1、Designation: D850 16Standard 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 U.S. Department of Defense.1. Scope*1.1 This test method covers the di
3、stillation 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 asstandard. No other units of measurement are included in thisstandard.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 E29.1.4 WarningMercury
5、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 should be taken when handling mercury andmercury-containing products. See the a
6、pplicable productSafety Data Sheet (SDS) for details and EPAs website (http:/www.epa.gov/mercury/faq.htm) for additional information.Users should be aware that selling mercury or mercury-containing products, or both, in your state may be prohibited bystate law.1.5 The values stated in SI units are t
7、o be regarded asstandard. No other units of measurement are included in thisstandard.1.6 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 an
8、d determine the applica-bility of regulatory limitations prior to use. For specific hazardstatements, 6.6.1 and Section 7.2. Referenced Documents2.1 ASTM Standards:2D1078 Test Method for Distillation Range of Volatile Or-ganic LiquidsD3437 Practice for Sampling and Handling Liquid CyclicProductsD479
9、0 Terminology of Aromatic Hydrocarbons and RelatedChemicalsD6809 Guide for Quality Control and Quality AssuranceProcedures for Aromatic Hydrocarbons and Related Ma-terialsE1 Specification for ASTM Liquid-in-Glass ThermometersE29 Practice for Using Significant Digits in Test Data toDetermine Conforma
10、nce 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 Test Method2.2 Other Document:OSHA Regulations, 29 CFR paragraphs 1910.100
11、0 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 related materials is carried out via acarefully controlled distillation
12、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 responsibility ofSubcommittee D16.04 on Instrumental Analysis.Current edition ap
13、proved June 1, 2016. Published July 2016. Originally approvedin 1945. Last previous edition approved in 2011 as D850 11. DOI: 10.1520/D0850-16.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards vo
14、lume 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:/www.access.gpo.gov.*A Summary of Changes section appears at the end of thi
15、s standardCopyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States1each additional 10 up to 90, and 95 % of the sample hasdistilled over. The temperature corresponding to the dry pointis also noted.5. Significance and Use5.1 This test method i
16、s 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 and can also indicate presence of excessive moisture
17、. 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:Diameter of bulb, outside, mm 76 1.5Diameter of neck, inside, mm 21 1H
18、eight of flask, outside, mm 179 3Vertical distance from bottom of bulb outside tobottom of vapor-tube opening in neck, mm1203Length of side tube, mm 100 3Diameter of side tube, outside, mm 7 0.5Angle of side tube with vertical axis of bulb andneck, 753The flask does not comply with Flask C of Specif
19、icationE133.6.2 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 tested. Ifno thermometer is specified in the material specification, selectone from Tab
20、le 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 aromatic hydrocarbons, andwhich meet the requirements of Specification E1.6.2.2 Automati
21、c Distillation Temperature SensorTemperature measurement 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
22、 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 is todistill pure toluene and compare the temperature indicated bythe thermocouple or resistance
23、 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 pointand distillation range.4It is recommended that such a materialbe used when replacing a tem
24、perature 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 DeviceThe temperature sensor shall be mounted througha snug-fitting device designed to mec
25、hanically 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 areshown in Fig. 2.6.2.2.2 The electronic circuitry or algorithms, or both, usedshall include t
26、he 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 dampening software.6.2.2.3 Alternatively, the sensor can also be placed in acasing with the
27、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 temperature is changing rapidly duringthe distillation, the temperature lag of a thermometer can
28、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 SpecificationE133.4Such a material is available from Spectrum Quality Standards.FIG. 1 Disti
29、llation 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 126 0.241C solvents distillation 98 to 152 0.242C solvents distillation 95 to 255 0.5102C
30、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 0.2106C solvents distillation 224 to 276 0.2111C solvents distillation 170 to 250 0.2D850 1626.3.1.2 As an alternative, the condenser tube may c
31、onsist 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. Clearance between the co
32、ndenser 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 tube is set at
33、 an angle of 75with the vertical. To minimize the turbulence in the receiverduring the run, provisions shall be made to enable the flow ofthe distillate to run down the side of the receiving cylinder.This can be accomplished by using a drip-deflector, which isattached to the outlet of the tube.6.3.2
34、 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, of uniform diameter, with a pressed or moldedbase and
35、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 longer line. It shall be numbered from the bottom up a
36、tintervals 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-plies with Section 9, Graduate B Fig. 4, of Specificatio
37、n 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 Automatic Distillation Level FollowerFor auto-matic ap
38、paratus, 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 typical calibration procedure involves verifyingthe
39、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 placement of a flask supportboard (see 6.5.2) above the e
40、lectric 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 and toluene,the opening shall be 25 mm in diameter; fo
41、r 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 heat to the flaskonly comes from the central opening
42、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 supportboard is approximately 50 mm higher than the top
43、 of theburner.6.6 Heater:FIG. 2 Examples of Centering Device Designs for Straight-Bore Neck FlasksD850 1636.6.1 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 us
44、ed, as described in 7.1 and 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 electricheaters than with bunsen burners as heat sources. This problemis discuss
45、ed in the section on Preparation of Apparatus in TestMethod D1078.)7. Hazards7.1 Consult current OSHA regulations and suppliers SafetyData Sheets, and local regulations, for all materials used in thistest method.8. Sampling8.1 Sampling should follow safe rules in order to adhere toall safety precaut
46、ions 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. Any separated water may ordinarily be elimi-nated by care in pouri
47、ng 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 filters rapidly, avoid drafts, cover the funnel with awatch glass
48、, 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 thatcan be significant with respect to this test. When it can beshown
49、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 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 dimensions, with the side tubeexte
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