1、Designation: D 850 03Standard Test Method forDistillation of Industrial Aromatic Hydrocarbons and RelatedMaterials1This standard is issued under the fixed designation D 850; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year
2、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.This standard has been approved for use by agencies of the Department of Defense.1. Scope *1.1 This test method covers the dis
3、tillation of industrialaromatic hydrocarbons and related materials of relativelynarrow boiling ranges from 30 to 250C.1.2 The values stated in SI units are to be regarded as thestandard. The values given in parentheses are for informationonly.1.3 The following applies to all specified limits in this
4、 testmethod: for the purposes of determining conformance to thistest method, an observed or calculated value shall be roundedoff “to the nearest unit” in the last right-hand digit used inexpressing the specification limit, in accordance with therounding-off method of Practice E 29.1.4 This standard
5、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 applica-bility of regulatory limitations prior to use. For specific hazardstatements, 6
6、.6.1and Section 7.2. Referenced Documents2.1 ASTM Standards:D 1078 Test Method for Distillation Range of VolatileOrganic Liquids2D 3437 Practice for Sampling and Handling Liquid CyclicProducts2D 4790 Terminology of Aromatic Hydrocarbons and Re-lated Chemicals2E 1 Specification for ASTM Thermometers3
7、E 29 Practice for Using Significant Digits in Test Data toDetermine Conformance with Specifications4E 133 Specification for Distillation Equipment5E 220 Test Method for Calibration of Thermocouples byComparison Techniques3E 691 Practice for Conducting an Interlaboratory Study toDetermine the Precisi
8、on of a Test Method42.2 Other Document:OSHA Regulations, 29 CFR, paragraphs 1910.1000 and1910.120063. Terminology3.1 Definitions:3.1.1 See Terminology D 4790 for definitions of terms usedin this test method.4. Summary of Test Method4.1 The distillation of a 100-mL sample of industrial aro-matic hydr
9、ocarbons and related materials is carried out via acarefully controlled distillation wherein temperature readingsare noted for the first drop of distillate and when 5, 10, andeach additional 10 up to 90, and 95 % of the sample hasdistilled over. The temperature corresponding to the dry pointis also
10、noted.5. Significance and Use5.1 This test method is suitable for setting specifications, foruse as an internal quality control tool, and for use in develop-ment or research work on industrial aromatic hydrocarbons andrelated materials.5.2 This test method gives a broad indication of generalpurity a
11、nd can also indicate presence of excessive moisture. Itwill not differentiate between products of similar boiling range.6. Apparatus6.1 Distillation FlaskA standard 200-mL side-tube, heat-resistant glass distillation flask as shown in Fig. 1, conformingto the following dimensions:1This test method i
12、s under the jurisdiction of ASTM Committee D16 onAromatic Hydrocarbons and Related Chemicals and is the direct responsibility ofSubcommittee D16.04 on Instrumental Analysis.Current edition approved Jan. 10, 2003. Published March 2003. Originallyapproved in 1945. Last previous edition approved in 200
13、2 as D 850 02e1.2Annual Book of ASTM Standards, Vol 06.04.3Annual Book of ASTM Standards, Vol 14.03.4Annual Book of ASTM Standards, Vol 14.02.5Annual Book of ASTM Standards, Vol 14.04.6Available from Superintendent of Documents, U.S. Government PrintingOffice, Washington, DC 20402.1*A Summary of Cha
14、nges section appears at the end of this standard.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.Diameter of bulb, outside, mm 76 6 1.5Diameter of neck, inside, mm 21 6 1Height of flask, outside, mm 179 6 3Vertical distance from botto
15、m of bulb outside tobottom of vapor-tube opening in neck, mm120 6 3Length of side tube, mm 100 6 3Diameter of side tube, outside, mm 7 6 0.5Angle of side tube with vertical axis of bulb andneck, 75 6 3The flask does not comply with Flask C of SpecificationE 133.6.2 Temperature Measurement Devices:6.
16、2.1 Manual Distillation Thermometer The ASTM Sol-vents Distillation Thermometer used in the test shall be asprescribed in the specifications for the material being tested. Ifno thermometer is specified in the material specification, selectone from Table 1 with the smallest graduations that will cove
17、rthe entire distillation range of the material being tested. Table1 lists several ASTM solvents distillation thermometers whichare suitable for testing industrial aromatic hydrocarbons, andwhich meet the requirements of Specification E 1.6.2.2 Automatic Distillation Temperature SensorTemperature mea
18、surement systems using thermocouples orresistance thermometers, otherwise referred to as the “tempera-ture measuring devices,” must exhibit the same temperature lagand accuracy as the equivalent mercury glass thermometer.Confirmation of the calibration of these temperature sensors isto be done at re
19、gular intervals. This may be accomplished asprescribed in Test Method E 220, or some similar means usinga precision resistance decade box. Another technique is todistill pure toluene and compare the temperature indicated bythe thermocouple or resistance thermometer with that shownby the thermometer.
20、 When installing a new automatic distilla-tion analyzer, a toluene sample with a known distillation rangeof approximately 1.0C must be used to verify the dry pointand distillation range.7It is recommended that such a materialbe used when replacing a temperature measuring device.Alternatively a mater
21、ial of known distillation range and drypoint may be used when replacing a temperature measuringdevice.6.2.2.1 Automatic Distillation Temperature Sensor Center-ing DeviceThe temperature sensor shall be mounted througha snug-fitting device designed to mechanically center thesensor in the neck of the f
22、lask. The use of a cork or siliconestopper with a hole drilled through the center is not acceptablefor this purpose. Examples of acceptable centering devices areshown in Fig. 2.6.2.2.2 The electronic circuitry or algorithms, or both, usedshall include the capability to simulate the temperature lag o
23、fa mercury-in-glass thermometer. For that reason the knowntoluene sample with a distillation range of approximately 1.0Cmust be used to verify the algorithm and dampening software.6.2.2.3 Alternatively, the sensor can also be placed in acasing with the tip of the sensor covered, so that the assembly
24、,because of its adjusted thermal mass and conductivity, has atemperature lag similar to that of a mercury-in-glass thermom-eter.NOTE 1In a region where the temperature is changing rapidly duringthe distillation, the temperature lag of a thermometer can be as much as3s.6.3 Condenser and Cooling Bath:
25、6.3.1 Manual Distillation Condenser and Cooling Bath:6.3.1.1 The manual distillation condenser and cooling bathshall be as specified in Section 5, and Fig. 1 of SpecificationE 133.6.3.1.2 As an alternative, the condenser tube may consist ofa straight glass tube 600 to 610 mm in length and 12 mm inin
26、side diameter, of standard wall thickness (about 1.25 mm)with the exit end cut off square and ground flat. It shall be setin a cooling trough so that at least 380 mm of the tube is incontact with the water. Clearance between the condenser tubeand any parallel side of the trough shall be not less tha
27、n 19 mm.The water in the cooling trough shall be maintained at 10 to20C. This may be done by adding ice to the water or bycirculating chilled water through the trough. The trough shallbe so mounted that the condenser tube is set at an angle of 75with the vertical.6.3.2 Automatic Distillation and Coo
28、ling BathThe auto-matic distillation and cooling bath shall be as specified inSection 5, Fig. 2 of Specification E 133.6.4 Distillation Receiver:6.4.1 Manual Distillation ReceiverA graduate of the cy-lindrical type, of uniform diameter, with a pressed or molded7Such a material is available from Spec
29、trum Quality Standards.FIG. 1 Distillation FlaskTABLE 1 ASTM Thermometers for Distillation Test of IndustrialAromatic HydrocarbonsASTMTher-mometerNo.Name Range, CSubdivision,C39C solvents distillation 48 to 102 0.240C solvents distillation 72 to 126 0.241C solvents distillation 98 to 152 0.242C solv
30、ents distillation 95 to 255 0.5102C solvents distillation 123 to 177 0.2103C solvents distillation 148 to 202 0.2104C solvents distillation 173 to 227 0.2105C solvents distillation 198 to 252 0.2D850032base and a lipped top. The cylinder shall be marked to contain100 mL, and the 0 to 100 mL receiver
31、 portion shall be not lessthan 178 nor more than 203 mm in length. It shall be graduatedin single millilitres and each fifth mark shall be distinguishedby a longer line. It shall be numbered from the bottom up atintervals of 10 mL. The overall height of the receiver shall notbe less than 248 nor mor
32、e than 260 mm. The graduations shallnot be in error by more than 1 mL at any point on the scale. Thebottom 1-mL graduation may be omitted. The receiver com-plies with Section 9, Graduate B Fig. 4, of Specification E 133.6.4.2 Automatic Distillation ReceiverA receiver to beused with measurements in a
33、ccordance with the instrumentmanufacturer and conform to the physical specifications de-scribed in this section, with the exception of the graduations.6.4.2.1 Automatic Distillation Level FollowerFor auto-matic apparatus, the level follower or recording mechanism ofthe apparatus will have a resoluti
34、on of 0.1 mL with an accuracyof 6 1 mL. The calibration of the assembly should beconfirmed according to the manufacturers instructions atregular intervals. The typical calibration procedure involvesverifying the output with the receiver containing 5 and 100 mLof material respectively.6.5 Flask Suppo
35、rt Assembly:6.5.1 For Units Using Electric HeatersThe assemblyconsists of an adjustable system onto which the electric heateris mounted with provision for placement of a flask supportboard (see 6.5.2) above the electric heater. The whole assemblyis adjustable from the outside of the shield.6.5.2 Fla
36、sk Support BoardThe flask support board shallbe constructed of ceramic or other heat-resistant material witha centrally located opening. For tests of benzene and toluene,the opening shall be 25 mm in diameter; for tests of materialsboiling above toluene but mostly below 145C, the openingshall be 38
37、mm in diameter, and for higher boiling materials, itshall be 50 mm in diameter. The flask support board shall be ofsufficient dimension to ensure that thermal heat to the flaskonly comes from the central opening and that extraneous heatto the flask other than through the central opening is mini-mize
38、d. (WarningAsbestos-containing materials shall not beused in the construction of the flask support board.)6.5.3 For Units Using Bunsen BurnerThe flask supportboard is approximately 50 mm higher than the top of theburner.6.6 Heater:6.6.1 Manual Distillation HeaterAn electric heater or abunsen burner,
39、 fully adjustable and capable of giving sufficientheat to distill the product at the required rate. When a bunsenburner is used, as described in 7.1 and Fig. 1 of SpecificationE 133, the burner shall be adjusted so as to produce an entirelyblue flame. (WarningSuperheating of the flask can causeerron
40、eous results and is more likely to occur with electricheaters than with bunsen burners as heat sources. This problemis discussed in the section on Preparation of Apparatus in TestMethod D 1078.)7. Hazards7.1 Consult current OSHA regulations and suppliers Mate-rial Safety Data Sheets, and local regul
41、ations, for all materialsused in this test method.8. Sampling8.1 Sampling should follow safe rules in order to adhere toall safety precautions as outlined in the latest OSHA regula-tions. Refer to Practice D 3437 for proper sampling andhandling of aromatic hydrocarbons analyzed by this testmethod.FI
42、G. 2 Examples of Centering Device Designs for Straight-Bore Neck FlasksD8500338.2 The sample under test shall be transparent and free ofseparated water. Any separated water may ordinarily be elimi-nated by care in pouring the 100-mL specimen (10.1) into thegraduated cylinder. If necessary, any separ
43、ated water or cloudi-ness may be removed by filtration, in which case the followingprecautions shall be taken: Use a soft paper through which thespecimen filters rapidly, avoid drafts, cover the funnel with awatch glass, and filter at least 200 mL from which to take the100 mL for distillation. Dehyd
44、ration (that is, removal ofdissolved water) is not permissible. Note, however, that certainmaterials, especially benzene, may absorb traces of water thatcan be significant with respect to this test. When it can beshown that failure to pass this distillation test is due to thepresence of dissolved wa
45、ter, it shall be permissible, if mutuallyagreeable to the purchaser and the seller, to dry the specimenby any method agreed to by both the purchaser and the seller.9. Assembly of Apparatus9.1 Manual Distillation Apparatus:9.1.1 Remove any residual liquid in the condenser tube byswabbing with a piece
46、 of lint-free cloth attached to a cord orwire.9.1.2 Assemble the apparatus. Mount the flask on theinsulation board of appropriate dimensions, with the side tubeextending through a tightly fitting silicone or cork stopperabout 50 mm into the condenser tube.9.1.3 Support the distillation thermometer i
47、n the neck of theflask by means of a cork or silicone stopper with the thermom-eter vertical and centered in the neck of the flask and in sucha position that the top of the bulb (or top of contraction bulb ifpresent) is level with the lowest point of juncture between theside tube and the neck of the
48、 flask (see Fig. 3).9.1.4 Place the burner directly under the center of the holein the insulation board.9.2 Automatic Distillation ApparatusFor assembly of au-tomatic distillation apparatus, consult the instrument manufac-turers operating manual.NOTE 2The centering device must be as stated in 6.2.2.
49、1 (Fig. 2).9.3 Carefully measure a 100-mL specimen of the material tobe tested in the 100-mL graduated cylinder at room tempera-ture and transfer to the distillation flask, draining the cylinderat least 15 s. This is preferably done before mounting the flaskin position, in order to prevent liquid from entering the sidearm. Do not rinse out the graduated cylinder used to measurethe sample for distillation, but place under the lower end of thecondenser tube to receive the distillate.9.4 Fit the flask vapor tube, provided with a snug fittingsilicone rubber sto
