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1.
Anal Sci ; 34(6): 675-679, 2018.
Artigo em Inglês | MEDLINE | ID: mdl-29887555

RESUMO

A novel microwave-induced helium plasma optical emission spectrometry (He-MIP-OES) combined with a thermal hydrolysis sample introduction system was newly established for the determination of fluorine (F) compounds in slags. The MIP maintained through an Okamoto cavity was adopted, which was quite stable and provided a higher detection capability of F by helium plasma. The basic analytical performance of He-MIP-OES combined with an ultrasonic nebulizer for F analysis was also examined, and expected results could be obtained. The thermal hydrolysis behavior of CaF2, Ca4(Si2O7)(F,OH)2 and Ca5(PO4)3F, as known F chemical structures in slag, was also examined by thermal hydrolysis He-MIP-OES; F compounds in actual slag could be successfully identified and determined by this developed system.

2.
Anal Sci ; 29(3): 291-5, 2013.
Artigo em Inglês | MEDLINE | ID: mdl-23474717

RESUMO

Laser post-ionization of sputtered molecules by pulsed Ga focused ion-beam (Ga-FIB) bombardment was examined for the detection and imaging of polycyclic aromatic hydrocarbons (PAHs) on particles. As model samples, pyrene and pelyrene adsorbed on TiO2, blended regents of pyrene and n-heneicosan were used. The TiO2 particle size was selected to be several micro-meters. Laser light and Ga-FIB were synchronized with each other. The repetition rate synchronized with Ga-FIB was 1 kHz for pyrene analysis and 2 kHz for perylene, respectively. The laser wavelength was set to 266 nm. The wavelength was a generated fourth harmonic of a Nd:YAG DPSS (diode-pumped solid-state) micro-chip laser (UV microchip laser). By using a UV microchip laser, laser-SNMS (laser post-ionized sputtered neutral mass spectrometry) analysis and imaging were performed. The imaging of pyrene (m/z = 202, C16H10) and perylene (m/z = 252, C20H12) has been successful. Both the scanning ion microscopy image of TiO2 and the PAHs image in laser-SNMS analysis were well-fitted with each other.

3.
Chemosphere ; 80(8): 881-7, 2010 Aug.
Artigo em Inglês | MEDLINE | ID: mdl-20570315

RESUMO

The chemical states of boron in coal fly ash, which may control its leaching into the environment, were investigated by focused-ion-beam time-of-flight secondary ion mass spectrometry (FIB-TOF-SIMS) and satellite-transition magic angle spinning nuclear magnetic resonance (STMAS NMR) spectroscopy. The distribution of boron on the surface and in the interior of micron-sized fly ash particles was directly observed by FIB-TOF-SIMS. Coordination numbers of boron and its bonding with different atoms from particles of bulk samples were investigated by STMAS NMR. Boron in coal fly ash with relatively poor leaching characteristics appears as trigonal BO(3) and coexists with Ca and Fe at the outer layer of every particle and inside CaO-MgO particles. In contrast, boron in coal fly ash with better leaching characteristics appears as CaO- or MgO-trigonal BO(3) and tetragonal BO(4), and it is distributed only on the outer surface of each ash particle without showing any correlation with a particular element.


Assuntos
Boro/química , Carbono/química , Espectroscopia de Ressonância Magnética , Material Particulado/química , Espectrometria de Massa de Íon Secundário , Boro/análise , Cinza de Carvão , Resíduos Perigosos/análise , Tamanho da Partícula
4.
Anal Sci ; 21(8): 991-6, 2005 Aug.
Artigo em Inglês | MEDLINE | ID: mdl-16122174

RESUMO

For the analysis of trace amounts of hazardous organic compounds, we developed a new ion detection system for supersonic jet resonance-enhanced multiphoton laser ionization mass spectrometry. High sensitivity and selectivity have been achieved by combining a proto-type Daly detector, a newly designed conical ion lens, and a potential switch that can perform the function of a mass selector. This ion detection system enables us to bring the jet nozzle closer to the ionization point. The detection sensitivity has thus been improved totally by more than 100 times compared with that obtained by the parallel-plate electrodes and micro-channel plate. We succeeded in assembling a flangeon-type ion extraction electrode consisting of a conical ion lens and a potential switch.

5.
Eur J Gastroenterol Hepatol ; 14(6): 635-40, 2002 Jun.
Artigo em Inglês | MEDLINE | ID: mdl-12072597

RESUMO

OBJECTIVE: There are a number of views on the indication for endoscopic papillary balloon dilation (EPBD) in the management of bile duct stones. In this study, we have evaluated the efficacy and safety of EPBD compared with endoscopic sphincterotomy (EST). DESIGN: Prospective randomized trial. SETTING: One university hospital and one general hospital. PARTICIPANTS AND MAIN OUTCOME MEASURES: One hundred and forty patients were randomly allocated to EPBD or EST. Outcomes and complications were observed for a median period of 30 months. RESULTS: Both treatment approaches finally achieved similar success rates and needed similar numbers of treatment sessions for patients with stones less than 10 mm in diameter. However, for patients with stones of 10 mm or more, EPBD required a significantly greater mean number of treatment sessions than EST (2.4 vs 1.6, P < 0.01). Early complications occurred in seven EPBD (four pancreatitis, two cholangitis and one basket impaction) and eight EST (three pancreatitis, two bleeding and three cholangitis) patients. Late complications occurred in four EPBD (three recurrent bile duct stones and one cholecystitis) and six EST (three recurrent stones and three cholecystitis) patients. CONCLUSIONS: EPBD has little risk of bleeding. The technique removed small bile duct stones just as easily as did EST. These two procedures had approximately the same risk of pancreatitis and incidence of recurrent bile duct stones. Therefore, both procedures appear to be appropriate treatments for small bile duct stones. Whether or not EPBD becomes an established treatment will depend on further long-term studies.


Assuntos
Ampola Hepatopancreática , Cateterismo , Colelitíase/terapia , Adulto , Idoso , Idoso de 80 Anos ou mais , Cateterismo/efeitos adversos , Cateterismo/métodos , Colecistite/etiologia , Feminino , Humanos , Masculino , Pessoa de Meia-Idade , Pancreatite/etiologia , Estudos Prospectivos , Recidiva , Segurança , Esfinterotomia Endoscópica/efeitos adversos , Resultado do Tratamento
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