Mechanistic Studies of Chromium Speciation with Thermospray

2002 ◽  
Vol 56 (9) ◽  
pp. 1152-1160 ◽  
Author(s):  
Xiaohua Zhang ◽  
John A. Koropchak

Thermospray (TSP) coupled with inductively coupled plasma-atomic emission spectroscopy (ICP-AES) or inductively coupled plasma-mass spectrometry (ICP-MS) has been developed as a non-chromatographic method for chromium speciation to quantitatively separate and determine two chromium oxidation states: Cr(III) and Cr(VI). The limits of detection can reach 0.5 ng/mL with ICP-AES detection and 50 pg/mL with ICP-MS detection. The basis for this speciation method is that Cr(III) can selectively and nearly quantitatively deposit inside a thermospray system as Cr2O3, while Cr(VI) does not. To fully understand the mechanism of this deposition process, four questions were investigated: is aerosol formation necessary for the reaction to occur? Does the deposition occur in the aerosol or liquid regime? Does the deposit tend to be retained on the surface of the fused silica capillary? Can the reaction be predicted from thermodynamic calculations? These studies show that this reaction happens before solvent evaporates (i.e., the liquid regime). The high temperature inside the thermospray system is the major factor triggering this reaction. At the same time, the high pressure is important for its influence on the solvent boiling point, which affects the residence time (the time that the analyte spends in the solution before the solvent evaporates) and the kinetics of the reaction. The effects of the other parameters (vaporizer length, heating length, drawn tip, etc.) on the efficiency of the deposition reaction, represented as background residual signal (BRS), were also studied.

2000 ◽  
Vol 655 ◽  
Author(s):  
M. Tarutani ◽  
T. Sato ◽  
M. Yamamuka ◽  
T. Kawahara ◽  
T. Horikawa ◽  
...  

Abstract(Ba,Sr)TiO3 [BST] films were deposited by the flash vaporization CVD method with a unique liquid delivery system. An inductively coupled plasma mass spectrometry [ICP-MS] analysis revealed the decline of (Ba+Sr)/Ti molar ratio of the initial BST-layer on Ru. By readjusting the flow ratio of liquid sources and using a two-step deposition method, we obtained 30-nm-thick BST films with uniform composition profile, exhibiting good electrical properties. The leakage property, however, was severely deteriorated in BST films less than 24 nm thick. A SEM observation showed the presence of micro-roughness or micro-hillocks in these films, which were confirmed to be caused by Ru oxidation. Therefore, an annealing process of the Ru electrode was added for its planarization, and the CVD process was also improved. As a result, we obtained smooth and finely crystallized ∼ 20-nm-thick BST films with good electrical properties of equivalent SiO2 thickness (teq) ∼ 0.45 nm and leakage current < 1 × 10−7 A/cm2. We also measured properties of BST films deposited on the 3-D Ru electrode. The results are briefly discussed.


2011 ◽  
Vol 383-390 ◽  
pp. 790-795
Author(s):  
Bao Hui Li ◽  
Bao Juan Tian

A method for mercury high throughput rapid speciation analysis was built by short column capillary electrophoresis (SC-CE) coupled with inductively coupled plasma mass spectrometry (ICP-MS). A micromist nebulizer was employed to increase the nebulization efficiency and a laboratory-made removable SC-CE-ICP-MS interface on the basis of cross design was applied to alleviate buffer contamination of ICP-MS. In less than 60 s methylmercury (MeHg(I)) and inorganic mercury (Hg(II)) were separated in a 16 × 75 μm i.d. short column fused-silica capillary at 21 kV, while a mixture of 30 mmol/L boric aicd + 5% (v/v) CH3OH (pH=8.60) acted as running electrolyte. The precisions (RSD, n=5) of migration time and peak area for MeHg(I) and Hg(II) were in the range of 1.4-2.6% and 3.3-3.4%, respectively. The limits of detection (3σ) mercury species were 9.7 and 12.0 μg/L, respectively. The recoveries for Hg(II) MeHg(I) were in the range of 96-107% and 99-105%.


2020 ◽  
Vol 21 (3) ◽  
pp. 119
Author(s):  
Hasria Hasria ◽  
Arifudin Idrus ◽  
I Wayan Warmada

Pada proses alterasi hidrotermal, reaksi batuan samping dengan fluida hidrotermal yang melewatinya akan  menyebabkan perubahan komposisi (oksida/unsur) pada batuan yang dilewati maupun pada fluida itu sendiri. Perhitungan perubahan oksida/unsur bertujuan untuk menentukan oksida/unsur dalam batuan yang bertambah atau berkurang karena proses alterasi hidrotemal, dilakukan dengan menggunakan analisis ICP-AES (Inductively Coupled Plasma Atomic Emission  Spectroscopy) dan ICP-MS (Inductively Coupled Plasma Mass Spectrometry). Hasil penelitian menunjukkan bahwa oksida/unsur yang immobile umumnya relatif tidak mengalami perubahan komposisi selama proses alterasi hidrotermal berlangsung,  sedangkan oksida/unsur mobile umumnya mengalami penambahan dan pengurangan selama proses alterasi hidrotermal berlangsung. Pada alterasi propilitik, oksida/unsur mobile yang mengalami penambahan adalah As, Zr, Cu, Sb, Ca, CaO, MgO, MnO dan SiO2 dan yang mengalami pengurangan adalah U, Th, Co, Sn, Sr, Nb, Ba, K, Au, Pb, Zn, V, Fe, K2O, Na2O dan Fe2O3. Pada alterasi serisitik, oksida/unsur mobile yang mengalami penambahan adalah Sb, Zr, Ag, Pb, K, Na2O, SiO2 dan yang mengalami pengurangan  adalah U, Th, Co, As, Nb, Ba, Sn, Sr, Ca, S, Au, V, Zn, Cu, Fe, K2O, MnO, CaO, MgO, Fe2O3. Pada alterasi argilik, oksida/unsur mobile yang mengalami penambahan adalah  Sb, Fe, S, Cu, Zr, Ba, As, Au, Zn, V, dan SiO2 sedangkan yang cenderung mengalami pengurangan adalah Ca, U, Th, Nb, Sn, Sr, Co, Pb, K, CaO, Na2O, MnO, MgO, K2O dan Fe2O3.Katakunci : Alterasi hidrotermal, Pegunungan Rumbia, Kabupaten Bombana, perubahan oksida/unsur, mobile, immobile.


2019 ◽  
Vol 40 (3) ◽  
pp. 115-133 ◽  
Author(s):  
Scott Wilschefski ◽  
Matthew Baxter

Inductively coupled plasma mass spectrometry (ICP-MS) is an analytical technique that can be used to measure elements at trace levels in biological fluids. Although older techniques such as atomic absorption and atomic emission are still in use by some laboratories, there has been a slow shift toward ICP-MS, particularly in the last decade. As this shift is likely to continue, clinical scientists should be aware of the analytical aspects of ICP-MS, as well as the potential for both spectroscopic and non-spectroscopic interference, and strategies that can be employed to eliminate or mitigate these issues.


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