Modern Instrumental Methods of Elemental Analysis of Petroleum Products and Lubricants

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STP 1109 Modern Instrumental Methods of Elemental Analysis of Petroleum Products and Lubricants R. A. Nadkarni, editor ASTM Publication Code Number (PCN): 04-0t 1090-12 ASTM 1916 Race Street Philadelphia, PA 19106

Library of Congress Cataloging-in-Publication Data Analysis of petroleum products and lubricants / R. A. Nadkarni, editor. "STP 1109." "The ASTM Symposium on Modern Instrumental Methods of Elemental Analysis of Petroleum Products and Lubricants was held in New Orleans, Louisiana, on 11-13 December 1989"--Foreword. Includes bibliographical references and index. ISBN 0-8031-1416-8 1. Petroleum products--analysis--congresses. 2. Lubrication and lubricants--analysis--congresses. I. Nadkarni, R.A. II. ASTM Symposium on Modern Instrumental Methods of Elemental Analysis of Petroleum Products and Lubricants (1989: New Orleans, La.) III. American Society for Testing and Materials. TP691.A68 1991 665.5--dc20 91-10488 CIP Copyright 9 AMERICAN SOCIETY FOR TESTING AND MATERIALS, Philadelphia, Pa. All rights reserved. This material may not be reproduced or copied, in whole or in part, in any printed, mechanical, electronic, film, or other distribution and storage media, without the written consent of the publisher. Photocopy Rights Authorization to photocopy items for internal or personal use, or the internal or personal use of specific clients, is granted by the AMERICAN SOCIETY FOR TESTING AND MATERIALS for users registered with the Copyright Clearance Center (CCC) Transactional Reporting Service, provided that the base fee of $2.50 per copy, plus $0.50 per page is paid directly to CCC, 27 Congress St., Salem, MA 01970; (508) 744-3350. For those organizations that have been granted a photocopy license by CCC, a separate system of payment has been arranged. The fee code for users of the Transactional Reporting Service is 0-8031-1416-8/91 $2.50 +.50. Peer Review Policy Each paper published in this volume was evaluated by three peer reviewers. The authors addressed all of the reviewer's comments to the satisfaction of both the technical editor(s) and the ASTM Committee on Publications. The quality of the papers in this publication reflects not only the obvious efforts of the authors and the technical editor(s), but also the work of these peer reviewers. The ASTM Committee on Publications acknowledges with appreciation their dedication and contribution to time and effort on behalf of ASTM. Printed in Baltimore, MD May 1991

Foreword The ASTM Symposium on Modern Instrumental Methods of Elemental Analysis of Petroleum Products and Lubricants was held in New Orleans, Louisiana, on 11-13 December 1989. The event was sponsored by ASTM Committee D-2 on Petroleum Products and Lubricants. R. A. Nadkarni, Exxon Chemical Company, served as symposium chairman and has also edited this publication.

Contents Overview A Review of Modern Instrumental Methods of Elemental Analysis of Petroleum Related Material: Part l--occurrence and Significance of Trace Metals in Petroleum and Lubricants--R. A. NADKARNI A Review of Modern Instrumental Methods of Elemental Analysis of Petroleum Related Material: Part ll--analytical Techniques--R. A. NADKARNI Analysis of Additive Metals in Lubricating Oils--J. R. MACKEY, S. T. WATT, C. A. CARDY, S. I. SMITH, AND C. A. MEUNIER Methods Development for Trace Metal Characterization of Crude Oil by Inductively Coupled Plasma Atomic Emission Spectroscopy--M. GONZALES AND A. W. LYNCH Automated Rapid Muitielement Analysis of Oils for Wear Metals by Flame Atomic Absorption Using a Single Aspiration Per Sample--L M. CARTER, W. BATIE, AND A. E. BERNHARD Correlation Between Inductively Coupled Plasma and Rotating Disk Electrode Spark Emission Spectrometry for Used Diesel Engine Oils--D. NYGAARD, F. BULMAN, AND T. ALAVOSUS Techniques to Improve the Ability of Spectroscopy to Detect Large Wear Particles in Lubricating Oils--M. LUKAS AND D. P. ANDERSON Elemental Analysis of Waste Oils by Inductively Coupled Plasma Mass Spectrometry--M. c. WILLIAMS Precious Metal Assay Analysis of Fresh Reforming Catalyst by X-Ray Fluorescence Spectrometry--F. c, McELROY AND J. M. MULHALL Analysis of Lubricant Additive Elements by X-Ray Fluorescence and Supporting Methods--J. R. SIEBER, S. G. SALMON, AND M. C. WILLIAMS Energy Dispersive X-Ray Fluorescence Spectrometric Determination of Vanadium, Nickel, and Iron in Petroleum and Petroleum Residua--J. v. SHAY AND P. W. WOODWARD 19 52 62 70 77 83 96 105 118 128

Elemental Analysis of Crude and Lubricating Oils by Energy Dispersive X-Ray Fluorescence--B. D. WHEELER 136 Improved Performance for Trace Halide Determination in Hydrocarbons-- G. G. OHLSON AND Y. TAKAHASHI 148

ISBN 0-8031-1416-8