1、Designation: D1465 10Technical 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 year oforiginal ad
2、option 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. Scope*1.1 This test method covers the determination of the block-ing point and
3、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 taken when handling me
4、rcury 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 or countrymay be p
5、rohibited 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 the user of this sta
6、ndard 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 PetroleumWaxes, Inc
7、luding 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 the test strips a
8、re 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 ablocking plate. The p
9、late 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 specimenwidth is disr
10、upted (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 occur, can be a majo
11、r 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 range at or above
12、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 other device for cu
13、tting paper strips.6.3 Paper Scales, sensitive to 0.002 g, or suitable balancefor measuring basis weights of unwaxed and waxed paper.6.4 Blocking Plate Assembly, consisting of a metal plate 305mm (12 in.) wide, 13 to 51 mm (12 to 2 in.) thick, and 559 to914 mm (22 to 36 in.) long. It is heated at on
14、e end and cooled1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products and Lubricants and is the direct responsibility of SubcommitteeD02.10.0A on Physical/Chemical Properties. This test method was prepared jointlyby the Technical Association of the Pulp and Paper Ind
15、ustry and the AmericanSociety for Testing and Materials.Current edition approved May 1, 2010. Published June 2010. Originallyapproved in 1957. Last previous edition approved in 2004 as D146504. DOI:10.1520/D1465-10.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM
16、Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.1*A Summary of Changes section appears at the end of this standard.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshoho
17、cken, PA 19428-2959, United States.at the other end to provide a 457 to 762-mm (18 to 30-in.) testsection having an average temperature gradient of 0.8 to 2.2C(1.5 to 4.0F)/in. The temperature gradient across the width ofthe plate from the longitudinal axis to 25 mm (1 in.) from theedge must not exc
18、eed 0.3C (0.5F). The temperature at anypoint should not vary more than 0.3C (0.5F). Details of twoacceptable blocking plates are given in Fig. 1 and Fig. 2.6.4.1 Eight Foam Rubber Strips,25to38mm(1to112 in.)wide by 6 to 13 mm (14 to12 in.) thick, extending the lengthof the test section on the blocki
19、ng plate.6.4.2 Eight Sets of Steel Weights, 25 by 25 mm (1 by 1 in.)in cross section made from stock having a density range from7800 to 8000 kg/m3(0.28 to 0.29 lb/in3). The weights may bein single lengths or in sections to give sets equaling the lengthof the test section of the blocking plate.6.5 Te
20、mperature Recorder, or indicator for measuring thetemperature gradient of the blocking plate. The instrument andthermocouples when calibrated shall consistently be accurateto 6 0.3C (0.5F).6.6 Temperature Measuring Devices:6.6.1 ThermometersFor water bath and wax bath on thewaxing device, use two AS
21、TM Tag Closed Tester Thermom-eters having a range from 5 to 110C (20 to 230F), graduatedin 0.5C (1F) subdivisions, and conforming to Thermometer9C or 9F as prescribed in Specification E1.6.6.2 Alternatively, bath temperatures may be monitoredwith a calibrated thermometer containing a liquid other th
22、anmercury 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 to 51 g/m2(28.5 to 31.5 lb/3000 ft2).8. Sampling8.1 Select a portion of the wax that is representative of thewh
23、ole 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 hminimum) for the plate to reach an equilibrium temperaturecondition.9.2
24、Calibrate a 30-gauge “test” thermocouple as follows:Heat a beaker of water to about 43.3C (110F) and measure itstemperature with a temperature measuring device which isaccurate to 0.3C (0.5F). Insert the “test” thermocouple in thewater and measure the temperature with a manual potentiom-eter which i
25、s accurate to at least 60.5C (61F). A portableprecision type potentiometer or a type K potentiometer, both ofwhich are accurate to at least 0.5F (0.3C) in this temperaturerange, is preferred.9.3 Lay the calibrated “test” thermocouple across the widthof the plate with its junction directly over one o
26、f the imbeddedthermocouples. Be sure that one of the sponge rubber stripscovers the junction completely. Replace the weights on therubber strips.After 3 to 4 min, note the temperature readings onthe hand potentiometer and the corresponding point on therecorder. If the reading of the test thermocoupl
27、e plus itscalibration factor is more than 0.5C (1F) from that of therecorder reading, check the accuracy of the recorder separately.If the recorder is satisfactory, the trouble may result from thethermocouple being damaged or not in solid contact with theplate. Replace this thermocouple, taking care
28、 to tamp it intoplace so that its junction is held firmly against the plate metal.FIG. 1 Type A Blocking PlateD1465 102Check the new thermocouple and each of the other imbeddedthermocouples in a like manner. Note the calibration factor ofeach.9.4 For best operation, install the blocking plate in aco
29、nstant temperature room. Check the plate calibration peri-odically, after installing new thermocouples, or if the platetemperatures vary more than 0.5C (1F) from the normalconditions.10. Preparation of Waxed Paper Test Specimens10.1 Heat the wax sample to at least 22C (40F) above itsexpected melting
30、 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 to be tested. Hold thewax bath and the doctor rods or squeeze rolls at a temperatureat leas
31、t 22C (40F) 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 infrared lamps or precontact the rolls withhot wax to heat them to about the wax bath temperature.10
32、.2 Use paper conditioned at least a week at 23 6 2.0C(73 6 3.5F) and 50 6 5 % relative humidity. Load the waxcoating device with the paper passing through the wax bath.Coat the paper with 6.5 to 10 g/m2(4 to 6 lb/3000 ft2)ofwaxon one side and 3.2 to 10 g/m2(2 to 6 lb/3000 ft2) of wax onthe other.10.
33、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. There is evidence, however, thewater quenching can cause variation in picking and blocking point valuesobtained on some waxes.10.4 Measu
34、re the coating weight using Test Method D2423,with the exception of substituting the blocking point strips inTest Method D1465 for the 100 by 100-mm square of waxedpaper in Test Method D2423. If the weights are other than 6.5to 10 g/m2(4 to 6 lb/ream) of wax on the test surface and 3.2to 10 g/m2(2 t
35、o 6 lb/ream) of wax on the back side, prepareanother waxed paper specimen.10.5 If the coating weights are satisfactory, cut two testspecimens from the waxed test paper, each specimen 25 mm (1in.) wide and twice the length of the test section of the blockingplate.10.6 Condition the waxed specimens fo
36、r at least 24 h at 236 2.0C (73 6 3.5F) and 50 6 5 % relative humidity.11. Procedure11.1 The blocking plate may be left on continuously. 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 temperatur
37、e recorder to be sure theplate is at the desired temperature.11.2 The blocking plates have room for seven or eight rowsof specimens across 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)
38、the samesize as the folded, waxed test specimen. Insert the foldedwaxed specimen between the two unwaxed strips and place itlongitudinally 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
39、firstspecimen. Not more than two of these test specimens should beplaced in each testing space. Carefully smooth out the wrinklesin 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
40、, insertsponge rubber pads and weights in the empty spaces.11.3 After 17-h exposure on the blocking plate, remove thespecimens together with the unwaxed spacer strips. Cool themfor a minimum of 5 min. Carefully peel off the unwaxed stripsFIG. 2 Type B Blocking PlateD1465 103and pull the specimens ap
41、art starting at cold end at a rate ofabout 152 mm (6 in.)/s.11.4 Examine the test surfaces closely and mark the pickingpoint and 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 fi
42、rst pointnearest the cold end where 50 % of the width of the strip showsfilm disruption. Fine, isolated lines across the strip 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 fo
43、r viewing the test strips.These include viewing against reflected light, dusting the strips withgraphite, or placing an opaque 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 g
44、auze pad.12. Calculation and Report12.1 Plot the temperature gradient curve for the instrumentfrom the temperature recorder readings. Aside from a slightrise in temperature when the specimens are first placed on theplate, the temperature of any single point should not vary morethan 0.3C (0.5F).12.2
45、Measure the distance from the fold to the two blockingpoint marks for each specimen with the wax sample beingtested. Note the blocking temperatures on the temperaturegradient curve corresponding to these distances.12.3 Report the average results to the nearest 0.5C (1F).Awax with a 41C (106F) initia
46、l film disruption and a 50 %blocking point of 43C (110F) would be reported as:12.3.1 Picking Point41C (106F).12.3.2 Blocking Point43C (110F).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
47、operator and apparatus), 2.8C(5F).13.1.1.2 Reproducibility (different operators and appara-tus), 3.6C (6.5F).13.1.2 Blocking Point:13.1.2.1 Repeatability (one operator and apparatus), 1.7C(3F).13.1.2.2 Reproducibility (different operators and appara-tus), 3.3C (6F).NOTE 4The precision as stated in S
48、ection 13 was obtained by acooperative program among seven laboratories using two standard refer-ence waxes which 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.
49、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; waxedpaperSUMMARY OF CHANGESSubcommittee D02.10 has identified the location of selected changes to this standard since the last issue(D146504) that may impact the use of this standard.(1) Revised and reorganized 6.6.(2) Added 6.6.2.(3) Revised 9.2.ASTM International takes no position respecting
