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1.
Anal Chem ; 95(2): 594-601, 2023 01 17.
Artículo en Inglés | MEDLINE | ID: mdl-36541929

RESUMEN

In this work, following a metal-ceramic heater (MCH) as an electrothermal vaporizer (ETV), a novel composite Pt/Ni trap based on platinizing the foamed nickel was first fabricated to trap Hg and Cd simultaneously. So, a solid sampling Hg-Cd analyzer was developed to simultaneously detect trace Hg and Cd in soil samples, mainly consisting of an MCH, a composite Pt/Ni trap, and an atomic fluorescence spectrometer (AFS). This small-size MCH-ETV system only consumes 100 W for the complete vaporization of Hg and Cd in soil matrices. The Pt/Ni trap fulfills the complete trapping of Hg and Cd following the solid sampling MCH-ETV system and then fast releases them by heating. It was proved that trapped and released Hg and Cd by the Pt/Ni trap are atomic species using X-ray photoelectron spectroscopy (XPS) and other approaches; specially, the effective cotrapping of Hg and Cd might be due to forming alloys of Hg + Pt and Cd + Ni on the Pt/Ni trap. Under the optimized conditions, the method detection limits (LODs) of Hg and Cd reached 0.4 µg/kg and 0.04 µg/kg for a 20 mg sample size, the relative standard deviations (RSDs) were within 12% and 8% for soil samples, respectively, and the recoveries ranged from 96% to 105%, indicating favorable analytical sensitivity, precision, and accuracy. The whole analysis time can be controlled within 5 min without the soil digestion process. The proposed Hg-Cd analyzer is thus suitable for rapid detection of Hg and Cd in soil samples with advantages such as simplicity, green, and safety. Further, the proposed solid sampling ETV-composite trap method has a promising application potential in the field and rapid detection for multielements.


Asunto(s)
Cadmio , Mercurio , Cadmio/análisis , Níquel/análisis , Mercurio/análisis , Platino (Metal)/análisis , Suelo
2.
Talanta ; 202: 178-185, 2019 Sep 01.
Artículo en Inglés | MEDLINE | ID: mdl-31171167

RESUMEN

A novel direct sampling (DS-HG) system consisting of an enlarged gas liquid separator (GLS) coupled with a foam breaker was firstly utilized for the in-situ dielectric barrier discharge atomic fluorescence spectrometer (DBD-AFS). After direct dilution using 5% HCl (v:v), a prepared blood sample was introduced into the DS-HG with a UV digestion unit, of which arsenic hydrides directly generated from sample under 5% HCl (v:v) and 5 g/L KBH4 in 1.5 g/L KOH. Herein, the newly designed DS-HG is capable of effectively eliminating foam generation deriving from protein in blood sample. Then, arsenic hydrides were trapped by 11 kV discharging at 110 mL/min air, and released by 13 kV at 180 mL/min H2 orderly. Under the optimized conditions, the linearity ranged from 0.05 to 50 ng/mL with a regression coefficient (R2) = 0.996. The method detection limit (LOD) was 7 pg arsenic (0.14 ng/mL), and relative standard deviation (RSD) of 10 repeated measurements for a real blood sample was 4.2%, indicating a good precision. The spiked recoveries for real samples were in the range of 97%-102%. Furthermore, arsenic presence in real blood samples measured by the proposed method were consistent (P > 0.05) with the microwave digestion ICP-MS. The whole analytical time can be controlled within 8 min including sample dilution. As a matter of fact, it is a favorable progress for DBD technique to eliminate matrix interferences of real samples based on the gas phase enrichment (GPE) principle, with advantages such as excellent sensitivity, digestion-free, fast and simple operation. Thus, the recommended DS-HG-in-situ DBD-AFS are suitable to the fast analysis of ultratrace arsenic in blood samples to protect human's health.


Asunto(s)
Arsénico/sangre , Gases/química , Borohidruros/química , Humanos , Ácido Clorhídrico/química , Hidróxidos/química , Compuestos de Potasio/química , Espectrometría de Fluorescencia/instrumentación , Espectrofotometría Atómica/instrumentación
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