Application of pressurized sample preparation methods for the analysis of steels and copper alloys

Borszéki, J.; Halmos, Pál; Gegus, E.; Kárpáti, Péter

doi:10.1016/0039-9140(94)80076-6

Cited by 8 publications

(8 citation statements)

References 2 publications

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“…The slurry technique is based on the idea that a powdered sample of suitable small particle size held in an aqueous suspension of a certain percentage can be directly aspired into the plasma and analyzed. 4,5 Taking into account that many types of samples such as silicate minerals, refractory compounds, and ceramics are not easily completely dissolved without contamination and losses of analytes, a number of methods have been developed to introduce slurries into plasmas. [4][5][6] Some of the experimental factors that can influence the signal intensities for analytes in slurry nebulization are: the particle size distribution and atomization efficiency.…”

Section: Introductionmentioning

confidence: 99%

“…4,5 Taking into account that many types of samples such as silicate minerals, refractory compounds, and ceramics are not easily completely dissolved without contamination and losses of analytes, a number of methods have been developed to introduce slurries into plasmas. [4][5][6] Some of the experimental factors that can influence the signal intensities for analytes in slurry nebulization are: the particle size distribution and atomization efficiency. [4][5][6] In a review Ebdon et al discussed the importance of particle size distribution measurements for the powder to be brought into suspension, the influence of the slurry concentration, and the calibration in slurry nebulization in ICP.…”

Section: Introductionmentioning

confidence: 99%

“…[4][5][6] Some of the experimental factors that can influence the signal intensities for analytes in slurry nebulization are: the particle size distribution and atomization efficiency. [4][5][6] In a review Ebdon et al discussed the importance of particle size distribution measurements for the powder to be brought into suspension, the influence of the slurry concentration, and the calibration in slurry nebulization in ICP. 7 Sanchez et al described a practical method for the direct determination of Al, Ca, Fe, K, Mg, Mn, Na, Si, and Ti in slag samples by the introduction of suspensions into the ICP OES.…”

Section: Introductionmentioning

confidence: 99%

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Clay and refractory materials slurries in inductively coupled plasma optical emission spectrometry: effects of mechanochemical synthesis on emission intensities of analytes

Santos¹,

Nogueira²,

Nóbrega³

2005

J. Braz. Chem. Soc.

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Neste trabalho foi investigada a aplicação da síntese mecanoquímica para promover reações na amostra e sintetizar novos compostos visando aumentar as intensidades de emissão de elementos presentes em suspensões de argilas e materiais refratários quando introduzidas em espectrômetro de emissão óptica com plasma acoplado indutivamente com configuração axial. A hipótese formulada é que é possível gerar compostos mais voláteis durante a moagem e esses novos compostos causam aumento da intensidade dos sinais de emissão para os analitos em suspensões introduzidas no plasma. A ação de dois modificadores, LiBO 2 e Na 2 CO 3 , adicionados durante a etapa de moagem foi investigada.As argilas e materiais refratários foram moídos juntamente com os modificadores químicos durante 2 h usando um moinho de bolas de alto impacto com recipiente e bolas de carbeto de tungstênio. As suspensões foram preparadas dispersando as argilas e os materiais refratários modificados em solução 10% v v -1 HNO 3 e, posteriormente, sonicadas em banho de ultra-som para melhorar a homogeneização. Os compostos produzidos durante a etapa de moagem foram caracterizados por difração de raios X e análise termogravimétrica. Ambas as técnicas indicaram a formação de novos compostos nas argilas e materiais refratários por síntese mecanoquímica. Os efeitos da modificação química foram avaliados pelas mudanças nas intensidades de emissão dos analitos Al, Ca, Fe, K, Mg, P, Si e Ti. Ambos modificadores causaram aumento na sensibilidade para todos os analitos de até 665% (Na 2 CO 3 ) e 583% (LiBO 2 ) quando comparados às intensidades dos sinais de emissão obtidos para os analitos nas suspensões preparadas com as amostras sem modificação química.The developed work investigated the application of mechanochemical synthesis for promoting reactions in the samples and for synthesizing new compounds for increment of emission intensities of analytes in clays and refractory materials slurries in inductively coupled plasma optical emission spectrometry with axial viewing. The hypothesis is that it is possible to generate more volatile compounds during the grinding step and these new compounds will increase the intensities of emission signals for slurries introduced in the plasma. The action of two chemical modifiers, LiBO 2 and Na 2 CO 3 , added during the grinding step was evaluated. The clays and refractory materials mixed with the chemical modifier were ground for 2 h using a high impact ball mill with a tungsten carbide grinding container and balls. Slurries were prepared by dispersing the modified clays and refractory materials in 10% v v -1 HNO 3 solution and by shaking them in an ultrasonic bath to ensure good dispersion. The compounds produced during the grinding step were characterised by X-ray diffraction and thermogravimetric analysis. Both techniques indicated the formation of new compounds in clays and refractory materials by mechanochemical synthesis. Chemical modification effects were evaluated by changes of the emission intensities of Al, Ca, Fe, K, Mg, P, ...

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Section: Introductionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

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Clay and refractory materials slurries in inductively coupled plasma optical emission spectrometry: effects of mechanochemical synthesis on emission intensities of analytes

Santos¹,

Nogueira²,

Nóbrega³

2005

J. Braz. Chem. Soc.

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“…Standards for calibration curves can be either in the form of a solution or slurries. 14 The successful application of slurries in the references cited resulted in an investigation into the use of ICP-OES for analysis of cement. This approach should result in a rapid, convenient and contamination-free method of analysis, which could be employed on a routine basis for analysis of cement.…”

Section: Introductionmentioning

confidence: 99%

Analysis of cement by inductively coupled plasma optical emission spectrometry using slurry nebulization

Marjanović¹,

McCrindle²,

Botha³

et al. 2000

J. Anal. At. Spectrom.

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An investigation was conducted to determine the feasibility of analysing cement by introducing it as a slurry into an inductively coupled plasma optical emission spectrometer (ICP-OES). A complete analysis of cement for major (Ca, Si, Mg, Al, Fe) and minor and trace elements (S, K, Ti, Na, P, Mn and Sr) was accomplished. Calibration was performed either by using reference materials as slurries or by using simple aqueous standards. A combination of hydrochloric acid (1% v/v), glycerol (0.01% m/v) and agitation in an ultrasonic bath (10 min) was employed to ensure well dispersed and stable slurries. Measurements were made on a simultaneous ICP-OES instrument with both axial and radial plasma viewing. Values obtained for selected elements were compared to those measured on an X-ray ¯uorescence (XRF) instrument. It was found that ICP-OES gave an elegant and effective alternative to XRF for the analysis of cement. Accuracy of the technique, was checked by analysing a certi®ed reference material. This proved that the method could be easily employed on a routine basis for analysis of cement. Cost effectiveness and simplicity of sample preparation contributed to this conclusion.

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“…Accordingly, no precipitates might be due to the combined action of borate and tartaric acid ions. In several previous reports, 3,11,12) a mixture of sulfuric acid and phosphoric acid has been applied for tungsten wet analysis, where the water content is often vaporized and the concentrated acid is fumed well. 3,11) And then, aqueous dilution of the resulting solution is time-consuming because of the exothermic process.…”

Section: Solution Preparationmentioning

confidence: 99%

Rapid Borate Fusion Pre-treatment for ICP-AES Determination of Tungsten in High-speed Steel

Nakayama

Wagatsuma

2016

ISIJ Int.

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This paper suggests a rapid decomposition and dissolution method for stable solution preparation in inductively coupled plasma atomic emission spectrometry when tungsten in a highspeed steel is quantified. The steel sample was decomposed with a mixture of hydrofluoric and nitric acid, and then the resulting solution was fused with lithium tetraborate. The vitrified borate was able to dissolve in nitric acid containing tartaric acid to prepare the final sample solutions. This pre-treatment method has a superior feature: borate could effectively prevent tungsten hydrolysis in the prepared solution. The standard for quantification could be prepared in a similar procedure using metal standard solutions. The present method enabled more rapid and accurate determination of tungsten in certified reference materials of high-speed steel compared to the conventional dissolution procedure.

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Application of pressurized sample preparation methods for the analysis of steels and copper alloys

Cited by 8 publications

References 2 publications

Clay and refractory materials slurries in inductively coupled plasma optical emission spectrometry: effects of mechanochemical synthesis on emission intensities of analytes

Clay and refractory materials slurries in inductively coupled plasma optical emission spectrometry: effects of mechanochemical synthesis on emission intensities of analytes

Analysis of cement by inductively coupled plasma optical emission spectrometry using slurry nebulization

Rapid Borate Fusion Pre-treatment for ICP-AES Determination of Tungsten in High-speed Steel

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