Optimization of chemical and instrumental parameters in hydride generation laser-induced breakdown spectrometry for the determination of arsenic, antimony, lead and germanium in aqueous samples

Yeşiller, Semira Ünal; Yalçın, Şerife

doi:10.1016/j.aca.2013.02.014

Cited by 26 publications

(6 citation statements)

References 42 publications

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“…The details of the experimental set-up for continuous flow HG-LIBS system has been given elsewhere (Ünal and Yalçın 2010;Yeşiller and Yalçın 2013). The system is comprised a hydride generation unit, a plasma cell, and a detection unit.…”

Section: Methodsmentioning

confidence: 99%

“…To investigate the presence of alkali/alkali earth metals, namely Na, K, Ca, and Mg on arsenic signal intensity, initially, optimization of instrumental LIBS parameters (gate delay, gate width, laser pulse energy), and chemical hydride generation parameters (acid and reductant concentration, sample, and carrier gas flow rate) was performed. The details of optimization process for HG-LIBS systems have been given previously (Ünal and Yalçın 2010;Yeşiller and Yalçın 2013); therefore, only optimal conditions used throughout this study for maximum arsenic signal is listed in Table 1.…”

Section: Effect Of Presence Of Alkali/alkali Earth Metals On As Signal Intensitymentioning

confidence: 99%

“…Recently, some studies based on hydride generation (HG) sample introduction coupled with LIBS detection, for the analysis of some hydride forming elements like As, Sb, Sn, Pb, and Ge has been introduced (Simeonsson and Williamson 2011;Singh et al 1996;Unal 2010;Yesiller and Yalçın 2013). Our group has previously reported optimum chemical and instrumental parameters for the determination of Sn (Unal 2010), As, Sb, Pb, Ge (Yeşiller and Yalçın 2013) in aqueous environments by HG-LIBS. A strong enhancement in signal strength and improvement in the limit of detection values of the studied elements, compared to direct analysis of bulk liquid samples by LIBS, was obtained.…”

Section: Introductionmentioning

confidence: 99%

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Determination of Arsenic by Hydride Generation—Laser-Induced Breakdown Spectroscopy: Characterization of Interelement Interferences

2018

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In this study, interelement interferences were evaluated for the determination of arsenic in aqueous samples through laser-induced breakdown spectroscopy (LIBS) hyphenated with a hydride generation sample introduction system. Optimum instrumental and chemical parameters were selected and variation in LIBS signal intensity was recorded for As solution in the presence of comparable concentrations of interfering elements. No significant change in the signal intensity of As(I) 228.8 nm line was observed in the presence of alkali/alkali earth metals; however, the presence of hydride-forming elements has shown a noticeable decrease in the line emission strength of arsenic. The least variation in arsenic signal was observed in the presence of Ge, the most volatile of all. However, the signal has decreased to a greater extent in the presence of Sn, Sb, and Pb. The presence of interfering elements on electron temperature and electron number density of arsenic plasma has also been studied. Plasma temperatures calculated using both As and Ar emission lines in the Boltzmann equation were similar, being around 5000 K. The McWhirter criterion for stationary and homogenous plasmas was utilized for the establishment of the local thermodynamic equilibrium under the plasma conditions studied. Applicability of the technique for multielemental analysis of water samples was tested through spiking experiments. Arsenic signal showed 26% decrease in the multielemental mixture solution. LIBS is among a few atomic spectroscopic techniques that facilitate rapid and simultaneous multielemental analysis without extensive sample preparation steps. However, the analytical performance of the technique still requires more serious efforts to compete with other conventional techniques for routine analysis of environmental samples.

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Section: Methodsmentioning

confidence: 99%

Section: Effect Of Presence Of Alkali/alkali Earth Metals On As Signal Intensitymentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

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Determination of Arsenic by Hydride Generation—Laser-Induced Breakdown Spectroscopy: Characterization of Interelement Interferences

2018

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“…Such examples are HG-AFS and CV-AFS [ 14 , 15 , 16 , 17 , 18 , 19 ], HG coupled with high-resolution continuum source electrothermal atomic absorption spectrometry or quartz furnace atomic absorption spectrometry (HG-HR-CS-ETAAS, HG-HR-CS-QFAAS) [ 20 , 21 , 22 ] and graphite furnace atomic absorption spectrometry (HG-GFAAS) [ 23 ]. Other ways are HG-ICP OES [ 24 ], HG-ICP-MS [ 25 , 26 ], and hydride generation laser-induced breakdown spectrometry (HG-LIBS) [ 27 ]. In addition, the use of UV photochemical vapor generation (UV-PVG) [ 28 , 29 ] coupled with spectrometric methods such as UV-PVG-AFS [ 30 ], UV-PVG-GFAAS [ 31 , 32 ], and UV-PVG-ICP-MS [ 33 , 34 ] resulted in enhanced sensitivity and lower susceptibility to non-spectral interference compared to conventional HG.…”

Section: Introductionmentioning

confidence: 99%

Simultaneous Determination of As, Bi, Sb, Se, Te, Hg, Pb and Sn by Small-Sized Electrothermal Vaporization Capacitively Coupled Plasma Microtorch Optical Emission Spectrometry Using Direct Liquid Microsampling

et al. 2021

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The simultaneous determination of chemical vapor-generating elements involving derivatization is difficult even by inductively coupled plasma optical emission spectrometry or mass spectrometry. This study proposes a new direct liquid microsampling method for the simultaneous determination of As, Bi, Se, Te, Hg, Pb, and Sn, using a fully miniaturized set-up based on electrothermal vaporization capacitively coupled plasma microtorch optical emission spectrometry. The method is cost-effective, free from non-spectral interference, and easy to run by avoiding derivatization. The method involves the vaporization of analytes from the 10 µL sample and recording of episodic spectra generated in low-power (15 W) and low-Ar consumption (150 mL min−1) plasma microtorch interfaced with low-resolution microspectrometers. Selective vaporization at 1300 °C ensured the avoidance of non-spectral effects and allowed the use of external calibration. Several spectral lines for each element even in the range 180–210 nm could be selected. Generally, this spectral range is examined with large-scale instrumentation. Even in the absence of derivatization, the obtained detection limits were low (0.02–0.75 mg kg−1) and allowed analysis of environmental samples, such as cave and river sediments. The recovery was in the range of 86–116%, and the accuracy was better than 10%. The method is of general interest and could be implemented on any miniaturized or classical laboratory spectrometric instrumentation.

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“…Plasma formation on flowing jet liquids [3][4][5], inside bubbles [6], on liquid droplets [7][8], on aerosols formed by nebulization [9,10] or by electro-spray ionization [11,12], on samples in which physical conditions are changed by freezing [13,14] or by chemical derivatization [15][16][17][18], liquids adsorbed on solid substrates [19][20][21][22][23] or on sol-gels [24] and use of sequential laser pulses [25][26][27][28][29] are some of the efforts devoted in the last decade to increase the analytical capability of the LIBS technique for liquids analysis. Also, filtration based approaches, collection of the suspended particles like pollen, bacteria, fungi and viruses on filters enabled analysis of biological materials in water [30].…”

Section: Introductionmentioning

confidence: 99%

Development and validation of a laser-induced breakdown spectroscopic method for ultra-trace determination of Cu, Mn, Cd and Pb metals in aqueous droplets after drying

Aras

Yalçın

2016

Talanta

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Keywords:Laser-induced breakdown spectroscopy Liquid droplet analysis Oxidized silicon wafer substrate (Si þ SiO 2 ) a b s t r a c tThe present study reports a fast and accurate methodology for laser-induced breakdown spectroscopic, LIBS, analysis of aqueous samples for environmental monitoring purposes. This methodology has two important attributes: one is the use of a 300 nm oxide coated silicon wafer substrate (Siþ SiO 2 ) for the first time for manual injection of 0.5 microliter aqueous metal solutions, and two is the use of high energy laser pulses focused outside the minimum focus position of a plano convex lens at which relatively large laser beam spot covers the entire droplet area for plasma formation. Optimization of instrumental LIBS parameters like detector delay time, gate width and laser energy has been performed to maximize atomic emission signal of target analytes; Cu, Mn, Cd and Pb. Under the optimal conditions, calibration curves were constructed and enhancements in the LIBS emission signal were obtained compared to the results of similar studies given in the literature. The analytical capability of the LIBS technique in liquid analysis has been improved. Absolute detection limits of 1.3 pg Cu, 3.3 pg Mn, 79 pg Cd and 48 pg Pb in 0.5 microliter volume of droplets were obtained from single shot analysis of five sequential droplets. The applicability of the proposed methodology to real water samples was tested on the Certified Reference Material, Trace Metals in Drinking Water, CRM-TMDW and on ICP multi-element standard samples. The accuracy of the method was found at a level of minimum 92% with relative standard deviations of at most 20%. Results suggest that 300 nm oxide coated silicon wafer has an excellent potential to be used as a substrate for direct analysis of contaminants in water supplies by LIBS and further research, development and engineering will increase the performance and applicability of the methodology.

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Optimization of chemical and instrumental parameters in hydride generation laser-induced breakdown spectrometry for the determination of arsenic, antimony, lead and germanium in aqueous samples

Cited by 26 publications

References 42 publications

Determination of Arsenic by Hydride Generation—Laser-Induced Breakdown Spectroscopy: Characterization of Interelement Interferences

Determination of Arsenic by Hydride Generation—Laser-Induced Breakdown Spectroscopy: Characterization of Interelement Interferences

Simultaneous Determination of As, Bi, Sb, Se, Te, Hg, Pb and Sn by Small-Sized Electrothermal Vaporization Capacitively Coupled Plasma Microtorch Optical Emission Spectrometry Using Direct Liquid Microsampling

Development and validation of a laser-induced breakdown spectroscopic method for ultra-trace determination of Cu, Mn, Cd and Pb metals in aqueous droplets after drying

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