ASTM D7345-23
(Test Method)Standard Test Method for Distillation of Petroleum Products and Liquid Fuels at Atmospheric Pressure (Micro Distillation Method)
Standard Test Method for Distillation of Petroleum Products and Liquid Fuels at Atmospheric Pressure (Micro Distillation Method)
SIGNIFICANCE AND USE
5.1 The distillation (volatility) characteristics of hydrocarbons and other liquids have an important effect on their safety and performance, especially in the case of fuels and solvents. The boiling range gives information on the composition, the properties, and the behavior of the fuel during storage and use. Volatility is the major determinant of the tendency of a hydrocarbon mixture to produce potentially explosive vapors.
5.2 The distillation characteristics are critically important for both automotive and aviation gasolines, affecting starting, warm-up, and tendency to vapor lock at high operating temperature or at high altitude, or both. The presence of high boiling point components in these and other fuels can significantly affect the degree of formation of solid combustion deposits.
5.3 Distillation limits are often included in petroleum product specifications, in commercial contract agreements, process refinery/control applications, and for compliance to regulatory rules.
5.4 This test method can be applied to contaminated products or hydrocarbon mixtures. This is valuable for fast product quality screening, refining process monitoring, fuel adulteration control, or other purposes including use as a portable apparatus for field testing.
5.5 This test method uses an automatic micro distillation apparatus, provides fast results using small sample volume, and eliminates much of the operator time and subjectivity in comparison to Test Method D86.
SCOPE
1.1 This test method covers a procedure for determination of the distillation characteristics of petroleum products and liquid fuels having boiling range between 20 °C to 400 °C at atmospheric pressure using an automatic micro distillation apparatus.
1.2 This test method is applicable to such products as; light and middle distillates, automotive spark-ignition engine fuels, automotive spark-ignition engine fuels containing up to 20 % ethanol, aviation gasolines, aviation turbine fuels, regular and low sulfur diesel fuels, biodiesel (B100), biodiesel blends up to 20 % biodiesel, special petroleum spirits, naphthas, white spirits, kerosines, burner fuels, and marine fuels.
1.3 The test method is also applicable to hydrocarbons with a narrow boiling range, like organic solvents or oxygenated compounds.
1.4 The test method is designed for the analysis of distillate products; it is not applicable to products containing appreciable quantities of residual material.
1.5 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.6 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.
1.7 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.
General Information
- Status
- Published
- Publication Date
- 30-Nov-2023
- Technical Committee
- D02 - Petroleum Products, Liquid Fuels, and Lubricants
- Drafting Committee
- D02.08 - Volatility
Relations
- Effective Date
- 01-Dec-2023
- Effective Date
- 01-Mar-2024
- Effective Date
- 01-Mar-2024
- Effective Date
- 01-Dec-2023
- Effective Date
- 01-Dec-2023
- Effective Date
- 01-Dec-2023
- Effective Date
- 01-Mar-2023
- Effective Date
- 01-May-2021
- Effective Date
- 01-Dec-2023
- Effective Date
- 01-Dec-2023
- Effective Date
- 01-Dec-2023
- Effective Date
- 01-Dec-2023
- Effective Date
- 01-Dec-2023
- Referred By
ASTM E3050-22 - Standard Specification for Denatured Ethanol for Use as Cooking and Appliance Fuel - Effective Date
- 01-Dec-2023
- Effective Date
- 01-Dec-2023
Overview
ASTM D7345-23 is a standard test method developed by ASTM International for determining the distillation characteristics of petroleum products and liquid fuels at atmospheric pressure using the micro distillation method. This standard provides a procedure for analyzing fuels and hydrocarbons with boiling ranges between 20 °C and 400 °C, using an automatic micro distillation apparatus. ASTM D7345-23 streamlines the measurement of volatility-a critical parameter affecting both safety and performance in fuels and solvents-while significantly reducing sample size, operator involvement, and test time compared to traditional methods.
Key Topics
- Distillation Characteristics: The test method assesses the boiling range and volatility of hydrocarbons and other liquids, which are essential for evaluating fuel composition, stability, and performance during storage and use.
- Micro Distillation Apparatus: Utilizes an automatic, microprocessor-controlled system to ensure accuracy, repeatability, and operator-independent results.
- Sample Types: Applicable to a wide range of petroleum products, including automotive and aviation gasolines (with or without ethanol), diesel fuels (regular and low sulfur), biodiesel, biodiesel blends, kerosine, naphthas, white spirits, burner fuels, organic solvents, and marine fuels.
- Precision and Quality Control: Incorporates strict procedural and calibration guidelines for high repeatability and reproducibility, as well as compatibility with industry reference methods such as ASTM D86.
- Barometric Correction: Temperature readings are corrected to standard atmospheric pressure to ensure consistent results.
Applications
ASTM D7345-23 is used industry-wide for rapid and accurate assessment of distillation (volatility) characteristics in:
- Petroleum Refining and Production: Monitoring of fractionation processes, quality control of fuel blends, and ensuring compliance with commercial and regulatory specifications.
- Product Quality Assurance: Fast screening of fuels and solvents for impurities, adulteration, or contamination-crucial in transportation and storage operations.
- Automotive and Aviation Industries: Evaluation of gasoline and kerosene volatility parameters, influencing cold start, warm-up, vapor lock tendency, and deposit formation in engines.
- Environmental Compliance: Supports adherence to environmental regulations regarding fuel composition and volatility emissions.
- Field and Laboratory Testing: Compact, automated apparatus enables efficient laboratory and portable field testing with minimal sample volume, suited for on-site analysis and rapid decision-making.
- Contractual and Specification Purposes: Determining compliance with product contract agreements and international fuel standards through reliable distillation profiling.
Related Standards
ASTM D7345-23 references and aligns with several key standards to provide comprehensive and harmonized test procedures:
- ASTM D86: Standard Test Method for Distillation of Petroleum Products at Atmospheric Pressure – the primary reference method for distillation analysis.
- ASTM D323: Test Method for Vapor Pressure of Petroleum Products (Reid Method).
- ASTM D4057 / D4177: Practices for sampling of petroleum and petroleum products.
- ASTM D4953, D5190, D5191, D5482: Methods related to vapor pressure testing.
- ASTM D5854: Practice for mixing and handling of liquid samples.
- ASTM D6299 / D6300: Quality assurance and statistical assessment methods.
- ISO 17034 / ISO Guide 35: International standards for reference material producers and statistical certification.
- Energy Institute IP 69 / IP 394: Comparable international methods for vapour pressure.
Value and Benefits
Implementing ASTM D7345-23 in petroleum product testing delivers:
- Rapid Results with Small Samples: Efficient micro distillation using as little as 10 mL allows fast throughput and suitability for limited or valuable samples.
- Reduced Operator Error: Automation minimizes subjective influences, enhances precision, and improves laboratory productivity.
- Versatility: Broad applicability across multiple fuel types and industrial applications, with relevance for both field and lab settings.
- Regulatory Confidence: Clear, consistent correlation with established reference methods ensures reliability for specification and compliance testing.
Keywords: ASTM D7345-23, distillation test method, micro distillation, petroleum product volatility, liquid fuel analysis, automatic distillation apparatus, fuel quality control, ASTM D86 alternative, refinery process monitoring, field and lab petroleum testing.
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Frequently Asked Questions
ASTM D7345-23 is a standard published by ASTM International. Its full title is "Standard Test Method for Distillation of Petroleum Products and Liquid Fuels at Atmospheric Pressure (Micro Distillation Method)". This standard covers: SIGNIFICANCE AND USE 5.1 The distillation (volatility) characteristics of hydrocarbons and other liquids have an important effect on their safety and performance, especially in the case of fuels and solvents. The boiling range gives information on the composition, the properties, and the behavior of the fuel during storage and use. Volatility is the major determinant of the tendency of a hydrocarbon mixture to produce potentially explosive vapors. 5.2 The distillation characteristics are critically important for both automotive and aviation gasolines, affecting starting, warm-up, and tendency to vapor lock at high operating temperature or at high altitude, or both. The presence of high boiling point components in these and other fuels can significantly affect the degree of formation of solid combustion deposits. 5.3 Distillation limits are often included in petroleum product specifications, in commercial contract agreements, process refinery/control applications, and for compliance to regulatory rules. 5.4 This test method can be applied to contaminated products or hydrocarbon mixtures. This is valuable for fast product quality screening, refining process monitoring, fuel adulteration control, or other purposes including use as a portable apparatus for field testing. 5.5 This test method uses an automatic micro distillation apparatus, provides fast results using small sample volume, and eliminates much of the operator time and subjectivity in comparison to Test Method D86. SCOPE 1.1 This test method covers a procedure for determination of the distillation characteristics of petroleum products and liquid fuels having boiling range between 20 °C to 400 °C at atmospheric pressure using an automatic micro distillation apparatus. 1.2 This test method is applicable to such products as; light and middle distillates, automotive spark-ignition engine fuels, automotive spark-ignition engine fuels containing up to 20 % ethanol, aviation gasolines, aviation turbine fuels, regular and low sulfur diesel fuels, biodiesel (B100), biodiesel blends up to 20 % biodiesel, special petroleum spirits, naphthas, white spirits, kerosines, burner fuels, and marine fuels. 1.3 The test method is also applicable to hydrocarbons with a narrow boiling range, like organic solvents or oxygenated compounds. 1.4 The test method is designed for the analysis of distillate products; it is not applicable to products containing appreciable quantities of residual material. 1.5 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard. 1.6 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. 1.7 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.
SIGNIFICANCE AND USE 5.1 The distillation (volatility) characteristics of hydrocarbons and other liquids have an important effect on their safety and performance, especially in the case of fuels and solvents. The boiling range gives information on the composition, the properties, and the behavior of the fuel during storage and use. Volatility is the major determinant of the tendency of a hydrocarbon mixture to produce potentially explosive vapors. 5.2 The distillation characteristics are critically important for both automotive and aviation gasolines, affecting starting, warm-up, and tendency to vapor lock at high operating temperature or at high altitude, or both. The presence of high boiling point components in these and other fuels can significantly affect the degree of formation of solid combustion deposits. 5.3 Distillation limits are often included in petroleum product specifications, in commercial contract agreements, process refinery/control applications, and for compliance to regulatory rules. 5.4 This test method can be applied to contaminated products or hydrocarbon mixtures. This is valuable for fast product quality screening, refining process monitoring, fuel adulteration control, or other purposes including use as a portable apparatus for field testing. 5.5 This test method uses an automatic micro distillation apparatus, provides fast results using small sample volume, and eliminates much of the operator time and subjectivity in comparison to Test Method D86. SCOPE 1.1 This test method covers a procedure for determination of the distillation characteristics of petroleum products and liquid fuels having boiling range between 20 °C to 400 °C at atmospheric pressure using an automatic micro distillation apparatus. 1.2 This test method is applicable to such products as; light and middle distillates, automotive spark-ignition engine fuels, automotive spark-ignition engine fuels containing up to 20 % ethanol, aviation gasolines, aviation turbine fuels, regular and low sulfur diesel fuels, biodiesel (B100), biodiesel blends up to 20 % biodiesel, special petroleum spirits, naphthas, white spirits, kerosines, burner fuels, and marine fuels. 1.3 The test method is also applicable to hydrocarbons with a narrow boiling range, like organic solvents or oxygenated compounds. 1.4 The test method is designed for the analysis of distillate products; it is not applicable to products containing appreciable quantities of residual material. 1.5 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard. 1.6 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. 1.7 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.
ASTM D7345-23 is classified under the following ICS (International Classification for Standards) categories: 75.180.20 - Processing equipment. The ICS classification helps identify the subject area and facilitates finding related standards.
ASTM D7345-23 has the following relationships with other standards: It is inter standard links to ASTM D7345-17, ASTM D6708-24, ASTM D6300-24, ASTM D86-23ae1, ASTM D6300-23a, ASTM D86-23a, ASTM D86-23, ASTM D6708-21, ASTM D7467-23, ASTM D4814-23a, ASTM D975-23a, ASTM D6751-23a, ASTM D2880-23, ASTM E3050-22, ASTM D396-21. Understanding these relationships helps ensure you are using the most current and applicable version of the standard.
ASTM D7345-23 is available in PDF format for immediate download after purchase. The document can be added to your cart and obtained through the secure checkout process. Digital delivery ensures instant access to the complete standard document.
Standards Content (Sample)
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.
Designation: D7345 − 23
596/17 (21)
Standard Test Method for
Distillation of Petroleum Products and Liquid Fuels at
1,2
Atmospheric Pressure (Micro Distillation Method)
This standard is issued under the fixed designation D7345; 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.
1. Scope* 1.7 This international standard was developed in accor-
dance with internationally recognized principles on standard-
1.1 This test method covers a procedure for determination
ization established in the Decision on Principles for the
of the distillation characteristics of petroleum products and
Development of International Standards, Guides and Recom-
liquid fuels having boiling range between 20 °C to 400 °C at
mendations issued by the World Trade Organization Technical
atmospheric pressure using an automatic micro distillation
Barriers to Trade (TBT) Committee.
apparatus.
2. Referenced Documents
1.2 This test method is applicable to such products as; light
and middle distillates, automotive spark-ignition engine fuels,
2.1 All standards are subject to revision, and parties to
automotive spark-ignition engine fuels containing up to 20 %
agreement on this test method are to apply the most recent
ethanol, aviation gasolines, aviation turbine fuels, regular and
edition of the standards indicated below, unless otherwise
low sulfur diesel fuels, biodiesel (B100), biodiesel blends up to
specified, such as in contractual agreements or regulatory rules
20 % biodiesel, special petroleum spirits, naphthas, white
where earlier versions of the method(s) identified may be
spirits, kerosines, burner fuels, and marine fuels.
required.
1.3 The test method is also applicable to hydrocarbons with
2.2 ASTM Standards:
a narrow boiling range, like organic solvents or oxygenated
D86 Test Method for Distillation of Petroleum Products and
compounds.
Liquid Fuels at Atmospheric Pressure
D323 Test Method for Vapor Pressure of Petroleum Products
1.4 The test method is designed for the analysis of distillate
(Reid Method)
products; it is not applicable to products containing appreciable
D1160 Test Method for Distillation of Petroleum Products at
quantities of residual material.
Reduced Pressure
1.5 The values stated in SI units are to be regarded as
D4057 Practice for Manual Sampling of Petroleum and
standard. No other units of measurement are included in this
Petroleum Products
standard.
D4175 Terminology Relating to Petroleum Products, Liquid
1.6 This standard does not purport to address all of the Fuels, and Lubricants
safety concerns, if any, associated with its use. It is the
D4177 Practice for Automatic Sampling of Petroleum and
responsibility of the user of this standard to establish appro- Petroleum Products
priate safety, health, and environmental practices and deter-
D4953 Test Method for Vapor Pressure of Gasoline and
mine the applicability of regulatory limitations prior to use. Gasoline-Oxygenate Blends (Dry Method)
D5190 Test Method for Vapor Pressure of Petroleum Prod-
ucts (Automatic Method) (Withdrawn 2012)
D5191 Test Method for Vapor Pressure of Petroleum Prod-
This test method is under the jurisdiction of ASTM International Committee
ucts and Liquid Fuels (Mini Method)
D02 on Petroleum Products, Liquid Fuels, and Lubricants and is the direct
responsibility of ASTM Subcommittee D02.08 on Volatility. The technically
D5482 Test Method for Vapor Pressure of Petroleum Prod-
equivalent standard as referenced is under the jurisdiction of the Energy Institute
ucts and Liquid Fuels (Mini Method—Atmospheric)
Subcommittee SC-B-9.
Current edition approved Dec. 1, 2023. Published January 2024. Originally
approved in 2007. Last previous edition approved in 2017 as D7345 – 17. DOI: For referenced ASTM standards, visit the ASTM website, www.astm.org, or
10.1520/D7345-23. contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
This test method has been developed through the cooperative effort between Standards volume information, refer to the standard’s Document Summary page on
ASTM and the Energy Institute, London. ASTM and IP standards were approved by the ASTM website.
ASTM and EI technical committees as being technically equivalent but that does not The last approved version of this historical standard is referenced on
imply both standards are identical. www.astm.org.
*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
D7345 − 23
D5854 Practice for Mixing and Handling of Liquid Samples 3.2.5 initial boiling point (IBP), n—corrected temperature
of Petroleum and Petroleum Products readings that corresponds to the instant of the flask internal
D6299 Practice for Applying Statistical Quality Assurance pressure rise registered by automatic apparatus.
and Control Charting Techniques to Evaluate Analytical
3.2.6 liquid temperature, n—temperature of the liquid speci-
Measurement System Performance
men in the distillation flask during the test obtained by a liquid
D6300 Practice for Determination of Precision and Bias
temperature measuring device of automatic apparatus.
Data for Use in Test Methods for Petroleum Products,
3.2.7 percent evaporated, n—percent recovered corrected to
Liquid Fuels, and Lubricants
a predicted by automatic analyzer evaporation loss percent.
D6708 Practice for Statistical Assessment and Improvement
Percent evaporated is automatically reported for ASTM 7C
of Expected Agreement Between Two Test Methods that
thermometer correlation.
Purport to Measure the Same Property of a Material
3.2.8 percent recovered, n—volume percent automatically
2.3 Energy Institute Standards:
reported by the analyzer; expressed as a percentage of the
IP 69 Petroleum Products—Determination of Vapour
charge volume, associated with a simultaneous temperature
Pressure—Reid Method
readings. Percent recovered is reported for ASTM 8C ther-
IP 394 Liquid Petroleum Products—Vapour Pressure—Part
mometer correlation.
1: Determination of Air Saturated Vapour Pressure
(ASVP)
3.2.9 percent recovery, n—percent recovery predicted by the
2.4 ISO Standards:
automatic apparatus and expressed as a percentage of the
ISO 17034 General Requirements for the Competence of charge volume.
Reference Material Producers
3.2.10 percent residue, n—volume of residue in the distil-
Guide 35 Reference Materials—Guidance for characteriza-
lation flask predicted by the automatic apparatus and expressed
tion and assessment of homogeneity and stability
as a percentage of the charge volume.
3.2.11 reference method, n—ASTM D86 test method or its
3. Terminology
analogs which is widely used for expression of the distillation
3.1 Definitions:
characteristics of petroleum products in industry.
3.1.1 For definitions of terms used in this test method, refer
3.2.12 temperature readings, n—vapor and liquid tempera-
to Terminology D4175.
ture has through use of an algorithm of the automatic apparatus
3.2 Definitions of Terms Specific to This Standard:
been adjusted to mimic the same temperature lag and emergent
3.2.1 automatic apparatus, n—microprocessor-controlled
stem effects as would be seen when using an ASTM 7C/7F or
unit that performs the procedures of automatically controlling
8C/8F liquid-in-glass thermometer to determine the distillation
the evaporation of a liquid specimen under specific conditions
characteristics of the material under test by industry recognized
of this test method, collecting measurement data and convert-
reference method.
ing this data by patented algorithm in order to predict distilla-
tion results in correlation with industry recognized reference
3.2.13 vapor temperature, n—temperature of the vapors in
method.
the distillation flask during the test obtained by a vapor
3.2.2 corrected temperature reading, n— temperature temperature measuring device of automatic apparatus.
readings, as described in 3.2.12, corrected to 101.3 kPa
barometric pressure. 4. Summary of Test Method
3.2.3 end point (EP) or final boiling point (FBP),
4.1 A specimen of the sample is transferred into the distil-
n—maximum corrected temperature readings obtained during
lation flask, the distillation flask is placed into position on the
the test at the instant the flask internal pressure returns to the
automatic apparatus, and heat is applied to the bottom of the
initial pressure level registered by automatic apparatus.
distillation flask.
3.2.3.1 Discussion—This usually occurs after the evapora-
4.2 The automatic apparatus measures and records speci-
tion of all liquid from the bottom of the distillation flask. The
men vapor and liquid temperatures, and pressure in the
term maximum temperature is a frequently used synonym.
distillation flask as the sample gradually distills under atmo-
3.2.4 flask internal pressure, n—pressure within the distil-
spheric pressure conditions. Automatic recordings are made
lation flask obtained during the test by a differential pressure
throughout the distillation and the data stored into the appara-
sensor of automatic apparatus.
tus memory.
3.2.4.1 Discussion—The flask internal pressure data re-
4.3 At the conclusion of the distillation, the collected data is
corded during the test is automatically converted to the volume
treated by the data processing system, converted to distillation
percent recovered or evaporated data by patented algorithm
characteristics and corrected for barometric pressure.
employed by automatic apparatus.
4.4 Test results are commonly expressed as percent recov-
ered or evaporated versus corresponding temperature in com-
Available from Energy Institute, 61 New Cavendish St., London, WIG 7AR,
pliance with industry recognized standard form and reference
U.K., http://www.energyinst.org.uk.
method either in a table or graphically, as a plot of the
Available from International Organization for Standardization (ISO), 1 rue de
Varembé, Case postale 56, CH-1211, Geneva 20, Switzerland, http://www.iso.ch. distillation curve.
D7345 − 23
5. Significance and Use 6.3.2 (Warning—Do not take readings from ordinary aner-
oid barometers, such as those used at weather stations and
5.1 The distillation (volatility) characteristics of hydrocar-
airports, since these are precorrected to give sea level read-
bons and other liquids have an important effect on their safety
ings.)
and performance, especially in the case of fuels and solvents.
6.4 Sampling Device—Glass or plastics syringe capacity
The boiling range gives information on the composition, the
properties, and the behavior of the fuel during storage and use. 10 mL 6 0.3 mL or constant volume dispenser capacity 10 mL
6 0.3 mL.
Volatility is the major determinant of the tendency of a
hydrocarbon mixture to produce potentially explosive vapors.
6.5 Waste Beaker—Glass approximately 200 mL capacity,
outside diameter approximately 70 mm and height approxi-
5.2 The distillation characteristics are critically important
mately 130 mm fitted with a cover to reduce evaporation. The
for both automotive and aviation gasolines, affecting starting,
cover design shall allow the beaker to remain open to atmo-
warm-up, and tendency to vapor lock at high operating
spheric pressure.
temperature or at high altitude, or both. The presence of high
boiling point components in these and other fuels can signifi-
7. Reagents and Materials
cantly affect the degree of formation of solid combustion
deposits.
7.1 Cleaning Solvents, suitable for cleaning and drying the
test flask such as; petroleum naphtha and acetone. (Warning—
5.3 Distillation limits are often included in petroleum prod-
Flammable. Liquid causes eye burns. Vapor harmful. May be
uct specifications, in commercial contract agreements, process
fatal or cause blindness if swallowed or inhaled.)
refinery/control applications, and for compliance to regulatory
rules.
7.2 Toluene, 99.5 % purity. (Warning—Extremely flam-
mable. Harmful if inhaled. Skin irritant on repeated contact.
5.4 This test method can be applied to contaminated prod-
Aspiration hazard.)
ucts or hydrocarbon mixtures. This is valuable for fast product
quality screening, refining process monitoring, fuel adultera- 7.3 n-Hexadecane, 99 % purity. (Warning—Extremely
tion control, or other purposes including use as a portable flammable. Harmful if inhaled. Skin irritant on repeated
apparatus for field testing. contact. Aspiration hazard.)
5.5 This test method uses an automatic micro distillation 7.4 Chemicals of at least 99 % purity shall be used in the
calibration procedure (see 10.2). Unless otherwise indicated, it
apparatus, provides fast results using small sample volume, and
eliminates much of the operator time and subjectivity in is intended that all reagents conform to the specifications of the
Committee on Analytical Reagents of the American Chemical
comparison to Test Method D86.
Society.
6. Apparatus
7.5 Granular Pumice Stones, clean and dry fine grade
pumice stones of diameter 0.8 mm to 3.0 mm, approximately
6.1 Basic Components of the Automatic Apparatus:
10 grains are necessary for each test.
6.1.1 The basic components of the micro distillation unit are
the distillation flask, a condensate recovery area with waste
7.6 Sample Drying Agent—Anhydrous sodium sulfate has
beaker, an enclosure for the distillation flask with the heat
been found to be suitable.
source and flask support, the specimen liquid temperature
measuring device, the specimen vapor temperature measuring 8. Sampling, Storage, and Sample Conditioning
device, the distillation flask internal pressure measuring device,
8.1 Sampling:
the ambient pressure measuring device, the control systems for
8.1.1 The extreme sensitivity of volatility measurements to
regulating the distillation process, and the data processing
losses through evaporation and the resulting changes in com-
system for converting recorded information into typical indus-
position is such as to require the utmost precaution in the
try recognized standard report form.
drawing and handling of volatile product samples.
8.1.2 Obtain a sample and test specimen in accordance with
6.2 A detailed description of the apparatus is given in Annex
Practice D4057, D4177, or D5854 when appropriate. At least
A1.
50 mL of sample is recommended.
6.3 Barometer for Calibration—A pressure measuring de-
8.1.3 Sample shall be free from any suspended solids or
vice capable of measuring local station pressure with an
other insoluble contaminations. Obtain another sample or
accuracy of 0.1 kPa (1 mmHg) or better, at the same elevation
remove solid particle by filtration. During filtration operation
relative to sea level where the apparatus is located.
take care to minimize any loss of light ends.
6.3.1 The barometer is only required for periodic calibration
8.2 Sample Storage:
of the external and internal pressure measuring devices.
ACS Reagent Chemicals, Specifications and Procedures for Reagents and
The sole source of supply of the apparatus known to the committee at this time Standard-Grade Reference Materials, American Chemical Society, Washington,
is ISL /PAC, B.P. 70285 Verson, 14653 CARPIQUET – FRANCE. If you are aware DC. For suggestions on the testing of reagents not listed by the American Chemical
of alternative suppliers, please provide this information to ASTM International Society, see Analar Standards for Laboratory Chemicals, BDH Ltd., Poole, Dorset,
Headquarters. Your comments will receive careful consideration at a meeting of the U.K., and the United States Pharmacopeia and National Formulary, U.S. Pharma-
responsible technical committee, which you may attend. copeial Convention, Inc. (USPC), Rockville, MD.
D7345 − 23
8.2.1 All samples shall be stored in a tightly closed and 10.3.1 Certified Reference Material (CRM)—CRM is a
leak-free container away from direct sunlight or sources of stable mixture of hydrocarbon or other stable petroleum
direct heat. product with a method-specific distillation characteristic estab-
8.2.2 Protect samples containing light materials having lished by a method-specific interlaboratory study following
expected initial boiling point lower than 100 °C from excessive Practice D6300 or ISO 17034 and Guide 35. Suppliers of
temperatures prior to testing. This can be accomplished by CRMs will provide certificates stating the method-specific
storage of the sample container in an appropriate ice bath or distillation characteristic for each material of the current
refrigerator at a temperature below 10 °C. Other samples can production batch.
be stored at ambient or lower temperature.
10.3.2 Secondary Working Standard (SWS)—SWS is a
8.2.3 If the sample has partially or completely solidified stable mixture of pure hydrocarbons, or other petroleum
during storage, it is to be carefully heated to a temperature
product whose composition is known to remain appreciably
when it is completely fluid. It shall be vigorously shaken after stable. Establish the mean value of control points and the
melting, prior to opening the sample container, to ensure
statistical control limits for the SWS using standard statistical
homogeneity. techniques. See Practice D6299.
8.3 Wet Samples:
11. Calibration
8.3.1 Samples of materials that visibly contain water are not
suitable for testing by this test method. If the sample is not dry,
11.1 Follow the manufacturer’s instructions for verifying
obtain another sample that is free from suspended water.
the correct operation of the apparatus.
8.3.2 If such a sample cannot be obtained, remove any free
11.2 Temperature Measurement System—At intervals of not
water by placing approximately 30 mL of the sample to be
more than six months or after the system has been replaced or
tested in a glass conical flask containing approximately 10 g of
repaired, or both, following the apparatus instruction manual,
the drying agent. Stopper and shake gently. Allow the mixture
check the calibration of the liquid and vapor temperature
to settle for approximately 15 min. Once the sample shows no
measuring sensors by distilling of pure compounds, like
visible signs of water, use a decanted portion of the sample for
toluene and n-hexadecane.
the analysis. It is recommended to filter the test portion from
NOTE 2—The melting point of n-hexadecane is 18 °C. If the sample is
the residual or suspended drying agent. During this drying and
solid, heat it to about 25 °C and wait until all the material is liquid before
filtration operations take care to minimize any loss of light
starting the test.
ends. Report that the sample has been dried by the addition of
11.3 External Pressure Measuring Device—At intervals of
a drying agent.
not more than six months, or after the system has been replaced
or repaired, or both, the external pressure measuring device
9. Preparation of Apparatus
reading of the apparatus shall be verified against a barometer,
9.1 Install the analyzer for operation in accordance with the
as described in 6.3.
manufacturer’s instructions.
11.4 Differential Pressure Measuring Device—At intervals
9.2 This instrument shall be located away from direct
of not more than six months, or after the system has been
sunlight, sources of direct heat or air draft.
replaced or repaired, or both, the differential pressure measur-
9.3 Turn on the main power switch of the analyzer.
ing device reading of the apparatus shall be verified in
accordance with the manufacturer’s instructions.
10. Verification Quality Control Checks
10.1 To verify the temperature measurement system, distill
12. Procedure
high purity toluene in accordance with this test method and
12.1 Material with an Initial Boiling Point of 100 °C and
comparing the temperature reading at 50 % distilled. If the
Below—Bring the temperature of the sample and container to a
temperature reading differs more than 0.5 °C from the expected
temperature at least 10 °C below the expected initial boiling
temperature of 109.3 °C (see Note 1), then check the instru-
point of the material before opening the sample container.
ment calibration (see Section 11).
12.2 Material with a Boiling Point above 100 °C—Bring the
10.2 To verify the temperature measurement system at
sample and its container to ambient temperature. If the sample
elevated temperatures, use n-hexadecane and record the tem-
has partially or completely solidified during storage warm until
perature at 50 % distilled. If the temperature reading differs
fluid, then mix by gentle shaking.
more than 1.0 °C from the expected temperature of 278.6 °C
NOTE 3—Not respecting the requirements given in 12.1 can lead to
(see Note 1, then check the instrument calibration (see Section
improper IBP detection on samples containing volatile materials. If
11).
expected initial boiling point of the sample to be tested is unknown, it is
NOTE 1—These temperatures are those that would be obtained if the
advised to make a test at ambient conditions. If the distillation result
toluene and hexadecane were distilled using Test Method D86 and are not
shows that the requirements of 12.1 were not respected, discard the result
the figures that are given as the boiling points of these materials in
and repeat the test strictly respecting the conditions.
literature.
12.3 Ensure that the distillation measuring head of auto-
10.3 Verification of apparatus performance under dynamic
matic apparatus has been allowed to reach ambient temperature
conditions and wide temperature range can be done by distil-
and that any residual condensate has been removed.
lation of a Certified Reference Material (CRM) or Secondary
Working Standard (SWS). 12.4 Check that the distillation flask is clean and dry.
D7345 − 23
12.5 Place at least 10 grains of clean and dry granular 13.1.1 If required, the percent loss is calculated by the
pumice stones into the distillation flask. Some apparatus supply following equation:
a suitable boiling stone dispenser. When the sample is biodiesel
loss % 5 100 2 percent recovery1percent residue (1)
~ !
(B100), do not use any pumice stones.
13.2 Report all volumetric percentages to the nearest 0.1 %
12.6 Measure 10 mL 6 0.3 mL test portion using the
(V/V).
sampling device (see Section 6). When the sample is biodiesel
13.3 Report all temperature readings to the nearest 0.1 °C
(B100), measure 5 mL 6 0.3 mL test portion. Check for the
(see Note 3).
presence of any bubbles and if present discard the test portion
and refill with bubble free material. Transfer the bubble free 13.4 Report if a drying agent, as described in 8.3.2, was
used.
test portion to the prepared distillation flask, taking care that
none of the liquid flows into the vapor tube.
13.5 The test report shall contain at least the following
NOTE 4—Use new disposable syringe or disposable dispenser tip for
information:
each new sampling to avoid any products cross contamination which can
13.5.1 Sufficient details for complete identification of the
cause erroneous distillation results.
product tested;
12.7 Fit the distillation measurement head into its position
13.5.2 A reference to this standard;
on the distillation flask securely in accordance with the
13.5.3 The result of the test;
manufacturer’s instructions.
13.5.4 Any deviation, by agreement or otherwise, from the
12.8 Place the distillation flask into the heating enclosure
procedure specified; and
and insert the sidearm of the distillation flask into the sealing
13.5.5 The date of the test.
of the condenser tube, while also attaching the measurement
14. Precision and Bias
head holder.
14.1 Precision—The precision of this test method as deter-
12.9 Position the heating source/flask support around the
9-11
mined by the statistical examination of the interlaboratory
lower section of the distillation flask.
test results is as follows:
12.10 Close heating enclosure by positioning the protection
NOTE 6—Typically samples for distillation are classified according to a
shield to its position.
Group number (see Test Method D86). However, this test method does not
12.11 Check that a waste collection beaker is placed under
require this classification, but for the purposes of precision and between-
method reproducibility comparisons, the precisions and bias have been
the projecting lower end of the condenser tube. Ensure that the
derived according to the group number in the following fashion. Group 1,
waste collection beaker remains open to atmospheric pressure.
2, and 3 samples are labeled as NOT4, and Group 4 samples are labeled
NOTE 5—Monitor that the liquid level in the waste beaker does not
GRP4. See Appendix X1 for further information on typical samples and
exceed two thirds of its total capacity and drain it on periodic intervals.
group classification.
12.12 Without delay initiate the distillation process accord-
NOTE 7—Information on the precision of % evaporated or % recovered
at a prescribed temperature can be found in Annex A4.
ing to the apparatus manufacturer’s instructions.
12.12.1 From this point up to and including the termination
14.1.1 Repeatability—The difference between successive
of the measurement, the apparatus automatically controls all
test results, obtained by the same operator using the same
operations. The instrument applies heating to the specimen and
apparatus under constant operating conditions on identical test
regulates automatically heating power during the distillation
material, would in the long run, in the normal and correct
run using specimen liquid temperature data. The distillation
operation of this test method, exceed the following only in one
conditions; distillation flask internal pressure, specimen liquid
case in twenty.
temperature, and specimen vapor temperature are automati-
Group NOT4:
cally measured and recorded during the test by the control
IBP: r = 3.3 valid range: 20 °C – 50 °C
E5/E10: r = 1.1 valid range: 25 °C – 65 °C
system. The distillation is automatically terminated when the
E20: r = 1.2 valid range: 40 °C – 70 °C
flask internal pressure returns to its initial pressure level. The
E30: r = 1.8 valid range: 50 °C – 85 °C
collected test data is automatically processed and reported on E40: r = 2.7 valid range: 55 °C – 100 °C
E50: r = 2.4 valid range: 60 °C – 120 °C
the display and printed out at the conclusion of the test run. The
E60: r = 2.4 valid range: 75 °C – 125 °C
heating enclosure cooling fan is automatically activated.
E70: r = 1.8 valid range: 100 °C – 140 °C
E80: r = 2.1 valid range: 115 °C – 160 °C
12.13 Record the test data.
E90/E95: r = 2.0 valid range: 140 °C – 200 °C
FBP: r = 3.0 valid range: 140 °C – 260 °C
12.14 Allow the distillation flask to cool and remove it from
the apparatus.
13. Report
Supporting data have been filed at ASTM International Headquarters and may
be obtained by requesting Research Report RR:D02-1621. Contact ASTM Customer
13.1 In cases in which no specific data requirements have
Service at service@astm.org.
been set by the operator, corrected temperatures readings
Supporting data have been filed at ASTM International Headquarters and may
be obtained by requesting Research Report RR:D02-1831. Contact ASTM Customer
versus corresponding percent recovered or evaporated are
Service at service@astm.org.
typically reported by the apparatus. Report typically contains
Supporting data have been filed at ASTM International Headquarters and may
the IBP, FBP, 5 %, 95 % and each 10 % increment from 10 %
be obtained by requesting Research Report RR:D02-2067. Contact ASTM Customer
to 90 %, as well as percent recovery and percent residue. Service at service@astm.org.
D7345 − 23
IBP:
Group GRP4: Refer to Annex A2 for tables of calculated repeatability.
IBP: r = 3.9 valid range: 145 °C – 195 °C
NOT4
T5: r = T × 0.01194 valid range: 175 °C – 250 °C
The degree of agreement between results from Test Method D7345 and Test
T10: r = T × 0.00954 valid range: 160 °C – 265 °C
Method D86 (automated) can be further improved by applying the bias-
T20: r = T × 0.00932 valid range: 180 °C – 275 °C
correction outlined in Eq 2. Sample-specific bias, as defined in Practice D6708,
T30: r = T × 0.00782 valid range: 190 °C – 285 °C
was observed for some samples after applying the bias-correction.
T40: r = T × 0.00822 valid range: 200 °C – 290 °C
T50: r = T × 0.00614 valid range: 170 °C – 295 °C
T60: r = T × 0.00534 valid range: 220 °C – 305 °C
Bias-corrected X 5 predicted Y 5 X11.42 °C (2)
T70: r = T × 0.00405 valid range: 230 °C – 315 °C
T80: r = T × 0.00441 valid range: 240 °C – 325 °C
T90: r = T × 0.0041 valid range: 180 °C – 340 °C
where:
T95: r = 2.03 valid range: 260 °C – 360 °C
X = result obtained by Test Method D7345 (this test method), and bias-
FBP: r = 3.93 valid range: 195 °C – 365 °C
corrected X = predicted Y = result that would have been obtained by Test
where:
Method D86 (automated) on the same sample.
E = evaporated temperature at x percent within valid range prescribed (°C)
T = recovered temperature at x percent within valid range prescribed (°C)
Differences between bias-corrected results from Eq 2 and Test Method D86, for
the sample types and property ranges studied, are expected to exceed the fol-
NOTE 8—For naphthas, solvents, and other similar materials where
lowing between-method reproducibility (R ), as defined in Practice D6708,
xy
2 2 0.5
percent recovered is reported and the percent loss is typically less than one
about 5 % of the time. R (°C) = (0.629 RX + 0.629 RY )
xy
percent, the percent recovered temperatures can be considered identical to
where:
the percent evaporated temperatures, and precision can be calculated as
RX = reproducibility of Test Method D7345 (this test method)
shown for Group NOT4.
RY = reproducibility of Test Method D86 (automated)
14.1.2 Reproducibility—The difference between two single
GRP4
and independent test results, obtained by different operators
No bias-correction considered in Practice D6708 can further improve agreement
working in different laboratories on identical test material,
between results from Test Method D7345 and Test Method D86 (automated), for
sample types and property ranges studied. Sample-specific bias, as defined in
would in the long run, in normal and correct operation of this
Practice D6708, was observed for some samples.
test method, exceed the following only in one case in twenty.
Differences between results from Test Method D7345 and Test Method D86
Group NOT4:
(automated), for the sample types and property ranges studied, are expected to
IBP: R = 5.9 valid range: 20 °C – 50 °C
exceed the following between-method reproducibility (R ), as defined in Prac-
E5/E10: R = 2.5 valid range: 25 °C – 65 °C xy
tice D6708, about 5 % of the time.
E20: R = 2.2 valid range: 40 °C – 70 °C
E30: R = 2.6 valid range: 50 °C – 85 °C
Group GRP4: Refer to Annex A3.
E40: R = 3.6 valid range: 55 °C – 100 °C
E50: R = 4.1 valid range: 60 °C – 120 °C
T5:
E60: R = 4.5 valid range: 75 °C – 125 °C
E70: R = 3.5 valid range: 100 °C – 140 °C
NOT4
E80: R = 3.7 valid range: 115 °C – 160 °C
The degree of agreement between results from Test Method D7345 and Test
E90/E95: R = 5.8 valid range: 140 °C – 200 °C
Method D86 (automated) can be further improved by applying the bias-
FBP: R = 5.7 valid range: 175 °C – 220 °C
correction outlined in Eq 3. Sample-specific bias, as defined in Practice D6708,
was observed for some samples after applying the bias-correction.
Group GRP4: Refer to Annex A2 for tables of calculated reproducibility.
IBP: R = 6.0 valid range: 145 °C – 195 °C
T5: R = T × 0.0172 valid range: 175 °C – 250 °C
Bias-corrected X = predicted Y = 0.82 X + 11.25 °C (3)
T10: R = T × 0.0177 valid range: 160 °C – 265 °C
T20: R = T × 0.0117 valid range: 180 °C – 275 °C
T30: R = T × 0.0122 valid range: 190 °C – 285 °C
Differences between results from Test Method D7345 and Test Method D86
T40: R = T × 0.0122 valid range: 200 °C – 290 °C
(automated), for the sample types and property ranges studied, are expected to
T50: R = T × 0.0103 valid range: 170 °C – 295 °C
exceed the following between-method reproducibility (R ), as defined in Prac-
xy
T60: R = T × 0.0092 valid range: 220 °C – 305 °C 2 2 0.5
tice D6708, about 5 % of the time. R (°C) = (0.995 RX + 1.468 RY )
xy
T70: R = T × 0.0084 valid range: 230 °C – 315 °C
T80: R = T × 0.0084 valid range: 240 °C – 325 °C
where:
T90: R = T × 0.0081 valid range: 180 °C – 340 °C
RX = reproducibility of Test Method D7345 (this test method)
T95 R = 3.23 valid range: 260 °C – 360 °C
RY = reproducibility of Test Method D86 (automated)
FBP: R = 7.7 valid range: 195 °C – 365 °C
where:
GRP4
E = evaporated temperature at x percent within valid range prescribed (°C)
The degree of agreement between results from Test Method D7345 and Test
T = recovered temperature at x percent within valid range prescribed (°C)
Method D86 (automated) can be further improved by applying the bias-
correction outlined in Eq 4. Sample-specific bias, as defined in Practice D6708,
NOTE 9—See Note 8.
was observed for some samples after applying the bias-correction.
14.2 Bias—Since there is no accepted reference material
Bias-corrected X = predicted Y = 1.1 X 2 18.43 °C (4)
suitable for determining the bias for the procedure in this Test
Method, bias has not been determined.
where:
X = result obtained by Test Method D7345 (this test method), and bias-
14.3 Between-Method Bias—The Degree of Agreement be-
corrected X = predicted Y = result that would have been obtained by Test
tween results by Test Method D7345 and Test Method D86
Method D86 (automated) on the same sample.
(automated)—Results on the same materials produced by Test
Method D7345 and Test Method D86 have been assessed in
9-11
accordance with procedures outlined in Practice D6708.
The findings are:
D7345 − 23
Differences between bias-corrected results from Eq 4 and Test Method D86, for where:
the sample types and property ranges studied, are expected to exceed the fol- X = result obtained by Test Method D7345 (this test method), and bias-
lowing between-method reproducibility (R ), as defined in Practice D6708, corrected X = predicted Y = result that would have been obtained by Test
xy
about 5 % of the time. Method D86 (automated) on the same sample.
Group GRP4: Refer to Annex A3. Differences between bias-corrected results from Eq 8 and Test Method D86, for
the sample types and property ranges studied, are expected to exceed the fol-
lowing between-method reproducibility (R ), as defined in Practice D6708,
T10: xy
about 5 % of the time.
NOT4
The degree of agreement between results from Test Method D7345 and Test
Group GRP4: Refer to Annex A3.
Method D86 (automated) can be further improved by applying the bias-
correction outlined in Eq 5. Sample-specific bias, as defined in Practice D6708,
T30:
was observed for some samples after applying the bias-correction.
No bias-correction considered in Practice D6708 can further improve the agree-
ment between results from Test Method D7345 and Test Method D86 (auto-
Bias-corrected X = predicted Y = 0.82 X + 11.1 °C (5)
mated) for the material types and property ranges studied. Sample-specific bias,
as defined in Practice D6708, was observed for some samples.
Differences between results from Test Method D7345 and Test Method D86
Differences between results from Test Method D7345 and Test Method D86
(automated), for the sample types and property ranges studied, are expected to
(automated), for the sample types and property ranges studied, are expected to
exceed the following between-method reproducibility (R ), as defined in Prac-
xy exceed the following between-method reproducibility (R ), as defined in Prac-
xy
2 2 0.5
2 2 0.5
tice D6708, about 5 % of the time. R (°C) = (1.078 RX + 1.618 RY )
xy tice D6708, about 5 % of the time. R (°C) = (1.468 RX + 1.468 RY )
xy
where:
where:
RX = reproducibility of Test Method D7345 (this test method)
RX = reproducibility of Test Method D7345 (this test method)
RY = reproducibility of Test Method D86 (automated)
RY = reproducibility of Test Method D86 (automated)
GRP4
GRP4
The degree of agreement between results from Test Method D7345 and Test
The degree of agreement between results from Test Method D7345 and Test
Method D86 (automated) can be further improved by applying the bias-
Method D86 (automated) can be further improved by applying the bias-
correction outlined in Eq 6. Sample-specific bias, as defined in Practice D6708,
correction outlined in Eq 9. Sample-specific bias, as defined in Practice D6708,
was observed for some samples after applying the bias-correction.
was observed for some samples after applying the bias-correction.
Bias-corrected X 5 predicted Y 5 1.09 X 2 16.4 °C (6)
Bias-corrected X = predicted Y = 1.08X 2 18.5 °C (9)
where:
where:
X = result obtained by Test Method D7345 (this test method), and bias-
X = result obtained by Test Method D7345 (this test method), and bias-
corrected X = predicted Y = result that would have been obtained by Test
corrected X = predicted Y = result that would have been obtained by Test
Method D86 (automated) on the same sample.
Method D86 (automated) on the same sample.
Differences between bias-corrected results from Eq 9 and Test Method D86, for
Differences between bias-corrected results from Eq 6 and Test Method D86, for
the sample types and property ranges studied, are expected to exceed the fol-
the sample types and property ranges studied, are expected to exceed the fol-
lowing between-method reproducibility (R ), as defined in Practice D6708,
xy
lowing between-method reproducibility (R ), as defined in Practice D6708,
xy
about 5 % of the time.
about 5 % of the time.
Group GRP4: Refer to Annex A3.
Group GRP4: Refer to Annex A3.
T40:
T20:
No bias-correction considered in Practice D6708 can further improve the agree-
The degree of agreement between results from Test Method D7345 and Test
ment between results from Test Method D7345 and Test Method D86 (auto-
Method D86 (automated) can be further improved by applying the bias-
mated) for the material types and property ranges studied. Sample-specific bias,
correction outlined in Eq 7. Sample-specific bias, as defined in Practice D6708,
as defined in Practice D6708, was observed for some samples.
was observed for some samples after applying the bias-correction.
Differences between results from Test Method D7345 and Test Method D86
(automated), for the sample types and property ranges studied, are expected to
Bias-corrected X = predicted Y = X +0.96 °C (7)
exceed the following between-method reproducibility (R ), as defined in Prac-
xy
2 2 0.5
tice D6708, about 5 % of the time. R (°C) = (1.615 RX + 1.615 RY )
xy
Differences between results from Test Method D7345 and Test Method D86
where:
(automated), for the sample types and property ranges studied, are expected to
RX = reproducibility of Test Method D7345 (this test method)
exceed the following between-method reproducibility (R ), as defined in Prac-
xy
RY = reproducibility of Test Method D86 (automated)
2 2 0.5
tice D6708, about 5 % of the time. R (°C) = (1.905 RX + 1.905 RY )
xy
GRP4
where:
The degree of agreement between results from Test Method D7345 and Test
RX = reproducibility of Test Method D7345 (this test method)
Method D86 (automated) can be further improved by applying the bias-
RY = reproducibility of Test Method D86 (automated)
correction outlined in Eq 10. Sample-specific bias, as defined in Practice
D6708, was observed for some samples after applying the bias-correction.
GRP4
The degree of agreement between results from Test Method D7345 and Test
Method D86 (automated) can be further improved by applying the bias-
Bias-corrected X = predicted Y = 1.06 X 2 15.71 °C (10)
correction outlined in Eq 8. Sample-specific bias, as defined in Practice D6708,
was observed for some samples after applying the bias-correction.
where:
X = result obtained by Test Method D7345 (this test method), and bias-
corrected X = predicted Y = result that would have been obtained by Test
Bias-corrected X = predicted Y = 1.09 X 2 18.88 °C (8)
Method D86 (automated) on the same sample.
D7345 − 23
where:
Differences between bias-corrected results from Eq 10 and Test Method D86, X = result obtained by Test Method D7345 (this test method), and bias-
for the sample types and property ranges studied, are expected to exceed the corrected X = predicted Y = result that would have been obtained by Test
following between-method reproducibility (R ), as defined in Practice D6708, Method D86 (automated) on the same sample.
xy
about 5 % of the time.
Differences between bias-corrected results from Eq 13 and Test Method D86,
Group GRP4: Refer to Annex A3. for the sample types and property ranges studied, are expected to exceed the
following between-method reproducibility (R ), as defined in Practice D6708,
xy
about 5 % of the time.
T50:
NOT4
Group GRP4: Refer to Annex A3.
No bias-correction considered in Practice D6708 can further improve the agree-
ment between results from Test Method D7345 and Test Method D86 (auto-
T70:
mated) for the material types and property ranges studied. Sample-specific bias,
as defined in Practice D6708, was observed for some samples. The degree of agreement between results from Test Method D7345 and Test
Method D86 (automated) can be further improved by applying the bias-
Differences between results from Test Method D7345 and Test Method D86 correction outlined in Eq 14. Sample-specific bias, as defined in Practice
(automated), for the sample types and property ranges studied, are expected to
D6708, was observed for some samples after applying the bias-correction.
exceed the following between-method reproducibility (R ), as defined in Prac-
xy
2 2 0.5
tice D6708, about 5 % of the time. R (°C) = (3.219 RX + 3.219 RY )
xy
Bias-corrected X = predicted Y = 0.8X + 24.27 °C (14)
where:
RX = reproducibility of Test Method D7345 (this test method)
RY = reproducibility of Test Method D86 (automated) Differences between results from Test Method D7345 and Test Method D86
(automated), for the sample types and property ranges studied, are expected to
GRP4 exceed the following between-method reproducibility (R ), as defined in Prac-
xy
2 2 0.5
tice D6708, about 5 % of the time. R (°C) = (0.74 RX + 1.164 RY )
The degree of agreement between results from Test Method D7345 and Test
xy
Method D86 (automated) can be further improved by applying the bias-
correction outlined in Eq 11. Sample-specific bias, as defined in Practice D6708, where:
was observed for some samples after applying the bias-correction. RX = reproducibility of Test Method D7345 (this test method)
RY = reproducibility of Test Method D86 (automated)
Bias-corrected X 5 predicted Y 5 X 2 2.015 °C (11)
GRP4
The degree of agreement between results from Test Method D7345 and Test
Method D86 (automated) can be further improved by applying the bias-
where: correction outlined in Eq 15. Sample-specific bias, as defined in Practice
X = result obtained by Test Method D7345 (this test method), and bias-
D6708, was observed for some samples after applying the bias-correction.
corrected X = predicted Y = result that would have been obtained by Test
Method D86 (automated) on the same sample.
Bias-corrected X = predicted Y = X 2 1.79 °C (15)
Differences between bias-corrected results from Test Method D7345 and Test
where:
Method D86 (automated), for the sample types and property ranges studied, are
X = result obtained by Test Method D7345 (this test method), and bias-
expected to exceed the following between-method reproducibility (R ), as de-
xy
corrected X = predicted Y = result that would have been obtained by Test
fined in Practice D6708, about 5 % of the time.
Method D86 (automated) on the same sample.
Group GRP4: Refer to Annex A3.
Differences between bias-corrected results from Eq 15 and Test Method D86,
for the sample types and property ranges studied, are expected to exceed the
T60:
following between-method reproducibility (R ), as defined in Practice D6708,
xy
The degree of agreement between results from Test Method D7345 and Test about 5 % of the time.
Method D86 (automated) can be further improved by applying the bias-
correction outlined in Eq 12. Sample-sp
...
This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Because
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.
Designation: D7345 − 17 D7345 − 23
596/12596/17 (21)
Standard Test Method for
Distillation of Petroleum Products and Liquid Fuels at
1,2
Atmospheric Pressure (Micro Distillation Method)
This standard is issued under the fixed designation D7345; 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.
1. Scope*
1.1 This test method covers a procedure for determination of the distillation characteristics of petroleum products and liquid fuels
having boiling range between 20 °C to 400 °C at atmospheric pressure using an automatic micro distillation apparatus.
1.2 This test method is applicable to such products as; light and middle distillates, automotive spark-ignition engine fuels,
automotive spark-ignition engine fuels containing up to 20 % ethanol, aviation gasolines, aviation turbine fuels, regular and low
sulfur diesel fuels, biodiesel (B100), biodiesel blends up to 20 % biodiesel, special petroleum spirits, naphthas, white spirits,
kerosines, burner fuels, and marine fuels.
1.3 The test method is also applicable to hydrocarbons with a narrow boiling range, like organic solvents or oxygenated
compounds.
1.4 The test method is designed for the analysis of distillate products; it is not applicable to products containing appreciable
quantities of residual material.
1.5 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.6 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 and healthsafety, health, and environmental practices and determine
the applicability of regulatory limitations prior to use.
1.7 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.
2. Referenced Documents
2.1 All standards are subject to revision, and parties to agreement on this test method are to apply the most recent edition of the
standards indicated below, unless otherwise specified, such as in contractual agreements or regulatory rules where earlier versions
of the method(s) identified may be required.
This test method is under the jurisdiction of ASTM International Committee D02 on Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility
of ASTM Subcommittee D02.08 on Volatility. The technically equivalent standard as referenced is under the jurisdiction of the Energy Institute Subcommittee SC-B-9.
Current edition approved May 1, 2017Dec. 1, 2023. Published June 2017January 2024. Originally approved in 2007. Last previous edition approved in 20162017 as
D7345 – 16.D7345 – 17. DOI: 10.1520/D7345-17.10.1520/D7345-23.
This test method has been developed through the cooperative effort between ASTM and the Energy Institute, London. ASTM and IP standards were approved by ASTM
and EI technical committees as being technically equivalent but that does not imply both standards are identical.
*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
D7345 − 23
2.2 ASTM Standards:
D86 Test Method for Distillation of Petroleum Products and Liquid Fuels at Atmospheric Pressure
D323 Test Method for Vapor Pressure of Petroleum Products (Reid Method)
D1160 Test Method for Distillation of Petroleum Products at Reduced Pressure
D4057 Practice for Manual Sampling of Petroleum and Petroleum Products
D4175 Terminology Relating to Petroleum Products, Liquid Fuels, and Lubricants
D4177 Practice for Automatic Sampling of Petroleum and Petroleum Products
D4953 Test Method for Vapor Pressure of Gasoline and Gasoline-Oxygenate Blends (Dry Method)
D5190 Test Method for Vapor Pressure of Petroleum Products (Automatic Method) (Withdrawn 2012)
D5191 Test Method for Vapor Pressure of Petroleum Products and Liquid Fuels (Mini Method)
D5482 Test Method for Vapor Pressure of Petroleum Products and Liquid Fuels (Mini Method—Atmospheric)
D5854 Practice for Mixing and Handling of Liquid Samples of Petroleum and Petroleum Products
D6299 Practice for Applying Statistical Quality Assurance and Control Charting Techniques to Evaluate Analytical Measure-
ment System Performance
D6300 Practice for Determination of Precision and Bias Data for Use in Test Methods for Petroleum Products, Liquid Fuels, and
Lubricants
D6708 Practice for Statistical Assessment and Improvement of Expected Agreement Between Two Test Methods that Purport
to Measure the Same Property of a Material
2.3 Energy Institute Standards:
IP 69 Petroleum Products—Determination of Vapour Pressure—Reid Method
IP 394 Liquid Petroleum Products—Vapour Pressure—Part 1: Determination of Air Saturated Vapour Pressure (ASVP)
2.4 ISO Standards:
Guide 34ISO 17034 General Requirements for the Competence of Reference Material Producers
Guide 35 Reference Materials—General and Statistical Principles for CertificationMaterials—Guidance for characterization and
assessment of homogeneity and stability
3. Terminology
3.1 Definitions:
3.1.1 For definitions of terms used in this test method, refer to Terminology D4175.
3.2 Definitions of Terms Specific to This Standard:
3.2.1 automatic apparatus, n—microprocessor-controlled unit that performs the procedures of automatically controlling the
evaporation of a liquid specimen under specific conditions of this test method, collecting measurement data and converting this
data by patented algorithm in order to predict distillation results in correlation with industry recognized reference method.
3.2.2 corrected temperature reading, n— temperature readings, as described in 3.1.123.2.12, corrected to 101.3 kPa barometric
pressure.
3.2.3 end point (EP) or final boiling point (FBP), n—maximum corrected temperature readings obtained during the test at the
instant the flask internal pressure returns to the initial pressure level registered by automatic apparatus.
3.2.3.1 Discussion—
This usually occurs after the evaporation of all liquid from the bottom of the distillation flask. The term maximum temperature
is a frequently used synonym.
3.2.4 flask internal pressure, n—pressure within the distillation flask obtained during the test by a differential pressure sensor of
automatic apparatus.
3.2.4.1 Discussion—
The flask internal pressure data recorded during the test is automatically converted to the volume percent recovered or evaporated
data by patented algorithm employed by automatic apparatus.
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.
The last approved version of this historical standard is referenced on www.astm.org.
Available from Energy Institute, 61 New Cavendish St., London, WIG 7AR, U.K., http://www.energyinst.org.uk.
Available from International Organization for Standardization (ISO), 1 rue de Varembé, Case postale 56, CH-1211, Geneva 20, Switzerland, http://www.iso.ch.
D7345 − 23
3.2.5 initial boiling point (IBP), n—corrected temperature readings that corresponds to the instant of the flask internal pressure rise
registered by automatic apparatus.
3.2.6 liquid temperature, n—temperature of the liquid specimen in the distillation flask during the test obtained by a liquid
temperature measuring device of automatic apparatus.
3.2.7 percent evaporated, n—percent recovered corrected to a predicted by automatic analyzer evaporation loss percent. Percent
evaporated is automatically reported for ASTM 7C thermometer correlation.
3.2.8 percent recovered, n—volume percent automatically reported by the analyzer; expressed as a percentage of the charge
volume, associated with a simultaneous temperature readings. Percent recovered is reported for ASTM 8C thermometer
correlation.
3.2.9 percent recovery, n—percent recovery predicted by the automatic apparatus and expressed as a percentage of the charge
volume.
3.2.10 percent residue, n—volume of residue in the distillation flask predicted by the automatic apparatus and expressed as a
percentage of the charge volume.
3.2.11 reference method, n—ASTM D86 test method or its analogs which is widely used for expression of the distillation
characteristics of petroleum products in industry.
3.2.12 temperature readings, n—vapor and liquid temperature has through use of an algorithm of the automatic apparatus been
adjusted to mimic the same temperature lag and emergent stem effects as would be seen when using an ASTM 7C/7F or 8C/8F
liquid-in-glass thermometer to determine the distillation characteristics of the material under test by industry recognized reference
method.
3.2.13 vapor temperature, n—temperature of the vapors in the distillation flask during the test obtained by a vapor temperature
measuring device of automatic apparatus.
4. Summary of Test Method
4.1 A specimen of the sample is transferred into the distillation flask, the distillation flask is placed into position on the automatic
apparatus, and heat is applied to the bottom of the distillation flask.
4.2 The automatic apparatus measures and records specimen vapor and liquid temperatures, and pressure in the distillation flask
as the sample gradually distills under atmospheric pressure conditions. Automatic recordings are made throughout the distillation
and the data stored into the apparatus memory.
4.3 At the conclusion of the distillation, the collected data is treated by the data processing system, converted to distillation
characteristics and corrected for barometric pressure.
4.4 Test results are commonly expressed as percent recovered or evaporated versus corresponding temperature in compliance with
industry recognized standard form and reference method either in a table or graphically, as a plot of the distillation curve.
5. Significance and Use
5.1 The distillation (volatility) characteristics of hydrocarbons and other liquids have an important effect on their safety and
performance, especially in the case of fuels and solvents. The boiling range gives information on the composition, the properties,
and the behavior of the fuel during storage and use. Volatility is the major determinant of the tendency of a hydrocarbon mixture
to produce potentially explosive vapors.
5.2 The distillation characteristics are critically important for both automotive and aviation gasolines, affecting starting, warm-up,
D7345 − 23
and tendency to vapor lock at high operating temperature or at high altitude, or both. The presence of high boiling point
components in these and other fuels can significantly affect the degree of formation of solid combustion deposits.
5.3 Distillation limits are often included in petroleum product specifications, in commercial contract agreements, process
refinery/control applications, and for compliance to regulatory rules.
5.4 This test method can be applied to contaminated products or hydrocarbon mixtures. This is valuable for fast product quality
screening, refining process monitoring, fuel adulteration control, or other purposes including use as a portable apparatus for field
testing.
5.5 This test method uses an automatic micro distillation apparatus, provides fast results using small sample volume, and
eliminates much of the operator time and subjectivity in comparison to Test Method D86.
6. Apparatus
6.1 Basic Components of the Automatic Apparatus:
6.1.1 The basic components of the micro distillation unit are the distillation flask, a condensate recovery area with waste beaker,
an enclosure for the distillation flask with the heat source and flask support, the specimen liquid temperature measuring device,
the specimen vapor temperature measuring device, the distillation flask internal pressure measuring device, the ambient pressure
measuring device, the control systems for regulating the distillation process, and the data processing system for converting
recorded information into typical industry recognized standard report form.
6.2 A detailed description of the apparatus is given in Annex A1.
6.3 Barometer for Calibration—A pressure measuring device capable of measuring local station pressure with an accuracy of
0.1 kPa (1 mmHg) or better, at the same elevation relative to sea level where the apparatus is located.
6.3.1 The barometer is only required for periodic calibration of the external and internal pressure measuring devices.
6.3.2 (Warning—Do not take readings from ordinary aneroid barometers, such as those used at weather stations and airports,
since these are precorrected to give sea level readings.)
6.4 Sampling Device—Glass or plastics syringe capacity 10 mL 6 0.3 mL or constant volume dispenser capacity 10 mL 6 0.3 mL.
6.5 Waste Beaker—Glass approximately 200 mL capacity, outside diameter approximately 70 mm and height approximately
130 mm fitted with a cover to reduce evaporation. The cover design shall allow the beaker to remain open to atmospheric pressure.
7. Reagents and Materials
7.1 Cleaning Solvents, suitable for cleaning and drying the test flask such as; petroleum naphtha and acetone. (Warning—
Flammable. Liquid causes eye burns. Vapor harmful. May be fatal or cause blindness if swallowed or inhaled.)
7.2 Toluene, 99.5 % purity. (Warning—Extremely flammable. Harmful if inhaled. Skin irritant on repeated contact. Aspiration
hazard.)
7.3 n-Hexadecane, 99 % purity. (Warning—Extremely flammable. Harmful if inhaled. Skin irritant on repeated contact.
Aspiration hazard.)
The sole source of supply of the apparatus known to the committee at this time is ISL /PAC, B.P. 70285 Verson, 14653 CARPIQUET – FRANCE. If you are aware of
alternative suppliers, please provide this information to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of the responsible
technical committee, which you may attend.
D7345 − 23
7.4 Chemicals of at least 99 % purity shall be used in the calibration procedure (see 10.2). Unless otherwise indicated, it is
intended that all reagents conform to the specifications of the Committee on Analytical Reagents of the American Chemical
Society.
7.5 Granular Pumice Stones, clean and dry fine grade pumice stones of diameter 0.8 mm to 3.0 mm, approximately 10 grains are
necessary for each test.
7.6 Sample Drying Agent—Anhydrous sodium sulfate has been found to be suitable.
8. Sampling, Storage, and Sample Conditioning
8.1 Sampling:
8.1.1 The extreme sensitivity of volatility measurements to losses through evaporation and the resulting changes in composition
is such as to require the utmost precaution in the drawing and handling of volatile product samples.
8.1.2 Obtain a sample and test specimen in accordance with Practice D4057, D4177, or D5854 when appropriate. At least 50 mL
of sample is recommended.
8.1.3 Sample shall be free from any suspended solids or other insoluble contaminations. Obtain another sample or remove solid
particle by filtration. During filtration operation take care to minimize any loss of light ends.
8.2 Sample Storage:
8.2.1 All samples shall be stored in a tightly closed and leak-free container away from direct sunlight or sources of direct heat.
8.2.2 Protect samples containing light materials having expected initial boiling point lower than 100 °C from excessive
temperatures prior to testing. This can be accomplished by storage of the sample container in an appropriate ice bath or refrigerator
at a temperature below 10 °C. Other samples can be stored at ambient or lower temperature.
8.2.3 If the sample has partially or completely solidified during storage, it is to be carefully heated to a temperature when it is
completely fluid. It shall be vigorously shaken after melting, prior to opening the sample container, to ensure homogeneity.
8.3 Wet Samples:
8.3.1 Samples of materials that visibly contain water are not suitable for testing by this test method. If the sample is not dry, obtain
another sample that is free from suspended water.
8.3.2 If such a sample cannot be obtained, remove any free water by placing approximately 30 mL of the sample to be tested in
a glass conical flask containing approximately 10 g of the drying agent. Stopper and shake gently. Allow the mixture to settle for
approximately 15 min. Once the sample shows no visible signs of water, use a decanted portion of the sample for the analysis. It
is recommended to filter the test portion from the residual or suspended drying agent. During this drying and filtration operations
take care to minimize any loss of light ends. Report that the sample has been dried by the addition of a drying agent.
9. Preparation of Apparatus
9.1 Install the analyzer for operation in accordance with the manufacturer’s instructions.
9.2 This instrument shall be located away from direct sunlight, sources of direct heat or air draft.
9.3 Turn on the main power switch of the analyzer.
Reagent Chemicals, American Chemical Society Specifications,ACS Reagent Chemicals, Specifications and Procedures for Reagents and Standard-Grade Reference
Materials, American Chemical Society, Washington, DC. For Suggestionssuggestions on the testing of reagents not listed by the American Chemical Society, see
AnnualAnalar Standards for Laboratory Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia and National Formulary, U.S. Pharmacopeial
Convention, Inc. (USPC), Rockville, MD.
D7345 − 23
10. Verification Quality Control Checks
10.1 To verify the temperature measurement system, distill high purity toluene in accordance with this test method and comparing
the temperature reading at 50 % distilled. If the temperature reading differs more than 0.5 °C from the expected temperature of
109.3 °C (see Note 1), then check the instrument calibration (see Section 11).
10.2 To verify the temperature measurement system at elevated temperatures, use n-hexadecane and record the temperature at
50 % distilled. If the temperature reading differs more than 1.0 °C from the expected temperature of 278.6 °C (see Note 1, then
check the instrument calibration (see Section 11).
NOTE 1—These temperatures are those that would be obtained if the toluene and hexadecane were distilled using Test Method D86 and are not the figures
that are given as the boiling points of these materials in literature.
10.3 Verification of apparatus performance under dynamic conditions and wide temperature range can be done by distillation of
a Certified Reference Material (CRM) or Secondary Working Standard (SWS).
10.3.1 Certified Reference Material (CRM)—CRM is a stable mixture of hydrocarbon or other stable petroleum product with a
method-specific distillation characteristic established by a method-specific interlaboratory study following Practice D6300 or ISO
Guide 34 17034 and Guide 35. Suppliers of CRMs will provide certificates stating the method-specific distillation characteristic
for each material of the current production batch.
10.3.2 Secondary Working Standard (SWS)—SWS is a stable mixture of pure hydrocarbons, or other petroleum product whose
composition is known to remain appreciably stable. Establish the mean value of control points and the statistical control limits for
the SWS using standard statistical techniques. See Practice D6299.
11. Calibration
11.1 Follow the manufacturer’s instructions for verifying the correct operation of the apparatus.
11.2 Temperature Measurement System—At intervals of not more than six months or after the system has been replaced or
repaired, or both, following the apparatus instruction manual, check the calibration of the liquid and vapor temperature measuring
sensors by distilling of pure compounds, like toluene and n-hexadecane.
NOTE 2—The melting point of n-hexadecane is 18 °C. If the sample is solid, heat it to about 25 °C and wait until all the material is liquid before starting
the test.
11.3 External Pressure Measuring Device—At intervals of not more than six months, or after the system has been replaced or
repaired, or both, the external pressure measuring device reading of the apparatus shall be verified against a barometer, as described
in 6.3.
11.4 Differential Pressure Measuring Device—At intervals of not more than six months, or after the system has been replaced or
repaired, or both, the differential pressure measuring device reading of the apparatus shall be verified in accordance with the
manufacturer’s instructions.
12. Procedure
12.1 Material with an Initial Boiling Point of 100 °C and Below—Bring the temperature of the sample and container to a
temperature at least 10 °C below the expected initial boiling point of the material before opening the sample container.
12.2 Material with a Boiling Point above 100 °C—Bring the sample and its container to ambient temperature. If the sample has
partially or completely solidified during storage warm until fluid, then mix by gentle shaking.
NOTE 3—Not respecting the requirements given in 12.1 can lead to improper IBP detection on samples containing volatile materials. If expected initial
boiling point of the sample to be tested is unknown, it is advised to make a test at ambient conditions. If the distillation result shows that the requirements
of 12.1 were not respected, discard the result and repeat the test strictly respecting the conditions.
D7345 − 23
12.3 Ensure that the distillation measuring head of automatic apparatus has been allowed to reach ambient temperature and that
any residual condensate has been removed.
12.4 Check that the distillation flask is clean and dry.
12.5 Place at least 10 grains of clean and dry granular pumice stones into the distillation flask. Some apparatus supply a suitable
boiling stone dispenser. When the sample is biodiesel (B100), do not use any pumice stones.
12.6 Measure 10 mL 6 0.3 mL test portion using the sampling device (see Section 6). When the sample is biodiesel (B100),
measure 5 mL 6 0.3 mL test portion. Check for the presence of any bubbles and if present discard the test portion and refill with
bubble free material. Transfer the bubble free test portion to the prepared distillation flask, taking care that none of the liquid flows
into the vapor tube.
NOTE 4—Use new disposable syringe or disposable dispenser tip for each new sampling to avoid any products cross contamination which can cause
erroneous distillation results.
12.7 Fit the distillation measurement head into its position on the distillation flask securely in accordance with the manufacturer’s
instructions.
12.8 Place the distillation flask into the heating enclosure and insert the sidearm of the distillation flask into the sealing of the
condenser tube, while also attaching the measurement head holder.
12.9 Position the heating source/flask support around the lower section of the distillation flask.
12.10 Close heating enclosure by positioning the protection shield to its position.
12.11 Check that a waste collection beaker is placed under the projecting lower end of the condenser tube. Ensure that the waste
collection beaker remains open to atmospheric pressure.
NOTE 5—Monitor that the liquid level in the waste beaker does not exceed two thirds of its total capacity and drain it on periodic intervals.
12.12 Without delay initiate the distillation process according to the apparatus manufacturer’s instructions.
12.12.1 From this point up to and including the termination of the measurement, the apparatus automatically controls all
operations. The instrument applies heating to the specimen and regulates automatically heating power during the distillation run
using specimen liquid temperature data. The distillation conditions; distillation flask internal pressure, specimen liquid
temperature, and specimen vapor temperature are automatically measured and recorded during the test by the control system. The
distillation is automatically terminated when the flask internal pressure returns to its initial pressure level. The collected test data
is automatically processed and reported on the display and printed out at the conclusion of the test run. The heating enclosure
cooling fan is automatically activated.
12.13 Record the test data.
12.14 Allow the distillation flask to cool and remove it from the apparatus.
13. Report
13.1 In cases in which no specific data requirements have been set by the operator, corrected temperatures readings versus
corresponding percent recovered or evaporated are typically reported by the apparatus. Report typically contains the IBP, FBP, 5 %,
95 % and each 10 % increment from 10 % to 90 %, as well as percent recovery and percent residue.
13.1.1 If required, the percent loss is calculated by the following equation:
loss %5 100 2 percent recovery1percent residue (1)
~ !
D7345 − 23
13.2 Report all volumetric percentages to the nearest 0.1 % (V/V).
13.3 Report all temperature readings to the nearest 0.1 °C (see Note 3).
13.4 Report if a drying agent, as described in 8.3.2, was used.
13.5 The test report shall contain at least the following information:
13.5.1 Sufficient details for complete identification of the product tested;
13.5.2 A reference to this standard;
13.5.3 The result of the test;
13.5.4 Any deviation, by agreement or otherwise, from the procedure specified; and
13.5.5 The date of the test.
14. Precision and Bias
9-11
14.1 Precision—The precision of this test method as determined by the statistical examination of the interlaboratory test results
is as follows:
NOTE 6—Typically samples for distillation are classified according to a Group number (see Test Method D86). However, this test method does not require
this classification, but for the purposes of precision and cross method between-method reproducibility comparisons, the precisions and bias have been
derived according to the group number in the following fashion. Group 1, 2, and 3 samples are labeled as NOT4, and Group 4 samples are labeled GRP4.
See Appendix X1 for further information on typical samples and group classification.
NOTE 7—Information on the precision of % evaporated or % recovered at a prescribed temperature can be found in Annex A4.
14.1.1 Repeatability—The difference between successive test results, obtained by the same operator using the same apparatus
under constant operating conditions on identical test material, would in the long run, in the normal and correct operation of this
test method, exceed the following only in one case in twenty.
Group NOT4:
IBP: r = 3.3 valid range: 20 °C – 50 °C
E5: r = 1.1 valid range: 25 °C – 60 °C
E5/E10: r = 1.1 valid range: 25 °C – 65 °C
E10: r = 1.1 valid range: 30 °C – 65 °C
E20: r = 1.2 valid range: 40 °C – 70 °C
E30: r = 1.8 valid range: 50 °C – 85 °C
E40: r = 2.7 valid range: 55 °C – 100 °C
E50: r = 2.4 valid range: 60 °C – 120 °C
E60: r = 2.4 valid range: 75 °C – 125 °C
E70: r = 1.8 valid range: 100 °C – 140 °C
E80: r = 2.1 valid range: 115 °C – 160 °C
E90: r = 1.9 valid range: 140 °C – 180 °C
E90/E95: r = 2.0 valid range: 140 °C – 200 °C
E95: r = 2.0 valid range: 150 °C – 200 °C
FBP: r = 3.0 valid range: 140 °C – 260 °C
Group GRP4: Refer to Annex A2 for tables of calculated repeatability.
IBP: r = 3.9 valid range: 145 °C – 195 °C
T5: r = T × 0.01194 valid range: 175 °C – 250 °C
T10: r = T × 0.00954 valid range: 160 °C – 265 °C
Supporting data have been filed at ASTM International Headquarters and may be obtained by requesting Research Report RR:D02-1621. Contact ASTM Customer
Service at service@astm.org.
Supporting data have been filed at ASTM International Headquarters and may be obtained by requesting Research Report RR:D02-1831. Contact ASTM Customer
Service at service@astm.org.
Supporting data have been filed at ASTM International Headquarters and may be obtained by requesting Research Report RR:D02-2067. Contact ASTM Customer
Service at service@astm.org.
D7345 − 23
T20: r = T × 0.00932 valid range: 180 °C – 275 °C
T30: r = T × 0.00782 valid range: 190 °C – 285 °C
T40: r = T × 0.00822 valid range: 200 °C – 290 °C
T50: r = T × 0.00614 valid range: 170 °C – 295 °C
T60: r = T × 0.00534 valid range: 220 °C – 305 °C
T70: r = T × 0.00405 valid range: 230 °C – 315 °C
T80: r = T × 0.00441 valid range: 240 °C – 325 °C
T90: r = T × 0.0041 valid range: 180 °C – 340 °C
T95: r = 2.03 valid range: 260 °C – 360 °C
FBP: r = 3.93 valid range: 195 °C – 365 °C
where:
E = evaporated temperature at x percent within valid range prescribed (°C)
T = recovered temperature at x percent within valid range prescribed (°C)
NOTE 8—For naphthas, solvents, and other similar materials where percent recovered is reported and the percent loss is typically less than one percent,
the percent recovered temperatures can be considered identical to the percent evaporated temperatures, and precision can be calculated as shown for Group
NOT4.
14.1.2 Reproducibility—The difference between two single and independent test results, obtained by different operators working
in different laboratories on identical test material, would in the long run, in normal and correct operation of this test method, exceed
the following only in one case in twenty.
Group NOT4:
IBP: R = 5.9 valid range: 20 °C – 50 °C
E5: R = 2.5 valid range: 25 °C – 60 °C
E5/E10: R = 2.5 valid range: 25 °C – 65 °C
E10: R = 2.1 valid range: 30 °C – 65 °C
E20: R = 2.2 valid range: 40 °C – 70 °C
E30: R = 2.6 valid range: 50 °C – 85 °C
E40: R = 3.6 valid range: 55 °C – 100 °C
E50: R = 4.1 valid range: 60 °C – 120 °C
E60: R = 4.5 valid range: 75 °C – 125 °C
E70: R = 3.5 valid range: 100 °C – 140 °C
E80: R = 3.7 valid range: 115 °C – 160 °C
E90: R = 5.8 valid range: 140 °C – 180 °C
E90/E95: R = 5.8 valid range: 140 °C – 200 °C
E95: R = 5.4 valid range: 150 °C – 200 °C
FBP: R = 5.7 valid range: 175 °C – 220 °C
Group GRP4: Refer to Annex A2 for tables of calculated reproducibility.
IBP: R = 6.0 valid range: 145 °C – 195 °C
T5: R = T × 0.0172 valid range: 175 °C – 250 °C
T10: R = T × 0.0177 valid range: 160 °C – 265 °C
T20: R = T × 0.0117 valid range: 180 °C – 275 °C
T30: R = T × 0.0122 valid range: 190 °C – 285 °C
T40: R = T × 0.0122 valid range: 200 °C – 290 °C
T50: R = T × 0.0103 valid range: 170 °C – 295 °C
T60: R = T × 0.0092 valid range: 220 °C – 305 °C
T70: R = T × 0.0084 valid range: 230 °C – 315 °C
T80: R = T × 0.0084 valid range: 240 °C – 325 °C
T90: R = T × 0.0081 valid range: 180 °C – 340 °C
T95 R = 3.23 valid range: 260 °C – 360 °C
FBP: R = 7.7 valid range: 195 °C – 365 °C
where:
E = evaporated temperature at x percent within valid range prescribed (°C)
T = recovered temperature at x percent within valid range prescribed (°C)
NOTE 9—See Note 8.
NOTE 10—The degrees of freedom associated with the reproducibility estimate from this interlaboratory study for D7345 Group NOT4 precision for E5
are 25. Since the minimum requirement of 30 (in accordance with Practice D6300) is not met, users are cautioned that the actual reproducibility may
be significantly different than these estimates.
NOTE 11—The degrees of freedom associated with the reproducibility estimate from this interlaboratory study for D7345 Group NOT4 precision for E10
are 27. Since the minimum requirement of 30 (in accordance with Practice D6300) is not met, users are cautioned that the actual reproducibility may
be significantly different than these estimates.
NOTE 12—The degrees of freedom associated with the reproducibility estimate from this interlaboratory study for D7345 Group NOT4 precision for E95
are 25. Since the minimum requirement of 30 (in accordance with Practice D6300) is not met, users are cautioned that the actual reproducibility may
be significantly different than these estimates.
D7345 − 23
14.2 Bias—Since there is no accepted reference material suitable for determining the bias for the procedure in this Test Method,
bias has not been determined.
14.3 Between-Method Bias—The Degree of Agreement between results by Test Method D7345 and Test Method D86
(automated)—Results on the same materials produced by Test Method D7345 and Test Method D86 have been assessed in
9-11
accordance with procedures outlined in Practice D6708. The findings are:
D7345 − 23
IBP:
NOT4
The degree of agreement between results from Test Method D7345 and Test Method D86 (automated)
can be further improved by applying the bias-correction outlined in Eq 2. Sample-specific bias, as de-
fined in Practice D6708, was observed for some samples after applying the bias-correction.
Bias-correctedX5predicted Y5 X11.42°C (2)
where:
X = result obtained by Test Method D7345 (this test method), and bias-corrected X = predicted Y = re-
sult that would have been obtained by Test Method D86 (automated) on the same sample.
Differences between bias-corrected results from Eq 2 and Test Method D86, for the sample types and
property ranges studied, are expected to exceed the following cross method reproducibility (R ), as
xy
defined in Practice D6708, about 5 % of the time.
Differences between bias-corrected results from Eq 2 and Test Method D86, for the sample types and
property ranges studied, are expected to exceed the following between-method reproducibility (R ), as
xy
2 2 0.5
defined in Practice D6708, about 5 % of the time. R (°C) = (0.629 RX + 0.629 RY )
xy
Group
NOT4: Refer to Annex A3.
where:
RX = reproducibility of Test Method D7345 (this test method)
RY = reproducibility of Test Method D86 (automated)
GRP4
No bias-correction considered in Practice D6708 can further improve agreement between results from
Test Method D7345 and Test Method D86 (automated), for sample types and property ranges studied.
Sample-specific bias, as defined in Practice D6708, was observed for some samples.
Differences between results from Test Method D7345 and Test Method D86 (automated), for the
sample types and property ranges studied, are expected to exceed the following cross method repro-
ducibility (R ), as defined in Practice D6708, about 5 % of the time.
xy
Differences between results from Test Method D7345 and Test Method D86 (automated), for the
sample types and property ranges studied, are expected to exceed the following between-method re-
producibility (R ), as defined in Practice D6708, about 5 % of the time.
xy
Group GRP4: Refer to Annex A3.
T5:
NOT4
The degree of agreement between results from Test Method D7345 and Test Method D86 (automated) can be further improved by applying the bias-correction out-
lined in Eq 3. Sample-specific bias, as defined in Practice D6708, was observed for some samples after applying the bias-correction.
Bias-corrected X = predicted Y = 0.82 X + 11.25 °C (3)
Differences between results from Test Method D7345 and Test Method D86 (automated), for the sample types and property ranges studied, are expected to exceed
the following cross method reproducibility (R ), as defined in Practice D6708, about 5 % of the time.
xy
Differences between results from Test Method D7345 and Test Method D86 (automated), for the sample types and property ranges studied, are expected to exceed
2 2 0.5
the following between-method reproducibility (R ), as defined in Practice D6708, about 5 % of the time. R (°C) = (0.995 RX + 1.468 RY )
xy xy
Group
NOT4: Refer to Annex A3.
where:
RX = reproducibility of Test Method D7345 (this test method)
RY = reproducibility of Test Method D86 (automated)
GRP4
The degree of agreement between results from Test Method D7345 and Test Method D86 (automated) can be further improved by applying the bias-correction out-
lined in Eq 4. Sample-specific bias, as defined in Practice D6708, was observed for some samples after applying the bias-correction.
Bias-corrected X =predicted Y = 1.1X218.43 °C (4)
where:
X = result obtained by Test Method D7345 (this test method), and bias-corrected X = predicted Y = result that would have been obtained by Test Method D86 (auto-
mated) on the same sample.
D7345 − 23
Differences between bias-corrected results from Eq 4 and Test Method D86, for the sample types and property ranges studied, are expected to exceed the following
cross method reproducibility (R ), as defined in Practice D6708, about 5 % of the time.
xy
Differences between bias-corrected results from Eq 4 and Test Method D86, for the sample types and property ranges studied, are expected to exceed the following
between-method reproducibility (R ), as defined in Practice D6708, about 5 % of the time.
xy
Group GRP4: Refer to Annex A3.
T10:
NOT4
The degree of agreement between results from Test Method D7345 and Test Method D86 (automated)
can be further improved by applying the bias-correction outlined in Eq 5. Sample-specific bias, as de-
fined in Practice D6708, was observed for some samples after applying the bias-correction.
Bias-corrected X = predicted Y = 0.82 X + 11.1 °C (5)
Differences between results from Test Method D7345 and Test Method D86 (automated), for the sample
types and property ranges studied, are expected to exceed the following cross method reproducibility
(R ), as defined in Practice D6708, about 5 % of the time.
xy
Differences between results from Test Method D7345 and Test Method D86 (automated), for the sample
types and property ranges studied, are expected to exceed the following between-method reproducibility
2 2 0.5
(R ), as defined in Practice D6708, about 5 % of the time. R (°C) = (1.078 RX + 1.618 RY )
xy xy
Group
NOT4: Refer to Annex A3.
where:
RX = reproducibility of Test Method D7345 (this test method)
RY = reproducibility of Test Method D86 (automated)
GRP4
The degree of agreement between results from Test Method D7345 and Test Method D86 (automated)
can be further improved by applying the bias-correction outlined in Eq 6. Sample-specific bias, as de-
fined in Practice D6708, was observed for some samples after applying the bias-correction.
Bias-corrected X 5predicted Y51.09 X216.4°C (6)
where:
X = result obtained by Test Method D7345 (this test method), and bias-corrected X = predicted Y = re-
sult that would have been obtained by Test Method D86 (automated) on the same sample.
Differences between bias-corrected results from Eq 6 and Test Method D86, for the sample types and
property ranges studied, are expected to exceed the following cross method reproducibility (R ), as de-
xy
fined in Practice D6708, about 5 % of the time.
Differences between bias-corrected results from Eq 6 and Test Method D86, for the sample types and
property ranges studied, are expected to exceed the following between-method reproducibility (R ), as
xy
defined in Practice D6708, about 5 % of the time.
Group GRP4: Refer to Annex A3.
T20:
The degree of agreement between results from Test Method D7345 and Test Method D86 (automated) can be further improved by applying the bias-correction out-
lined in Eq 7. Sample-specific bias, as defined in Practice D6708, was observed for some samples after applying the bias-correction.
Bias-corrected X =predicted Y = X +0.96 °C (7)
Differences between results from Test Method D7345 and Test Method D86 (automated), for the sample types and property ranges studied, are expected to exceed
the following cross method reproducibility (R ), as defined in Practice D6708, about 5 % of the time.
xy
Differences between results from Test Method D7345 and Test Method D86 (automated), for the sample types and property ranges studied, are expected to exceed
2 2 0.5
the following between-method reproducibility (R ), as defined in Practice D6708, about 5 % of the time. R (°C) = (1.905 RX + 1.905 RY )
xy xy
Group
NOT4: Refer to Annex A3.
where:
RX = reproducibility of Test Method D7345 (this test method)
RY = reproducibility of Test Method D86 (automated)
GRP4
D7345 − 23
The degree of agreement between results from Test Method D7345 and Test Method D86 (automated) can be further improved by applying the bias-correction out-
lined in Eq 8. Sample-specific bias, as defined in Practice D6708, was observed for some samples after applying the bias-correction.
Bias-corrected X =predicted Y = 1.09X218.88 °C (8)
where:
X = result obtained by Test Method D7345 (this test method), and bias-corrected X = predicted Y = result that would have been obtained by Test Method D86 (auto-
mated) on the same sample.
Differences between bias-corrected results from Eq 8 and Test Method D86, for the sample types and property ranges studied, are expected to exceed the following
cross method reproducibility (R ), as defined in Practice D6708, about 5 % of the time.
xy
Differences between bias-corrected results from Eq 8 and Test Method D86, for the sample types and property ranges studied, are expected to exceed the following
between-method reproducibility (R ), as defined in Practice D6708, about 5 % of the time.
xy
Group GRP4: Refer to Annex A3.
T30:
No bias-correction considered in Practice D6708 can further improve the agreement between results from Test Method D7345 and Test Method D86 (automated) for
the material types and property ranges studied. Sample-specific bias, as defined in Practice D6708, was observed for some samples.
Differences between results from Test Method D7345 and Test Method D86 (automated), for the sample types and property ranges studied, are expected to exceed
the following cross method reproducibility (R ), as defined in Practice D6708, about 5 % of the time.
xy
Differences between results from Test Method D7345 and Test Method D86 (automated), for the sample types and property ranges studied, are expected to exceed
2 2 0.5
the following between-method reproducibility (R ), as defined in Practice D6708, about 5 % of the time. R (°C) = (1.468 RX + 1.468 RY )
xy xy
Group
NOT4: Refer to Annex A3.
where:
RX = reproducibility of Test Method D7345 (this test method)
RY = reproducibility of Test Method D86 (automated)
GRP4
The degree of agreement between results from Test Method D7345 and Test Method D86 (automated) can be further improved by applying the bias-correction out-
lined in Eq 9. Sample-specific bias, as defined in Practice D6708, was observed for some samples after applying the bias-correction.
Bias-corrected X =predicted Y = 1.08X218.5 °C (9)
where:
X = result obtained by Test Method D7345 (this test method), and bias-corrected X = predicted Y = result that would have been obtained by Test Method D86 (auto-
mated) on the same sample.
Differences between bias-corrected results from Eq 9 and Test Method D86, for the sample types and property ranges studied, are expected to exceed the following
cross method reproducibility (R ), as defined in Practice D6708, about 5 % of the time.
xy
Differences between bias-corrected results from Eq 9 and Test Method D86, for the sample types and property ranges studied, are expected to exceed the following
between-method reproducibility (R ), as defined in Practice D6708, about 5 % of the time.
xy
Group GRP4: Refer to Annex A3.
T40:
No bias-correction considered in Practice D6708 can further improve the agreement between results from Test Method D7345 and Test Method D86 (automated) for
the material types and property ranges studied. Sample-specific bias, as defined in Practice D6708, was observed for some samples.
Differences between results from Test Method D7345 and Test Method D86 (automated), for the sample types and property ranges studied, are expected to exceed
the following cross method reproducibility (R ), as defined in Practice D6708, about 5 % of the time.
xy
Differences between results from Test Method D7345 and Test Method D86 (automated), for the sample types and pro
...








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