1、Designation: D 889 99 (Reapproved 2009)Standard Test Method forVolatile Oil in Rosin1This standard is issued under the fixed designation D 889; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revision. A number in
2、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 volatileoil content of rosin or similar material. The oil may consist ofnaturally occurring terp
3、ene oil, such as heavy fractions ofturpentine, resulting from incomplete distillation in the pro-cessing of the rosin, or of foreign nonterpene oil resulting fromincomplete removal of mineral or coal-tar solvent used toextract the rosin from wood or still wastes. In certain cases thevolatile oil cou
4、ld consist of decarboxylated rosin formedduring the processing of the rosin.1.2 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.3 This standard does not purport to address all of thesafety concerns, if any, associated with its
5、 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.2. Referenced Documents2.1 ASTM Standards:2D 233 Test Methods of Sampling and Testing TurpentineE1 Specification fo
6、r ASTM Liquid-in-Glass Thermometers3. Significance and Use3.1 Rosin and similar materials such as rosin derivativesoften contain volatile material derived from the raw materialused or formed as a result of the processing of the rosin. Thisvolatile material can have a significant effect on the physic
7、aland chemical properties of the rosin and so a standard methodfor its determination is required.4. Apparatus4.1 Flask, 500-mL round-bottom having a thermometer welland a 24/40 standard-taper ground joint for connection with thetrap (see Fig. 1).4.2 Trap (Fig. 2), designed so as to overcome the tend
8、encyfor droplets of oil to remain below the surface of the water, dueto the greater viscosity of the volatile oils recovered from rosin,and thus be returned to the flask (Note 1). The trap shall befitted with 24/40 standard-taper ground joints to provide tightconnections with the flask and condenser
9、, in order to avoidvapor loss.NOTE 1This trap is a modification of the original Clevenger trap usedto recover oils lighter than water. In that trap the oil and water condensatedrop directly into the graduated part of the trap. Due to the viscouscharacter, density, and surface tension of the oils rec
10、overed from rosin,cylindrical columns of oil were formed below the surface of the water inthe graduated section of the trap, which were not penetrated by the watercondensed immediately thereafter. This resulted in alternate columns of oiland water in the graduated section. These were returned to the
11、 distillingflask in the same order as they occurred, through the side arm of the trap.As this condition continued indefinitely, it was impossible to completelyremove all the oil from the rosin. By raising the opening of the side armof the trap to the position shown, to bring the surface of the liqui
12、d into thewide part of the trap above the narrow graduated section, the oil iscollected in a thinner film that can be penetrated readily by the droplets ofwater falling from the end of the condenser, and only the water is thuscollected in the narrow graduated section. At the end of the test, the oil
13、 isslowly brought down into the graduated section and its volume read. Thesystem or apparatus loss amounts to not more than 0.1 mL of oil.4.3 Condenser, straight-tube, 300-mm, water-jacketed re-flux type, with a 24/40 standard-taper ground joint for connec-tion with the trap.4.4 Heat SourceAn oil ba
14、th containing high-temperature-resistant oil, or an electric heater of the mantle type in whichthe heating elements are encased in a glass cloth mantle of suchshape as to partially or completely surround the flask beingheated.4.5 Thermometer, having a range from 30 to 200 C, ASTM16C or equivalent (s
15、ee Specification E1).4.6 Glass Beads.5. Procedure5.1 Place 50 g of the crushed sample in the flask, add 125mL of a glycerin-water solution (4 + 1), add a few glass beads,insert an ebullition tube, and connect the flask with the trap.Fill the trap (Fig. 2) with water through the top opening untilthe
16、water level is even with the bottom of the seal of the smallreturn tube to the side arm. Insert the thermometer, and connectthe condenser.1This test method is under the jurisdiction of ASTM Committee D01 on Paintand Related Coatings, Materials, and Applications and is the direct responsibility ofSub
17、committee D01.34 on Naval Stores.Current edition approved June 1, 2009. Published June 2009. Originallyapproved in 1946. Last previous edition approved in 2004 as D 889 99 (2004).2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org.
18、 For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.5.2 Regulate the applied heat until the liquid in the flask isbroug
19、ht to a boil and distillation continues at a constanttemperature, which will be about 125C at the start. At thisstage, open the stopcock slightly and withdraw the water fromthe trap into a small graduated cylinder at the rate of 1 drop to5 drops off the lower end of the condenser. Control the reflux
20、rate so that no uncondensed vapors escape from the top of thecondenser. The withdrawal of water from the system should beat the rate of about 1 mL/min. Increase the heat from time totime to maintain uniform continuous operation with slowlyrising temperature. Discontinue the distillation when the tem
21、-perature reaches 180C.5.3 Remove the source of heat and allow the distillation tosubside (Note 2). Draw off water until all the oil is brought intothe graduated section of the trap and note the volume. Thedensity of the oil is usually very close to 1.00.FIG. 1 FlaskFIG. 2 TrapD 889 99 (2009)2NOTE 2
22、The contents of the flask should be poured out while stillwarm, before the rosin has become viscous or solid, to facilitate cleaningand avoid strain on the glass when the rosin becomes cold.6. Report6.1 Properly made rosin yields not more than 0.5 mL ofresidual volatile oil per 50 g of sample. If th
23、e recovered oil iswithin such limit, report the rosin as free of excess volatile oil.If more than 0.5 mL of oil is recovered, report the total volumeobtained.NOTE 3The volatile oil recovered from gum rosin consists primarilyof high-boiling terpene components of the crude gum, most of whichunder prop
24、er distillation will have been recovered as turpentine by thetime the rosin is drawn from the still. Faulty distillation or prematurewithdrawal may yield a rosin giving a higher than normal recovery of oil,with a refractive index below 1.483. The polymerization residue shouldhave a refractive index
25、not lower than 1.500. In the case of wood rosins,generally obtained by extraction from stumpwood with a petroleum ornaphtha solvent, any recovered oil would probably consist of unrecoveredsolvent. The refractive index of both the recovered oil and the polymer-ization residue therefrom would be well
26、under the above figures for gumrosin.7. Additional Examination of Oil7.1 Drain off the water, transfer the oil to a small glasscontainer, stopper, and allow to settle until clear. Note the odorand determine the refractive index. For further information onthe nature of the oil, volume permitting, mak
27、e a polymerizationtest according to the procedure given in Test Methods D 233.8. Precision and Bias8.1 This test method is not often used for the determinationof volatile oil in rosin and so it is not practical to measure itsprecision and bias.9. Keywords9.1 rosin; volatile oilASTM International tak
28、es 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 such rights, are entirely their own re
29、sponsibility.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 additional standardsand should be addres
30、sed 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 Standards, at th
31、e 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 889 99 (2009)3
