1、Designation: D850 181Standard 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 o
2、f 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.1NOTEEditorial corrections were made in 12
3、.1 and 12.2 in September 2018.1. Scope*1.1 This test method covers the distillation of industrialaromatic hydrocarbons and related materials of relativelynarrow boiling ranges from 30 to 250C.1.2 The following applies to all specified limits in this testmethod: for the purposes of determining confor
4、mance 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 E29.1.3 WarningMercury has been designated by EPA andmany state agencies a
5、s 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 applicable productSafety Data Sheet (SDS) for detail
6、s 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.1.4 The values stated in SI units are to be regarded asstandard. No other units of measure
7、ment are included in thisstandard.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, health, and environmental practices and deter-mine the applicability of r
8、egulatory limitations prior to use.For specific hazard statements, see 6.5.2, 6.6.1 and Section 7.1.6 This international standard was developed in accor-dance with internationally recognized principles on standard-ization established in the Decision on Principles for theDevelopment of International
9、Standards, Guides and Recom-mendations issued by the World Trade Organization TechnicalBarriers to Trade (TBT) Committee.2. Referenced Documents2.1 ASTM Standards:2D1078 Test Method for Distillation Range of Volatile Or-ganic LiquidsD3437 Practice for Sampling and Handling Liquid CyclicProductsD4790
10、 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 Conforman
11、ce 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 1910.1000
12、 and1910.120033. Terminology3.1 Definitions:3.1.1 See Terminology D4790 for definitions of terms usedin this test method.1This test method is under the jurisdiction of ASTM Committee D16 onAromatic, Industrial, Specialty and Related Chemicals and is the direct responsi-bility of Subcommittee D16.04
13、on Instrumental Analysis.Current edition approved June 1, 2018. Published June 2018. Originallyapproved in 1945. Last previous edition approved in 2016 as D850 16. DOI:10.1520/D0850-18E01.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at service
14、astm.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:/www.access.gpo.gov.*A Summary
15、 of Changes section appears at the end of this standardCopyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United StatesThis international standard was developed in accordance with internationally recognized principles on standardization established in
16、 the Decision on Principles for theDevelopment of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.14. Summary of Test Method4.1 The distillation of a 100-mL sample of industrial aro-matic hydrocarbons and related
17、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 noted.5. Significance
18、 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 and can also indicate
19、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:Diameter of bulb, outside, mm 76 1.5Diam
20、eter of neck, inside, mm 21 1Height 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
21、 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 material being tested. Ifno thermometer is specified in the material spe
22、cification, 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 aromatic hydrocarbons, andwhich meet the requirements of S
23、pecification 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 lagand accuracy as the equivalent mercury glass thermometer.C
24、onfirmation 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 is todistill pure toluene and compare the temperature indicated by
25、the 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 pointand distillation range.4It is recommended that such a materi
26、albe 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 DeviceThe temperature sensor shall be mounted througha snug-
27、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 areshown in Fig. 2.6.2.2.2 The electronic circuitry or algorithms
28、, 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 dampening software.6.2.2.3 Alternatively, the sensor can also
29、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 temperature is changing rapidly duringthe distillation, the tempera
30、ture lag of a thermometer can be as much as3s.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 0.240
31、C 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 solvents distillation 173 to 227 0.2105C solvents distillation 198 to 252 0.2106C solvents distill
32、ation 224 to 276 0.2111C solvents distillation 170 to 250 0.2D850 18126.3 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 SpecificationE133.6.3.1.2 As an altern
33、ative, the condenser 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
34、water. Clearance 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 th
35、at the condenser tube is set at 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
36、to the outlet of the tube.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, of uniform diameter, wi
37、th 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 longer line. It shall b
38、e 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-plies with Section 9, Gra
39、duate 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 Automatic Distillation
40、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 typical calibration p
41、rocedure 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 placement of a flask suppo
42、rtboard (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 and toluene,the opening
43、 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 heat to the flaskonly
44、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.)FIG. 2 Examples of Centering Device Designs for Straight-Bore Neck Fl
45、asksD850 18136.5.3 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, fully adjustable and capable of giving sufficientheat to distill the product at the required
46、 rate. When a bunsenburner is used, 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
47、 sources. This problemis discussed 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 orde
48、r 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. Any separated water may ordinarily
49、 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 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 a
