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ASTM Selected Technical Papers
Fifty Years of Progress in Metallographic Techniques
By
Committee E-4
Committee E-4
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ISBN-10:
0-8031-6181-6
ISBN:
978-0-8031-6181-8
No. of Pages:
417
Publisher:
ASTM International
Publication date:
1968

The magnitude of systematic and statistical errors in electron probe microanalysis due to faulty specimen preparation is discussed theoretically and experimentally. It is shown that this error increases as the energy of the X-ray line being monitored decreases and also as the X-ray emergence angle decreases. Specific specimens are chosen to illustrate various preparation problems in metallurgy, petrography, and biology. Generalizing from these, certain useful instrumental adjuncts can be listed; these adjuncts tend to allow the effects of the specimen surface on the analysis to be controlled more rigorously. Several conductive coatings commonly used are evaluated in terms of electron and optical transparency, adherence, X-ray attenuation, and thermal and electrical conductivity. Finally, a brief survey of standards employed in electron probe microanalysis is made. Situations for which nonelemental standards are required are outlined. The choice of standards for various types of work is discussed.

1.
Birks
,
L. S.
and
Seebold
,
R. E.
, “
Effect of Take-Off Angle on Electron Probe Calibration
,”
Analytical Chemistry
 0003-2700, Vol.
33
,
1961
, p. 687.
2.
Yakowitz
,
H.
and
Heinrich
,
K. F. J.
, “
Quantitative Electron Probe Microanalysis: Absorption Correction Uncertainty
,”
Mikrochimica Acta
 0026-3672, in press.
3.
Yakowitz
,
H.
 et al
, “
Homogeneity Characterization of NBS Spectrometric Standards II: Cartridge Brass and Low-Alloy Steel
,” National Bureau of Standards Miscellaneous Publication 260-10, issued
14
12
1965
, 28 pp.
4.
Picklesimer
,
M. L.
and
Hallerman
,
G.
, “
The Influence of the Preparation of Metal Specimens on the Precision of Electron Probe Microanalysis
,” Report ORNL-TM-1591,
1966
, 46 pp.
5.
Kiessling
,
R.
and
Lange
,
N.
, “
Non-Metallic Inclusions in Steel
,” Special Report 90,
The Iron and Steel Institute
, London SWI,
1964
.
6.
Perryman
,
E. C. W.
, “
Recent Developments in Metallography
,”
Metal Industry, London
, Vol.
79
,
1951
, pp. 23, 71, 111, 131.
7.
Hutchins
,
G. A.
, “
Thickness Determination of Thin Films by Electron Probe Microanalysis
,”
The Electron Microprobe
,
McKinley
,
T. D.
,
Heinrich
,
K. F. J.
, and
Wittry
,
D. B.
, eds.,
Wiley
,
New York
,
1966
, p. 390.
8.
Picklesimer
,
M. L.
, “
Anodizing as a Metallographic Technique for Zirconium Base Alloys
,” Report ORNL-2296,
1957
.
9.
Wyman
,
L. L.
 et al
, “
Intermediate Phases in Superconducting Niobium-Tin Alloys
,”
Journal of Research, National Bureau of Standards
 0160-1741 Vol.
66A
,
1962
, p. 351.
10.
Macres
,
V. G.
, presented at Methods and Applications of Electron Probe Analysis Course,
University of Southern California
,
1962
.
11.
Tousimis
,
A. I.
, “
Electron Probe X-ray Microanalysis of Medical and Biological Specimens
,”
X-ray and Electron Probe Analysis
, ASTM STP 349,
American Society for Testing and Materials
,
1963
, p. 193.
12.
Hall
,
T. A.
,
Hale
,
A. J.
, and
Switsur
,
V. R.
, “
Some Applications of Microprobe Analysis in Biology and Medicine
,”
The Electron Microprobe
,
McKinley
,
T. D.
,
Heinrich
,
K. F. J.
, and
Wittry
,
D. B.
, eds.,
Wiley
,
New York
,
1966
, p. 805.
13.
Duncumb
,
P.
and
Melford
,
D. A.
, “
A Simple Correction Procedure for Ultra-soft X-ray Microanalysis
,”
Tube Investment Research Laboratories
, Technical Report 195,
1965
, 27 pp.
14.
Nelms
,
A. T.
, “
Energy Loss and Range of Electrons and Positions
,”
National Bureau of Standards
, Circular 577,
1956
, 30 pp.
15.
Heinrich
,
K. F. J.
, “
X-ray Absorption Uncertainty
,”
The Electron Microprobe
,
McKinley
,
T. D.
,
Heinrich
,
K. F. J.
, and
Wittry
,
D. B.
, eds.,
Wiley
,
New York
,
1966
, p. 296.
16.
Adler
,
I.
, “
Electron Probe Analysis of Minerals
,”
X-ray and Electron Probe Analysis
, ASTM STP 349,
American Society for Testing and Materials
,
1963
, p. 183.
17.
Smith
,
J. V.
, “
Production of X-rays
,” notes of a course taught at
California Institute of Technology
,
Pasadena, Calif.
,
04
1965
, pp. 16, 29.
18.
Tousimis
,
A. J.
, Symposium Specimen Preparation at First National Conference on Electron Probe Microanalysis,
College Park, Md.
,
1966
. (Available from Biodynamics Research Corp., Rockville, Md.)
19.
Wittry
,
D. B.
, “
Methods of Quantitative Electron Probe Analysis
,”
X-ray and Electron Probe Analysis
, ASTM STP 345,
American Society for Testing and Materials
,
1963
, p. 128.
20.
Adler
,
I.
and
Goldstein
,
J. I.
, “
Absorption Tables for Electron Probe Microanalysis
,” NASA Technical Note D-2984,
1965
.
21.
Macres
,
V. G.
, “
Application of Electron Microanalysis to Cu-Zn Diffusion
,” Sc.D. thesis,
Massachusetts Institute of Technology
, Cambridge, Mass.,
1958
.
22.
Goldstein
,
J. I.
and
Wood
,
F.
, “
Experimental Procedure for Trace Determination with the Electron Probe
,” presented at First National Conference on Electron Probe Microanalysis,
College Park, Md.
,
05
1966
.
23.
Goldstein
,
J. I.
,
Majeske
,
F. J.
, and
Yakowitz
,
H.
, “
Preparation of Electron Probe Microanalyzer Standards Using a Rapid Quench Method
,”
Advances in X-Ray Analysis
 0376-0308, Vol.
10
,
1967
, p. 431.
24.
ASTM
, “
Methods of Metallographic Specimen Preparation
,” ASTM STP 285,
1960
, 134 pp. Includes eight articles and discussion-a paper on ceramic materials is also given.
25.
Phillips
,
V. A.
, “
Direct Observations on Structure of Ultramicrotomed Metals and Alloys
,” ASTM STP 317,
1962
, p. 34.
26.
Anderson
,
R. L.
, “
Revealing Microstructures in Metals
,”
Westinghouse Research Laboratories
, Scientific Paper 425-COOO-P2,
1961
, 344 pp. Contains a comprehensive bibliography and 106 general references.
27.
Cadwell
,
D. E.
and
Weiblen
,
P. W.
, “
Diamond Disc Preparation of Polished Thin Sections for Electron Microprobe Analysis
,”
Economic Geology
 0361-0128, Vol.
60
,
1965
, p. 1320.
28.
Frazier
,
P. D.
, “
Electron Probe Analysis of Human Teeth: Some Problems in Sample Preparation
,”
Norelco Reporter
, Vol.
13
,
1966
, p. 25.
29.
Holland
,
L.
,
Vacuum Deposition of Thin Films
,
Wiley
,
New York
,
1956
.
30.
Kehl
,
G. L.
,
Principles of Metallographic Laboratory Practice
, 3rd ed.,
McGraw-Hill
,
New York
,
1949
.
31.
Laidley
,
R. A.
,
Hoffmann
,
V. J.
, and
Wyckoff
,
R. W. G.
, “
Some Applications of the Electron Probe to Minerals
,”
Norelco Reporter
, Vol.
11
,
1964
, p. 104.
32.
Taylor
,
C. M.
and
Radtke
,
A. S.
, “
Preparation and Polishing of Ores and Mill Products for Microscopic Examination and Electron Microprobe Analysis
,”
Economic Geology
 0361-0128, Vol.
60
,
1965
, p. 1306.
33.
Tegart
,
W.
,
Electrolytic and Chemical Polishing of Metals in Research and Industry
, 2nd rev. ed.,
Pergamon Press
,
London and New York
,
1959
.
34.
See also Symposium on Specimen Preparation presented at the First National Conference on Electron Probe Microanalysis: (1) Metallurgy by M. L. Picklesimer (2) Mineralogy by K. Frederiksson and G. Moreland, and (3) Biology by A. J. Tousimis.
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