Depentanization of Gasoline and Naphthas: Standard Test Method For
Depentanization of Gasoline and Naphthas: Standard Test Method For
for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
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The sole source of supply of the apparatus known to the committee at this time
1
This test method is under the jurisdiction of ASTM Committee D02 on is Thermometer No. ME510-1 available from Metro Scientific Inc., 11 Willow Park
Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of Center, East Farmingdale, NY 11735.
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Subcommittee D02.04.0C on Liquid Chromatography. If you are aware of alternative suppliers, please provide this information to
Current edition approved Dec. 1, 2017. Published December 2017. Originally ASTM International Headquarters. Your comments will receive careful consider-
approved in 1962. Last previous edition approved in 2012 as D2001 – 07 (2012). ation at a meeting of the responsible technical committee,1 which you may attend.
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DOI: 10.1520/D2001-07R17. The sole source of supply of the apparatus known to the committee at this time
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or is Reliance Glass Works Inc., Gateway Rd., PO Box 825, Bensenville, IL 60106.
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contact ASTM Customer Service at [email protected]. For Annual Book of ASTM The sole source of supply of the apparatus known to the committee at this time
Standards volume information, refer to the standard’s Document Summary page on is Cannon protruded metal packing available from Scientific Development Co., Box
the ASTM website. 795, State College, PA.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
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D2001 − 07 (2017)
5.3 Distillation Flask, round-bottom, 100 mL, with NOTE 1—The calibration of the thermometer at the cut temperature
⁄ standard-taper female joint.
24 40 should be checked by refluxing a pure compound. Such a calibration can
show a need for a correction.
5.4 Distillation Flask Heating Mantle, Glas-Col, spherical,
6.4 Immerse the receiver in a Dewar flask containing a
for 100 mL flask.
mixture of solid carbon dioxide (Warning—Extremely cold.)
5.5 Variable Transformer, for regulating power to heating in a suitable liquid. 1,1,2 Trichloro Ethene is recommended.
mantle. (Warning—Health hazard.)
5.6 Water Cooling Bath—If a supply of chilled water for the 6.5 Circulate water, chilled to a temperature between 4 °C
reflux condenser is not available, a satisfactory means for and 10 °C (40 °F and 50 °F), through the reflux condenser.
supplying chilled water can be provided by circulating tap
water through coiled copper tubing immersed in an ice-water 7. Procedure
bath.
7.1 Lubricate the joint at the bottom of the column with a
6. Preparation of Apparatus hydrocarbon-insoluble grease, such as silicone, starch-
glycerol, or metallic soap. Place the heating mantle around the
6.1 Fill the fractionating column with packing as follows:
flask. With a 50 mL graduated cylinder, measure 50 mL of the
Place about 25 mm (1 in.) of the Heli-Pak column packing, size
sample. Determine its temperature, and transfer it to the flask.
C or the Cannon packing on the indentations at the bottom of
Connect the flask immediately to the column.
the column. This packing assures ample free space to prevent
flooding at the bottom of the column. Fill the column to within 7.2 Connect the mantle, through the variable transformer, to
25 mm (1 in.) of the top of the jacket with Heli-Pak column the power supply.
packing, size B. (The performance of this packing is not 7.3 Apply heat to the contents of the flask at a uniform rate.
sensitive to the exact manner of pouring into the column.)
NOTE 2—With the apparatus prepared as described in Section 6, a
6.2 Assemble and connect the column, head, light-ends trap, setting of 30 on the transformer usually provides a satisfactory initial
and the receiver. Mount the assembly on a suitable support. heating rate; voltage is increased as required.
6.3 Insert the thermometer through the side-arm at the top of 7.4 As soon as drops of liquid reflux form at the column
the column. head, adjust the position of the condenser so that one drip-tip
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D2001 − 07 (2017)
feeds to the take-off line, and the other back to the (Warning— Volume of bottoms, percent 5 ~ A/B ! 3 100 (1)
Extremely flammable liquid.) column. The reflux condenser
where:
remains in this position throughout the distillation to provide
about a 1 + 1 reflux ratio. A = volume of bottoms, mL and
B = volume of the charge, mL.
NOTE 3—Low-boiling light ends will condense on the light-ends trap
and collect in the receiver before drops of liquid reflux form at the column 9. Precision and Bias
head.
9.1 The following criteria should be used for judging the
7.5 The distillation rate should not exceed 30 drops ⁄30 s to acceptability of results (95 % confidence) (Note 4):
40 drops ⁄30 s from each tip of the reflux condenser. 9.1.1 Repeatability—The difference between two test
7.6 Continue the distillation until the thermometer indicates results, obtained by the same operator with the same apparatus
a temperature of 49 °C (120 °F). When this temperature is under constant operating conditions on identical test material,
reached, shut off the heat and drop the lower portion of the would in the long run, in the normal and correct operation of
heating mantle. Turn the reflux condenser so that drops from the test method, exceed 2 % by volume only in one case in
both drippers are returned to the column. Direct a stream of air twenty.
on the top surface of the flask. Perform the above steps in rapid 9.1.2 Reproducibility—The difference between two single
succession. and independent results obtained by different operators work-
ing in different laboratories on identical test material would, in
7.7 Allow the column to drain and the contents of the flask
the long run, in the normal and correct operation of the test
to cool for 30 min.
method, exceed 4 % by volume only in one case in twenty.
7.8 Remove the flask from the column, and carefully
9.2 Bias—The quantities determined are defined by the
transfer the contents to the same graduated cylinder which was
conditions used in this empirical test method, and a statement
used to measure the charge. Measure the volume of the bottoms
of bias is therefore not appropriate.
fraction and determine its temperature.
NOTE 4—Precision data are based on results obtained by five laborato-
8. Calculation ries testing four samples in duplicate. The samples contained C5-and-
lighter fractions covering a range of 5 % by volume to 25 % by volume.
8.1 If the temperatures of the distillation charge and bottoms
differ by more than 11 °C (20 °F), correct the measured 10. Keywords
volumes to volumes at 15 °C (60 °F) by Guide D1250. 10.1 depentanization; fractionations; hydrocarbon types;
8.2 Calculate the volume of bottoms in percent as follows: pentanes
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