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Methods for Geochemical Analysis \ o 70 n m O n U.S. GEOLOGICAL SURVEY BULLETIN 1770 o r Methods for Geochemical Analysis Edited by PHILIP A. BAEDECKER Analytical methods used in the Geologic Division laboratories of the U.S. Geological Survey for the inorganic chemical analysis of rock and mineral samples U.S. GEOLOGICAL SURVEY BULLETIN 1770 DEPARTMENT OF THE INTERIOR DONALD PAUL MODEL, Secretary U.S. GEOLOGICAL SURVEY Dallas L. Peck, Director UNITED STATES GOVERNMENT PRINTING OFFICE: 1987 For sale by the Books and Open-File Reports Section, U.S. Geological Survey, Federal Center, Box 25425, Denver, CO 80225 Library of Congress Cataloging in Publication Data Methods for geochemical analysis. (U.S. Geological Survey bulletin ; 1770) Bibliography: p. Supt. of Docs, no.: I 19.3:1770 1. Geochemistry, Analytic. I. Baedecker, Philip A. II. Series. QE75.B9 no. 1770 [QE516.3] 557.3s 87-600387 [551.9] CONTENTS INTRODUCTION P. A. Baedecker INI CHAPTER A Analysis of geologic materials by direct-current arc emission spectrography and spectrometry Al D. W. Golightly, A. F. Dorrzapf, Jr., R. E. Mays, T. L. Fries, and N. M. Cbnklin CHAPTER B Inductively coupled plasma-atomic emission spectrometry Bl F. E. Lichte, D. W. Golightly, and P. J. Lamothe CHAPTER C Atomic absorption methods Cl P. J. Aruscavage and J. G. Crock CHAPTER D Chemical methods of separation for optical emission, atomic absorption spectrometry, and colorimetry Dl S. A. Wilson, J. S. Kane, J. G. Crock, and D. B. Hatfield CHAPTER E Analysis of geologic materials by wavelength-dispersive X-ray fluorescence spectrometry El J. E. Taggart, Jr., J. R. Lindsay, B. A. Scott, D. V. Vivit, A. J. Bartel, and K. C. Stewart CHAPTER F Energy-dispersive X-ray fluorescence spectrometry Fl R. G. Johnson and B.-S. L. King CHAPTER G Major and minor elements requiring individual determination, classical whole rock analysis, and rapid rock analysis Gl L. L. Jackson, F. W. Brown, and S. T. Neil CHAPTER H Instrumental neutron activation analysis of geochemical samples HI P. A. Baedecker and D. M. McKown CHAPTER I Determination of uranium and thorium by delayed neutron counting II D. M. McKown and H. T. Millard, Jr. CHAPTER J Radiochemical neutron activation analysis of geologic materials Jl G. A. Wandless CHAPTER K Isotope-dilution mass spectrometry Kl J. A. Philpotts Any use of trade names is for descriptive purposes only and does not imply endorsement by the U.S. Geological Survey Volume Contents INTRODUCTION By P. A. Baedecker The laboratories for analytical chemistry within the the quality of that data and the challenges and complexity Geologic Division of the U.S. Geological Survey are of analytical chemistry as a scientific discipline. The administered by the Office of Mineral Resources. The committee report stated, "...clearly, an increased under­ laboratory analysts provide analytical support to those standing of modern analytical techniques by all potential programs of the Geologic Division that require chemical users of chemical data in the Geologic Division is a highly information and conduct basic research in analytical and desirable goal. Toward that end we are recommending geochemical areas vital to the furtherance of Division that a publication entitled Methods for Geochemical Anal­ program goals. Laboratories for research and geochemi­ ysis be prepared, which will cover all aspects of the cal analysis are maintained at the three major centers in techniques currently available." This volume is in Reston, Virginia, Denver, Colorado, and Menlo Park, response to that recommendation. California. The Division has an expertise in a broad In many respects, the current volume supplants two spectrum of analytical techniques, and the analytical previous publications that were designed to familiarize research is designed to advance the state of the art of scientists within the Geologic Division with the analytical existing techniques and to develop new methods of capabilities that were (or are) available in the laboratories analysis in response to special problems in geochemical of the Division. The first edition of the Manual of Labo­ analysis. The geochemical research and analytical results ratory Services of the Division's Geochemistry and Petrol­ are applied to the solution of fundamental geochemical ogy Branch was published in 1956. That document was problems relating to the origin of mineral deposits and subsequently revised in 1974 by the Office of Geoche­ fossil fuels, as well as to studies relating to the distribution mistry and Geophysics. This volume is more restricted of elements in varied geologic systems, the mechanisms by than either of the above publications in that the previous which they are transported, and their impact on the reports contained sections on geochronology, electron environment. optics, X-ray crystallography and diffraction, mineralogic In 1984, a review of the role of analytical chemistry and petrographic analysis, organic analysis, thermody­ within the Geologic Division was conducted by an ad hoc namics, geophysical methods, and so forth; the coverage committee of senior Division managers. The committee offered by this volume, however, is limited to modern concluded that a lack of familiarity on the part of those methods of inorganic analysis. In the preparation of submitting samples for geochemical analysis with the Methods for Geochemical Analysis, the authors also have wide range of analytical techniques available could result adopted a different approach to the subject matter. in the misapplication of some techniques to various Rather than to provide a simple documentation of avail­ geochemical problems; for example, highly precise able services, they have attempted to treat each topic in analyses could be applied to problems for which only much greater depth. Thus, each chapter contains sections approximate answers are needed or can be obtained in on fundamental principles, an overview of the method as other ways. Conversely, investigators might request too practiced in each center, the limitations of the technique few analyses or data by techniques that are not precise (such as matrix, chemical, and spectral interferences), enough for the problem at hand; for example, potential and the sensitivity, precision, and accuracy of each tech­ waste occurs when data on a desired element, such as nique. The goal was to prepare a single volume that would cesium, is obtained by requesting a broad-spectrum provide the nonchemist reader with a broad coverage of Instrumental Neutron Activation Analysis, which requires geochemical analysis as a scientific discipline, a good perhaps an order of magnitude more time and effort than understanding of the inherent difficulty of analyzing if cesium alone were determined by the same method or complex geologic matrices that are highly variable in possibly another. In addition to these concerns, analytical composition, and sufficient technical detail to understand chemists often are concerned that those who use analyt­ the factors that can affect the quality (precision and ical data have little appreciation for the factors that affect accuracy) of the analysis of the geologic sample. To again Introduction INI quote the 1984 analytical chemistry review report, "It is As an introduction to the topics covered in this hoped that a widespread familiarization with this docu­ publication and as a guide to alternative methods of ment by members of the Division will provide the basis for analysis, the following table may prove useful. Listed for a more informed dialogue on chemical problems between each element are estimates of sensitivity for the most geologists and analytical chemists." common techniques used for their determination in geo- At this point, I think it worthwhile to repeat a few chemical samples. The term "sensitivity" is a general term sections from the introduction to the 1956 Manual of for the lower limits of measurement for a given analytical Laboratory Services because, although the technology of test and is most often expressed as either a "detection analytical chemistry has changed dramatically, the follow­ limit" or "determination limit." The detection limit is the ing general comments regarding routine and nonroutine minimum concentration of analyte required for a positive analysis and analytical accuracy remain as valid today as decision that an analysis indicates a qualitative detection, they were 30 years ago: and the determination limit is a higher level of concentra­ The service work of the Branch falls into two tion that will give a satisfactory quantitative result with a categories, routine and research (including custom), given relative standard deviation (such as ±10 percent). which are neither completely nor even too sharply Both estimates are dependent on the analytical "noise" separated at any time. Depending on the circum­ associated with measurement above the background or stances, a routine determination may become a "blank" level for a given analytical procedure, and, for research problem, or what was originally a research multielement analytical methods, the sensitivity limits are problem may in time become a routine process. The often matrix dependent and, therefore, may vary from Branch is constantly testing new methods with the aim sample to sample. The sensitivity levels provided by the of developing rapid routine determinations as the geol­ table should be looked upon as "working" determination ogists indicate their need for them....Research determi­ limits for a silicate rock matrix. As stated above, the nations are those made by methods we do not ordinarily method with the greatest sensitivity should not be identi­ use; they may include determinations made on samples fied as the "best" method for any given problem. The of unusual composition, or the analysis for some ele­ most sensitive methods are most often the most labor ment or elements at lower concentration ranges than intensive. The method of choice is based on the answers to previously handled, or the development of new chemi­ the following questions: What minimum levels of preci­ cal, spectrographic, mineralogical, X-ray, or other meth­ sion, accuracy, and sensitivity are required to solve the ods.
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