths or in sections to give setsequaling the length of t
20、he test section of the blocking plate.6.5 Temperature Recorder, or indicator for measuring thetemperature gradient of the blocking plate. The instrument andthermocouples when calibrated shall consistently be accurateto 60.3 C (0.5 F).6.6 Temperature Measuring Devices:6.6.1 ThermometersFor water bath
21、 and wax bath on thewaxing device, use two ASTM Tag Closed Tester Thermom-eters having a range from 5 C to 110 C (20 F to 230 F),graduated in 0.5 C (1 F) subdivisions, and conforming toThermometer 9C or 9F as prescribed in Specification E1.6.6.2 Alternatively, bath temperatures may be monitoredwith
22、a calibrated thermometer containing a liquid other thanmercury or an electronic temperature measuring device ofequivalent precision and accuracy to the thermometers de-scribed in 6.6.1.7. Test Paper7.1 PaperCereal glassine of basis weight 46 g m2to51 g m2(28.5 lb 3000 ft2to 31.5 lb 3000 ft2).8. Samp
23、ling8.1 Select a portion of the wax that is representative of thewhole sample. The amount required will depend on the size ofthe waxing device used.9. Standardization of Apparatus9.1 Turn the blocking plate on with all sponge rubber stripsand metal blocks in position. Allow sufficient time (3 hminim
24、um) for the plate to reach an equilibrium temperaturecondition.9.2 Calibrate a 30-gauge “test” thermocouple as follows:Heat a beaker of water to about 43.3 C (110 F) and measureits temperature with a temperature measuring device which isaccurate to 0.3 C (0.5 F). Insert the “test” thermocouple inthe
25、 water and measure the temperature with a manual poten-tiometer which is accurate to at least 60.5 C (61 F). Aportable precision type potentiometer or a type Kpotentiometer, both of which are accurate to at least 0.5 F(0.3 C) in this temperature range, is preferred.9.3 Lay the calibrated “test” ther
26、mocouple across the widthof the plate with its junction directly over one of the imbeddedthermocouples. Be sure that one of the sponge rubber stripscovers the junction completely. Replace the weights on therubber strips. After 3 min to 4 min, note the temperaturereadings on the hand potentiometer an
27、d the correspondingpoint on the recorder. If the reading of the test thermocoupleplus its calibration factor is more than 0.5 C (1 F) from thatof the recorder reading, check the accuracy of the recorderseparately. If the recorder is satisfactory, the trouble may resultFIG. 1 Type A Blocking PlateD14
28、65 10 (2015)2from the thermocouple being damaged or not in solid contactwith the plate. Replace this thermocouple, taking care to tampit into place so that its junction is held firmly against the platemetal. Check the new thermocouple and each of the otherimbedded thermocouples in a like manner. Not
29、e the calibrationfactor of each.9.4 For best operation, install the blocking plate in aconstant temperature room. Check the plate calibrationperiodically, after installing new thermocouples, or if the platetemperatures vary more than 0.5 C (1 F) from the normalconditions.10. Preparation of Waxed Pap
30、er Test Specimens10.1 Heat the wax sample to at least 22 C (40 F) above itsexpected melting or congealing point according to Test MethodD87 or Test Method D938, using an air or water bath so as notto overheat portions of the sample. After cleaning the waxingdevice, fill the wax bath with the sample
31、to be tested. Hold thewax bath and the doctor rods or squeeze rolls at a temperatureat least 22 C (40 F) above the expected melting or congealingpoint of the wax. For machines not having positive temperaturecontrol (heated electrically or by hot water) of the doctor rodsor squeeze rolls, use infrare
32、d lamps or precontact the rolls withhot wax to heat them to about the wax bath temperature.10.2 Use paper conditioned at least a week at 23 C 62.0 C (73 F 6 3.5 F) and 50 % 6 5 % relative humidity.Load the wax coating device with the paper passing throughthe wax bath. Coat the paper with 6.5 g m2to
33、10 g m2(4 lb 3000 ft2to 6 lb 3000 ft2) of wax on one side and3.2 g m2to 10 g/m2(2 lb 3000 ft2to 6 lb 3000 ft2) of wax onthe other.10.3 Cool the wax coated paper to room temperature inambient air.NOTE 1As an alternative procedure, the wax coated paper may becooled by passage through a water bath. The
34、re is evidence, however, thewater quenching can cause variation in picking and blocking point valuesobtained on some waxes.10.4 Measure the coating weight using Test Method D2423,with the exception of substituting the blocking point strips inTest Method D1465 for the 100 mm by 100 mm square ofwaxed
35、paper in Test Method D2423. If the weights are otherthan 6.5 g m2to 10 g m2(4 lb ream to 6 lb ream) of wax onthe test surface and 3.2 g m2to 10 g m2(2 lb ream to6 lb ream) of wax on the back side, prepare another waxedpaper specimen.10.5 If the coating weights are satisfactory, cut two testspecimens
36、 from the waxed test paper, each specimen 25 mm(1 in.) wide and twice the length of the test section of theblocking plate.10.6 Condition the waxed specimens for at least 24 h at23 C 6 2.0 C (73 F 6 3.5 F) and 50 % 6 5 % relativehumidity.11. Procedure11.1 The blocking plate may be left on continuousl
37、y. Ifstarting with a cold plate, allow at least 3 h for the plate to heatup and reach an equilibrium condition with the pads andweights in place. Check the temperature recorder to be sure theplate is at the desired temperature.11.2 The blocking plates have room for seven or eight rowsof specimens ac
38、ross the plate. Fold the specimens to the lengthof the test section with the surfaces face to face. Cut singleunwaxed glassine paper strips (or glassine, if desired) the samesize as the folded, waxed test specimen. Insert the foldedwaxed specimen between the two unwaxed strips and place itlongitudin
39、ally on the blocking plate with the folded end on the“start” line at the hot end. Place a second waxed specimen andan unwaxed strip in a similar manner on top of the firstspecimen. Not more than two of these test specimens should beplaced in each testing space. Carefully smooth out the wrinklesFIG.
40、2 Type B Blocking PlateD1465 10 (2015)3in the specimens. Place any other specimens to be tested inother rows on the blocking bar in the same manner. If theblocking plate is not filled to capacity with specimens, insertsponge rubber pads and weights in the empty spaces.11.3 After 17 h exposure on the
41、 blocking plate, remove thespecimens together with the unwaxed spacer strips. Cool themfor a minimum of 5 min. Carefully peel off the unwaxed stripsand pull the specimens apart starting at cold end at a rate ofabout 152 mm (6 in.) s.11.4 Examine the test surfaces closely and mark the pickingpoint an
42、d the 50 % blocking point. The picking point is the firstof a series of spots of actual film disruption nearest the “cold”end of the strip. The 50 % blocking point is the first pointnearest the cold end where 50 % of the width of the strip showsfilm disruption. Fine, isolated lines across the strip
43、are not ratedas the 50 % blocking point. Loss of gloss or spotting withoutfilm disruption is not considered as blocking or picking.NOTE 2Several techniques have been used for viewing the test strips.These include viewing against reflected light, dusting the strips withgraphite, or placing an opaque
44、object behind the test strip.NOTE 3Loss of gloss (blooming) can sometimes be distinguishedfrom film disruption by lightly wiping the surface of the test paper with acotton gauze pad.12. Calculation and Report12.1 Plot the temperature gradient curve for the instrumentfrom the temperature recorder rea
45、dings. Aside from a slightrise in temperature when the specimens are first placed on theplate, the temperature of any single point should not vary morethan 0.3 C (0.5 F).12.2 Measure the distance from the fold to the two blockingpoint marks for each specimen with the wax sample beingtested. Note the
46、 blocking temperatures on the temperaturegradient curve corresponding to these distances.12.3 Report the average results to the nearest 0.5 C (1 F).A wax with a 41 C (106 F) initial film disruption and a 50 %blocking point of 43 C (110 F) would be reported as:12.3.1 Picking Point41 C (106 F).12.3.2
47、Blocking Point43 C (110 F).13. Precision and Bias13.1 PrecisionResults should not differ from the mean bymore than the following amounts:13.1.1 Picking Point:13.1.1.1 Repeatability (one operator and apparatus), 2.8 C(5 F).13.1.1.2 Reproducibility (different operators and apparatus),3.6 C (6.5 F).13.
48、1.2 Blocking Point:13.1.2.1 Repeatability (one operator and apparatus), 1.7 C(3 F).13.1.2.2 Reproducibility (different operators and apparatus),3.3 C (6 F).NOTE 4The precision as stated in Section 13 was obtained by acooperative program among seven laboratories using two standard refer-ence waxes wh
49、ich have sharp blocking points. Where a sharp blockingpoint cannot be obtained because of the composition of the wax samplebeing tested, poorer precision in test results will be encountered.13.2 BiasThe procedure in this test method has no biasbecause the measurement of blocking and picking points canbe defined only in terms of a test method.14. Keywords14.1 blocking point; picking point; waxed coating; waxedpaperASTM International takes no position respecting the validity o
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