Statistical Considerations in Microanalysis by Energy-Dispersive 
Spectrometry

Lifshin, Eric; Doganaksoy, Necip; Sirois, Jane; Gauvin, Raynald

doi:10.1017/s1431927698980576

Cited by 20 publications

(10 citation statements)

References 6 publications

(9 reference statements)

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“…This value is taken from a consideration of a large number of WDS measurements, in which 95% of the values were within ± 5% relative of the accepted value. Other authors suggest that, in the best case, WDS analysis is capable of a 2% relative error (Lifshin et al 1999). The latter authors did not comment on quantitative EDS measurements.…”

Section: Introductionmentioning

confidence: 99%

Accuracy and precision of quantitative energy‐dispersive x‐ray spectrometry in the environmental scanning electron microscope

Carlton¹,

Lyman

Roberts

2004

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The accuracy and precision of quantitative energy-dispersive x-ray spectrometry in the environmental scanning electron microscope have been estimated using a series of copper / gold alloys of known composition. The mean values (five to six replicate experiments) had relative errors within +/- 5%, and most were within +/- 3.5%. All relative standard deviations were < 5% and most were < 3%. Since the standard specimens were large (approximately 500 microm) in diameter, electron scattering in the 2 torr of water vapor above the specimen did not affect the results. This level of accuracy and precision was possible only by using a novel specimen surface charge neutralization scheme.

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Section: Introductionmentioning

confidence: 99%

Accuracy and precision of quantitative energy‐dispersive x‐ray spectrometry in the environmental scanning electron microscope

Carlton¹,

Lyman

Roberts

2004

Scanning

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“…Relationship between detection limit (in oxides of Al, Ti, Ca, P, Na, Cr, Ni, Mn, Zn, Co) calculated by equation (1) The accuracy of measurement by WDS for trace as well as for major elements depends on many factors including sample preparation, the type and thickness of the coating, stability under the electron beam, accurate knowledge of the composition of the primary standards, and the quality of algorithms used for matrix (i.e., the ZAF, φ(ρz)) and interference corrections (e.g., [1,10,[45][46][47]). Jercinovic et al [10] showed that the accuracy of EPMA decreases at low concentrations because most random and systematic errors encountered during major element analysis are magnified at trace level and specific errors appear.…”

Section: Figurementioning

confidence: 99%

Trace element analysis by EPMA in geosciences: detection limit, precision and accuracy

Batanova

Sobolev

Magnin

2018

IOP Conf. Ser.: Mater. Sci. Eng.

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Abstract. Use of the electron probe microanalyser (EPMA) for trace element analysis has increased over the last decade, mainly because of improved stability of spectrometers and the electron column when operated at high probe current; development of new large-area crystal monochromators and ultra-high count rate spectrometers; full integration of energy-dispersive / wavelength-dispersive X-ray spectrometry (EDS/WDS) signals; and the development of powerful software packages. For phases that are stable under a dense electron beam, the detection limit and precision can be decreased to the ppm level by using high acceleration voltage and beam current combined with long counting time. Data on 10 elements (Na, Al, P, Ca, Ti, Cr, Mn, Co, Ni, Zn) in olivine obtained on a JEOL JXA-8230 microprobe with tungsten filament show that the detection limit decreases proportionally to the square root of counting time and probe current. For all elements equal or heavier than phosphorus (Z = 15), the detection limit decreases with increasing accelerating voltage. The analytical precision for minor and trace elements analysed in olivine at 25 kV accelerating voltage and 900 nA beam current is 4 -18 ppm (2 standard deviations of repeated measurements of the olivine reference sample) and is similar to the detection limit of corresponding elements. To analyse trace elements accurately requires careful estimation of background, and consideration of sample damage under the beam and secondary fluorescence from phase boundaries. The development and use of matrix reference samples with well-characterised trace elements of interest is important for monitoring and improving of the accuracy. An evaluation of the accuracy of trace element analyses in olivine has been made by comparing EPMA data for new reference samples with data obtained by different in-situ and bulk analytical methods in six different laboratories worldwide. For all elements, the measured concentrations in the olivine reference sample were found to be identical (within internal precision) to reference values, suggesting that achieved precision and accuracy are similar. The spatial resolution of EPMA in a silicate matrix, even at very extreme conditions (accelerating voltage 25 kV), does not exceed 7 -8 µm and thus is still better than laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) or secondary ion mass spectrometry (SIMS) of similar precision. These make the electron microprobe an indispensable method with applications in experimental petrology, geochemistry and cosmochemistry. IntroductionThere is no rigorous definition of a trace element, and typically accepted definitions depend on the field of science. For example, in analytical chemistry, a trace element is one whose concentration is less than 100 parts per million (ppm) or less than 100 micrograms per gram; while in geochemistry, a trace element has a concentration less than 1000 ppm or 0.1 wt% of a rock's mass and substitutes for major elements in the rock-forming minerals. Reed [1] defines a...

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“…The precision of EDS depends on the X-ray counting statistics and is improved by long acquisition times [7]. Given the high number of spectra in a 3-D EDS stack, the time spent per spectrum needs to be limited to keep the total acquisition time reasonable.…”

Section: Introductionmentioning

confidence: 99%

Three-dimensional chemical analysis of laser-welded NiTi–stainless steel wires using a dual-beam FIB

et al. 2013

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The biomedical industry has an increasing demand for processes to join dissimilar metals, such as laser welding of NiTi and stainless steel wires. A region of the weld close to the NiTi interface, which previously was shown to be prone to cracking, was further analyzed by energy dispersive spectrometry (EDS) extended in the third dimension using a focused ion beam. As the spatial resolution of EDS analysis is not precise enough to resolve the finest parts of the microstructure, a new segmentation method that uses in addition secondaryelectron images of higher spatial resolution was developed. Applying these tools, it is shown that this region of the weld close to the NiTi interface does not comprise a homogeneous intermetallic layer, but is rather constituted by a succession of different intermetallics, the composition of which can be directly correlated with the solidification path in the ternary Fe-Ni-Ti Gibbs simplex.

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Statistical Considerations in Microanalysis by Energy-Dispersive Spectrometry

Cited by 20 publications

References 6 publications

Accuracy and precision of quantitative energy‐dispersive x‐ray spectrometry in the environmental scanning electron microscope

Accuracy and precision of quantitative energy‐dispersive x‐ray spectrometry in the environmental scanning electron microscope

Trace element analysis by EPMA in geosciences: detection limit, precision and accuracy

Three-dimensional chemical analysis of laser-welded NiTi–stainless steel wires using a dual-beam FIB

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