distillation and vapor pressure measurement in petroleum products

2EY'-ONTEMAYOR %DITOR Distillation and Vapor Pressure Measurement in Petroleum Products Distillation and Vapor Pressure Measurement in Petroleum Products ASTM International 100 Barr Harbor Drive PO Box C700 West Conshohocken, PA 19428–2959 Printed in the U.S.A. ASTM Stock Number: MNL51 Rey G. Montemayor, editor Library of Congress Cataloging-in-Publication Data Montemayor, Rey G., 1944– Distillation and vapor pressure measurement in petroleum products / Rey G. Montemayor. p. cm. — ͑ASTM Manual Series: MNL 51͒ ASTM stock number: “MNL51.” ISBN 978-0-8031-6227-3 1. Petroleum—Refining—Standards. 2. Petroleum refineries—Standards. 3. Distillation—Standards. 4. Vapor pressure—Standards. I. ASTM International. II. Title. TP690.45.M66 2008 665.5 Ј 3—dc22 2007039107 Copyright © 2008 ASTM International, West Conshohocken, PA. All rights reserved. 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Printed in Mayfield, PA September 2008 Foreword THIS PUBLICATION, Manual on Distillation and Vapor Pressure Measurement in Petroleum Products, was spon- sored by ASTM International Committee D02 on Petroleum Products and Lubricants, and edited by Rey G. Montemayor, Imperial Oil Ltd., Sarnia, Ontario, Canada. This publication is Manual 51 of ASTM International’s Manual Series. iii Preface ASTM International has been developing standards that is widely used world-wide since 1898. The technical content and quality of these standards are excellent, and these are largely due to the thousands of technical experts who volunteer and devote considerable amount of their time and effort in the standards development activities. In ASTM Committee D02 on Petroleum Products and Lubricants, one of the largest ASTM committees, a tremendous amount of activity is spent in developing new test methods, and revising existing test methods to meet ever increasing demands for high quality standards in the industry. ASTM D02 is blessed with a consid- erable number of technical experts who, in one way or another, have contributed tremendously to standards development related to petroleum products and lubricants. This manual is the result of the selfless effort, time, dedication, and considerable expertise of some of these experts. v Acknowledgment This manual would not have been possible without the help and contribution from a number of individuals. I would like to sincerely thank the authors of the different chapters who have been very responsive in submitting their manuscripts, and who have been very patient in waiting for all the publication protocols to be satisfied. Their time, effort, dedication and expertise have proven to be invaluable in the preparation of this manual. To the anonymous reviewers who have provided very helpful and constructive suggestions on their review of the content of the various chapters thereby making them easier to understand and minimize any potential misun- derstanding, I would like to extend my heartfelt gratitude. Special thanks to a number of ASTM Staff who are instrumental in bringing this work to become a reality: to Lisa Drennen of Committee D02 who provided a number of ASTM historical documents; and to Monica Siperko and Kathy Dernoga of the ASTM Publications Department who provided support, guidance, and encouragement throughout the preparation of the various chapter manuscripts. I wish to thank Imperial Oil Ltd., for its continued support in the time and effort spent with this work, and other ASTM International activities. I would also like to acknowledge ASTM International and Committee D02 for sponsoring this work. And last, but not least, to Susanna, my sincere thanks for being so understanding and supportive of my involvement with ASTM International. Rey G. Montemayor Imperial Oil Ltd. vi Contents Preface v Acknowledgment vi Chapter 1: Introduction and a Brief Historical Background, R. G. Montemayor 1 Coverage Of The Manual 1 Distillation Measurement 1 Vapor Pressure Measurement 2 Simulated Distillation Measurement 2 A Bit Of History 2 Distillation Measurement at Atmospheric Pressure 2 Distillation Measurement at Reduced Pressure 3 Simulated Distillation 4 Vapor Pressure Measurement 5 Chapter 2: Distillation Measurement at Atmospheric Pressure, R. G. Montemayor 6 ASTM D86—Distillation At Atmospheric Pressure 6 Scope 6 Terminology 6 Summary of the Method 6 Significance and Use 7 Sampling . . 7 Group Characteristic 7 Sample Storage and Conditioning 8 Wet Samples 8 Manual and Automated D86 Apparatus 8 Distillation Flask 9 Flask Support Hole Dimension 9 Condenser and Cooling Systems 9 Heat Source and Heat Control 10 Temperature Measurement Device 13 Calibration . . 13 Temperature Measurement Device 13 Receiving Cylinder and Level Follower 14 Barometer or Pressure Measuring Device 14 Calculations 15 Correcting Temperature Readings to 101.3 kPa ͑760 mm Hg͒ Pressure Device 15 Sample Calculation 15 Percent Total Recovery and Percent Loss 16 Corrected Percent Loss and Corrected Percent Recovery 16 Percent Evaporated and Percent Recovered 16 Temperature Readings at Prescribed Percent Evaporated 16 Percent Evaporated or Percent Recovered at a Prescribed Temperature Reading 17 Slope or Rate of Change of Temperature 18 Calculation of Precision 18 Report 19 Precision 19 Bias 19 ASTM D850 And D1078: Distillation At Atmospheric Pressure For Aromatic Materials And Volatile Organic Solvents 20 ASTM D850 . . . . . . . . 20 ASTM D1078 20 Comparison Of ASTM D86, D850, And D1078 22 Potential Troubleshooting Guide 22 Safety 23 Statistical Quality Control 24 Cross-Reference Of Distillation At Atmospheric Pressure Test Methods 24 New Test Methods For Distillation At Atmospheric Pressure 25 Micro Method 25 Mini Method 25 ASTM D402 Distillation Of Cut-Back Asphaltic Product 25 Chapter 3: Distillation Measurement at Reduced Pressure, R. M. Daane 27 Distillation Of Crude Petroleum By ASTM D2892 27 Introduction 27 Field Of Application 27 Important Parameters 27 Temperature 27 Distillation Pressure 28 Separation Sharpness ͑Efficiency͒ 29 Other Factors Affecting Results 30 Precision 31 Summary 31 Vacuum Distillation 31 ASTM D5236 31 Introduction 31 Field of Application 31 Important Parameters 32 Temperature 32 Distillation Pressure 32 Separation Sharpness 33 Other Factors 34 Boiling Point, TBP, and AET 34 Comparison of ASTM D5236 and D2892 34 Precision 35 ASTM D1160 35 Introduction 35 Field of Application 35 Important Parameters 36 Temperature 36 Distillation Pressure 36 Volume Measurement 36 Precision 36 Accuracy 37 Closing Remarks 37 Chapter 4: Simulated Distillation Measurement, D. S. Workman 38 Introduction 38 Gas Chromatography and Simulated Distillation 38 ASTM Simulated Distillation Methods 38 Important Considerations 40 Instrument Requirements 40 Column Selection 40 Carrier Gas Flow Control 42 Data Collection 42 Analysis Software 42 Data Interpretation 42 Comparison To Physical Distillation TBP 43 Correlations Using Simulated Distillation Data 44 D86 Correlated Data from D2887 Data 44 Correlation of Flash Point and D2887 44 Future Work In The Area Of Simulated Distillation 46 Accelerated Simulated Distillation 46 Chapter 5: Vapor Pressure Measurement, R. G. Montemayor 48 ASTM D323—Vapor Pressure Measurement By The Reid Method †2‡ 48 Scope 48 Summary and Significance of the Test Method 48 Apparatus . . 49 Sampling . . 50 Calibration . . 51 Report, Precision, and Bias . . 51 ASTM D4953—Vapor Pressure By The Dry Reid Method †5‡ 51 Scope 51 Summary of the Test Method, Significance and Use, and Apparatus 52 Precision and Bias 52 ASTM D5191—Vapor Pressure of Petroleum Products „Mini Method…†5‡ 52 Scope 52 Summary and Significance of the Test Method 53 Apparatus . . 53 Sampling and Sample Handling 53 Calibration . . 54 Calculation 55 Report, Precision, and Bias . . 55 ASTM D5190—Vapor Pressure Of Petroleum Products „Automatic Method…†5‡ 56 Summary of the Test Method 56 Apparatus . . 56 Calibration . . 57 Calculation 57 Precision and Bias 57 ASTM D5482—Vapor Pressure Of Petroleum Products „Mini Method-Atmospheric…†5‡ 57 Summary of the Test Method 57 Apparatus . . 57 Calculation 57 Precision and Bias 57 ASTM D6377—Vapor Pressure Of Crude Oil: VPCR X „Expansion Method…†9‡ 58 Scope 58 Terminology 58 Summary and Significance of the Test Method 58 Apparatus and Calibration 58 Sampling . . 58 Report, Precision, and Bias . . 59 ASTM D6378—Vapor Pressure „VP X … Of Petroleum Products, Hydrocarbons, And Hydrocarbon-Oxygenate Mixtures „Triple Expansion Method…†9‡ 59 Scope 59 Summary and Significance of the Test Method 59 Apparatus and Calibration 59 Sampling and Sample Handling 60 Calculation 60 Report, Precision, and Bias . . 60 Proposed Revision to D6378 Being Considered 60 ASTM D1267—Vapor Pressure Of Liquefied Petroleum „LP… Gases „LP-Gas Method…†2‡ 61 Scope 61 Summary and Significance of the Test Method 61 Apparatus . . 61 Sampling and Calculation . . 62 Report, Precision, and Bias . . 62 ASTM D6897—Vapor Pressure Of Liquefied Petroleum Gases „LPG…„Expansion Method…†9‡ 62 Scope 62 Summary and Significance of the Test Method 62 Apparatus and Calibration 63 Calculation, Report, Precision, and Bias 63 Vapor-Liquid Ratio Temperature Measurements 63 ASTM D2533—Vapor-Liquid Ratio of Spark-Ignition Fuels ͓2͔ 63 Scope 63 Summary and Significance of the Test Method 63 Critical Apparatus, Calibration, Sampling, and Sample Handling 64 Calculation, Report, Precision, and Bias 64 ASTM D5188—Vapor-Liquid Ratio Temperature of Fuels ͑Evacuated Chamber Method͒ 65 Scope 65 Summary and Significance of the Test 65 Apparatus, Calibration, Sampling, and Sample Handling 65 Calculation, Report, Precision, and Bias 65 Other Vapor Pressure Measurements 65 ASTM D2878—Estimating Apparent Vapor Pressures and Molecular Weights of Lubricating Oils ͓4͔ 65 ASTM D2879—Vapor Pressure-Temperature Relationship and Initial Decomposition Temperature of Liquids by Isoteniscope ͓4͔ 65 ASTM E1194—Vapor Pressure ͓12͔ 66 ASTM E1719—Vapor Pressure of Liquids by Ebulliometry ͓13͔ 66 Comparison Of Vapor Pressure And Vapor/Liquid Ratio Test Methods 66 [...]... Method for Vapor Pressure of Gasoline and Gasoline-Oxygenate Blends ͑Dry Method͒” ͓5͔, ASTM D5190 “Standard Test Method for Vapor Pressure of Petroleum Products ͑Automated Method͒” ͓5͔, ASTM D5191 “Standard Test Method for Vapor Pressure of Petroleum Products ͑Mini Method͒” ͓5͔, ASTM D5482 “Standard Test Method for Vapor Pressure of Petroleum Products ͑Mini Method—Atmospheric͒” ͓5͔, ASTM D6377 “Standard... provide information and discussions on the different aspects of measuring distillation and vapor pressure characteristics, with the purpose of clarifying and providing a better understanding of the various test methods This work focuses on current standard test methods used by practitioners of distillation and vapor pressure measurements in the petroleum industry world-wide Specifically, the standard... IN PETROLEUM PRODUCTS of Heavy Hydrocarbon Mixtures ͑Vacuum Potstill Method͒” ͓5͔ Vapor Pressure Measurement The vapor pressure measurement test methods covered in this manual are: ASTM D323 “Standard Test Method for Vapor Pressure of Petroleum Products ͑Reid Method͒” ͓1͔, ASTM D1267 “Standard Test Method for Gage Vapor Pressure of Liquefied Petroleum ͑LP͒ Gases ͑LP-Gas Method͒” ͓1͔, ASTM D4953 “Standard... conducted in 2001 to determine the relative bias ͑if any͒ of manual and automated D86 distillation results In addition, data from the recently concluded interlaboratory study ͑2003͒ ͓10͔ comparing vapor pressure results using D5191 and D6378 test methods will be presented These data on D86, D5191, and D6378 are in the process of being included in the existing standards A Bit Of History Distillation Measurement. .. was made to include precision statements for automated and manual D1078 distillation Distillation Measurement at Reduced Pressure In 1938, Fenske described in a review ͓20͔ of laboratory and small-scale distillation of petroleum products, and several apparatuses and procedures for distillation at reduced pressure These have evolved in a number of standard test methods to determine the distillation. .. characteristics of petroleum products and fractions that would decompose if distilled at atmospheric pressure ASTM D1160 was first 4 DISTILLATION AND VAPOR PRESSURE MEASUREMENT IN PETROLEUM PRODUCTS ᭿ Fig 2—Nomograph showing precision of D86-52 published in 1951; ASTM D2892 for crude oil distillation first approved and published in 1970; and ASTM D5236 for heavy hydrocarbon mixtures such as heavy crude oils, petroleum. .. for the petroleum refining industry ͓3͔ Vapor Pressure Measurement ͓7͔ It is said that the Reid vapor pressure test method was the result of a competition in the 1920s to improve upon the original U.S Bureau of Mines vapor tension” method ͑essentially a pressure gage on a specified length of 2 in pipe͒ to measure the vapor pressure of gasoline ͓24͔ The competition was won by W Reid, and the resulting test... lowest point in the distillation flask The end point or final boiling point, rather than dry point, is intended for general use The dry point is normally reported for special purpose naphthas such as hydrocarbon solvents used in the paint and coatings industry Dry point is also substituted for the end point ͑final boiling point͒ whenever the sample is of such nature that the precision of the end point ͑final... glass joint 14 DISTILLATION AND VAPOR PRESSURE MEASUREMENT IN PETROLEUM PRODUCTS TABLE 6—Expected 50 % boiling point of n-hexadecane for 7C and 8C thermometers ASTM 7C 8C IP 5C 6C n-hexadecane 50 % boiling point 275.0± 1.0 ° C 278.6± 1.0 ° C TABLE 7—Updated 50 % boiling points of toluene and n-hexadecanea Thermometer Toluene n-hexadecane used to correct the temperature reading to atmospheric pressure. .. ͑final boiling point͒ cannot consistently meet the requirements given in the precision section of the method Front End Loss—Loss due to evaporation during transfer from the receiving cylinder to the distillation flask, vapor loss during the distillation, and uncondensed vapor in the flask at the end of the distillation Percent Recovered—The volume of condensate observed in the receiving cylinder, expressed . 2EY'-ONTEMAYOR %DITOR Distillation and Vapor Pressure Measurement in Petroleum Products Distillation and Vapor Pressure Measurement in Petroleum Products ASTM International 100 Barr Harbor. PUBLICATION, Manual on Distillation and Vapor Pressure Measurement in Petroleum Products, was spon- sored by ASTM International Committee D02 on Petroleum Products and Lubricants, and edited by Rey. Sampling, and Sample Handling 65 Calculation, Report, Precision, and Bias 65 Other Vapor Pressure Measurements 65 ASTM D2878—Estimating Apparent Vapor Pressures and Molecular Weights of Lubricating