ANALYTICAL PERFORMANCE OF A HANDHELD EDXRF SPECTROMETER WITH MINIATURE X-RAY TUBE EXCITATION
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1 JPACSM 56 ANALYTICAL PERFORMANCE OF A HANDHELD EDXRF SPECTROMETER WITH MINIATURE X-RAY TUBE EXCITATION Volker Thomsen and Debbie Schatzlein NITON LLC Billerica, MA ABSTRACT The analytical performance of a handheld energy dispersive x-ray fluorescence (EDXRF) spectrometer using miniature x-ray tube excitation is presented in terms of precision, accuracy, long-term stability, and detection limits. The new spectrometer also compares favorably with laboratory arc/spark spectrometers in terms of precision and accuracy. INTRODUCTION The advent of field portable x-ray fluorescence spectrometers using x-ray tube excitation was successfully predicted several years ago [1]. In this paper we present data generated by such a new generation of handheld EDXRF spectrometer using miniature x-ray tube excitation. Analytical data from alloy analysis is presented showing the precision, accuracy, long-term stability and detection limits for this instrument. In addition, a comparison with laboratory optical emission spectrometers is presented. EXPERIMENTAL The experimental results presented here were produced with a NITON Model XLt 8 Series analyzer. The instrument itself will not be discussed in this note as this information may be found elsewhere [2]. We note, however, that excitation was provided by a miniature x- ray tube with a silver transmission anode, run at 35 kv and 5 µa. Detection was by means of a thermoelectrically cooled Si PIN detector. Unless otherwise stated, all results presented in this paper are based on 2 second measurement times. All precision data consists of 11 replicate measurements. Samples used were alloys of iron, nickel, and cobalt, generally superalloys. Results: Precision Table 1 shows precision data for several alloys in standard tabular format with mean, one standard deviation, and percent relative standard deviation (RSD). [Note: %RSD is defined as 1 times the standard deviation divided by the mean.] We note RSDs of less than one percent for all elements at major concentrations (greater than five percent) in all cases but one (Ni in Stellite 25). The bar graph of Figure 1 shows a precision comparison for four elements in Hastelloy X. We compare the new miniature x-ray tube excitation with the previous generation of handheld EDXRF spectrometer (model XL), which used 1 mci Cd-19 radioisotope excitation. We see an average factor two improvement in the precision with the x-ray tube excitation. Results: Accuracy Correlation curves provide the best means of assessing the accuracy of an analytical method. Such curves plot the certified or nominal concentrations along the x-axis versus the measured values along the y-axis. To quantify the accuracy as expressed by the correlation curve, there are two criteria: a) A correlation coefficient (R²) must be calculated. A value of 1. indicates perfect agreement and while a zero means no correlation. Good agreement or accuracy, in our case, is ensured with a correlation coefficient greater than about.99. b) The slope of the regression line calculated through the data points must approximate 1. and the y- intercept. Deviations from this 45º straight line would indicate bias in the analytical method under investigation. Figures 2 and 3 show correlation curves for the elements molybdenum and chromium in alloys of iron, cobalt, and nickel. The agreement between measured and certified values is excellent and the conditions a) and b) of the preceding paragraph are clearly met. Furthermore, it is interesting to note that not only do these curves cover a wide range of alloys, but they are also not limited to a single matrix (base).
2 JPACSM 57 Hastelloy X Incoloy 825 Stellite 25 Elements Mean Std.Dev %RSD Mean Std.Dev %RSD Mean Std.Dev %RSD... Ti Cr Mn Fe Co Ni Cu Mo Nb W Table 1: Precision Data as Measured for Several Superalloys Standard Deviations Cr (22%) Fe (2%) Mo (9%) Ni (45%) Figure 1: Comparative Precision, Miniature X-ray Tube (blue) vs. Radioisotope
3 JPACSM y =.9948x R 2 =.9995 XLt Results (%) Certified Values (%) Figure 2: Correlation Curve for Molybdenum in Superalloys y =.9971x R 2 =.9989 XLt Results (%) Certified Values (%) Figure 3: Correlation Curve for Chromium in Superalloys Results: Long Term Stability Figures 4 and 5 show long-term stability for the elements nickel and iron in various alloys over a 24-hour period. In this test, seven different alloys were analyzed three times each during 15 time periods covering the 24 hours. Each individual reading is plotted for each measurement time. Note that there was a three hour pause between measurement set 7 and set 8 during which the instrument was shut off and transported. The same is true between set 11 and 12. The instrument displays excellent long-term stability. In fact, for major alloying elements (C i > 1%), we find that the instrument long-term stability is essentially identical to the short-term precision (Table 2). Here long-term stability is as defined above and the shortterm precision results noted are the result of 11 replicate 2 second measurements.
4 JPACSM Concentration Nickel (%) SS39 INVAR36 Monel4 HastC276 Linear (SS39) Linear (INVAR36) Linear (Monel4) Linear (HastC276) Time (Hours) Figure 4: Long-Term Stability of Nickel in Various Alloys Concentration Iron (%) SS39 Tool steel Monel 4 Hast C Linear (SS39) Linear (Tool steel) Linear (Monel 4) Linear (Hast C) Time (Hours) Figure 5: Long-Term Stability of Iron in Various Alloys
5 JPACSM 6 Element: Nickel Chromium Iron Alloy: SS39 Invar 36 C276 SS39 Tool C276 SS39 Monel C276 Short Mean Term Std.Dev %RSD Long Mean Term Std.Dev %RSD Table 2: Comparison of Short Term Precision and Long Term Stability Results: Detection Limits and %RSD vs. Concentration Curves Because of the wealth of precision data generated in this study, it was possible to produce curves such as those shown in Figure 6 and 7. These have the form typical of a graph of precision vs. concentration with the precision decreasing (i.e., percent RSD increasing) with decreasing concentration. At the limit of detection (LOD) the %RSD is, by definition, 33%. Therefore one could use such a curve to determine the limit of detection. In the case shown for chromium in nickel-base alloys, we compute an LOD of.47% from this curve. This compares quite favorably with.52%, the LOD for Cr in Fe-base found using the traditional method of three times the standard deviation of the blank times the sensitivity (see Table 3). Although data is not directly available for LODs in Ni-base alloys as determined in the traditional manner, we expect them to be comparable to those found for Fe-base. 3 Relative Standard Deviation (%RSD) y = 5.511x R 2 = Concentration Tungsten (%) 18 Figure 6: Concentration vs. %RSD for Tungsten in Nickel-base Alloys
6 JPACSM Relative Standard Deviation (%RSD) y = 4.286x R 2 = Concentration Chromium (%) Figure 7: Concentration vs. %RSD for Chromium in Nickel-base Alloys Element Fe-Base Ni-Base Cu-Base Ti.14 V.64 Cr Mn Fe.32 Co.2 Ni Cu.97 Zn.27 Zr.96 Nb.2 Mo.28.9 Sn.18 W Pb.42 Table 3: LODs (weight percent) in Metal Matrices
7 JPACSM 62 Results: Comparison with Laboratory Instrumentation Table 4 presents a comparison of the handheld EDXRF spectrometer with miniature x-ray tube excitation and various laboratory spectrometers. Spectrometer A Spectrometer B Spectrometer C Handheld Spark OES Spark OES Spark OES Element EDXRF PMT, ca PMT, ca Benchtop, CCD Ni Mean Std.Dev %RSD Cr Mean Std.Dev %RSD Mo Mean Std.Dev %RSD Fe Mean Std.Dev %RSD W Mean Std.Dev %RSD Mn Mean Std.Dev %RSD Table 4: Comparison With Laboratory Spectrometers Spectrometer A is a floor-standing arc/spark optical emission spectrometer of mid-198s vintage. The vacuum optical system has a.75 meter focal length and uses photomultiplier (PMT) detectors. Spectrometer B is a state-of-the-art laboratory arc/spark optical emission spectrometer produced in about It contains four.5 meter optical systems plus a monochromator, all with PMT detectors. Spectrometer C is a benchtop arc/spark spectrometer with a.35 meter focal length optical system utilizing CCD detectors. All three spectrometers employ a uni-directional spark discharge in an argon atmosphere. The results shown are for eleven measurements on a single sample of Hastelloy C-276. The handheld EDXRF spectrometer used 2 second integration times. The arc/spark used times appropriate for this technique, generally about 15 second pre-spark and 5 second integration, making the total time per measurement about the same. We see that the handheld EDXRF spectrometer with miniature x-ray tube excitation compares favorably in terms of precision with laboratory spectrometers.
8 JPACSM 63 SUMMARY We note first that handheld EDXRF is not appropriate for the light elements (Z < 2) due to a lack of gas purge or vacuum and detector resolution. It is also not the method of choice for trace element analysis in metals, where the element concentration is less than about 5 ppm. However, for the elements and concentration ranges over which this instrumental method is valid, laboratory quality analytical data may be produced. The latest generation of hand-held EDXRF instrumentation using minature x-ray tube excitation demonstrates substantial improvement in analytical performance over the previous generation. This performance compares favorably with that of laboratory spectrometers. REFERENCES 1. Piorek, S. Field-Portable X-Ray Fluorescence Spectrometry: Past, Present, and Future. Field Analytical Chemistry and Technology, 1(6): , Piorek, S. A Lightweight, Hand-Held Portable X-Ray Analyzer with Minature X-Ray Tube. The European Conference on Energy Dispersive X-Ray Spectrometry, Berlin, Germany, June 16-21, Thomsen, V., Schatzlein, D. Analytical Performance of a New Generation of Handheld EDXRF Spectrometers. Paper F-6, Denver X- ray Conference, Colorado Springs, CO, July 22. ACKNOWLEDGEMENT Portions of this paper were presented at the 22 Denver X-ray Conference [3].
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