1、Designation: D850 11Standard Test Method forDistillation of Industrial Aromatic Hydrocarbons and RelatedMaterials1This standard is issued under the fixed designation D850; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of
2、 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.1. Scope*1.1 This test method covers the distill
3、ation 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 tes
4、tmethod: 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 E29.1.4 WarningMercury has
5、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 should be taken when handling mercury andmercury-containing products. See the appli
6、cable 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 both, in your state may be prohibited bystate law.1.5 This standard does not pur
7、port 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, 6.6.1 and Sec
8、tion 7.2. Referenced Documents2.1 ASTM Standards:2D1078 Test Method for Distillation Range of Volatile Or-ganic LiquidsD3437 Practice for Sampling and Handling Liquid CyclicProductsD4790 Terminology ofAromatic Hydrocarbons and RelatedChemicalsE1 Specification for ASTM Liquid-in-Glass ThermometersE29
9、 Practice for Using Significant Digits in Test Data toDetermine Conformance with SpecificationsE133 Specification for Distillation EquipmentE220 Test Method for Calibration of Thermocouples ByComparison TechniquesE691 Practice for Conducting an Interlaboratory Study toDetermine the Precision of a Te
10、st Method2.2 Other Document:OSHA Regulations, 29 CFR paragraphs 1910.1000 and1910.120033. Terminology3.1 Definitions:3.1.1 See Terminology D4790 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 hydrocarbons and
11、related materials is carried out via acarefully controlled distillation wherein temperature readingsare noted for the first drop of distillate and when 5, 10, and1This test method is under the jurisdiction of ASTM Committee D16 onAromatic Hydrocarbons and Related Chemicals and is the direct responsi
12、bility ofSubcommittee D16.04 on Instrumental Analysis.Current edition approved July 1, 2011. Published July 2011. Originally approvedin 1945. Last previous edition approved in 2008 as D850 03 (2008)1. DOI:10.1520/D0850-11.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontac
13、t ASTM 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, h
14、ttp:/www.access.gpo.gov.1*A Summary of Changes 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.each additional 10 up to 90, and 95 % of the sample hasdistilled over. The temperature correspo
15、nding to the 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
16、 indication 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
17、dimensions: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 sid
18、e tube with vertical axis of bulb andneck, 75 6 3The flask does not comply with Flask C of SpecificationE133.6.2 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 mater
19、ial being 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 in
20、dustrial aromatic 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 temper
21、ature lagand 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 E220, or some similar means usinga precision resistance decade box. Another technique
22、 is todistill 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 dr
23、y pointand 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 Cent
24、er-ing DeviceThe 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 device
25、s areshown 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
26、 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,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
27、temperature 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.
28、1 of SpecificationE133.6.3.1.2 As an alternative, the condenser tube may consist ofa straight glass tube 600 to 610 mm in length and 12 mm in4Such a material is available from Spectrum Quality Standards.FIG. 1 Distillation FlaskTABLE 1 ASTM Thermometers for Distillation Test of IndustrialAromatic Hy
29、drocarbonsASTMThermometerNo.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 solvents distillation 95 to 255 0.5102C solvents distillation 123 to 177 0.2103C solvents distillation 148 to 202 0.2104C sol
30、vents distillation 173 to 227 0.2105C solvents distillation 198 to 252 0.2D850 112inside 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
31、 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 condenser
32、 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 E133.6.4 Distillation Receiver:6.4.1 Manual Distillation ReceiverA graduate of the cy-lindrical type, o
33、f 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 a l
34、onger 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-pli
35、es with Section 9, Graduate B Fig. 4, of Specification E133.6.4.2 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.6.4.2.1 A
36、utomatic 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. The
37、 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 plac
38、ement 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 benzene a
39、nd 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 thermal
40、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 resistant-containing materials shallnot be used in the construction of the flask support board.)6.5.3 For Units Using Bunsen BurnerThe flask su
41、pportboard 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 and
42、Fig. 1 of SpecificationE133, the burner shall be adjusted so as to produce an entirelyblue flame. (WarningSuperheating of the flask can causeerroneous results and is more likely to occur with electricFIG. 2 Examples of Centering Device Designs for Straight-Bore Neck FlasksD850 113heaters than with b
43、unsen burners as heat sources. This problemis discussed in the section on Preparation of Apparatus in TestMethod D1078.)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. Sampling8.1 Sampling
44、should follow safe rules in order to adhere toall safety precautions as outlined in the latest OSHA regula-tions. Refer to Practice D3437 for proper sampling andhandling of aromatic hydrocarbons analyzed by this testmethod.8.2 The sample under test shall be transparent and free ofseparated water. An
45、y 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 which thespecimen f
46、ilters 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 traces of water thatca
47、n 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 purchaser and th
48、e 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 dimensions, with the side
49、 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 insulation board.9.2 Aut
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