1、Designation: D3235 06 (Reapproved 2011)D3235 15Standard Test Method forSolvent Extractables in Petroleum Waxes1This standard is issued under the fixed designation D3235; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of l
2、ast 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 Scope*1.1 This test method covers the determination of solvent extractables in petroleum waxes.1.2 The values stated in SI
3、 units are to be regarded as standard. The values given in parentheses are for information only.1.3 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibilityof the user of this standard to establish appropriate safety and health p
4、ractices and determine the applicability of regulatorylimitations prior to use.2. Referenced Documents2.1 ASTM Standards:2E1 Specification for ASTM Liquid-in-Glass ThermometersE128 Test Method for Maximum Pore Diameter and Permeability of Rigid Porous Filters for Laboratory Use3. Summary of Test Met
5、hod3.1 The sample is dissolved in a mixture consisting of 50 volume % methyl ethyl ketone and 50 volume % toluene. The solutionis cooled to 32C (25F)32 C (25 F) to precipitate the wax, then filtered. The solvent extractables content is determined byevaporating the solvent from the filtrate and weigh
6、ing the residue.4. Significance and Use4.1 The solvent extractables in a wax may have significant effects on several of its properties such as strength, hardness,flexibility, scuff resistance, coefficient of friction, coefficient of expansion, melting point, and staining characteristics. Whetherthes
7、e effects are desirable or undesirable depends on the intended use of the wax.5. Apparatus5.1 Filter Stick and Assembly, consisting of a 10-mm10 mm diameter sintered glass filter stick of 1010 m to 15 m 15 mmaximum pore diameter as determined by the method in Appendix X1, provided with an air pressu
8、re inlet tube and deliverynozzle. It is provided with a ground-glass joint to fit a 2525 mm by 170-mm170 mm test tube. The dimensions for a suitablefiltration assembly are shown in Fig. 1.NOTE 1A metallic filter stick may be employed if desired. A filter stick3 made of stainless steel and having a 1
9、2.7-mm (0.50-in.)12.7 mm (0.50 in.)disk of 1010 nm to 15 nm 15 nm maximum pore diameter, as determined by Test Method E128, has been found to be satisfactory. The metallic apparatusis inserted into a 2525 mm by 150-mm150 mm test tube and held in place by means of a cork.5.2 Cooling Bath, consisting
10、of an insulated box with 3030 mm65-mm (1.25 mm (1.2 in.60.2-in.)0.2 in.) holes in the centerto accommodate any desired number of test tubes. The bath may be filled with a suitable medium such as kerosine, and may becooled by circulating a refrigerant through coils, or by using solid carbon dioxide.
11、A suitable cooling bath to accommodate threetest tubes is shown in Fig. 2.1 This test method is under the jurisdiction ofASTM Committee D02 on Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of SubcommitteeD02.10.0A on Physical/Chemical Properties.Current edition ap
12、proved Oct. 1, 2011April 1, 2015. Published October 2011April 2015. Originally approved in 1973. Last previous edition approved in 20062011 asD3235 - 06.D3235 06 (2011). DOI: 10.1520/D3235-06R11.10.1520/D3235-15.2 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Cust
13、omer Service at serviceastm.org. For Annual Book of ASTM Standardsvolume information, refer to the standards Document Summary page on the ASTM website.3 The sole source of supply of a suitable metal filter stick with designated porosity G known to the committee at this time is the Pall Trinity Micro
14、 Corp., Route 281,Cortland, NY13045.Alist of United Kingdom suppliers can be obtained from Energy Institute, 61 New Cavendish St., London,W1G 7AR, United Kingdom. If you are awareof alternative suppliers, please provide this information toASTM International Headquarters.Your comments will receive ca
15、reful consideration at a meeting of the responsibletechnical committee,1 which you may attend.This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Becauseit may not be technically poss
16、ible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current versionof the standard as published by ASTM is to be considered the official document.*A Summary of Changes section appears at the end of this standardCop
17、yright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States15.3 Dropper Pipet, dispensing device capable of delivering 0.50.5 g 6 0.05 g 0.05 g of molten wax.5.4 Transfer Pipet, or equivalent volume dispensing device, capable of delivering 1515 mL 6
18、 0.06 mL.0.06 mL.5.5 Air Pressure Regulator, designed to supply air to the filtration assembly (8.5) at sufficient pressure to give an even flow offiltrate. Either a conventional pressure-reducing valve or a mercury bubbler-type regulator has been found satisfactory. The lattertype, illustrated in F
19、ig. 3, consists of a 250-mL250 mLglass cylinder and aT-tube held in the cylinder by means of a rubber stoppergrooved at the sides to permit the escape of excess air. The volume and pressure of the air supplied to the filtration assembly isregulated by the depth to which the T-tube is immersed in mer
20、cury at the bottom of the cylinder. Absorbent cotton placed in thespace above the mercury prevents the loss of mercury by spattering. The air pressure regulator is connected to the filter stick andassembly by means of rubber tubing.5.6 Temperature Measuring Devices:5.6.1 Thermometers, two, having a
21、range as shown below and conforming to the requirements as prescribed in Specification E1or in the specifications for IP Standard Thermometers. One thermometer is required for the cold bath and a second thermometeris required for the sample solution.Thermometer NumberTemperature Range ASTM IP37 to +
22、21C 71C 72C37 to +21 C 71C 72C35 to +70F 71F 72F35 to +70 F 71F 72F5.6.2 Temperature measuring devices other than those described in 5.6.1 are satisfactory for this test method, provided theyexhibit the same temperature response as the equivalent mercury-in-glass thermometers.5.7 Weighing Bottles, g
23、lass-stoppered, having a typical capacity of 15-25 mL.15 mL to 25 mL.5.8 Evaporation Assembly, consisting of an evaporating cabinet and connections, essentially as illustrated in Fig. 4, and capableof maintaining a temperature of 3535 C 6 1C (951 C (95 F 6 2F)2 F) around the evaporation flasks. Cons
24、truct the jets withan inside diameter of 44 mm 6 0.2 mm 0.2 mm for delivering a stream of clean, dry air vertically downward into the weighingbottle. Support each jet so that the tip is 1515 mm 6 5 mm 5 mm above the surface of the liquid at the start of the evaporation.Supply purified air at the rat
25、e of 22 Lmin to 33 L L/min min per jet. One way to purify the air is to pass it through a tube ofapproximately 1-cm1 cm bore packed loosely to a height of approximately 20 cm 20 cm with absorbent cotton. Periodically checkthe cleanliness of the air by evaporating 4 mL4 mLof the solvent mixture descr
26、ibed in 6.3 by the procedure specified in 8.5. Whenthe residue does not exceed 0.1 mg, 0.1 mg, the evaporation equipment is operating satisfactorily.All dimensions are in millimetres.FIG. 1 Filter StickD3235 152NOTE 2Investigations by the European World Federation have indicated that improved precis
27、ion may be achieved by individually calibrating eachnozzle to deliver a flow rate of 22 L min to 3 L/min.3 L min.5.9 Analytical Balance, capable of reproducing weights to 0.1 mg.0.1 mg.5.10 Wire StirrerA piece of stiff made of iron, stainless steel, or Nichrome wire of about No. 20 Bands (0.9 mm (0.
28、9 mm indiameter) or 16 swg. gage, 250 mm long. A 10-mm10 mm diameter loop is formed at each end, and the loop at the bottom endis bent so that the plane of the loop is perpendicular to the wire.6. Solvent6.1 Methyl Ethyl Ketone, conforming to the specifications of the Committee on Analytical Reagent
29、s of the American ChemicalSociety.46.2 Toluene, conforming to the specifications of the Committee on Analytical Reagents of the American Chemical Society.46.3 Solvent MixturePrepare a mixture of 50 volume % methyl ethyl ketone and 50 volume % toluene.6.4 Store the solvent mixture over a suitable dry
30、ing agent, such as anhydrous calcium sulfate (5 weight % (five mass percentof the solvent). Filter prior to use.4 Reagent Chemicals, American Chemical Society Specifications, American Chemical Society, Washington, DC. For Suggestions on the testing of reagents not listed bythe American Chemical Soci
31、ety, see Annual Standards for Laboratory Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia and NationalFormulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville, MD.All dimensions are in millimetres (inches).FIG. 2 Cooling BathD3235 1537. Sample7.1 Obtain a represen
32、tative portion by melting the entire sample and stirring thoroughly. This is necessary because theextractables may not be distributed uniformly throughout the solidified sample.8. Procedure8.1 Melt a representative portion of the sample, using a water bath or oven maintained at 7070 C to 100C (15810
33、0 C (158 Fto 212F).212 F). As soon as the wax is completely melted, thoroughly mix. Preheat the pipet or equivalent measuring device inorder to prevent the solidification of wax in the tip, and withdraw a portion of the sample as soon as possible after the wax hasmelted. The mass of wax transferred
34、to the test tube must be 1.001.00 g 6 0.05 g. 0.05 g. Allow the test tube to cool, and weighto at least the nearest 1 mg.1 mg.NOTE 3The weight of a test tube which is cleaned by means of solvent will not vary to a significant extent. Therefore, a tare weight may be obtainedand used repeatedly.8.2 Pi
35、pet 15 mL 15 mL of the solvent mixture into the test tube and place the latter just up to the level of its contents in a hotwater or steam bath. Heat the solvent-wax mixture, stirring up and down with the wire stirrer, until a homogeneous solution isobtained. Exercise care to avoid loss of solvent b
36、y prolonged boiling.NOTE 4Very high-melting wax samples may not form clear solutions. Stir until the undissolved material is well dispersed as a fine cloud.8.2.1 Plunge the test tube into an 800-mL800 mL beaker of ice water and continue to stir until the contents are cold. Removethe stirrer. Remove
37、the test tube from the ice bath, wipe dry on the outside with a cloth, and weigh to at least the nearest 0.1 g.0.1 g.NOTE 5During this operation the loss of solvent through vaporization should be less than 1 %. The weight of the solvent is, therefore, practicallya constant, and after a few samples a
38、re weighed, this weight can be used as a constant factor.8.3 Place the test tube containing the wax-solvent slurry in the cooling bath, which is maintained at 34.534.5 C 6 1.0C(30.01.0 C (30.0 F 6 2.0F).2.0 F). During this chilling operation, stir the contents of the tube by means of a temperatureme
39、asurement device placed in the tube. It is important that stirring by means of the temperature measurement device be almostcontinuous, in order to maintain a slurry of uniform consistency as the wax precipitates. Do not allow the wax to set up on thewalls of the cooling vessel nor permit any lumps o
40、f wax crystals to form. Continue stirring until the temperature reaches31.731.7 C 6 0.3C (25.00.3 C (25.0 F 6 0.5F).0.5 F).8.4 Remove the temperature measurement device from the tube and allow it to drain momentarily into the tube, thenimmediately immerse in the mixture the clean, dry filter stick,
41、which has previously been cooled by placing it in a test tube andholding at 34.534.5 C 6 1.0C (30.01.0 C (30.0 F 6 2.0F)2.0 F) in the cooling bath for a minimum of 10 min. 10 min.Seat the ground-glass joint of the filter so as to make an airtight seal. Place an unstoppered weighing bottle, previousl
42、y weighedtogether with the glass stopper to the nearest 0.1 mg, 0.1 mg, under the delivery nozzle of the filtration assembly.NOTE 6Take every precaution to ensure the accuracy of the weight of the stoppered weighing bottle. Prior to determining this weight, rinse the clean,dry weighing bottle and st
43、opper with the solvent mixture described in 6.3, wipe dry on the outside with a cloth, and place in the evaporation assemblyto dry for about 5 min. 5 min. Then remove the weighing bottle and stopper, place near the balance, and allow to stand for 10 min 10 min prior toAll dimensions are in millimetr
44、es.FIG. 3 Air Pressure RegulatorD3235 154weighing. Stopper the bottle during this cooling period. Once the weighing bottle and stopper have been dried in the evaporation assembly, lift only withforceps. Take care to remove and replace the glass stopper with a light touch.8.5 Apply air pressure to th
45、e filtration assembly and immediately collect about 4 mL 4 mL of filtrate in the weighing bottle.Release the air pressure to permit the liquid to drain back slowly from the delivery nozzle. Remove the weighing bottleimmediately, and stopper and weigh to at least the nearest 10 mg 10 mg without waiti
46、ng for it to come to room temperature.Unstopper the weighing bottle and place it under one of the jets in the evaporation assembly maintained at 3535 C61C (951 C(95 F 6 2F),2 F), with the air jet centered inside the neck, and the tip 1515 mm 6 5 mm 5 mm above the surface of the liquid.After the solv
47、ent has evaporated, which usually takes less than 30 min, 30 min, remove the bottle, stopper, and place near thebalance. Allow to stand for 10 min 10 min and weigh to the nearest 0.1 mg. 0.1 mg. Repeat the evaporation procedure, using 5min 5 min evaporation periods, until the loss between successive
48、 weighings is not over 0.2 mg.0.2 mg.9. Calculation9.1 Calculate the amount of extractables in the wax as follows:Solvent extractables,weight%5100 AC/BD (1)where:All dimensions are in millimetres (inches).FIG. 4 Evaporation AssemblyD3235 155A = weight of extractables residue, g,B = weight of wax sam
49、ple, g,C = weight of solvent, g, obtained by subtracting weight of test tube plus wax sample (8.1) from weight of test tube and contents(8.2), andC = weight of solvent, g, obtained by subtracting weight of test tube plus wax sample (8.1) from weight of test tube and contents(8.2), andD = weight of solvent evaporated, in g, obtained by subtracting weight of weighing bottle plus extractables residue from weightof weighing bottle plus filtrate (8.5).10. Report10.1 Report the result as solvent extract
