Time-Resolved Laser-Induced Breakdown Spectrometry for the Rapid Determination of Beryllium in Beryllium-Copper Alloys

Abstract

Time-resolved laser-induced breakdown spectrometry has been combined with the long spark technique and applied to the rapid determination of beryllium in beryllium-copper alloys. A calibration curve was developed which related the beryllium concentration in a solid copper matrix to the Be(I) 234.9-nm to Cu(II) 235.7-nm intensity ratio. The beryllium concentrations ranged from 0.001 to 0.22%. For the lowest concentration the relative standard deviation of replicate samples was 7%, implying a detection limit of 0.0002% (2 ppm) at a signal-to-noise ratio of 3. The excitation temperature was determined from Boltzmann plots on Cu(I) and Cu(II), assuming local thermodynamic equilibrium. The values from the two spectra agreed well, and averaged to 13,850 K at 1 μS into the plasma lifetime.

Quantitative absorption spectroscopy of laser-produced plasmas

“…The minimal preparation and small sample size required for LIBS study of beryllium also enables further study of its energetic properties and kinetic behavior in high-temperature, high-pressure environment using this apparatus whilst minimizing exposure to the sample. There has previously been work involving the use of LIBS for detection of beryllium to ensure low levels for maintaining safe work environments [70][71][72]. A bulk Be sample was ablated in H 2 at 100 torr with the same setup and laser conditions as for the previous samples.…”

History

“…These included analysis of beryllium in beryllium-copper alloys (Millard et al, 1986) and detection of cadmium, lead and zinc (Essien et al, 1988). The superconducting materials community published many papers on laser ablation for deposition of superconducting thin films, and sometimes addressed the optical emission as a diagnostic technique for process monitoring.…”

Effect of atmosphere on collinear double-pulse laser-induced breakdown spectroscopy

“…No sample preparation is necessary for LIBS, making it a very popular technique in many applications that include environmental monitoring [10][11][12], material analysis [13], forensics [14], characterization of fossils [15], biological identification [16,12], analysis of works of art [17], and space exploration [18,19]. Though the applications of LIBS are vast, LIBS suffers a disadvantage in sensitivity when compared to other spectroscopy techniques, such as inductively coupled plasma atomic emission spectroscopy (ICP-AES) [20][21][22][23][24]. Double-pulse laser-induced breakdown spectroscopy (DP-LIBS) is typically used to improve sensitivity compared to single-pulse LIBS (SP-LIBS) [25].…”