An American National Standard

Designation: D 1160 – 06

Standard Test Method for

Distillation of Petroleum Products at Reduced Pressure1
--`,,`,,``,`,`,```,`,`,,``,`,``-`-`,,`,,`,`,,`---

This standard is issued under the fixed designation D 1160; 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 (e) 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* 3. Terminology
1.1 This test method covers the determination, at reduced 3.1 Definitions of Terms Specific to This Standard:
pressures, of the range of boiling points for petroleum products 3.1.1 atmospheric equivalent temperature (AET)—the tem-
that can be partially or completely vaporized at a maximum perature converted from the measured vapor temperature using
liquid temperature of 400°C. Both a manual method and an Eq A7.1. The AET is the expected distillate temperature if the
automatic method are specified. distillation was performed at atmospheric pressure and there
1.2 In cases of dispute, the referee test method is the manual was no thermal decomposition.
test method at a mutually agreed upon pressure. 3.1.2 end point (EP) or final boiling point (FBP)—the
1.3 The values stated in SI units are to be regarded as the maximum vapor temperature reached during the test.
standard. The values in parentheses are for information only. 3.1.3 initial boiling point (IBP)—the vapor temperature that
1.4 This standard does not purport to address all of the is measured at the instant the first drop of condensate falls from
safety concerns, if any, associated with its use. It is the the lower end of the condenser section drip tip.
responsibility of the user of this standard to establish appro- 3.1.3.1 Discussion—When a chain is attached to the drip tip
priate safety and health practices and determine the applica- the first drop will form and run down the chain. In automatic
bility of regulatory limitations prior to use. For specific hazard apparatus, the first drop detection device shall be located as
statements, see 6.1.4, 6.1.8.1, 10.11, and A3.2.1. near to the lower end of the drip tip as practical.
3.1.4 spillover point—the highest point of the lower internal
2. Referenced Documents 2 junction of the distillation column and the condensing section
2.1 ASTM Standards: of the vacuum-jacketed column assembly.
D 613 Test Method for Cetane Number of Diesel Fuel Oil
D 1193 Specification for Reagent Water 4. Summary of Test Method
D 1250 Guide for Use of the Petroleum Measurement 4.1 The sample is distilled at an accurately controlled
Tables pressure between 0.13 and 6.7 kPa (1 and 50 mm Hg) under
D 1298 Test Method for Density, Relative Density (Specific conditions that are designed to provide approximately one
Gravity), or API Gravity of Crude Petroleum and Liquid theoretical plate fractionation. Data are obtained from which
Petroleum Products by Hydrometer Method the initial boiling point, the final boiling point, and a distillation
D 4052 Test Method for Density and Relative Density of curve relating volume percent distilled and atmospheric
Liquids by Digital Density Meter equivalent boiling point temperature can be prepared.
D 4057 Practice for Manual Sampling of Petroleum and
Petroleum Products 5. Significance and Use
D 4177 Practice for Automatic Sampling of Petroleum and 5.1 This test method is used for the determination of the
Petroleum Products distillation characteristics of petroleum products and fractions
that may decompose if distilled at atmospheric pressure. This
boiling range, obtained at conditions designed to obtain ap-
proximately one theoretical plate fractionation, can be used in
1
This test method is under the jurisdiction of ASTM Committee D02 on engineering calculations to design distillation equipment, to
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee
D02.08 on Volatility. prepare appropriate blends for industrial purposes, to deter-
Current edition approved July 1, 2006. Published July 2006. Originally approved mine compliance with regulatory rules, to determine the
in 1951. Last previous edition approved in 2003 as D 1160–03.
2
suitability of the product as feed to a refining process, or for a
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
host of other purposes.
Standards volume information, refer to the standard’s Document Summary page on 5.2 The boiling range is directly related to viscosity, vapor
the ASTM website. pressure, heating value, average molecular weight, and many

*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.

Copyright ASTM International 1

Provided by IHS under license with ASTM Licensee=Esso Malaysia Berhard/5986012001, User=Petron Corporation, Refining Div
No reproduction or networking permitted without license from IHS Not for Resale, 08/30/2012 02:23:12 MDT
 D 1160 – 06
other chemical, physical, and mechanical properties. Any of the inner diameter of the connection to the distillation column
these properties can be the determining factor in the suitability not being less than the inner diameter of the distillation
of the product in its intended application. column. The use of the thermowell can be replaced by an
5.3 Petroleum product specifications often include distilla- encased temperature probe and the second side neck is present
tion limits based on data by this test method. on commercially available flasks used in this test method.
5.4 Many engineering design correlations have been devel- 6.1.2 Vacuum-Jacketed Column Assembly, of borosilicate
oped on data by this test method. These correlative methods are glass, consisting of a distilling head and an associated con-
used extensively in current engineering practice. denser section as illustrated in the lettered drawing, Fig. 4 and
6. Apparatus Table 1. The head shall be enclosed in a completely silvered
glass vacuum jacket with a permanent vacuum of less than
6.1 The vacuum distillation apparatus, shown schematically
10−5 Pa (10−7 mm Hg) (Note 1). The attached condenser
in Fig. 1, consists in part of the components described below
plus others that appear in Fig. 1 but are not specified, either as section shall be enclosed in water jackets as illustrated and
to design or performance. Some of these parts are not essential have an adapter at the top for connection to the vacuum source.
for obtaining satisfactory results from the tests but are desirable A light drip-chain shall hang from the drip tip of the condenser
components of the assembly for the purpose of promoting the to a point 5 mm below the 10-mL mark of the receiver as
efficient use of the apparatus and ease of its operation. Both shown in Fig. 5. Alternatively, instead of the metal drip-chain,
manual and automatic versions of the apparatus must conform a metal trough may be used to channel the distillate to the wall
to the following requirements. Additional requirements for the of the receiver. This trough may either be attached to the
automatic apparatus can be found in Annex A9. condenser drip tip as shown in Fig. 5 or it may also be located
6.1.1 Distillation Flask, of 500-mL capacity, made of boro- in the neck of the receiver.
silicate glass or of quartz conforming to the dimensions given NOTE 1—There is no simple method to determine the vacuum in the
in Fig. 2 or Fig. 3, and having a heating mantle with insulating jacket once it is completely sealed. A Tesla coil can be used, but the spark
top. These dimensions can vary slightly by manufacturer, and can actually create a pinhole in a weak spot in the jacket. Even the
are not considered critical dimensions, with the exception of slightest pinhole or crack not readily detectable by sight alone will negate
the position of the end of the temperature sensing probe, and the vacuum in the jacket.

--`,,`,,``,`,`,```,`,`,,``,`,``-`-`,,`,,`,`,,`---

NOTE—A cold trap can be inserted before the pressure transducer in Option No. 2, if desired, or if the design of the transducer, such as a mercury
McCleod gage, would require vapor protection.
FIG. 1 Assembly of Vacuum Distillation Apparatus

Copyright ASTM International 2

Provided by IHS under license with ASTM Licensee=Esso Malaysia Berhard/5986012001, User=Petron Corporation, Refining Div
No reproduction or networking permitted without license from IHS Not for Resale, 08/30/2012 02:23:12 MDT
 D 1160 – 06
--`,,`,,``,`,`,```,`,`,,``,`,``-`-`,,`,,`,`,,`---

FIG. 2 Distillation Flask and Heating Mantle

FIG. 3 Distillation Flask 500ML

6.1.3 Vapor Temperature Measuring Device and associated the measurement of the vapor temperature. The system must
signal conditioning and processing instruments (Annex A1) for produce readings with an accuracy of 60.5°C over the range 0

Copyright ASTM International 3

Provided by IHS under license with ASTM Licensee=Esso Malaysia Berhard/5986012001, User=Petron Corporation, Refining Div
No reproduction or networking permitted without license from IHS Not for Resale, 08/30/2012 02:23:12 MDT
 D 1160 – 06

--`,,`,,``,`,`,```,`,`,,``,`,``-`-`,,`,,`,`,,`---
FIG. 4 Vacuum-Jacketed Column

to 400°C and have a response time of less than 200 s as taper joint matched to the distillation column. In some distil-
described in Annex A2. The location of the vapor temperature lation apparatus configurations, the vacuum adapter at the top
sensor is extremely critical. As shown in Fig. 6, the vapor of the distillation column can be omitted. In these cases, the
temperature measuring device shall be centered in the upper position of the vapor temperature measuring device shall be
portion of the distillation column with the top of the sensing tip adjusted accordingly. The boiler temperature measuring device
3 6 1 mm below the spillover point (see 3.1). The vapor may be either a thermocouple or PRT and shall also be
temperature measuring device can consist of different configu- calibrated as above.
rations depending if it is a platinum resistance in glass or metal, 6.1.4 Receiver of borosilicate glass, conforming to the di-
or if it is a thermocouple in glass or metal. Figs. 7 and 8 show mensions shown in Fig. 9. If the receiver is part of an automatic
the proper positioning of these two types in relation to the unit and is mounted in a thermostatted chamber, the jacket is
spillover point. In glass platinum resistance devices the top of not required. (Warning—The glass parts of the apparatus are
the spiral winding is the top of the sensing tip, in thermo- subjected to severe thermal conditions and, to lessen the
couples it is the top of the thermocouple junction, in metal chances of failure during a test, only equipment shown to be
jacketed devices it is 1 6 1 mm above the bottom of the device. strain-free under polarized light should be used.)
An alignment procedure is described in Appendix X1. The 6.1.5 Vacuum Gage, capable of measuring absolute pres-
vapor temperature measuring device shall be mounted through sures with an accuracy of 0.01 kPa in the range below 1 kPa
a compression ring type seal mounted on the top of the glass absolute and with an accuracy of 1 % above this pressure. The
temperature sensor/vacuum adapter or fused into a ground McLeod gage can achieve this accuracy when properly used,

Copyright ASTM International 4

Provided by IHS under license with ASTM Licensee=Esso Malaysia Berhard/5986012001, User=Petron Corporation, Refining Div
No reproduction or networking permitted without license from IHS Not for Resale, 08/30/2012 02:23:12 MDT
 D 1160 – 06
TABLE 1 Vacuum-Jacketed Column Assembly Dimensions
NOTE 1—These dimensions are for guidance for verifying the appropriate construction of the assembly. The actual dimensions used by glassmakers
vary to some extent, and the dimensions they use to construct the assembly are not easily obtained after the assembly is fused together. Those dimensions
noted as critical shall be adhered to within the tolerance listed. The dimensions listed in this chart have been gathered from users of the various
manufactured manual and automatic apparatus who participated in the interlaboratory program to produce the precision for this test method.
NOTE 2—Important—Further study will progress to produce a set of dimensions which will be more restrictive in range of dimension, since it is
believed that the current wide variance in dimensions has resulted in precision for this test method to be significantly high. The target dimensions for
this assembly and other components of the apparatus are expected to be available within the next year, with implementation expected to occur after five
years of initial revised test method publication date.
Component Critical DimensionsA Notes
A no 265 6 10 ...
B yes 99 6 4 Spillover point
C yes 85 6 3 Internal measurement difficult, used by manufacturer for assembly. Dimension is where
center of angled inner tube intersects with the inner wall of the vertical column
D (OD) no 64.5 6 2 ...
E no 14/23 or 19/38 Tapered ground joint – femaleB
F no 35/25 Spherical ground joint – maleB
G no 35 6 10 This area to be covered by the insulating top of the heating mantle
H (ID) yes 24.7 6 1.2 Use of 28 mm OD tubing achieves this dimension
I no 2 − 12 Window allows observation of boil-up rate and column cleanliness, but also allows detri-
mental heat loss
J no 60 6 20 ...
K no 12 6 7 ...
L (OD) no 8 Minimum, cooling medium connections
M yes 230 6 13 This dimension determines condensed vapor run down time and affects temperature/
recovery results
N (OD) no 38 6 2 ...
O yes 140 6 20 This dimension affects vapor condensing efficiency which influences temperature/
recovery results
P (ID) yes 18.7 6 1.1 Use of 22 mm OD tubing achieves this dimension
Q yes 60 6 2° ...
R no not applicable Connection to vacuum system; any suitable means is allowed
S no not applicable Extension above condensing section; must maintain minimum or greater internal diam-
eter of condensing section
T (ID) yes 18.7 6 1.1 Use of 22 mm OD tubing achieves this dimension
U yes 140 6 5 This dimension affects vapor condensing efficiency which influences temperature/
recovery results
V no not applicable Extensions on the upper and lower portions of the condensing section vary by manufac-
turer and have no influence on the test
W no 12 6 7 ...
X yes 50 6 8 ...
Y yes 30 6 7 Distance to end of drip tip
A
All dimensions are in millimetres.
B
Ground glass joints from different sources may have one of a number of diameter to length ratios. For purposes of this test method, any are suitable, and in some
instances, the diameter itself is not critical. However, it is critical that the male and female parts of each joint are from the same series to avoid recession or protuberance.

rately). An electronic gage such as the Baratron is satisfactory

when calibrated from a McLeod gage but must be rechecked
periodically as described in Annex A3. A suitable pressure
calibration setup is illustrated in Fig. A3.1. Vacuum gages
based on hot wires, radiation, or conductivity detectors are not
recommended.
--`,,`,,``,`,`,```,`,`,,``,`,``-`-`,,`,,`,`,,`---

NOTE 2—Suitable instruments for measuring the pressure of the system

during the test are the tensimeter or an electronic pressure gage, provided
the output is traceable to a primary gage, such as the non-tilting McLeod
gage.
6.1.5.1 Connect the vacuum gage to the side tube of the
temperature sensor/vacuum adapter of the distillation column
(preferred location) or to the side tube of the sensor/vacuum
adapter of the condenser when assembling the apparatus.
Connections shall be as short in length as possible and have an
FIG. 5 Detail of Drip-Chain or Trough Attachment to Condenser inside diameter not less than 8 mm.
6.1.6 Pressure Regulating System, capable of maintaining
but a mercury manometer will permit this accuracy only down the pressure of the system constant within 0.01 kPa at pressures
to a pressure of about 1 kPa and then only when read with a of 1 kPa absolute and below and within 1 % of the absolute
good cathetometer (an instrument based on a telescope pressure at 1 kPa or higher. Suitable equipment for this purpose
mounted on a vernier scale to determine levels very accu- is described in Annex A4. Connect the pressure regulating

Copyright ASTM International 5

Provided by IHS under license with ASTM Licensee=Esso Malaysia Berhard/5986012001, User=Petron Corporation, Refining Div
No reproduction or networking permitted without license from IHS Not for Resale, 08/30/2012 02:23:12 MDT
 D 1160 – 06

NOTE—Dimensions are in millimetres.

FIG. 6 Location of Temperature Sensor
--`,,`,,``,`,`,```,`,`,,``,`,``-`-`,,`,,`,`,,`---

FIG. 7 Platinum Resistance Temperature Measuring Device

system to the tube at the top of the condenser when assembling 6.1.7 Vacuum Source, consisting of, for example, one or
the apparatus. Connections shall be as short in length as more vacuum pumps and several surge tanks, capable of
possible and have an inside diameter not less than 8 mm. maintaining the pressure constant within 1 % over the full

Copyright ASTM International 6

Provided by IHS under license with ASTM Licensee=Esso Malaysia Berhard/5986012001, User=Petron Corporation, Refining Div
No reproduction or networking permitted without license from IHS Not for Resale, 08/30/2012 02:23:12 MDT
 D 1160 – 06

FIG. 8 Thermocouple Temperature Measuring Device

range of operating pressures. A vacuum adapter is used to

connect the source to the top of the condenser (Fig. 1) with
tubing of 8 mm ID or larger and as short as practical. A single
stage pump of at least 850 L/min (30 cfm) capacity at 100 kPa
is suitable as a vacuum source, but a double stage pump of
similar or better capacity is recommended if distillations are to
be performed below 0.5 kPa. Surge tanks of at least 5 L
capacity are recommended to reduce pressure fluctuations.
6.1.8 Cold Traps:
--`,,`,,``,`,`,```,`,`,,``,`,``-`-`,,`,,`,`,,`---

6.1.8.1 Cold trap mounted between the top of the condenser

and the vacuum source to recover the light boiling components
in the distillate that are not condensed in the condenser section.
This trap shall be cooled with a coolant capable of maintaining
the temperature of the trap below − 40°C. Liquid nitrogen is
commonly used for this purpose. (Warning—If there is a large
air leak in the system and liquid nitrogen is used as the coolant,
it is possible to condense air (oxygen) in the trap. If hydrocar-
bons are also present in the trap, a fire or explosion can result
when the trap is warmed up in step 10.12.)
NOTE—Jacket is not required for automatic units when receiver is 6.1.8.2 Cold trap mounted between the temperature sensor/
placed in thermostatted chamber. If jacket is used, connections should not vacuum adapter and the vacuum gage to protect the gage from
interfere with reading of graduations. contamination by low boiling components in the distillate.
FIG. 9 Receiver
6.1.9 Low Pressure Air or Carbon Dioxide Source to cool
the flask and heater at the end of the distillation.

Copyright ASTM International 7

Provided by IHS under license with ASTM Licensee=Esso Malaysia Berhard/5986012001, User=Petron Corporation, Refining Div
No reproduction or networking permitted without license from IHS Not for Resale, 08/30/2012 02:23:12 MDT
 D 1160 – 06
6.1.10 Low Pressure Nitrogen Source to release the vacuum the sample size, viscosity, and other factors, to ensure unifor-
in the system. mity. If solids are still visible above 70°C, these particles are
6.1.11 Safety Screen or Safety Enclosure that adequately probably inorganic in nature and not part of the distillable
shields the operator from the distillation apparatus in the event portion of the sample. Remove most of these solids by filtering
of mishap. Reinforced glass, 6 mm thick clear plexiglass, or a or decanting the sample.
clear material of equivalent strength is recommended. 8.5.1 There are several substances, such as visbroken resi-
6.1.12 Coolant Circulating System, capable of supplying dues and high melting point waxes, that will not be completely
coolant to the receiver and condenser system, at a temperature fluid at 70°C. These solids and semi-solids should not be
controlled within 63°C in the range between 30 and 80°C. For removed since they are part of the hydrocarbon feed.
automatic units where the receiver is mounted in a thermostat-
ted chamber, the coolant circulating system has to be capable 9. Preparation, Calibration, and Quantification of
of supplying coolant to the condenser system only. Apparatus
9.1 Calibrate the temperature sensors and associated signal
7. Reagents and Materials conditioning and processing device as a unit in accordance
7.1 n-Tetradecane—Reagent grade conforming to the speci- with Annex A1.
fications of the Committee on Analytical Reagents of the 9.2 Check the operation of the pressure regulating system as
American Chemical Society.3 described in Annex A4.
7.2 ASTM Cetane Reference Fuel (n-Hexadecane), con- 9.3 Clean and dry the glass parts and relubricate the joints.
forming to the specification in Test Method D 613. Silicone high-vacuum grease can be used but no more than is
7.3 Silicone Grease—High vacuum silicone grease spe- necessary to give a uniform film on the ground glass surfaces.
cially manufactured for the use in high vacuum applications. An excess of grease can cause leaks and can contribute to
7.4 Silicone Oil, certified by the manufacturer to be appli- foaming at startup.
cable for prolonged use at temperatures above 350°C. 9.4 Assemble the empty apparatus and conduct a leak test as
7.5 Toluene—Technical grade. described in A3.3.2.
7.6 Cyclohexane—Technical grade. 9.5 Check the total apparatus using either of the two
reagents described in 7.1 and 7.2 and in accordance with Annex
8. Sample and Sampling Requirements A5.
8.1 Sampling shall be done in accordance with Practices
10. Procedure
D 4057 or D 4177. It is assumed that a 4- to 8-L sample,
representative of a shipment or of a plant operation, is received 10.1 Determine when the temperature sensor was last cali-
by the laboratory and that this sample is to be used for a series brated. Recalibrate according to Annex A1 if more time has
of tests and analyses. An aliquot portion slightly in excess of elapsed than that specified in Annex A1.
200 mL will be required for this test method. 10.2 Set the temperature of the condenser coolant to at least
8.2 The aliquot used for this test shall be moisture-free. If 30°C below the lowest vapor temperature to be observed in the
--`,,`,,``,`,`,```,`,`,,``,`,``-`-`,,`,,`,`,,`---

there is evidence of moisture (drops on the vessel wall, a liquid test.

layer on the bottom of the container, etc.) use the procedure NOTE 3—A suitable coolant temperature for distillation of many mate-
given in Annex A6, paragraph A6.1, to dehydrate a sufficient rials is 60°C.
quantity of sample to provide the 200-mL charge to the 10.3 From the density of the sample determine the weight,
distillation flask. to the nearest 0.1 g, equivalent to 200 mL of the sample at the
8.3 Determine the density of the oil sample at the tempera- temperature of the receiver. Weigh this quantity of oil into the
ture of the receiver by means of a hydrometer by Practice distillation flask.
D 1298, by means of a digital density meter by Test Method 10.4 Lubricate the spherical joints of the distillation appa-
D 4052, and by using either the mathematical subroutines or ratus with a suitable grease (Note 4). Make certain that the
tables of Guide D 1250, or a combination thereof. surfaces of the joints are clean before applying the grease, and
8.4 If the sample is not to be tested immediately upon use only the minimum quantity required. Connect the flask to
receipt, store at ambient temperature or below. If the sample is the lower spherical joint of the distilling head, place the heater
received in a plastic container, it shall be transferred to a under the flask, put the top mantle in place and connect the rest
container made out of glass or of metal prior to storage. of the apparatus using spring clamps to secure the joints.
8.5 The sample shall be completely liquid before charging.
If crystals are visible, the sample shall be heated to a NOTE 4—Silicone high-vacuum grease has been used for this purpose.
temperature that permits the crystals to dissolve. The sample An excess of this lubricant applied to the flask joint can cause the sample
to foam during distillation.
must then be stirred vigorously for 5 to 15 min, depending on
10.5 Place a few drops of silicone oil in the bottom of the
thermowell of the flask and insert the temperature sensor to the
3
Reagent Chemicals, American Chemical Society Specifications, American bottom. The sensor can be secured with a wad of glass wool at
Chemical Society, Washington, DC. For suggestions on the testing of reagents not the top of the thermowell.
listed by the American Chemical Society, see Analar Standards for Laboratory
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
10.6 Start the vacuum pump and observe the flask contents
and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville, for signs of foaming. If the sample foams, allow the pressure
MD. on the apparatus to increase slightly until the foaming subsides.

Copyright ASTM International 8

Provided by IHS under license with ASTM Licensee=Esso Malaysia Berhard/5986012001, User=Petron Corporation, Refining Div
No reproduction or networking permitted without license from IHS Not for Resale, 08/30/2012 02:23:12 MDT
 D 1160 – 06
Apply gentle heat to assist the removal of dissolved gas. For NOTE 8—A gentle stream of carbon dioxide is preferred to cool the
general directions for suppression of excessive foaming of the flask to prevent fire in the event the flask cracks during the test or during
sample, see A6.2. the cooling cycle.
10.7 Evacuate the apparatus until the pressure reaches the 10.12 Bring the temperature of the cold trap mounted before
level prescribed for the distillation (Note 5). Failure to reach the vacuum source back to ambient temperature. Recover,
the distillation pressure, or the presence of a steady increase in measure, and record the volume of the light products collected
pressure in the apparatus with the pump blocked off, is in the trap.
evidence of significant leakage into the system. Bring the 10.13 Remove the receiver, empty it, and place it back into
system to atmospheric condition using a nitrogen bleed and the instrument for the cleaning cycle, or use a separate, empty
relubricate all joints. If this does not result in a vacuum-tight receiver. Remove the flask and replace with a flask filled with
system, examine other parts of the system for leaks. a cleaning solvent (Note 9). Run a distillation at atmospheric
pressure to clean the unit. At the end of this cleaning run,
NOTE 5—The most commonly prescribed pressure is 1.3 kPa (10 mm
Hg). For heavy products with a substantial fraction boiling above 500°C, remove the flask and receiver and blow a gentle stream of air
an operating pressure of 0.13 kPa (1 mm Hg) or 0.26 kPa (2 mm Hg) is or nitrogen to dry the unit.
generally specified. NOTE 9—Toluene or cyclohexane can be used as cleaning solvent.
10.8 After the desired pressure level has been attained, turn
on the heater and apply heat as rapidly as possible to the flask, 11. Calculations and Report
without causing undue foaming of the sample. As soon as 11.1 Convert the recorded vapor temperature readings to
vapor or refluxing liquid appears at the neck of the flask, adjust Atmospheric Equivalent Temperatures (AET) using the equa-
the rate of heating so that the distillate is recovered at a uniform tions in Annex A7.
rate of 6 to 8 mL/min (Note 6). 11.2 Report the AET to the nearest degree Celsius corre-
sponding to the volumetric percentages of liquid recovered in
NOTE 6—It is extremely difficult to achieve the desired rate at the very
the receiver. Report also the identity of the sample, the density
beginning of the distillation, but this rate should be attainable after the first
10 % of the distillate has been recovered. (measured in 8.3), the total amount of liquid distillate recov-
ered in the receiver and in the cold trap before the vacuum
10.9 Record the vapor temperature, time, and the pressure at source, any unusual occurrence such as foaming or burping,
each of the following volume percentage fractions of the together with the measures that were taken to correct the
charge collected in the receiver: IBP, 5, 10, 20, 30, 40, 50, 60, problem.
70, 80, 90, 95, and at the end point. If the liquid temperature
reaches 400°C, or if the vapor reaches a maximum temperature 12. Precision and Bias 4
before the end point is observed, record the vapor temperature 12.1 Precision—The precision of this test method was
reading and the total volume recovered at the time the generated from data obtained in a 1983 cooperative interlabo-
distillation is discontinued. When a product is tested for ratory program with nine laboratories participating and eight
conformity with a given specification, record all requested samples being run. In this program, one laboratory used an
observations, whether or not they are listed above. automatic vacuum distillation analyzer and the results obtained
NOTE 7—The maximum vapor temperature will result either from with this equipment have been included in the data used to
complete distillation of the oil or from the onset of cracking. generate this precision statement. The precision of this test
method is as follows:
10.10 If a sudden increase in pressure is observed, coupled
12.1.1 Repeatability—The difference between two test re-
with the formation of white vapors and a drop in the vapor
sults, in degrees Celsius, obtained by the same operator with
temperature, the material being distilled is showing significant
the same apparatus under constant operating conditions on
cracking. Discontinue the distillation immediately and record
identical test materials would, in the long run, in the normal
the fact on the run sheet. If necessary, rerun the distillation with
and correct operation of this test method, exceed the values
a fresh sample at lower operating pressure.
indicated in Table 2 in only 1 case in 20.
10.11 Lower the flask heater 5 to 10 cm and cool the flask
12.1.2 Reproducibility—The difference between two single
and heater with a gentle stream of air or, preferably, with a
and independent results in degrees Celsius, obtained by differ-
stream of carbon dioxide (Note 8). Repressure the contents of
ent operators working in different laboratories on identical test
the still with dry nitrogen (Warning—Repressuring the con-
material would, in the long run, in the normal and correct
tents of the still with air while it contains hot oil vapors can
operation of this test method, exceed the values indicated in
result in fire or explosion.) if it is necessary to dismantle the
Table 2 in only 1 case in 20.
apparatus before it has cooled below 200°C. Carbon dioxide
12.1.3 In Table 2, the rate of change in degrees Celsius
can also be used for repressuring, provided liquid nitrogen
(AET) per percentage of liquid volume recovered is shown as
traps are not in use. (Warning—In addition to other precau-
C/V %. At any point between the 10 and the 90 % point this
tions, it is recommended to discontinue the distillation at a
value is assumed to be equal to the average value of C/V % of
maximum vapor temperature of 350°C. Operating the distilla-
the two data points that bracket the point in question. In no case
tion flask at temperatures above 350°C for prolonged periods at
pressures below 1 kPa may also result in thermal deformation
of the flask. In this case, discard the flask after use. Alterna- 4
Supporting data have been filed at ASTM International Headquarters and may
tively, use a quartz flask.) be obtained by requesting Research Report RR: D02–1206.

Copyright ASTM International

--`,,`,,``,`,`,```,`,`,,``,`,``-`-`,,`,,`,`,,`---
9
Provided by IHS under license with ASTM Licensee=Esso Malaysia Berhard/5986012001, User=Petron Corporation, Refining Div
No reproduction or networking permitted without license from IHS Not for Resale, 08/30/2012 02:23:12 MDT
 D 1160 – 06
TABLE 2 Precision
NOTE—The body of this table is in degrees Celsius atmospheric equivalent temperature.
Criteria Repeatability Reproducibility
Pressure
0.13 kPa (1 mm Hg) 1.3 kPa (10 mm Hg) 0.13 kPa (1 mm Hg) 1.3 kPa (10 mm Hg)
IBP 17 15 56 49
FBP 3.3 7.1 31 27
Volume
5–50 % 60–90 % 5–50 % 60–90 % 5–50 % 60–90 % 5–50 % 60–90 %
Recovered
C/V %
0.5 2.4 2.5 1.9 2.0 6.5 3.9 7.0 5.4
1.0 2.9 3.0 2.4 2.5 10 6.0 9.3 7.2
1.5 3.2 3.3 2.8 2.9 13 7.8 11 8.5
2.0 3.4 3.5 3.1 3.2 16 9.4 12 9.6
2.5 3.6 3.7 3.3 3.5 18 11 14 11
3.0 3.8 3.9 3.6 3.7 21 12 15 11
3.5 3.9 4.0 3.8 3.9 23 13 16 12
4.0 4.0 4.2 3.9 4.1 25 15 16 13
4.5 4.1 4.3 4.1 4.3 27 16 17 13
5.0 4.2 4.4 4.3 4.4 29 17 18 14
5.5 4.3 4.5 4.4 4.6 30 18 19 15
6.0 4.4 4.6 4.5 4.7 32 19 19 15
6.5 4.5 4.7 4.7 4.8 34 20 20 16
7.0 4.6 4.8 4.8 5.0 35 23 21 16
7.5 4.7 4.8 4.9 5.1 37 22 21 16
8.0 4.8 4.9 5.0 5.2 38 23 22 17
8.5 4.8 5.0 5.1 5.3 40 24 22 17
9.0 4.9 5.1 5.2 5.4 41 25 23 18
9.5 5.0 5.1 5.3 5.5 43 25 23 18
10.0 5.0 5.2 5.4 5.6 44 26 24 19
10.5 5.1 5.2 5.5 5.7 46 27 24 19
11.0 5.1 5.3 5.6 5.8 47 28 25 19
11.5 5.2 5.4 5.7 5.9 48 29 25 20
12.0 5.2 5.4 5.8 6.0 50 30 26 20
12.5 5.3 5.5 5.9 6.1 51 30 26 20
--`,,`,,``,`,`,```,`,`,,``,`,``-`-`,,`,,`,`,,`---

13.0 5.3 5.5 6.0 6.2 52 31 27 21

13.5 5.4 5.6 6.0 5.3 54 32 27 21
14.0 5.4 5.6 6.1 6.3 55 33 27 21
14.5 5.5 5.7 6.2 6.4 56 33 28 22
15.0 5.5 5.7 6.3 6.5 57 34 28 22

shall the span of these two points be more than 20 % recovered. where:
An exception is the 5 % point where the span shall be not more R = reproducibility, °C (AET),
than 10 %. See Annex A8 for an example. a8, b8, and M8 = constants from 12.5.2, and
12.2 The precision data in Table 2 have been computed from S = rate of temperature change (°C, AET) per
the following equations, which can be used to calculate volume percent recovered.
precision data for C/V % values not listed. 12.2.3 See Annex A8 for an example.
12.2.1 Repeatability (r) can be calculated using the follow- 12.3 To calculate precision data for pressures between 0.13
ing equation: and 1.3 kPa (1 and 10 mm Hg), use constants calculated by
linear interpolation from data given in 12.5.1 and 12.5.2.
r 5 M[e exp$a 1 b ln ~1.8 S!%#/1.8 (1)
12.4 Bias—Since there is no accepted reference material
suitable for determining the bias for the procedure in this test
where: method, no statement is being made.
r = repeatability, °C (AET), 12.5 Constants for Calculating: See Table 2.
e = base of natural logarithmic function, ap- 12.5.1 Constants for calculating repeatability (r):
proximately 2.718281828, Volume Recovered
a, b, and M = constants from 12.5.1, and IBP 5–50 % 60–95 % FBP
S = rate of temperature change (°C, AET) per At 0.13 kPa (1 mm a 2.372 0.439 0.439 0.718
Hg)
volume percent recovered. b 0 0.241 0.241 0
12.2.2 Reproducibility (R) can be calculated using the M 2.9 2.9 3.0 2.9
following equation: At 1.3 kPa (10 mm a 2.246 0.240 0.240 1.521
Hg)
R 5 M8[e exp$a8 1 b8 ln ~1.8 S!%#/1.8 (2) b 0 0.350 0.350 0
M 2.8 2.8 2.9 2.8

Copyright ASTM International 10

Provided by IHS under license with ASTM Licensee=Esso Malaysia Berhard/5986012001, User=Petron Corporation, Refining Div
No reproduction or networking permitted without license from IHS Not for Resale, 08/30/2012 02:23:12 MDT
 D 1160 – 06
12.5.2 Constants for calculating reproducibility (R): 13. Keywords
Volume Recovered
IBP 5–50 % 60–95 % FBP
13.1 atmospheric equivalent temperature (AET); boiling
At 0.13 kPa (1 mm a8 3.512 1.338 0.815 2.931 range; distillation; vacuum distillation
Hg)
b8 0 0.639 0.639 0
M8 3.0 3.3 3.3 3.0
At 1.3 kPa (10 mm a8 3.424 1.415 1.190 2.815
Hg)
b8 0 0.409 0.409 0
M8 2.9 3.2 3.1 2.9

ANNEXES

(Mandatory Information)

A1. PRACTICE FOR CALIBRATION OF TEMPERATURE SENSORS

A1.1 Principle—This section of the annex deals with the

basic calibration of the vapor temperature sensor against
primary temperature standards as recommended by the Na-
tional Institute for Science and Technology (NIST) in order to
avoid the problems associated with the use of secondary
temperature references. It can also be used for the calibration
of other temperature sensors.

A1.2 Sensors should be calibrated over the full range of

temperatures at the time of first use and whenever the sensor or
its associated instrument is repaired or serviced. Sensors used
in vapor temperature service should be checked monthly at one
or more temperatures.
--`,,`,,``,`,`,```,`,`,,``,`,``-`-`,,`,,`,`,,`---

A1.3 Calibrate the sensors with their associated instruments

by recording the temperatures of the freezing points of water
and of the selected pure metals and metal blends listed in A1.6.

A1.4 Apparatus—A suitable apparatus is shown in Fig.

A1.1. For the freezing point of water, a Dewar flask filled with
at least 50 % crushed ice in water may be substituted.

A1.5 Procedure: FIG. A1.1 Melting Point Bath for Temperature Standards
A1.5.1 For sensors that are mounted loosely in a thermow-
ell, place enough silicone oil or other inert liquid in the bottom A1.5.5 Apply a correction to be added to the reading, if
of the well so as to make good physical contact between the necessary, to give the correct temperature. A chart may be
sensor and the tip of the well. Those sensors that are fused into drawn of correction versus temperature for interpolation. In the
good contact with the tip of the well may be calibrated as is. case of automated instruments, the correction must be built into
A1.5.2 Place about 0.3 mL of silicone oil in the bottom of the record and must be adjustable.
the thermowell of the melting point bath and insert the sensors A1.5.6 If the freezing plateau is too short, it can be
to be calibrated. The oil must cover the tips. increased by applying some heat during the cooling cycle. Be
A1.5.3 Heat the melting point bath to a temperature 5 to aware of the possibility that the metal bath can become
10°C above the melting point of the metal inside and hold at contaminated or too oxidized. In this case, replace the metal.
this temperature for 5 min to ensure that all the metal inside is
A1.6 Reagents and Materials:
melted.
A1.5.4 Discontinue heat to the melting point bath and A1.6.1 Distilled Water—Reagent grade as defined by Type
observe and record the cooling curve. A paper strip chart III of Specification D 1193, freezing point 0.0°C.
recorder is recommended. When the cooling curve shows a A1.6.2 Metals Blend of Sn 50 wt %, Pb 32 wt %, Cd 18
plateau of constant temperature for at least 1 min, the tempera- wt %—Freezing point 145.0°C.
ture of the recorded plateau is accepted as the calibration A1.6.3 Sn—100 %, freezing point 231.9°C.
temperature. A1.6.4 Pb—100 %, freezing point 327.4°C.

Copyright ASTM International 11

Provided by IHS under license with ASTM Licensee=Esso Malaysia Berhard/5986012001, User=Petron Corporation, Refining Div
No reproduction or networking permitted without license from IHS Not for Resale, 08/30/2012 02:23:12 MDT
 D 1160 – 06

A2. PRACTICE FOR DETERMINATION OF TEMPERATURE RESPONSE TIME

A2.1 Scope—This practice is for the determination of the Alternatively, connect the sensor to a strip chart recorder of
temperature response time based on the rate of cooling of the suitable range that will allow interpolation to 0.1°C. Set the
sensor under prescribed conditions. chart speed to at least 30 cm/h for ease of reading.
A2.2 Significance and Use—This practice is performed to A2.3.3 Insert the sensor into a hole in the center of one side
ensure that the sensor is able to respond sufficiently rapidly to of a cardboard cube box of about 30 cm in each dimension. The
changes in temperature that no significant error due to lag is sensor should be held in place by friction fit of the joint in the
introduced in a rapidly rising temperature curve. hole. Record the temperature in the box when it becomes
stable.
A2.2.1 The importance of this test is greatest under the
lowest pressure conditions when the heat content of the vapors A2.3.4 Remove the sensor and insert it into the thermowell
is minimal. in the beaker of water. After the sensor has reached a
temperature of 80°C, remove it and immediately insert it into
A2.3 Procedure: the hole in the box.
A2.3.1 Arrange a 1-L beaker of water on a hot plate with a A2.3.5 Observe with a stopwatch, or record on the strip-
glass thermowell supported vertically in the water. Maintain chart, the time interval required by the sensor to cool from
the temperature of the water at 90 6 5°C. 30°C above to 5°C above the temperature recorded in A2.3.3.
A2.3.2 Connect the sensor to a suitable instrument prefer- A2.3.6 A time interval in excess of 200 s is not acceptable.
ably having a digital readout with a readability to 0.1°C.

A3. PRACTICE FOR CALIBRATION OF VACUUM GAGES

A3.1 Principle—The calibration of vacuum sensors is

based upon the use of the McLeod gage, which is the only
practical primary gage suitable for this pressure range.
NOTE A3.1—The general principles of construction of McLeod gages
are well-established. The dimensions and tolerances of a gage that, when
properly employed, fulfills the requirements of 6.1.5 for the pressure range
from 0.1 to 5 kPa are: capillary length of 200 6 5 mm, capillary diameter
of 2.7 mm (known to 0.002 mm), bulk volume + capillary volume, 10.5 6
0.5 mL (known to 0.05 mL). This gage is best used by adjusting the
mercury level in the system pressure arm to a point opposite the closed
end of the capillary tube. The system pressure is calculated by means of
the following equation:
P 5 Kbh 2 /~V 2 bh! (A3.1)

where: FIG. A3.1 Calibration of Vacuum Gages

K = 133.32. This is a dimensioned conversion factor to
convert mm to N/m2, steady within 1 % of the required pressure at pressures of 1 kPa
P = system pressure, Pa, and higher and within 0.01 kPa at pressures below 1 kPa.
b = volume of capillary per unit of length expressed as
A3.2.1 The McLeod gage, when used as the standard, must
mL/mm,
have been baked out hot and empty at a pressure below 0.01
h = length of capillary left unfilled by mercury, mm, and
V = combined volume of bulb and capillary, mL. kPa before refilling with clean mercury and thereafter be
This equation includes the correction term required when the protected from exposure to moisture such as that from atmo-
system pressure is an appreciable fraction of the length of the spheric air. The use of two McLeod gages of different pressure
capillary left unfilled with mercury. A requirement for the ranges is recommended as a precaution. If they agree at the test
successful operation of this gage to measure system pressures pressure, it is an indication that the system is free of moisture
in the range from 100 Pa to 200 Pa (0.75 mm Hg to 1.5 mm and other condensibles. (Warning—Hg is a poison. Harmful
Hg) is the determination of the length of capillary left unfilled or fatal if inhaled or ingested.)
with mercury with an accuracy of 0.2 mm. At pressures from A3.3 Procedure:
0.2 to 2 kPa (1.5 to 15 mm Hg), a precision in this measure-
A3.3.1 Set up a test manifold such as that shown in Fig.
ment of 0.5 mm is sufficient.
A3.1.
A3.2 Apparatus—A suitable test setup is shown in Fig. A3.3.2 Ensure that the test manifold is leak-free and can be
A3.1. It must be capable of maintaining pressures that are maintained at a steady pressure at the required level. A suitable
--`,,`,,``,`,`,```,`,`,,``,`,``-`-`,,`,,`,`,,`---

Copyright ASTM International 12

Provided by IHS under license with ASTM Licensee=Esso Malaysia Berhard/5986012001, User=Petron Corporation, Refining Div
No reproduction or networking permitted without license from IHS Not for Resale, 08/30/2012 02:23:12 MDT
 D 1160 – 06
leak test is to pump down to a pressure below 0.1 kPa and A3.3.4 Read and record the pressures indicated by all the
isolate the pump. Observe the pressure inside the unit for at gages as nearly simultaneously as possible.
least 1 min. If the pressure rises no more than 0.01 kPa in that A3.3.5 Repeat the above procedure at the pressure levels
period, the apparatus is considered acceptable. 0.13, 1.3, and 6.7 kPa (1, 10, and 50 mm Hg).
A3.3.3 Connect the primary vacuum gage(s) and the gage(s) A3.3.6 Make up a chart of corrections to be added at each
to be calibrated. Adjust the pressure to the required level for the pressure level for each gage tested. This can be used for
test and run a final leak test as above. interpolation when necessary.

A4. PRESSURE REGULATING SYSTEM

A4.1 The following is suggested as a satisfactory example A4.1.3 For multiple still arrangements, it is possible to use
of a pressure regulating system: A low-efficiency, high- a large pump and a large low-pressure surge tank. Several
capacity vacuum pump is connected to one of two surge tanks, smaller tanks operating at the pressures of the various distilla-
each having a capacity of 10 to 20 L and arranged in series. A tions can be attached to the large low-pressure surge tank with
solenoid valve or other type regulator is installed in the individual pressure regulators. Other arrangements can be
connection between the tanks so that the first tank is main- used, provided the pressure is maintained constant within the
tained at pump pressure and the second one at the pressure of limits specified in 6.1.7.
the distillation apparatus.
A4.1.1 With some apparatus it is desirable to have a slight NOTE A4.1—If a solenoid valve or other electrically operated regulator
is used, a suitable manostat is required for activation of the regulating
bleed to the second tank that will cause the controls to operate
device. Many such manostats are described in the literature or are
at regular intervals in order to provide smooth operation. available from laboratory supply houses. As an alternative for the separate
However, experience has shown that the bleed shall be held at manostat and solenoid, a Cartesian Manostat can be used. This device is
an absolute minimum in order to prevent loss of vapors through capable of maintaining the system pressure within the specified limits
the manometer connection at the top of the column. down to a pressure of about 1 kPa.
A4.1.2 Connecting lines from the second tank to the
vacuum distillation apparatus shall be as short in length and as
large in diameter as possible. A minimum internal diameter of
12 mm is suggested.

A5. APPARATUS CHECK WITH REAGENT FUEL

A5.1 Check the assembled apparatus, including the previ- t 5 [1831.316/~6.14438 2 log P!# 2 154.53 (A5.1)
ously calibrated pressure measuring and temperature sensor
and associated instrumentation, to indicate proper assembly where P is in kPa, and t is in °C, or
and operating control. Conduct the test procedure as described
at the test pressure in connection with a specific sample or at t 5 [1831.316/~7.01944 2 log P!# 2 154.53 (A5.2)
two or more pressures in connection with general checks of the where P is in mm Hg, and t is in °C.
equipment, using n-hexadecane or n-tetradecane.
A5.1.3 If n-tetradecane is used, the average of distillation
A5.1.1 If n-hexadecane is used, the average of distillation temperatures obtained in the 10 % to 90 % range, inclusive,
temperatures obtained in the 10 % to 90 % range, inclusive, should conform with the data in Table A5.1.
should conform with the data in Table A5.1.
A5.1.4 For pressures over 0.1 kPa not given in Table A5.1,
A5.1.2 For pressures over 0.1 kPa not given in Table A5.1,
and if n-tetradecane is used, the range of average temperatures
the range of average temperatures shall not deviate by more
than 1.5°C from a temperature, t, given by: shall not deviate by more than 1.5°C from a temperature, t14,
given by:
TABLE A5.1 Distillation Temperatures of Reference Compounds t14 5 [1747.452/~6.1471 2 log P!# 2 168.44 (A5.3)
Pressure Range of Temperatures,° C
kPa mm Hg n-tetradecane n-hexadecane
where P is in kPa, and t is in °C, or
0.13 1.0 78.9 to 81.9 104.3 to 107.6
0.67 5.0 106.4 to 109.4 133.1 to 136.4 t14 5 [1747.452/~7.02216 2 log P!# 2 168.44 (A5.4)
1.34 10.0 120.2 to 123.2 147.5 to 150.8
2.7 20.0 135.5 to 138.5 163.3 to 166.7
5.3 40.0 152.5 to 155.5 181.1 to 184.4 where P is in mm Hg, and t is in °C.
6.7 50.0 158.3 to 161.3 187.2 to 190.6

--`,,`,,``,`,`,```,`,`,,``,`,``-`-`,,`,,`,`,,`---

Copyright ASTM International 13

Provided by IHS under license with ASTM Licensee=Esso Malaysia Berhard/5986012001, User=Petron Corporation, Refining Div
No reproduction or networking permitted without license from IHS Not for Resale, 08/30/2012 02:23:12 MDT
 D 1160 – 06

A6. SAMPLE DEHYDRATION AND FOAMING SUPPRESSION

A6.1 Dehydration of Sample—The following is suggested Grade 2 steel wool, roll into five balls, each approximately 8 to
--`,,`,,``,`,`,```,`,`,,``,`,``-`-`,,`,,`,`,,`---

as a convenient means of dehydrating samples to be subjected 10 mm in diameter, and drop into the flask.
to this distillation test. Heat 300 mL of the sample to 80°C, add A6.2.4 Boiling Chips—These consist of broken pieces of
10 to 15 g of 8- to 12-mesh fused calcium chloride (CaCl2), and porcelain drying plates or broken alundum thimbles that are
stir vigorously for 10 to 15 min. Allow the mixture to cool dropped into the flask before starting a distillation. Hengar
without stirring, and remove the oil layer by decantation. granules of the plain type, as used in Kjeldahl nitrogen
determinations, are also used in the same way (Note A6.1).
A6.2 Suppression of Foaming and Bumping of the Sample:
NOTE A6.1—The use of anti-bumping aids can affect the distillation
A6.2.1 The tendency of samples to bump or foam exces- curve. Their use should therefore be limited to cases where they are
sively is frequently a serious obstacle to the successful distil- absolutely needed to perform the distillation.
lation of petroleum products under vacuum. In some cases, this
A6.2.5 Silicone Fluids—The addition of one or two drops
is due to the presence of water or dissolved gases, but many
of silicone fluid5 (350 cSt) to the sample in the flask is effective
samples foam even when apparently free from these contami-
in the suppression of foam in many cases. However, analytical
nants. There is no unanimity of opinion concerning the best
tests run on the products from this test method can be biased by
way to reduce excessive foaming to manageable proportions.
the presence of these fluids, so the report shall make note of
The following methods are offered solely as examples of
their use.
means that have been employed successfully for that purpose.
A6.2.6 Flask Preparation—Some laboratories have treated
A6.2.2 Degassing—The procedure described in 10.6 is
the inside of the flask, prior to use for distillation, in order to
intended to promote degassing. Slow rates of pressure reduc-
provide an active ebullition surface. Methods used for this
tion or temperature increase, or both, for the oil in the flask are
purpose include: boiling 100 mL of 33 % sodium hydroxide
important factors in achieving success by this means. Another
solution for 15 to 20 min, etching of the inside of the flask
technique for degassing is to filter the sample under vacuum
bottom with hydrofluoric acid fumes, and the infusion of fine
before weighing.
carborundum or fritted glass to the inside of the flask bottom.
A6.2.3 Application of Steel Wool—Separate about 10 g of a
folded pad of median-grade steel wool. Unfold, and separate
into 8 to 10 long, loose strands. Push each strand separately
5
into the bulk of the flask. Avoid packing tightly or forming The sole source of supply of Dow Corning Silicone Fluid No. 200 known to the
committee at this time is Dow Corning. If you are aware of alternative suppliers,
large void spaces. Fill the upper half of the bulb with steel
please provide this information to ASTM International Headquarters. Your com-
wool, but do not allow any strand to protrude more than 6 mm ments will receive careful consideration at a meeting of the responsible technical
into the neck of the flask. Alternatively, take 0.5 to 0.6 g of committee,1 which you may attend.

A7. PRACTICE FOR CONVERTING OBSERVED VAPOR TEMPERATURES TO ATMOSPHERIC EQUIVALENT

TEMPERATURES (AET)

A7.1 Scope where:

A7.1.1 This practice is for conversion of the actual distilla- AET = atmospheric equivalent temperature, °C, and
tion temperature obtained at sub-ambient pressure to atmo- T = observed vapor temperature, °C.
spheric equivalent temperature (AET) corresponding to the A7.3.1.1 Calculate A using Eq A7.2 or Eq A7.3:
equivalent boiling point at atmospheric pressure, 101.3 kPa 5.143222 – 0.972546 log10 P
(760 mm Hg), by means of equations derived by Maxwell and A 5 2579.329 – 95.76 log P (A7.2)
10
Bonnell.6
where:
A7.2 Significance and Use P = operating pressure, kPa, (operating pressure $0.266
A7.2.1 Final data on atmospheric equivalent temperatures kPa), or
are to be obtained by computation. 5.994295 – 0.972546 log10 P
A 5 2663.129 – 95.76 log P (A7.3)
A7.3 Calculation 10

A7.3.1 Convert observed vapor temperature to atmospheric where:

equivalent temperature using Eq A7.1: P = operating pressure, mm Hg (operating pressure $2 mm
748.1A Hg).
AET 5 – 273.1
@1/~T 1 273.1!# 1 0.3861A – 0.00051606 A7.3.1.2 If the operating pressure < 0.266 kPa (< 2 mm Hg),
(A7.1) calculate A using Eq A7.4 or Eq A7.5:
5.897249 – 0.987672 log10 P
6
Maxwell and Bonnell, Industrial Engineering Chemistry, Vol 49, 1957, p. 1187.
A 5 2962.909 – 43.00 log P (A7.4)
10

Copyright ASTM International 14

Provided by IHS under license with ASTM Licensee=Esso Malaysia Berhard/5986012001, User=Petron Corporation, Refining Div
No reproduction or networking permitted without license from IHS Not for Resale, 08/30/2012 02:23:12 MDT
 D 1160 – 06

where:
P = operating pressure, kPa, or
6.761559 – 0.987672 log10 P
A 5 3000.538 – 43.00 log P (A7.5)
10

where:
P = operating pressure, mm Hg.
A7.3.2 The equations are correct only for specimens that
have a Watson K-factor of 12.0 6 0.2. The K-factor shall be
assumed to be 12 and any effect of K-factor ignored unless
there is mutual agreement to the contrary.
A7.3.3 If correction is required, calculate the K-factor using
Eq A7.6:
3
= 1.8~B 1 273.1!
K5 D (A7.6)

where:
B = mean average boiling point, °C, and
D = relative density at 15.6/15.6°C.
A7.3.3.1 By custom, either the mid-point vapor temperature
of the specimen or the mid-point of a gas chromatographic
distillation of the specimen can be used for the mean average
boiling point. In either case the method must be specified.
A7.3.3.2 An estimate of the K-factor can be made using Fig.
A7.1.
A7.3.4 Calculate the correction to be applied to the AET
using Eq A7.7:

F S DG
Pa
t 5 –1.4[K – 12] log10 P
o
(A7.7)

where:
FIG. A7.1 Watson Characterization Factor of Petroleum Fractions
t = correction, °C,
Pa = atmospheric pressure, kPa (mm Hg), and
Po = observed pressure, kPa (mm Hg). A7.3.4.1 An estimate of the correction can be made using
Fig. A7.2.

--`,,`,,``,`,`,```,`,`,,``,`,``-`-`,,`,,`,`,,`---

Copyright ASTM International 15

Provided by IHS under license with ASTM Licensee=Esso Malaysia Berhard/5986012001, User=Petron Corporation, Refining Div
No reproduction or networking permitted without license from IHS Not for Resale, 08/30/2012 02:23:12 MDT
 --`,,`,,``,`,`,```,`,`,,``,`,``-`-`,,`,,`,`,,`---
D 1160 – 06

FIG. A7.2 Boiling Point Corrections for K-Factor

A8. EXAMPLE OF PRECISION CALCULATIONS

A8.1 Procedure AET (°C) 40 % 443

A8.1.1 For a given percentage recovered from a distillation AET (°C) 30 % 427
at a given pressure (0.13 or 1.3 kPa), calculate the change in AET (°C) 20 % 409
temperature per volume percent recovered {°C(AET)/V %}. °C/V % = (443 − 409)/(40 − 20) = 34/20 = 1.7
A8.1.2 Look up the desired precision (repeatability or From Table 2, Reproducibility, 0.13 kPa (1 mm Hg); recovery
reproducibility) from Table 2. Use linear interpolation to find between 5 and 50 % (inclusive):
the precision when °C(AET)/V % is not a whole number.
°C/V % of 1.5 = 13
A8.2 Example—Desired result: reproducibility of 30 % °C/V % of 2.0 = 16
recovered, 0.13 kPa (1 mm Hg), °C: Therefore: 13 + (0.2/0.5)(16 − 13) = 14.2, rounded = 14°C.

Copyright ASTM International 16

Provided by IHS under license with ASTM Licensee=Esso Malaysia Berhard/5986012001, User=Petron Corporation, Refining Div
No reproduction or networking permitted without license from IHS Not for Resale, 08/30/2012 02:23:12 MDT
 D 1160 – 06

A9. DISTILLATION OF PETROLEUM PRODUCTS AT REDUCED PRESSURE (AUTOMATIC)

A9.1 Scope—This test method covers the determination by A9.6.3 From the density of the sample, determine the
automatic equipment, at reduced pressures, of the range of weight, to the nearest 0.1 g, equivalent to 200 mL of the sample
boiling points for petroleum products that can be partially or at the temperature of the receiver. Weigh this quantity of oil
completely vaporized at a maximum liquid temperature of into the distillation flask.
400°C. A9.6.4 Lubricate the spherical joints of the distillation
apparatus with a suitable grease. Connect the flask to the lower
A9.2 Summary of Test Method—The sample is distilled in spherical joint of the distilling head, place the heater under the
an automatic distillation apparatus that duplicates the distilla- flask, put the top mantle in place, and connect the rest of the
tion conditions described in the manual procedure. Data are apparatus using spring clamps to secure the joints.
obtained from which the initial boiling point (IBP), the final A9.6.5 Insert the temperature sensor into the thermowell of
boiling point (FBP), and a distillation curve of atmospheric the flask.
equivalent temperature (AET) versus volume can be obtained.
A9.6.6 Set the operating pressure to the prescribed value for
A9.3 Apparatus—The automatic apparatus should be de- the distillation (see Note 3). The pressure should be automati-
signed to include the components as described in 6.1. Addi- cally reduced in stages to prevent foaming of the sample.
tional parts not specified can be included by the manufacturer A9.6.7 Set the initial heat rate to the desired value. The
that are not essential for obtaining satisfactory results but are apparatus should have the capability to adjust heat input so that
desirable components to the assembly for the purpose of the distillate recovered is at a uniform rate of 6 to 8 mL/min.
promoting efficient use of the apparatus and ease of operation. A9.6.8 After ensuring that the apparatus controls are set
A9.3.1 Level Follower/Recording Mechanism for the mea- according to the manufacturer’s instructions, initiate the distil-
--`,,`,,``,`,`,```,`,`,,``,`,``-`-`,,`,,`,`,,`---

surement of the volume of liquid recovered in the receiver. The lation.

system shall have a resolution of 0.1 mL with an accuracy of A9.6.9 The apparatus will automatically record the initial
61 mL. The calibration of the assembly should be confirmed boiling point, final boiling point, percent volumes recovered
according to the manufacturer’s instructions. with corresponding actual temperatures, and distillation rates.
A9.3.2 Vacuum Gage, capable of measuring the absolute Actual temperatures recorded are automatically converted to
pressure with an accuracy of 610 Pa (60.08 mm Hg) at 1 kPa Atmospheric Equivalent Temperatures (AET) using software
(7.5 mm) and below. The vacuum gage is usually an electronic supplied by the manufacturer. This conversion should be based
pressure measuring system. An accuracy of 61 % of the on (Eq A7.1).
observed reading is required in the range above 1 kPa. A9.6.10 If the liquid temperature reaches 400°C, or if the
Electronic diaphragm gages are capable of achieving this level vapor temperature reaches a maximum before the end point is
of accuracy, but they must be properly calibrated and re- observed, the distillation equipment shall switch off and
checked periodically, as described in Annex A3. terminate the distillation. The apparatus shall automatically
A9.3.3 Receiver Chamber Temperature Control System, ca- record the vapor temperature and total volume percent recov-
pable of controlling the receiver temperature between 32°C ered at the time the distillation is discontinued.
and 78°C. A9.6.11 Upon completion of the distillation, the apparatus
will automatically enter into a cooling cycle. After the tem-
A9.4 Sample and Sample Requirements—Sample and sam- perature drops below a safe limit, usually 100°C, the pressure
pling requirements are described in Section 8. in the distillation assembly is gradually increased to atmo-
spheric pressure. The flask and receiver can then be removed
A9.5 Preparation of Apparatus—The instrument is pre- for cleaning. If it is necessary to dismantle the apparatus before
pared in accordance with the manufacturer’s instructions. the contents have cooled below 100°C, use dry nitrogen to
A9.6 Procedure bring the system pressure back to atmospheric pressure.
A9.6.12 The unit is cleaned as described in 10.13.
A9.6.1 Set the temperature of the condenser coolant to at
least 30°C below the lowest vapor temperature to be observed A9.6.13 Any material in the cold trap is recovered as
in the test. A temperature near 60°C has been found satisfactory described in 10.12.
for most charges.
A9.6.2 Determine the density of the sample at the tempera- A9.7 Precision and Bias
ture of the receiver by means of a hydrometer by Test Method A9.7.1 The precision of the test method using automatic
D 1298, by means of a digital density meter using Test Method Test Method D 1160 equipment is being determined.
D 4052, or by using either the mathematical subroutines or A9.7.2 The bias between the manual and the automatic test
tables of Guide D 1250, or a combination thereof. method is being determined.

Copyright ASTM International 17

Provided by IHS under license with ASTM Licensee=Esso Malaysia Berhard/5986012001, User=Petron Corporation, Refining Div
No reproduction or networking permitted without license from IHS Not for Resale, 08/30/2012 02:23:12 MDT
 D 1160 – 06
APPENDIX

(Nonmandatory Information)

X1. VAPOR TEMPERATURE MEASURING DEVICE ALIGNMENT PROCEDURE

X1.1 A tool to help in determining the spillover point was X1.3 Once the spillover point has been determined, then
made out of an approximately 3 mm rod approximately 300 make a mark on both sides of the outside glass 3 mm 6 1 mm
mm in length. A 90° bend was made approximately 25 mm below the marks determined above. This is where the top of the
from one end. Then a 2 mm inside diameter (ID) flexible sensing tip should be aligned. (If possible, these two sets of
plastic tubing was placed over the end to a total distance of marks should be permanently made on the distillation column
about 30 mm. The flexible plastic tubing is used to prevent since they should not change unless repairs are made to the
scratching of the glassware. The length of the bend is depen- glassware).
dent upon the ID of the distillation column.
X1.2 This tool is then carefully moved up from the bottom X1.4 While holding the distillation column such that you
of the distillation column until the end can protrude into the can see through the distillation column, insert the thermo-
condensing arm. The tip of the bent end of the tool should then couple which has been placed in the tapered screw cap down
be rested on the highest point of the lower internal junction of into the distillation column. With the tapered fitting in its
the distillation column and the condensing section of the normal operating position adjust the thermocouple (up or
vacuum-jacketed column assembly. This is the spillover point. down) so that the top of the sensing tip is aligned with the
--`,,`,,``,`,`,```,`,`,,``,`,``-`-`,,`,,`,`,,`---

Then with a ballpoint pen make a mark on one side of the lower of the two marks made on the outside glass. Once in the
outside glass of the distillation column in line with the bottom proper position tighten the screw cap. Then mark the point
of the tool. Repeat this step on the opposite side of the where the thermocouple aligns with the top of the screw cap
distillation column. With two straight edge rulers confirm that with a permanent marker. This marking will be accurate for this
the distance from the top of the distillation column down to particular distillation column, tapered screw cap, and thermo-
each of the two marks is equal. If they are both equal, then this couple only and can be used to verify proper alignment.
is the spillover point. If they are not equal, repeat the steps
described above.

SUMMARY OF CHANGES

Subcommittee D02.08 has identified the location of selected changes to this standard since the last issue
(D 1160–03) that may impact the use of this standard.

(1) Updated 10.13.

ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentioned
in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk
of infringement of such rights, are entirely their own responsibility.

This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and
if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards
and should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of the
responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should
make your views known to the ASTM Committee on Standards, at the address shown below.

This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,
United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the above
address or at 610-832-9585 (phone), 610-832-9555 (fax), or service@astm.org (e-mail); or through the ASTM website
(www.astm.org).

Copyright ASTM International 18

Provided by IHS under license with ASTM Licensee=Esso Malaysia Berhard/5986012001, User=Petron Corporation, Refining Div
No reproduction or networking permitted without license from IHS Not for Resale, 08/30/2012 02:23:12 MDT