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PubMed1997

Ion-exchange separation of eight arsenic compounds by high-performance liquid chromatography-UV decomposition-hydride generation-atomic fluorescence spectrometry and stability tests for food treatment procedures.

A novel separation for cationic arsenic compounds on a polymer-based cation-exchange column was developed using an ion-pairing reagent (3-carboxy-4-hydroxybenzenesulphonic acid) in the mobile phase. An existing anion-exchange separation was used for anionic arsenic compounds. Combining both separation techniques, eight environmentally important arsenic compounds can be determined using on-line decomposition in a UV reactor prior to hydride generation (HG) and atomic fluorescence spectrometry (AFS). The method was applied for testing the stability of arsenic compounds (in aqueous media) related to food treatment procedures. Boiling and microwave treatment gave no degradation, whereas gamma-irradiation and dry heating resulted in partial decomposition of several arsenic compounds. No health hazards are to be expected when these data are extrapolated to commercial or domestic food treatment procedures.

Arsenicals↗

PubMed1992

Background correction by wavelength modulation for pulsed-laser-excited atomic fluorescence spectrometry.

Instrumentation was constructed to modulate the dye laser wavelength for background correction in laser-excited atomic fluorescence spectrometry (LEAFS). To achieve wavelength modulation a piezoelectric pusher was used to drive the wavelength tuning mirror in a laboratory-constructed grazing incidence dye laser. The laser pulses were synchronized with the piezoelectric pusher movement so that alternate laser pulses measured the atomic fluorescence signal at the analytical atomic spectral line (on-line) and the background signal at a wavelength displaced to one side of the atomic line (off-line). The background-corrected signal was obtained by subtracting the off-line "background" from the on-line "signal plus background". The spectral line width (fwhm) of the dye laser was 0.003 nm, while the wavelength modulation interval was controllable over the range from 0 to 0.2 nm with a spectral resolution limited only by the spectral line width of the laser. This type of background correction could, in principle, be applied to other types of tunable lasers such as pulsed Ti: sapphire lasers. The performance of background correction by wavelength modulation (WM) was demonstrated by measurement of sodium resonance fluorescence in an air-acetylene flame and by thallium nonresonance fluorescence in a graphite furnace. The experimental data indicated that the wavelength modulation corrected, effectively and quantitatively, for flame background, blackbody emission from a graphite furnace, and scatter of laser radiation off aluminum chloride (1 mg/mL as AI) matrix particles in both the furnace and the flame. Analytical results were in good agreement with certified values for the determination of sodium in standard reference materials by the use of modulated LEAFS.

Lasers↗

PubMed2005

[Speciation analysis of mercury in traditional Chinese medicine by vapor-generation atomic fluorescence spectrometry].

A sensitive method has been proposed for the determination of inorganic mercury and total organic mercury in traditional Chinese medicine (Wanshi Niuhuang Qingxin) by vapor-generation atomic fluorescence spectrometry. The experimental conditions that influence the atomic fluorescence signal intensity of Hg and the oxidization of organic mercury were investigated and optimized. Thiourea citric acid was selected as a sensitization agent, which greatly enhanced atomic fluorescence signal intensity of mercury. The influence of foreign ions and their elimination were studied. The detection limit of the method for Hg was 7.6 ng x L(-1) and the relative standard deviation was 1.56%-3.28% for Hg. The proposed method was successfully applied to the determination of mercury speciation in real samples with a recovery range of 90.3%-110.3%.

Citric Acid↗

PubMed2005

Characterization of intercalated iron(III) nanoparticles and oxidative adsorption of arsenite on them monitored by x-ray absorption fine structure combined with fluorescence spectrometry.

This paper first deals with the screening and optimization of Fe(III)-based adsorbents for arsenic adsorption from 0.2 to 16 ppm test solutions of arsenite/arsenate. The best adsorption capacity has been reported on alpha-FeO(OH) on an adsorbent weight basis. Better results were found on intercalated Fe-montmorillonites for arsenite adsorption below the equilibrium dissolved As concentration of 310 ppb and for arsenate adsorption in all of the concentrations studied. Next, the speciation of As adsorbed was performed by As K-edge x-ray absorption fine structure (XAFS) combined with high-energy-resolution fluorescence spectrometry. Major oxidative adsorption of arsenite was observed on Fe-montmorillonite from the 0.2-16 ppm test solutions. The reasons for the higher capacity of arsenic adsorption and oxidative adsorption of arsenite on Fe-montmorillonite are discussed.

Adsorption↗

PubMed2005

X-ray absorption fine structure combined with x-ray fluorescence spectrometry. Part 15. Monitoring of vanadium site transformations on titania and in mesoporous titania by selective detection of the vanadium K alpha1 fluorescence.

X-ray absorption fine structure combined with X-ray fluorescence spectrometry was applied to various V+TiO2 hybrid samples. Emitted V K alpha1 fluorescence from the sample was selectively counted by using a high-energy-resolution (0.4 eV) spectrometer equipped with a Ge(331) crystal. Two advantages of this method, extremely high signal/background ratio and the compatibility of measurements in the atmosphere of reaction gas (in situ study in relation to heterogeneous catalysis), were effective at the V K-edge. Structure transformation of the V sites was spectroscopically followed for the V/TiO2 catalyst. The monooxo tetrahedral vanadate site was demonstrated to exist at 473 K. It transformed into dispersed species of 5-fold coordination in ambient air and further into polymeric VO(x) species in 0.85 kPa of water at 290 K. In the presence of 3.2 kPa of 2-propanol, dissociative adsorption of 2-propanol on the dispersed V species was strongly suggested at 290-473 K. In situ structure changes of V sites on TiO2 were reported by means of XAFS for the first time. The V(V) sites for the V/TiO2 catalysts were essentially identical with those for V supported on mesoporous (high-surface-area) TiO2 and V-TiO2 sample prepared by the sol-gel method. However, predominant V(IV) sites were found for mesoporous V-TiO2. The V(IV) sites substituted on the Ti sites of TiO2. When the molar ratio of V/Ti increased from 1/100 to 1/5.0, major octahedral V sites in the TiO2 matrix looked to transform into tetrahedral ones.

Journal Article↗

PubMed2005

Micelle-sensitized constant-energy synchronous fluorescence spectrometry for the simultaneous determination of pyrene, benzo[a]pyrene and perylene.

The use of micellar media in constant-energy synchronous fluorescence spectrometry has been proposed. The influence of some aqueous micellar systems on the determination of pyrene, perylene and benzo[a]pyrene has been investigated. The presence of these micellar systems allows their determination in aqueous media, thus avoiding the use of an organic solvent, and greatly enhances the fluorescence signals. The combination of a constant-energy synchronous scanning technique and a micellar system provided a single spectrum for the simultaneous identification and quantitative determination of the three polycyclic aromatic hydrocarbons (PAHs). Further there was no energy transfer among them, making the measurement simple and fast. A constant-energy difference of 2800 cm(-1) was selected. The analytical characteristics of the proposed method in the presence of anionic micelles of sodium dodecylsulfate (SDS) were studied. The detection limits were at a level of ng ml(-1). Analysis of water samples from two different origins spiked with known amount of pyrene, perylene and benzo[a]pyrene also gave satisfactory results, and total average recoveries were greater than 97.1%.

Algorithms↗

PubMed2005

[Study on the interaction of water-soluble p-(N,N-dimethylaminomethyl) calix[8] arene with DNA by fluorescent spectrometry].

The interaction of water-soluble p-(N, N-dimethylaminomethyl) calix [8] arene (CX8) with DNA was studied using adriamycin(ADM) as a probe by fluorescent spectrometry. The effect factors such as, pH of solution, salt effect and unlinking DNA on the spectra were also investigated. The interaction mechanism was proposed. The authors observed that the fluorescence of ADM was quenched by calf thymus DNA, and the fluorescence intensity of DNA-ADM enhanced with the increasing of the CX8 gradually. The result indicates that the strong electrostatic interaction between the oxyphosphate anion of DNA and the CX8 existed. According to the plot of scatchard, the results imply that the influence of CX8 on interaction of DNA-ADM belongs to mixed model, on the one hand, in the condition of neutral and acidity, the oxyphosphate anion of DNA can be neutralized by CX8 partially, which induced the contraction of DNA and the conformational change of DNA, which led to release ADM from DNA partially, on the other hand, the CX8 can also compete the electrostatic sites with ADM directly.

Algorithms↗

PubMed2004

[Speciation analysis of arsenic in traditional Chinese medicines by hydride generation-atomic fluorescence spectrometry with ion exchange resin separation].

A method for the determination of arsenic species (arsenide, arsenate) in traditional Chinese medicines using hydride generation atomic fluorescence spectrometry (HG-AFS) with ion exchange resin separation has been studied. The ion exchange resin was used to separate the arsenide and arsenate, and the separation conditions were investigated. The experimental conditions that influence the fluorescence intensity and the reduction of arsenic(V) were investigated and optimized, and the influence of foreign ions and its elimination were studied. The proposed method was applied to the determination of arsenic species in water leachate of traditional Chinese medicines. A detection limit of 89.1 ng x mL(-1) and a recovery range of 91.1%-109.3% were obtained.

Arsenates↗

PubMed1998

Simultaneous determination of salicylamide and salsalate in serum and urine by first derivative variable-angle synchronous fluorescence spectrometry.

The determination of salicylamide and salsalate in human serum and urine is performed using a simple, rapid, sensitive, and selective method. The broad-band overlapping conventional spectra of both compounds are resolved by means of first derivative variable-angle synchronous fluorescence spectrometry. The method is based on the intrinsic fluorescence of both drugs in chloroformic solution. The measurements are performed in an alkaline medium, which is adjusted by adding 0.40 M pyrrolidine chloroformic solution to the organic phase. The method was applied for the simultaneous determination of salicylamide and salsalate, at concentrations between 0.100 and 1. 000 microg mL-1 for both components, by means of absolute values of a first derivative variable-angle synchronous scan at the emission/excitation wavelengths of 410/299 nm for salicylamide and 440/307 nm for salsalate. Serum and urine are extracted with chloroform, by adding acetate buffer solution to provide pH 4.8 in the aqueous phase. Finally, pyrrolidine chloroformic solution is added to organic phase, where both components are determined, without the need for a reextraction step to an aqueous phase.

Humans↗

PubMed2003

Screening pyrene metabolites in the hemolymph of dungeness crabs (Cancer magister) with synchronous fluorescence spectrometry: method development and application.

The present study examined the metabolic pathways of pyrene in dungeness crabs (Cancer magister) in the laboratory and the potential of using synchronous fluorescence spectrometry (SFS) to determine pyrene metabolite concentrations in the hemolymph of crabs exposed to polycyclic aromatic hydrocarbons (PAHs) in the field. Pyrene was metabolized by crabs mainly to 1-hydroxypyrene and pyrene-1-glucoside. Both pyrene metabolites could be detected by SFS in the hemolymph of crabs. A nondestructive hemolymph collection procedure was developed and used in conjunction with the SFS assay to assess the exposure of crabs to PAHs in Kitimat Arm (British Columbia, Canada). Our results showed that crabs obtained near the source of PAH contamination had the highest level of pyrene-related fluorescence in the hemolymph, whereas concentrations were lower at other sites downstream from the pollution source. In a separate study, the hepatopancreases of crabs were analyzed for parent PAHs by using gas chromatography-mass spectrometry. Pyrene-associated fluorescent responses of the hemolymph were found to correlate positively with the concentration of total PAHs in the hepatopancreas (r = 0.39, p < 0.05).

Animals↗

PubMed1987

Elements in normal and cirrhotic human liver tissue. II. Potassium, sulphur, chlorine and bromine measured by X-ray fluorescence spectrometry.

Elements (K, S, Cl, Br) were measured by X-ray fluorescence spectrometry in normal liver tissue obtained at autopsy from 74 subjects (44 male, 30 female), median age 62 years (range 20-87), and in cirrhotic liver tissue from 27 subjects (14 alcoholic, 13 non-alcoholic cirrhosis). The element content (median and 5-95 percentile interval) in normal livers in mmol/kg dry tissue was: K, 198.75 (150.95-256.42); S, 147.60 (73.86-233.97); Cl, 98.73 (69.51-163.55); Br, 0.1101 (0.0701-0.4205). None of the elements displayed any sex difference. There were correlations between the content of Br and Cl (r = 0.26, P less than 0.05) and Br and K (r = 0.24, p less than 0.05). In both groups of cirrhotic livers, K, S and Cl content was within the normal range. Median Br content was above normal both in alcoholic (0.2265 mmol/kg, P less than 0.01) and non-alcoholic cirrhotic livers (0.2228 mmol/kg, P less than 0.01).

Adult↗

PubMed2005

Determination of trace elements in sediment reference materials by monochromatic X-ray excitation X-ray fluorescence spectrometry.

A new reliable analytical method, "Monochromatic X-ray Excitation X-ray Fluorescence Spectrometry", has been proposed. For validating the method, trace elements in sediment certified reference materials were determined. In the method X-ray fluorescence spectra are measured for specimens and pure metals; in addition the mass-attenuation coefficients of the specimens for various X-ray wavelengths are also measured. The data are analyzed by the fundamental parameter method and the uncertainty of the analysis is evaluated. The obtained results were in satisfactory agreement with the certified values within their uncertainties. This method will be applicable to the certification of reference materials, in the field of which reliable results with uncertainty statements are required.

Geologic Sediments↗

PubMed1995

Spatial discrimination against background with different optical systems for collection of fluorescence in laser-excited atomic fluorescence spectrometry with a graphite tube electrothermal atomizer.

A single 90 degrees off-axis ellipsoidal mirror fragment was used in a dispersive detection system for electrothermal atomization laser-excited atomic fluorescence spectrometry. The performance of the new optical arrangement was compared with those of optical arrangements that employed a plane mirror in combination with biconvex or plano-convex lenses. All the optical arrangements collected fluorescence in a scheme called front surface illustration. BEAM-4, an optical ray tracing program, was used for calculations of spatial ray distributions and optical collection efficiency for the various optical configurations. Experimentally, the best collection efficiency was obtained by use of the ellipsoidal mirror, in qualitative agreement with simulations done by use of the BEAM-4 software. The best detection limit for cobalt with the new optical arrangement was 20 fg, which was a factor of 5 better than that obtained with conventional optical arrangements with otherwise the same instrumentation. The signal-to-background ratio and the fluorescence collection efficiency were also studied as a function of position of the optical components for the various optical arrangements. For both cobalt and phosphorus, the signal-to-background ratio with the new optical arrangement remained stable within 10-20% during +/- 8 mm shifts in the position of the detection system from the focal plane of the optics. Overall, the new optical arrangement offered high collection efficiency, excellent sensitivity, and facile optical alignment due to efficient spatial separation between the fluorescence signal and the background radiation. The advantages of the new optical arrangement were particularly important during measurements in the presence of high levels of blackbody radiation.

Data Display↗

PubMed2005

Sample preparation for evaluation of detection limits in X-ray fluorescence spectrometry.

The influence of analyte mass concentration on determination of detection limits in X-ray fluorescence spectrometry has been investigated experimentally. Both the total reflection X-ray fluorescence (TXRF) and the conventional energy-dispersive X-ray fluorescence techniques have been used to derive the dependence of analyte mass concentration on the values of detection limits. Results obtained indicate that values of detection limits are optimum, or in other words, they are closer to the true detection limit of the technique, when analyte concentrations are in the range of 10 times of the detection limit.

Journal Article↗

PubMed1996

Laser induced atomic fluorescence spectrometry for detection of elemental pollution in the environment.

Recently, laser induced atomic fluorescence spectrometry was successfully applied for the detection of trace elements in environmental objects. Due to the very high sensitivity of the LIF technique, either direct analysis of the environmental samples at and below the pg/g level can be done or the sample pretreatment may be considerably simplified. The results of the LIF analysis recently obtained by groups in the USA, Russia and Italy will be reviewed.

Journal Article↗

PubMed1999

Development of an electrothermal atomization laser-excited atomic fluorescence spectrometry procedure for direct measurements of arsenic in diluted serum.

A procedure for the direct determination of arsenic in diluted serum by electrothermal atomization laser-excited atomic fluorescence spectrometry (ETA-LEAFS) is reported. Laser radiation needed to excite As at 193.696 and 197.197 nm is generated as the second anti-Stokes stimulated Raman scattering output of a frequency-doubled dye laser operating near 230.5 and 235.5 nm, respectively. Two different LEAFS schemes have been utilized and provide limits of detection of 200-300 fg for As in aqueous standards. When measurements of serum samples diluted 1:10 with deionized water are performed, a stable background signal is observed that can be accounted for by taking measurements with the laser tuned off-wavelength. No As is detected in any of the bovine or human serum samples analyzed. Measurements of 100 pg/mL standard additions of As to a diluted bovine serum sample utilizing either inorganic or organic As species demonstrate a linear relationship of the fluorescence signal to As spike concentration, but exhibit a sensitivity of approximately half that observed in pure aqueous standards. The limit of detection for As in 1:10 diluted serum samples is 65 pg/mL or 650 fg absolute mass, which corresponds to 0.65 ng/mL As in undiluted serum. To our knowledge, the ETA-LEAFS procedure is currently the only one capable of directly measuring As in diluted serum at these levels.

Animals↗

PubMed2006

Selenium speciation by high-performance anion-exchange chromatography-post-column UV irradiation coupled with atomic fluorescence spectrometry.

A technique for the speciation of selenomethylcysteine (SeMeCys), selenocystine (SeCys), selenite [Se(IV)] and selenomethionine (SeMet) was established in this paper using high-performance anion-exchange chromatography coupled with atomic fluorescence spectrometry (HPAEC-AFS). Analytes were separated on an AminoPac PA10 column and then digested by on-line ultraviolet (UV) irradiation, which destroyed organic compound structure. Hydride generation was used as an available sample introduction technique for atomic fluorescence detection. The detection limits of four compounds were 1-5 microg/L (250 microL injection, 10 times of the baseline noise). The relative standard deviations (RSDs), calculated from seven consecutive injections of 100 microg/L standard mixtures, were from 2 to 4%. Selenious yeast tablet, which had been proposed as selenium supplement, and human urine collected from a volunteer were analyzed. Good spiked recoveries from 86 to 103% were obtained.

Chromatography, High Pressure Liquid↗

PubMedDate not supplied

Screening for selected trace elements in single cell populations by energy dispersive X-ray fluorescence spectrometry.

An adaptation of the thin film approach to energy dispersive X-ray fluorescence spectrometry (EDXRF) is described, which provides for a screening analysis for Fe, Ni, Cu, Zn, Se, and Cd in K-562 leukemic cells incubated in various metal-enhanced cultures. Valuable quantitative and semiquantitative data can be obtained on as few as 400,000 cells.

Cells, Cultured↗