ASTM D7345-07

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
An American National Standard
Designation:D7345–07
Standard Test Method for
Distillation of Petroleum Products at Atmospheric Pressure
(Micro Distillation Method)
This standard is issued under the fixed designation D 7345; 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.
1. Scope 2.2 ASTM Standards:
D86 Test Method for Distillation of Petroleum Products at
1.1 This test method covers a procedure for determination
Atmospheric Pressure
of the distillation characteristics of petroleum products having
D 323 Test Method for Vapor Pressure of Petroleum Prod-
boiling range between 20 to 400°C at atmospheric pressure
ucts (Reid Method)
using an automatic micro distillation apparatus.
D 4057 Practice for Manual Sampling of Petroleum and
1.2 This test method is applicable to such products as; light
Petroleum Products
and middle distillates, automotive spark-ignition engine fuels,
D 4177 Practice for Automatic Sampling of Petroleum and
aviation gasolines, aviation turbine fuels, regular and low
Petroleum Products
sulfur diesel fuels, biodiesel fuels, special petroleum spirits,
D 4953 Test Method for Vapor Pressure of Gasoline and
naphthas, white spirits, kerosines, burner fuels, and marine
Gasoline-Oxygenate Blends (Dry Method)
fuels.
D 5190 Test Method for Vapor Pressure of Petroleum Prod-
1.3 The test method is also applicable to hydrocarbons with
ucts (Automatic Method)
a narrow boiling range, like organic solvents or oxygenated
D 5191 Test Method for Vapor Pressure of Petroleum Prod-
compounds.
ucts (Mini Method)
1.4 The test method is designed for the analysis of distillate
D 5482 Test Method for Vapor Pressure of Petroleum Prod-
products;itisnotapplicabletoproductscontainingappreciable
ucts (Mini Method—Atmospheric)
quantities of residual material.
D 5854 Practice for Mixing and Handling of Liquid
1.5 The values stated in SI units are to be regarded as the
Samples of Petroleum and Petroleum Products
standard. The values given in parentheses are for information
D 6299 Practice for Applying Statistical Quality Assurance
only.
Techniques to Evaluate Analytical Measurement System
1.6 This standard does not purport to address all of the
Performance
safety concerns, if any, associated with its use. It is the
D 6300 Practice for Determination of Precision and Bias
responsibility of the user of this standard to establish appro-
Data for Use in Test Methods for Petroleum Products and
priate safety and health practices and determine the applica-
Lubricants
bility of regulatory limitations prior to use.
D 6708 Practice for Statistical Assessment and Improve-
2. Referenced Documents ment of Expected Agreement Between Two Test Methods
that Purport to Measure the Same Property of a Material
2.1 All standards are subject to revision, and parties to
2.3 Energy Institute Standards:
agreement on this test method are to apply the most recent
IP 69 Petroleum products - Determination of vapour pres-
edition of the standards indicated below, unless otherwise
sure - Reid method
specified, such as in contractual agreements or regulatory rules
IP394 Liquidpetroleumproducts-Vapourpressure-Part1:
where earlier versions of the method(s) identified may be
required.
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
This test method is under the jurisdiction of ASTM Committee D02 on Standards volume information, refer to the standard’s Document Summary page on
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee the ASTM website.
D02.08 on Volatility. Available from Energy Institute, 61 New Cavendish St., London, WIG 7AR,
Current edition approved July 15, 2007. Published August 2007. U.K., http://www.energyinst.org.uk.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D7345–07
Determination of air saturated vapour pressure (ASVP) 3.1.11 reference method, n—ASTMD86 test method or its
2.4 ISO Standards: analogs which is widely used for expression of the distillation
Guide 34 General requirements for the competence of characteristics of petroleum products in industry.
reference material producers 3.1.12 temperature readings, n—vapor and liquid tempera-
turehasthroughuseofanalgorithmoftheautomaticapparatus
Guide 35 Reference materials — General and statistical
principles for certification been adjusted to mimic the same temperature lag and emergent
stem effects as would be seen when using an ASTM 7C/7F or
3. Terminology 8C/8F liquid-in-glass thermometer to determine the distillation
characteristicsofthematerialundertestbyindustryrecognized
3.1 Definitions of Terms Specific to This Standard:
reference method.
3.1.1 automatic apparatus, n—microprocessor-controlled
3.1.13 vapor temperature, n—temperature of the vapors in
unit that performs the procedures of automatically controlling
the distillation flask during the test obtained by a vapor
the evaporation of a liquid specimen under specific conditions
temperature measuring device of automatic apparatus.
of this test method, collecting measurement data and convert-
ing this data by patented algorithm in order to predict distilla-
4. Summary of Test Method
tion results in correlation with industry recognized reference
method.
4.1 A specimen of the sample is transferred into the distil-
3.1.2 corrected temperature reading, n—temperature read- lation flask, the distillation flask is placed into position on the
ings, as described in 3.1.12, corrected to 101.3 kPa barometric
automatic apparatus, and heat is applied to the bottom of the
pressure. distillation flask.
3.1.3 end point (EP) or final boiling point (FBP),
4.2 The automatic apparatus measures and records speci-
n—maximum corrected temperature readings obtained during men vapor and liquid temperatures, and pressure in the
the test at the instant the flask internal pressure returns to the
distillation flask as the sample gradually distills under atmo-
initial pressure level registered by automatic apparatus. spheric pressure conditions. Automatic recordings are made
3.1.3.1 Discussion—This usually occurs after the evapora-
throughout the distillation and the data stored into the appara-
tion of all liquid from the bottom of the distillation flask. The
tus memory.
term maximum temperature is a frequently used synonym.
4.3 At the conclusion of the distillation, the collected data is
3.1.4 flask internal pressure, n—pressure within the distil-
treated by the data processing system, converted to distillation
lation flask obtained during the test by a differential pressure
characteristics and corrected for barometric pressure.
sensor of automatic apparatus.
4.4 Test results are commonly expressed as percent recov-
3.1.4.1 Discussion—The flask internal pressure data re-
ered or evaporated versus corresponding temperature in com-
corded during the test is automatically converted to the volume
pliance with industry recognized standard form and reference
percent recovered or evaporated data by patented algorithm
method either in a table or graphically, as a plot of the
employed by automatic apparatus.
distillation curve.
3.1.5 initial boiling point (IBP), n—corrected temperature
readings that corresponds to the instant of the flask internal
5. Significance and Use
pressure rise registered by automatic apparatus.
5.1 The distillation (volatility) characteristics of hydrocar-
3.1.6 liquid temperature, n—temperature of the liquid
bons have an important effect on their safety and performance,
specimen in the distillation flask during the test obtained by a
especially in the case of fuels and solvents. The boiling range
liquid temperature measuring device of automatic apparatus.
gives information on the composition, the properties, and the
3.1.7 percent evaporated, n—percentrecoveredcorrectedto
behavior of the fuel during storage and use. Volatility is the
a predicted by automatic analyzer evaporation loss percent.
major determinant of the tendency of a hydrocarbon mixture to
Percent evaporated is automatically reported for ASTM 7C
produce potentially explosive vapors.
thermometer correlation.
5.2 The distillation characteristics are critically important
3.1.8 percent recovered, n—volume percent automatically
for both automotive and aviation gasolines, affecting starting,
reported by the analyzer; expressed as a percentage of the
warm-up, and tendency to vapor lock at high operating
charge volume, associated with a simultaneous temperature
temperature or at high altitude, or both. The presence of high
readings. Percent recovered is reported for ASTM 8C ther-
boiling point components in these and other fuels can signifi-
mometer correlation.
cantly affect the degree of formation of solid combustion
3.1.9 percent recovery, n—percent recovery predicted by
deposits.
the automatic apparatus and expressed as a percentage of the
5.3 Distillation limits are often included in petroleum prod-
charge volume.
uct specifications, in commercial contract agreements, process
3.1.10 percent residue, n—volume of residue in the distil-
refinery/control applications, and for compliance to regulatory
lation flask predicted by the automatic apparatus and expressed
rules.
as a percentage of the charge volume.
5.4 This test method can be applied to contaminated prod-
ucts or hydrocarbon mixtures. This is valuable for fast product
quality screening, refining process monitoring, fuel adultera-
tion control, or other purposes including use as a portable
Available from International Organization for Standardization (ISO), 1 rue de
Varembé, Case postale 56, CH-1211, Geneva 20, Switzerland, http://www.iso.ch. apparatus for field testing.
D7345–07
5.5 This test method uses an automatic micro distillation isintendedthatallreagentsconformtothespecificationsofthe
apparatus,providesfastresultsusingsmallsamplevolume,and Committee on Analytical Reagents of the American Chemical
eliminates much of the operator time and subjectivity in Society.
comparison to Test MethodD86. 7.5 Granular Pumice Stones, clean and dry fine grade
pumice stones of diameter 0.8 to 3.0 mm, approximately 10
6. Apparatus grains are necessary for each test.
5 7.6 Sample Drying Agent—Anhydrous sodium sulfate has
6.1 Basic Components of the Automatic Apparatus:
been found to be suitable.
6.1.1 Thebasiccomponentsofthemicrodistillationunitare
the distillation flask, a condensate recovery area with waste
8. Sampling, Storage, and Sample Conditioning
beaker, an enclosure for the distillation flask with the heat
8.1 Sampling:
source and flask support, the specimen liquid temperature
8.1.1 The extreme sensitivity of volatility measurements to
measuring device, the specimen vapor temperature measuring
losses through evaporation and the resulting changes in com-
device,thedistillationflaskinternalpressuremeasuringdevice,
position is such as to require the utmost precaution in the
the ambient pressure measuring device, the control systems for
drawing and handling of volatile product samples.
regulating the distillation process, and the data processing
8.1.2 Obtain a sample and test specimen in accordance with
system for converting recorded information into typical indus-
Practice D 4057, D 4177 or D 5854 when appropriate.At least
try recognized standard report form.
50 mL of sample is recommended.
6.2 AdetaileddescriptionoftheapparatusisgiveninAnnex
8.1.3 Sample shall be free from any suspended solids or
A1.
other insoluble contaminations. Obtain another sample or
6.3 Barometer for Calibration—A pressure measuring de-
remove solid particle by filtration. During filtration operation
vice capable of measuring local station pressure with an
take care to minimize any loss of light ends.
accuracy of 0.1 kPa (1 mmHg) or better, at the same elevation
8.2 Sample Storage:
relative to sea level where the apparatus is located.
8.2.1 All samples shall be stored in a tightly closed and
6.3.1 Thebarometerisonlyrequiredforperiodiccalibration
leak-free container away from direct sunlight or sources of
of the external and internal pressure measuring devices.
direct heat.
6.3.2 (Warning—Do not take readings from ordinary aner-
8.2.2 Protect samples containing light materials having
oid barometers, such as those used at weather stations and
expected initial boiling point lower than 100°C (212°F) from
airports, since these are precorrected to give sea level read-
excessive temperatures prior to testing. This can be accom-
ings.)
plishedbystorageofthesamplecontainerinanappropriateice
6.4 Sampling Device—Glass or plastics syringe capacity
bath or refrigerator at a temperature below 10°C. Other
10 6 0.3 mL or constant volume dispenser capacity 10 6 0.3
samples can be stored at ambient or lower temperature.
mL.
8.2.3 If the sample has partially or completely solidified
6.5 Waste Beaker—Glass approximately 200 mL capacity,
during storage, it is to be carefully heated to a temperature
outside diameter approximately 70 mm and height approxi-
when it is completely fluid. It shall be vigorously shaken after
mately 130 mm fitted with a cover to reduce evaporation. The
melting, prior to opening the sample container, to ensure
cover design shall allow the beaker to remain open to atmo-
homogeneity.
spheric pressure.
8.3 Wet Samples:
8.3.1 Samples of materials that visibly contain water are not
7. Reagents and Materials
suitable for testing by this test method. If the sample is not dry,
7.1 Cleaning Solvents, suitable for cleaning and drying the
obtain another sample that is free from suspended water.
testflasksuchas;petroleumnaphthaandacetone.(Warning—
8.3.2 If such a sample cannot be obtained, remove any free
Flammable. Liquid causes eye burns. Vapor harmful. May be
water by placing approximately 30 mL of the sample to be
fatal or cause blindness if swallowed or inhaled.)
tested in a glass conical flask containing approximately 10 g of
7.2 Toluene, 99.5 % purity. (Warning—Extremely flam-
the drying agent. Stopper and shake gently.Allow the mixture
mable. Harmful if inhaled. Skin irritant on repeated contact.
to settle for approximately 15 min. Once the sample shows no
Aspiration hazard.)
visible signs of water, use a decanted portion of the sample for
7.3 n-Hexadecane, 99 % purity. (Warning—Extremely
the analysis. It is recommended to filter the test portion from
flammable. Harmful if inhaled. Skin irritant on repeated
the residual or suspended drying agent. During this drying a
...