1、Designation: D 850 03 (Reapproved 2008)e1Standard 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
2、 revision, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.This standard has been approved for use by agencies of the Department of Defense.e1NOTEMercury warning was
3、editorially added in June 2008.1. Scope1.1 This test method covers the distillation 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
4、 informationonly.1.3 The following applies to all specified limits in this 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
5、accordance with therounding-off method of Practice E29.1.4 WarningMercury has been designated by EPA andmany state agencies as a hazardous material that can causecentral nervous system, kidney and liver damage. Mercury, orits vapor, may be hazardous to health and corrosive tomaterials. Caution shoul
6、d be taken when handling mercury andmercury-containing products. See the applicable product Ma-terial Safety Data Sheet (MSDS) for details and EPAs website(http:/www.epa.gov/mercury/faq.htm) for additional informa-tion. Users should be aware that selling mercury or mercury-containing products, or bo
7、th, in your state may be prohibited bystate law.1.5 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 applica-bility of reg
8、ulatory limitations prior to use. For specific hazardstatements, 6.6.1and Section 7.2. Referenced Documents2.1 ASTM Standards:2D 1078 Test Method for Distillation Range of VolatileOrganic LiquidsD 3437 Practice for Sampling and Handling Liquid CyclicProductsD 4790 Terminology of Aromatic Hydrocarbon
9、s and Re-lated ChemicalsE1 Specification for ASTM Liquid-in-Glass ThermometersE29 Practice for Using Significant Digits in Test Data toDetermine Conformance with SpecificationsE 133 Specification for Distillation EquipmentE 220 Test Method for Calibration of Thermocouples ByComparison TechniquesE 69
10、1 Practice for Conducting an Interlaboratory Study toDetermine the Precision of a Test Method2.2 Other Document:OSHA Regulations, 29CFR paragraphs 1910.1000 and1910.120033. Terminology3.1 Definitions:3.1.1 See Terminology D 4790 for definitions of terms usedin this test method.4. Summary of Test Met
11、hod4.1 The distillation of a 100-mL sample of industrial aro-matic hydrocarbons and related materials is carried out via acarefully controlled distillation wherein temperature readings1This test method is under the jurisdiction of ASTM Committee D16 onAromatic Hydrocarbons and Related Chemicals and
12、is the direct responsibility ofSubcommittee D16.04 on Instrumental Analysis.Current edition approved June 1, 2008. Published June 2008. Originallyapproved in 1945. Last previous edition approved in 2003 as D 850 03.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM
13、Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3Available from U.S. Government Printing Office Superintendent of Documents,732 N. Capitol St., NW, Mail Stop: SDE, Washington, DC 20401, http:/ww
14、w.access.gpo.gov.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.are 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 th
15、e dry pointis also 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
16、 of generalpurity and 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:
17、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 bottom 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
18、 vertical axis of bulb andneck, 75 6 3The flask does not comply with Flask C of SpecificationE 133.6.2 Temperature Measurement Devices:6.2.1 Manual Distillation ThermometerThe ASTM Sol-vents Distillation Thermometer used in the test shall be asprescribed in the specifications for the material being
19、tested. Ifno thermometer is specified in the material specification, selectone from Table 1 with the smallest graduations that will coverthe entire distillation range of the material being tested. Table1 lists several ASTM solvents distillation thermometers whichare suitable for testing industrial a
20、romatic hydrocarbons, andwhich meet the requirements of Specification E1.6.2.2 Automatic Distillation Temperature SensorTemperature measurement systems using thermocouples orresistance thermometers, otherwise referred to as the “tempera-ture measuring devices,” must exhibit the same temperature laga
21、nd accuracy as the equivalent mercury glass thermometer.Confirmation of the calibration of these temperature sensors isto be done at regular intervals. This may be accomplished asprescribed in Test Method E 220, or some similar means usinga precision resistance decade box. Another technique is todis
22、till pure toluene and compare the temperature indicated bythe thermocouple or resistance thermometer with that shownby the thermometer. 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 pointan
23、d distillation range.4It is recommended that such a materialbe used when replacing a temperature measuring device.Alternatively a material of known distillation range and drypoint may be used when replacing a temperature measuringdevice.6.2.2.1 Automatic Distillation Temperature Sensor Center-ing De
24、viceThe temperature sensor shall be mounted througha snug-fitting device designed to mechanically center thesensor in the neck of the flask. The use of a cork or siliconestopper with a hole drilled through the center is not acceptablefor this purpose. Examples of acceptable centering devices areshow
25、n in Fig. 2.6.2.2.2 The electronic circuitry or algorithms, or both, usedshall include the capability to simulate the temperature lag ofa 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 damp
26、ening 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,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 temperatu
27、re is changing rapidly duringthe distillation, the temperature lag of a thermometer can be as much as3s.6.3 Condenser and Cooling Bath: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 Spec
28、ificationE 133.4Such a material is available from Spectrum Quality Standards.FIG. 1 Distillation FlaskTABLE 1 ASTM Thermometers for Distillation Test of IndustrialAromatic HydrocarbonsASTMThermometerNo.Name Range, CSubdivision,C39C solvents distillation 48 to 102 0.240C solvents distillation 72 to 1
29、26 0.241C solvents distillation 98 to 152 0.242C solvents 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 0.2D 850 03 (2008)e126.3.1.2 As an alternative, the con
30、denser tube may consist ofa straight glass tube 600 to 610 mm in length and 12 mm ininside 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. Clearan
31、ce between the condenser tubeand any parallel side of the trough shall be not less than 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 condens
32、er tube is set at an angle of 75with the vertical.6.3.2 Automatic Distillation and Cooling 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
33、, of uniform diameter, with a pressed or moldedbase and a lipped top. The cylinder shall be marked to contain100 mL, and the 0 to 100 mL receiver 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
34、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 more than 260 mm. The graduations shallnot be in error by more than 1 mLat any point on the scale. Thebottom 1-mL graduation may be omitted. The receiver com-
35、plies with Section 9, Graduate B Fig. 4, of Specification E 133.6.4.2 Automatic Distillation ReceiverA receiver to beused with measurements in accordance with the instrumentmanufacturer and conform to the physical specifications de-scribed in this section, with the exception of the graduations.6.4.2
36、.1 Automatic Distillation Level FollowerFor auto-matic apparatus, the level follower or recording mechanism ofthe apparatus will have a resolution of 0.1 mL with an accuracyof 61 mL. The calibration of the assembly should be con-firmed according to the manufacturers instructions at regularintervals.
37、 The typical calibration procedure involves verifyingthe output with the receiver containing 5 and 100 mL ofmaterial respectively.6.5 Flask Support Assembly:6.5.1 For Units Using Electric HeatersThe assemblyconsists of an adjustable system onto which the electric heateris mounted with provision for
38、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 Flask Support BoardThe flask support board shallbe constructed of ceramic or other heat-resistant material witha centrally located opening. For tests of benze
39、ne and toluene,the opening shall be 25 mm in diameter; for tests of materialsboiling above toluene but mostly below 145C, the openingshall be 38 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 ther
40、mal heat to the flaskonly comes from the central opening and that extraneous heatto the flask other than through the central opening is mini-mized. (WarningHeat rsisitant-containing materials shallnot be used in the construction of the flask support board.)6.5.3 For Units Using Bunsen BurnerThe flas
41、k 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, 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
42、and Fig. 1 of SpecificationE 133, the burner shall be adjusted so as to produce an entirelyblue flame. (WarningSuperheating of the flask can causeFIG. 2 Examples of Centering Device Designs for Straight-Bore Neck FlasksD 850 03 (2008)e13erroneous results and is more likely to occur with electricheat
43、ers 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 regulations, for all materialsused in this test method.8. Sampl
44、ing8.1 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.8.2 The sample under test shall be transparent and free ofse
45、parated 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 separated water or cloudi-ness may be removed by filtration, in which case the followingprecautions shall be taken: Use a soft paper through wh
46、ich 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. Dehydration (that is, removal ofdissolved water) is not permissible. Note, however, that certainmaterials, especially benzene, may absorb trace
47、s 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 water, it shall be permissible, if mutuallyagreeable to the purchaser and the seller, to dry the specimenby any method agreed to by both the
48、 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 of lint-free cloth attached to a cord orwire.9.1.2 Assemble the apparatus. Mount the flask on theinsulation board of appropriate dimensio
49、ns, 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 in 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 flask (see Fig. 3).9.1.4 Place the burner directly under the center of the holein the insulat
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