1、Designation: D 1465 04An American National StandardTechnical 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 D 1465; the number immediately following the designation i
2、ndicates the 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 (e) indicates an editorial change since the last revision or reapproval.1. Scope*1.1 This test method covers the determina
3、tion of the block-ing point and picking point of petroleum wax.1.2 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 applic
4、a-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D 87 Test Method for Melting Point of Petroleum Wax(Cooling Curve)D 938 Test Method for Congealing Point of PetroleumWaxes, Including PetrolatumD 2423 Test Method for Surface Wax on Waxed Paper orPaperboardE 1
5、 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 are separated.3.1.2 wax picking pointthe temperature at which the firstfilm disru
6、ption 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 plate is heated at one end and cooled at theother end to impose a measured temper
7、ature 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 disrupted (50 % blocking point) are noted. Thetemperatures of corresponding points o
8、n 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 major problem tothe paper-coating industry. For example, when the waxedsurfaces in a
9、 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 whichwaxed surfaces in contact with each other are likely to causesurface film i
10、njury.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 cutting paper strips.6.3 Paper Scales, sensitive to 0.002 g, or suitable balancefo
11、r 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 one end and cooledat the other end to provide a 457 to 762-mm (18 to 30-in.) tests
12、ection 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 exceed 0.3C (0.5F). The temperature at anypoint should not vary more than 0.3C (0.5F). Details of twoa
13、cceptable 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 blocking plate.6.4.2 Eight Sets of Steel Weights, 25 by 25 mm (1 by 1 in.)in cross section made from stoc
14、k having a density range from7800 to 8000 kg/m3(0.28 to 0.29 lb/in3). The weights may be1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products and Lubricants and is the direct responsibility of SubcommitteeD02.10 on Properties of Petroleum Wax. This test method was pr
15、epared jointly bythe Technical Association of the Pulp and Paper Industry and the American Societyfor Testing and Materials.Current edition approved Nov. 1, 2004. Published November 2004. Originallyapproved in 1957. Last previous edition approved in 2000 as D 146590(2000).2For referenced ASTM standa
16、rds, 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.1*A Summary of Changes section appears at the end of this standard.Copyright ASTM Intern
17、ational, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.in single lengths or in sections to give sets equaling the lengthof the test section of the blocking plate.6.5 Temperature Recorder, or indicator for measuring thetemperature gradient of the blocking plate.
18、The instrument andthermocouples when calibrated shall consistently be accurateto 6 0.3C (0.5F).6.6 ThermometersFor water bath and wax bath on thewaxing device, use two ASTM Tag Closed Tester Thermom-eters having a range from 5 to 110C (20 to 230F), graduatedin 0.5C (1F) subdivisions, and conforming
19、to Thermometer9C or 9F as prescribed in Specification E1.7. Test Paper7.1 PaperCereal glassine of basis weight 46 to 51 g/m2(28.5 to 31.5 lb/3000 ft2).FIG. 1 Type A Blocking PlateFIG. 2 Type B Blocking PlateD14650428. Sampling8.1 Select a portion of the wax that is representative of thewhole sample.
20、 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 Calibrate a
21、 30-gage “test” thermocouple as follows:Heat a beaker of water to about 43.3C (110F) and measure itstemperature with a standardized thermometer which is accurateto 0.3C (0.5F). Insert the “test” thermocouple in the waterand measure the temperature with a manual potentiometerwhich is accurate to at l
22、east 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 of the imbeddedther
23、mocouples. 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 thermocouple plus itscalibrat
24、ion 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 to tamp it intopl
25、ace so that its junction is held firmly against the plate metal.Check 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 aconstant temperature room. Check the plate calibration pe
26、ri-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 or congealing point according to Test MethodD87or Test
27、 Method D 938, 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 least 22C (40F) above the expected melting or congealingpoi
28、nt 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.10.2 Use paper conditioned at least a week at 23 6 2.0C(7
29、3 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.10.3 Cool the wax coated paper to room temperature inambie
30、nt 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 Measure the coating weight usingTest Method D 2423,with the
31、exception of substituting the blocking point strips inTest Method D 1465 for the 100 by 100-mm square of waxedpaper in Test Method D 2423. 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 to 6 lb/ream) of wax on the back side, prepareanother
32、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 for at least 24 h at 236 2.0C (73 6 3.5F) and 50 6 5 %
33、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 temperature recorder to be sure theplate is at the desired temp
34、erature.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) the samesize as the folded, waxed test specimen. Inse
35、rt 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 firstspecimen. Not more than two of these test specim
36、ens 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, insertsponge rubber pads and weights in the empty s
37、paces.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 stripsand pull the specimens apart starting at cold end at a rate ofabout 152 mm (6 in.)/s.11.4 Examine the test surfaces
38、 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 first pointnearest the cold end where 50 % of the width of the strip showsfilm disruption. F
39、ine, 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 for viewing the test strips.These include viewing against reflected light, dusting the strip
40、s withgraphite, or placing an opaque object behind the test strip.NOTE 3Loss of gloss (blooming) can sometimes be distinguishedD1465043from 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 th
41、e 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 Measure the distance from the fold to the two blockingpoint marks for each specime
42、n 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) initial film disruption and a 50 %blocking point of 43C (110F) would be reported as:12.3
43、.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 operator and apparatus), 2.8C(5F).13.1.1.2 Reproducibility (different operators an
44、d 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 Section 13 was obtained by acooperative program among seven laboratories using two
45、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.13.2 BiasThe procedure in this test method has no biasbecause the measurement of b
46、locking 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(D 146590(2000) that may impact
47、the use of this standard.(1) Added Test Method D 938 to the Referenced Documents.(2) Added Celsius thermometer scale graduation increment to6.6.(3) Revised 10.1 and 10.4.(4) Corrected Celsius value in 12.3.ASTM International takes no position respecting the validity of any patent rights asserted in
48、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 such rights, are entirely their own responsibility.This standard is subject to revision at any time by the res
49、ponsible 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 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 shouldmake your views known to the ASTM Committee on Standar
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