ASTM D850-21

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it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
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Designation: D850 − 18 D850 − 21
Standard Test Method for
Distillation of Industrial Aromatic Hydrocarbons and Related
Materials
This standard is issued under the fixed designation D850; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript 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.
ε NOTE—Editorial corrections were made in 12.1 and 12.2 in September 2018.
1. Scope*Scope
1.1 This test method covers the distillation of industrial aromatic hydrocarbons and related materials of relatively narrow boiling
ranges from 30 to 250°C. Warning—This test method is not applicable for styrene which will exothermically polymerize during
the distillation process.
1.2 The following applies to all specified limits in this test method: for the purposes of determining conformance to this test
method, an observed or calculated value shall be rounded off “to the nearest unit” in the last right-hand digit used in expressing
the specification limit, in accordance with the rounding-off method of Practice E29.
1.3 Warning—Mercury has been designated by EPA and many state agencies as a hazardous material that can cause central
nervous system, kidney and liver damage. Mercury, or its vapor, may be hazardous to health and corrosive to materials. Caution
should be taken when handling mercury and mercury-containing products. See the applicable product Safety Data Sheet (SDS) for
details and EPA’s 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 by state law.Warning—Mercury has been
designated by EPA and many state agencies as a hazardous material that can cause central nervous system, kidney and liver
damage. Mercury, or its vapor, may be hazardous to health and corrosive to materials. Caution should be taken when handling
mercury and mercury-containing products. See the applicable product Safety Data Sheet (SDS) for details and EPA’s 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 by state law.
1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.5 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility
of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of
regulatory 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 accordance with internationally recognized principles on standardization
established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued
by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
This test method is under the jurisdiction of ASTM Committee D16 on Aromatic, Industrial, Specialty and Related Chemicals and is the direct responsibility of
Subcommittee D16.04 on Instrumental Analysis.
Current edition approved June 1, 2018Feb. 1, 2021. Published June 2018February 2021. Originally approved in 1945. Last previous edition approved in 20162018 as
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D850 – 16.D850 – 18 . DOI: 10.1520/D0850-18E01.10.1520/D0850-21.
*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
D850 − 21
2. Referenced Documents
2.1 ASTM Standards:
D1078 Test Method for Distillation Range of Volatile Organic Liquids
D3437 Practice for Sampling and Handling Liquid Cyclic Products
D4790 Terminology of Aromatic Hydrocarbons and Related Chemicals
D6809 Guide for Quality Control and Quality Assurance Procedures for Aromatic Hydrocarbons and Related Materials
E1 Specification for ASTM Liquid-in-Glass Thermometers
E29 Practice for Using Significant Digits in Test Data to Determine Conformance with Specifications
E133 Specification for Distillation Equipment
E220 Test Method for Calibration of Thermocouples By Comparison Techniques
E691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
2.2 Other Document:
OSHA Regulations, 29 CFR paragraphs 1910.1000 and 1910.1200
3. Terminology
3.1 Definitions:
3.1.1 See Terminology D4790 for definitions of terms used in this test method.
4. Summary of Test Method
4.1 The distillation of a 100-mL sample of industrial aromatic hydrocarbons and related materials is carried out via a carefully
controlled distillation wherein temperature readings are noted for the first drop of distillate and when 5, 10, and each additional
10 up to 90, and 95 % of the sample has distilled over. The temperature corresponding to the dry point is also noted.
5. Significance and Use
5.1 This test method is suitable for setting specifications, for use as an internal quality control tool, and for use in development
or research work on industrial aromatic hydrocarbons and related materials.
5.2 This test method gives a broad indication of general purity and can also indicate presence of excessive moisture. It will not
differentiate between products of similar boiling range.
6. Apparatus
6.1 Distillation Flask—A standard 200-mL side-tube, heat-resistant glass distillation flask as shown in Fig. 1, conforming to the
following dimensions:
Diameter of bulb, outside, mm 76 ± 1.5
Diameter of neck, inside, mm 21 ± 1
Height of flask, outside, mm 179 ± 3
Vertical distance from bottom of bulb outside to 120 ± 3
bottom of vapor-tube opening in neck, mm
Length of side tube, mm 100 ± 3
Diameter of side tube, outside, mm 7 ± 0.5
Angle of side tube with vertical axis of bulb and 75 ± 3
neck, °
The flask does not comply with Flask C of Specification E133.
6.2 Temperature Measurement Devices:
6.2.1 Manual Distillation Thermometer—The ASTM Solvents Distillation Thermometer used in the test shall be as prescribed in
the specifications for the material being tested. If no thermometer is specified in the material specification, select one from Table
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
Available 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.
D850 − 21
FIG. 1 Distillation Flask
1 with the smallest graduations that will cover the entire distillation range of the material being tested. Table 1 lists several ASTM
solvents distillation thermometers which are suitable for testing industrial aromatic hydrocarbons, and which meet the requirements
of Specification E1.
6.2.2 Automatic Distillation Temperature Sensor—Temperature measurement systems using thermocouples or resistance
thermometers, otherwise referred to as the “temperature measuring devices,” must exhibit the same temperature lag and accuracy
as the equivalent mercury glass thermometer. Confirmation of the calibration of these temperature sensors is to be done at regular
intervals. This may be accomplished as prescribed in Test Method E220, or some similar means using a precision resistance decade
box. Another technique is to distill pure toluene and compare the temperature indicated by the thermocouple or resistance
thermometer with that shown by the thermometer. When installing a new automatic distillation analyzer, a toluene sample with
a known distillation range of approximately 1.0°C must be used to verify the dry point and distillation range. It is recommended
that such a material be used when replacing a temperature measuring device. Alternatively a material of known distillation range
and dry point may be used when replacing a temperature measuring device.
6.2.2.1 Automatic Distillation Temperature Sensor Centering Device—The temperature sensor shall be mounted through a
snug-fitting device designed to mechanically center the sensor in the neck of the flask. The use of a cork or silicone stopper with
a hole drilled through the center is not acceptable for this purpose. Examples of acceptable centering devices are shown in Fig.
2.
6.2.2.2 The electronic circuitry or algorithms, or both, used shall include the capability to simulate the temperature lag of a
mercury-in-glass thermometer. For that reason the known toluene sample with a distillation range of approximately 1.0°C must
be used to verify the algorithm and dampening software.
TABLE 1 ASTM Thermometers for Distillation Test of Industrial
Aromatic Hydrocarbons
ASTM
Subdivision,
Thermometer Name Range, °C
°C
No.
39C solvents distillation 48 to 102 0.2
40C solvents distillation 72 to 126 0.2
41C solvents distillation 98 to 152 0.2
42C solvents distillation 95 to 255 0.5
102C solvents distillation 123 to 177 0.2
103C solvents distillation 148 to 202 0.2
104C solvents distillation 173 to 227 0.2
105C solvents distillation 198 to 252 0.2
106C solvents distillation 224 to 276 0.2
111C solvents distillation 170 to 250 0.2
Such a material is available from Spectrum Quality Standards.
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FIG. 2 Examples of Centering Device Designs for Straight-Bore Neck Flasks
6.2.2.3 Alternatively, the sensor can also be placed in a casing with the tip of the sensor covered, so that the assembly, because
of its adjusted thermal mass and conductivity, has a temperature lag similar to that of a mercury-in-glass thermometer.
NOTE 1—In a region where the temperature is changing rapidly during the distillation, the temperature lag of a thermometer can be as much as
3 s.
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 bath shall be as specified in Section 5, and Fig. 1 of Specification E133.
6.3.1.2 As an alternative, the condenser tube may consist of a straight glass tube 600 to 610 mm in length and 12 mm in inside
diameter, of standard wall thickness (about 1.25 mm) with the exit end cut off square and ground flat. It shall be set in a cooling
trough so that at least 380 mm of the tube is in contact with the water. Clearance between the condenser tube and any parallel side
of the trough shall be not less than 19 mm. The water in the cooling trough shall be maintained at 10 to 20°C. This may be done
by adding ice to the water or by circulating chilled water through the trough. The trough shall be so mounted that the condenser
tube is set at an angle of 75° with the vertical. To minimize the turbulence in the receiver during the run, provisions shall be made
to enable the flow of the distillate to run down the side of the receiving cylinder. This can be accomplished by using a
drip-deflector, which is attached to the outlet of the tube.
6.3.2 Automatic Distillation and Cooling Bath—The automatic distillation and cooling bath shall be as specified in Section 5, Fig.
2 of Specification E133.
6.4 Distillation Receiver:
6.4.1 Manual Distillation Receiver—A graduate of the cylindrical type, of uniform diameter, with a pressed or molded base and
a lipped top. The cylinder shall be marked to contain 100 mL, and the 0 to 100 mL receiver portion shall be not less than 178 nor
more than 203 mm in length. It shall be graduated in single millilitres and each fifth mark shall be distinguished by a longer line.
It shall be numbered from the bottom up at intervals of 10 mL. The overall height of the receiver shall not be less than 248 nor
more than 260 mm. The graduations shall not be in error by more than 1 mL at any point on the scale. The bottom 1-mL graduation
may be omitted. The receiver complies with Section 9, Graduate B Fig. 4, of Specification E133.
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6.4.2 Automatic Distillation Receiver—A receiver to be used with measurements in accordance with the instrument manufacturer
and conform to the physical specifications described in this section, with the exception of the graduations.
6.4.2.1 Automatic Distillation Level Follower—For automatic apparatus, the level follower or recording mechanism of the
apparatus will have a resolution of 0.1 mL with an accuracy of 61 mL. 61 mL. The calibration of the assembly should be
confirmed according to the manufacturer’s instructions at regular intervals. The typical calibration procedure involves verifying
the output with the receiver containing 5 and 100 mL of material respectively.
6.5 Flask Support Assembly:
6.5.1 For Units Using Electric Heaters—The assembly consists of an adjustable system onto which the electric heater is mounted
with provision for placement of a flask support board (see 6.5.2) above the electric heater. The whole assembly is adjustable from
the outside of the shield.
6.5.2 Flask Support Board—The flask support board shall be constructed of ceramic or other heat-resistant material with a
centrally located opening. For tests of benzene and toluene, the opening shall be 25 mm in diameter; for tests of materials boiling
above toluene but mostly below 145°C, the opening shall be 38 mm in diameter, and for higher boiling materials, it shall be 50
mm in diameter. The flask support board shall be of sufficient dimension to ensure that thermal heat to the flask only comes from
the central opening and that extraneous heat to the flask other than through the central opening is minimized. (Warning—
Warning—Heat resistant-containing materials shall not be used in the construction of the flask support board.)
6.5.3 For Units Using Bunsen Burner—The flask support board is approximately 50 mm higher than the top of the burner.
6.6 Heater:
6.6.1 Manual Distillation Heater—An electric heater or a bunsen burner, fully adjustable and capable of giving sufficient heat to
distill the product at the required rate. When a bunsen burner is used, as described in 7.1 and Fig. 1 of Specification E133, the
burner shall be adjusted so as to produce an entirely blue flame. (Warning—WarningSuperheating—Superheating of the flask can
cause erroneous results and is more likely to occur with electric heaters than with bunsen burners as heat sources. This problem
is discussed in the section on Preparation of Apparatus in Test Method D1078.)
7. Hazards
7.1 Consult current OSHA regulations and supplier’s Safety Data Sheets, and local regulations, for all materials used in this test
method.
8. Sampling
8.1 Sampling should follow safe rules in order t
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