1、Designation: E 133 92 (Reapproved 2005)Standard Specification forDistillation Equipment1This standard is issued under the fixed designation E 133; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revision. A number
2、in parentheses indicates the year of last reapproval. Asuperscript epsilon (e) indicates an editorial change since the last revision or reapproval.This standard has been approved for use by agencies of the Department of Defense.1. Scope1.1 This specification covers distillation equipment used inthe
3、following ASTM test methods: D86, D 850, and (forapproved alternative requirements only) Test Method D 1078.1.2 Some items of equipment included in this specificationare common to all methods; other items are not. Therefore,those portions of this specification pertinent to the need mustbe selected.1
4、.3 The values stated in inch-pound units are to be regardedas standard. The values given in parentheses are mathematicalconversions to SI units that are provided for information onlyand are not considered standard.2. Referenced Documents2.1 ASTM Standards:2D86 Test Method for Distillation of Petrole
5、um Products atAtmospheric PressureD 850 Test Method for Distillation of Industrial AromaticHydrocarbons and Related MaterialsD 1078 Test Method for Distillation Range of VolatileOrganic LiquidsE1 Specification for ASTM Liquid-in-Glass ThermometersE 1272 Specification for Laboratory Glass Graduated C
6、yl-indersE 1405 Specification for Laboratory Glass DistillationFlasks3. Apparatus Assembly3.1 Typical assemblies of the apparatus are shown in Fig. 1and Fig. 2.4. Distillation Flasks4.1 Flasks of heat-resistant glass shall be provided asindicated in Fig. 3 and shall comply with the requirements ofSp
7、ecification E 1405.5. Condenser and Cooling Bath5.1 Typical approved types of condenser and cooling bathare included in Fig. 1 and Fig. 2. These items are common toall methods covered by this specification.5.2 The condenser shall be made of seamless brass tubing,22 in. (55.88 cm) in length. It shall
8、 be916 in. (14.29 mm) inoutside diameter, and shall have a wall thickness of 0.031 to0.036 in. (0.08 to 0.09 cm).5.3 The condenser shall be set so that approximately 15.5 in.(39.4 cm) of the tube will be in contact with the coolingmedium, with about 2 in. (5 cm) outside the cooling bath at theupper
9、end, and about 412 in. (11 cm) outside at the lower end.The length of tube projecting at the upper end shall be straightand shall be set at an angle of 75 with the vertical. The sectionof the tube inside the cooling bath may be either straight orbent in any suitable continuous, smooth curve. The ave
10、ragegradient shall be 0.26 in. (0.66 cm)/linear in. (2.54 cm) ofcondenser tube (sine of angle of 15), and no section of theimmersed portion of the condenser tube shall have a gradientless than 0.24 in. (0.61 cm) nor more than 0.28 in. (0.71 cm)/linear in. of tube. The projecting lower portion of the
11、 condensertube shall be curved downward for a length of 3 in. (7.62 cm)and slightly backward so as to ensure contact with the wall ofthe receiving graduate at a point approximately 1 to 114 in.(2.54 to 3.18 cm) below the top of the graduate when it is inposition to receive the distillate. The lower
12、end of the con-denser tube shall be cut off at an acute angle so that the tip maybe brought into contact with the wall of the cylinder.5.4 The capacity of the cooling bath shall be not less than340 in.3(5.55 L) of cooling medium. The arrangement of thetube in the cooling bath shall be such that its
13、center line shallbe not less than 114 in. (3.18 cm) below the plane of the top of1This specification is under the jurisdiction of ASTM Committee E41 onLaboratory Apparatus and is the direct responsibility of Subcommittee E41.01 onApparatus.Current edition approved Oct. 1, 2005. Published December 20
14、05. Originallyapproved in 1958. Last previous edition approved in 2000 as E 133 92 (2000)e1.2For 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 S
15、ummary page onthe ASTM website.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.the bath at its point of entrance and not less than34 in. (1.91cm) above the floor of the bath at its exit.5.5 Clearances between the condenser tube and t
16、he walls ofthe bath shall be at least12 in. (1.27 cm) except for the sectionsadjacent to the points of entrance and exit. Multiple installa-tions are permissible, provided they conform to the dimen-sional requirements and the capacity of the bath is not less than340 in.3(5.55 L)/tube.6. Metal Shield
17、 or Enclosure for Flask6.1 Type 1 Shield (Fig. 1) is 19 in. (48.26 cm) high, 11 in.(27.94 cm) long, and 8 in. (20.32 cm) wide, made of sheetmetal of approximately 22 gauge. It shall have a door on onenarrow side, and two openings 1 in. (2.54 cm) in diameter,equally spaced in each of the two narrow s
18、ides, with a slot cutin one side for the vapor tube. The centers of these fouropenings shall be 812 in. (21.59 cm) below the top of theshield. There shall be three14-in. (1.27 cm) holes in each of thefour sides, with their centers 1 in. above the base of the shield.6.2 Type 2 Shield (Fig. 2)is1714 i
19、n. (44.45 cm) high, 8 in.(20.32 cm) long, and 8 in. wide, made of sheet metal ofapproximately 22 gauge, with a window on the front side. Theopen bottom of the shield shall be spaced approximately 2 in.(5 cm) from the base of the unit. The rear of the shield shallhave an elliptical hole for the vapor
20、 tube. A flask-adjustingknob shall be located on front of the shield for adjusting theflask support. Also, a heat-adjusting indicating dial shall beused to provide stepless heat control when the electric heater isused. The entire mechanism shall be built into the bottomportion of the shield. When an
21、 electric heater is employed, theportion of the shield above the board shall be the same as withthe gas burner, but the part below may be omitted.7. Heat Source7.1 Gas Burner (Fig. 1), so constructed that sufficient heatfrom the available gas can be obtained to distill the product atthe specified ra
22、te. A sensitive regulating valve and gas pressuregovernor to give complete control of heating may be provided.7.2 Electric Heater (Fig. 2), may be used instead of a gasburner, provided it is capable of bringing over the first dropFIG. 1 Apparatus Assembly Using Gas BurnerFIG. 2 Apparatus Assembly Us
23、ing Electric HeaterE 133 92 (2005)2from a cold start within the time specified and of continuing thedistillation at the specified rate. Heater units of low heatretention, adjustable from 0 to 1000 W, have been foundsatisfactory.8. Flask Support8.1 Type 1 for Use with Gas Burner (Fig. 1)Aring support
24、of the ordinary laboratory type, 4 in. (10.2 cm) or larger indiameter, supported on a stand inside the shield or on aplatform, and adjustable from the outside of the shield, may beused.8.1.1 Two ceramic or hard heat-resistant boards,18 to14 in.(3.2 to 6.4 mm) in thickness, shall rest upon the ring o
25、r theplatform, whichever is used. The board immediately above thering or platform shall have a centered opening 3 to 4 in. (7.6 to10 cm) in diameter and outside line dimensions slightly smallerthan the inside boundaries of the shield.8.1.2 The second or flask-support board shall be slightlysmaller i
26、n outside dimensions than the first board and shallhave a centered opening conforming to the dimensions pre-scribed in Table 1. It shall be18 to14 in. in thickness at thecenter-hole rim. This flask-support board may be movedslightly in accordance with the directions for placing thedistillation flask
27、, and direct heat shall be applied to the flaskonly through the opening in this board.8.2 Type 2 for Use with Electric Heater (Fig. 2)The top ofthe electric heater shall consist of a ceramic or hard heat-resistant flask-support board with a centered hole as specifiedin Table 1, and a thickness of18
28、to14 in. at the center-hole rim.Provisions shall be made for moving the heater unit, with itstop, in order to place the distillation flask so that direct heatshall be applied to the flask only through the opening in theflask-support board.9. Graduated Cylinders9.1 Graduated cylinders shall be provid
29、ed as indicated inFig. 4 and shall comply with the requirements of SpecificationE 1272.10. Thermometers10.1 Thermometers meeting the requirements of Specifica-tion E1shall be provided (Table 2).11. Keywords11.1 apparatus; distillationType IIClass 3*Type IType IIClass 1*Type IIClass 5*NoteThe detaile
30、d construction requirements are found in Specification E 1405.FIG. 3 Distillation FlasksTABLE 1 Flask Support BoardsFlask Support Board Diameter of Opening, in. (cm)A114 (3.18)B112 (3.81)C 2 (5)D234 (6.91)E 133 92 (2005)3TABLE 4NoteThe detailed construction requirements are found in Specification E
31、1272.FIG. 4 Graduated CylindersE 133 92 (2005)4ASTM International takes 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,
32、and the riskof infringement of such rights, are entirely their own responsibility.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 revi
33、sion 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
34、shouldmake your views known to the ASTM Committee on Standards, at the 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 o
35、btained 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).TABLE 2 ThermometersASTMThermometerNo.ARangeSubdivisionsF C2C . 5 to 300 1C7F 30 to 580 . 2F7C . 2 to 300 1C8F 30 to 760 . 2F8C . 2 to
36、 400 1C37C . 2 to 52 0.2C38C . 24 to 78 0.2C39C . 48 to 102 0.2C40C . 72 to 126 0.2C41C . 98 to 152 0.2C42C . 95 to 255 0.5C102C . 123 to 177 0.2C103C . 148 to 202 0.2C104C . 173 to 227 0.2C105C . 198 to 252 0.2C106C . 223 to 277 0.2C107C . 248 to 302 0.2CAThe detailed constructional requirements for these thermometers are found inTable 1 of Specification E1.E 133 92 (2005)5
