Direct Determination of Trace Antimony in Natural Waters by Photochemical Vapor Generation ICPMS: Method Optimization and Comparison of Quantitation Strategies
Abstract:/npsi/ctrl?action=rtdoc&an=21276022&lang=en http://nparc.cisti-icist.nrc-cnrc.gc.ca/npsi/ctrl?action=rtdoc&an=21276022&lang=fr READ THESE TERMS AND CONDITIONS CAREFULLY BEFORE USING THIS WEBSITE.http://nparc.cisti-icist.nrc-cnrc.gc.ca/npsi/jsp/nparc_cp.jsp?lang=en Vous avez des questions? Nous pouvons vous aider. Pour communiquer directement avec un auteur, consultez la première page de la revue dans laquelle son article a été publié afin de trouver ses coordonnées. Si vous n'arrivez pas à les repérer, communi… Show more
“…[26][27][28][29][30][31][32][33][34][35][36] Furthermore, the impact of several additional parameters is generally not considered, including that of the temperature of the photoreactor on the intensity of the UV lamp (affected by the sample ow rate and inuencing photon ux) as well as independent supplies of Ar gas to the GLS (required for optimum phase separation and analyte transport efficiencies without causing excessive aerosol formation) and to the nebulizer such that the optimal observation height above the load coil can be achieved. [26][27][28][29][30][31][32][33][34][35][36] Furthermore, the impact of several additional parameters is generally not considered, including that of the temperature of the photoreactor on the intensity of the UV lamp (affected by the sample ow rate and inuencing photon ux) as well as independent supplies of Ar gas to the GLS (required for optimum phase separation and analyte transport efficiencies without causing excessive aerosol formation) and to the nebulizer such that the optimal observation height above the load coil can be achieved.…”
Section: Resultsmentioning
confidence: 99%
“…Use of this lamp for PVG relies on an averaging of the intensity over the length and diameter of the discharge. [32][33][34][35][36][37][38][39] These effects are less pronounced with the other two lamps ( Fig. 5 min for UV radiation and 10 min for temperature), water was introduced into each PVG reactor using a peristaltic pump and its impact on temperature and lamp intensity monitored for different ow rates.…”
Section: Inuence Of Uv Lamp Characteristicsmentioning
confidence: 99%
“…Based on previous reports, [19][20][21][22][23][24][25][26][27][28][29][30][31][32][33][34][35][36][37] the PVG efficiencies of most elements strongly depend on the type and concentration of LMW organic acid in the solution. Using the above established experimental conditions, solutions containing only Co(II) prepared in formic, acetic and propionic acids at concentrations ranging from 4 to 60% (v/v) were investigated in detail.…”
Section: Effect Of Lmw Organic Acidsmentioning
confidence: 99%
“…A batch mode of sample processing permits exible irradiation times to be achieved but generates transient signals and is typically less efficient. [33][34][35][36][37][38][39] Zheng et al 40 pointed to the possibility that speciation of mercury in a formic acid medium could be undertaken by exposing the sample to either 254 nm radiation for the determination of total mercury, or to a visible light source for selective reduction of inorganic mercury. 22,23 A combined spraychamber/UV photolysis unit has also been studied 24 but suffers from the inability to control the irradiation time and is functional only over a limited range of sample introduction rates.…”
An optimized photochemical vapor generation (PVG) approach for efficient synthesis of volatile cobalt species is described. Solutions containing Co(II) in a pH 3.3 medium of 50% formic acid were exposed to a source of deep UV (254 and 185 nm) radiation generated within a 19 W flow-through low pressure mercury discharge lamp. Following efficient phase separation, the analyte was transported to an ICP-OES system for detection at the 238.892 nm emission line of Co I. Several variables were investigated, including the type of UV lamp and gas-liquid separator, identity and concentration of the low molecular weight organic acid, solution pH, sample flow rate and exposure time to the UV irradiation as well as transport gas flow and mode of introduction of sample (continuous or segmented) to the ICP. In continuous mode, an optimum generation efficiency of 42 AE 2% was achieved with an irradiation time of 10 s, providing a 27-fold improvement in sensitivity compared to pneumatic nebulization and a limit of detection of 0.4 mg L À1 with a precision of 3% at 100 mg L À1 . Direct analysis of acid digested biological tissues (NRC TORT-2 and TORT-3) was hampered by strong matrix interferences from the presence of nitrate and other ions which could be circumvented by longer irradiation time and sufficient dilution such that accurate analysis of real samples by the method of additions could be achieved while maintaining high generation efficiency.
“…[26][27][28][29][30][31][32][33][34][35][36] Furthermore, the impact of several additional parameters is generally not considered, including that of the temperature of the photoreactor on the intensity of the UV lamp (affected by the sample ow rate and inuencing photon ux) as well as independent supplies of Ar gas to the GLS (required for optimum phase separation and analyte transport efficiencies without causing excessive aerosol formation) and to the nebulizer such that the optimal observation height above the load coil can be achieved. [26][27][28][29][30][31][32][33][34][35][36] Furthermore, the impact of several additional parameters is generally not considered, including that of the temperature of the photoreactor on the intensity of the UV lamp (affected by the sample ow rate and inuencing photon ux) as well as independent supplies of Ar gas to the GLS (required for optimum phase separation and analyte transport efficiencies without causing excessive aerosol formation) and to the nebulizer such that the optimal observation height above the load coil can be achieved.…”
Section: Resultsmentioning
confidence: 99%
“…Use of this lamp for PVG relies on an averaging of the intensity over the length and diameter of the discharge. [32][33][34][35][36][37][38][39] These effects are less pronounced with the other two lamps ( Fig. 5 min for UV radiation and 10 min for temperature), water was introduced into each PVG reactor using a peristaltic pump and its impact on temperature and lamp intensity monitored for different ow rates.…”
Section: Inuence Of Uv Lamp Characteristicsmentioning
confidence: 99%
“…Based on previous reports, [19][20][21][22][23][24][25][26][27][28][29][30][31][32][33][34][35][36][37] the PVG efficiencies of most elements strongly depend on the type and concentration of LMW organic acid in the solution. Using the above established experimental conditions, solutions containing only Co(II) prepared in formic, acetic and propionic acids at concentrations ranging from 4 to 60% (v/v) were investigated in detail.…”
Section: Effect Of Lmw Organic Acidsmentioning
confidence: 99%
“…A batch mode of sample processing permits exible irradiation times to be achieved but generates transient signals and is typically less efficient. [33][34][35][36][37][38][39] Zheng et al 40 pointed to the possibility that speciation of mercury in a formic acid medium could be undertaken by exposing the sample to either 254 nm radiation for the determination of total mercury, or to a visible light source for selective reduction of inorganic mercury. 22,23 A combined spraychamber/UV photolysis unit has also been studied 24 but suffers from the inability to control the irradiation time and is functional only over a limited range of sample introduction rates.…”
An optimized photochemical vapor generation (PVG) approach for efficient synthesis of volatile cobalt species is described. Solutions containing Co(II) in a pH 3.3 medium of 50% formic acid were exposed to a source of deep UV (254 and 185 nm) radiation generated within a 19 W flow-through low pressure mercury discharge lamp. Following efficient phase separation, the analyte was transported to an ICP-OES system for detection at the 238.892 nm emission line of Co I. Several variables were investigated, including the type of UV lamp and gas-liquid separator, identity and concentration of the low molecular weight organic acid, solution pH, sample flow rate and exposure time to the UV irradiation as well as transport gas flow and mode of introduction of sample (continuous or segmented) to the ICP. In continuous mode, an optimum generation efficiency of 42 AE 2% was achieved with an irradiation time of 10 s, providing a 27-fold improvement in sensitivity compared to pneumatic nebulization and a limit of detection of 0.4 mg L À1 with a precision of 3% at 100 mg L À1 . Direct analysis of acid digested biological tissues (NRC TORT-2 and TORT-3) was hampered by strong matrix interferences from the presence of nitrate and other ions which could be circumvented by longer irradiation time and sufficient dilution such that accurate analysis of real samples by the method of additions could be achieved while maintaining high generation efficiency.
“…The optimum concentrations of AA and FA for the PVG of As in standard solution were 15% (v/v) and 5% (v/v), respectively. As in the case of Sb [31], response of As in seawater was less than 35% of that from the same concentration of matrix-free standard solution due to the effect of sample matrix. Since the sample matrix have a significant influence on the PVG of As, NASS-6 seawater spiked with 1n gg À1 As was used to optimize the experimental conditions.…”
/npsi/ctrl?action=rtdoc&an=21277071&lang=en http://nparc.cisti-icist.nrc-cnrc.gc.ca/npsi/ctrl?action=rtdoc&an=21277071&lang=fr READ THESE TERMS AND CONDITIONS CAREFULLY BEFORE USING THIS WEBSITE.http://nparc.cisti-icist.nrc-cnrc.gc.ca/npsi/jsp/nparc_cp.jsp?lang=en Vous avez des questions? Nous pouvons vous aider. Pour communiquer directement avec un auteur, consultez la première page de la revue dans laquelle son article a été publié afin de trouver ses coordonnées. Si vous n'arrivez pas à les repérer, communiquez avec nous à PublicationsArchive-ArchivesPublications@nrc-cnrc.gc.ca.
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NRC Publications Archive Archives des publications du CNRCThis publication could be one of several versions: author's original, accepted manuscript or the publisher's version. / La version de cette publication peut être l'une des suivantes : la version prépublication de l'auteur, la version acceptée du manuscrit ou la version de l'éditeur. For the publisher's version, please access the DOI link below./ Pour consulter la version de l'éditeur, utilisez le lien DOI ci-dessous.http://doi.org/10.1016/j.aca.2015.10.020Analytica Chimica Acta, 2015-10 Multivariate optimization of photochemical vapor generation for direct determination of arsenic in seawater by inductively coupled plasma mass spectrometry Photochemical vapor generation (PVG) sample introduction coupled to inductively coupled plasma mass spectrometry (ICPMS) is described for the determination of As in seawater. A PlacketteBurman design (PBD) and central composite design (CCD) were employed to evaluate the significance of experimental variables relevant to the optimization of PVG-ICPMS detection. The impact of the saline matrix on the suppression of analyte signal was eliminated by use of a mixture of 20% (v/v) formic and 20% acetic acid (v/v) as the photochemical reductants. Optimized conditions yielded equivalent PVG generation efficiencies for As(III), As(V), monomethylarsonic acids (MMAs) and dimethylarsinic acids (DMAs), permitting direct and rapid determination of total arsenic in seawater without any other sample pretreatment. Quantitation was accomplished using one point gravimetric standard addition along with a spike of 82 Se internal standard to compensate for signal drift and fluctuation during analysis. The resulting method detection limit of 3 pg g À1 (3s) provided a 15-fold improvement over that obtained using direct solution nebulization, and is comparable to that for conventional chemical hydride generation (HG)-ICPMS. Accuracy was demonstrated by analysis of two Certified Reference Materials (NASS-6 and CASS-5 seawater) with satisfying results characterized by precisions of 3.5% and 3.2% RSD for CASS-5 and NASS-6, respectively. Crown
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