Determination on Heavy Metals Content of Achyranthes bidentata Blume. through Inductively Coupled Plasma Mass Spectrometry (ICP-MS)

[Objective] The inductively coupled plasma mass spectrometry(ICP-MS)was constructed to determine the contents of lead,cadmium,mercury and arsenic in Archyranthes bidentata Blume.[Method]Under the optimum operation condition of ICP-MS,the samples were digested by microwave.The element 114In was taken as an internal standard element to compensate body effect and ICP-MS method was used to determine the contents of lead,cadmium,mercury and arsenic.[Result]For the determined elements,the correlation coefficient(r)of standard curve was over 0.9995 and recovery rate was from 96.7% to 106.4% while RSD was less than 11.2%.The result of determination showed that the heavy metal content in Archyranthes bidentata Blume.beyond standard was serious.[Conclusion]The constructed ICP-MS method with simple operation,rapid response,accuracy and high sensitivity in this experiment could be used for quality control of Chinese medicinal materials by detecting heavy metal contents in different Chinese medicinal materials from original places.

Effects of external parameters on plasma characteristics and uniformity in a dual cylindrical inductively coupled plasma

The dual cylindrical inductively coupled plasma source,compared to the conventional structure of inductively coupled plasma source,can significantly improve the uniformity of plasma.It has an enhanced potential for application in processes,such as etching and ashing.A uniform plasma can be obtained by allowing the remote plasma from the upper chamber modulate the main plasma generated in the lower chamber.In this study,a fluid model was employed to investigate a dual cylindrical inductively coupled Ar/O_(2)discharge.The effects of external parameters on electron density,electron temperature,O atomic density,and plasma uniformity in the main chamber were studied,and the reasons were analyzed.The results of this study show that remote power can control the plasma uniformity and increase the plasma density in the main chamber.As the remote power increased,plasma uniformity improved initially and then deteriorated.The main power affected the plasma density at the edge of the main chamber and can modulate the plasma density in the main chamber.The gas pressure affected both the uniformity and density of the plasma.As the gas pressure increased,the plasma uniformity deteriorated,but the free radical density improved.

Effect of coil and chamber structure on plasma radial uniformity in radio frequency inductively coupled plasma

Enhancing plasma uniformity can be achieved by modifying coil and chamber structures in radio frequency inductively coupled plasma(ICP)to meet the demand for large-area and uniformly distributed plasma in industrial manufacturing.This study utilized a two-dimensional self-consistent fluid model to investigate how different coil configurations and chamber aspect ratios affect the radial uniformity of plasma in radio frequency ICP.The findings indicate that optimizing the radial spacing of the coil enhances plasma uniformity but with a reduction in electron density.Furthermore,optimizing the coil within the ICP reactor,using the interior point method in the Interior Point Optimizer significantly enhances plasma uniformity,elevating it from 56%to 96%within the range of the model sizes.Additionally,when the chamber aspect ratio k changes from 2.8 to 4.7,the plasma distribution changes from a center-high to a saddleshaped distribution.Moreover,the plasma uniformity becomes worse.Finally,adjusting process parameters,such as increasing source power and gas pressure,can enhance plasma uniformity.These findings contribute to optimizing the etching process by improving plasma radial uniformity.

Preliminary Study on Destruction of Freon 12 by Inductively Coupled Plasma--Development of ICP Technology for Waste Destruction

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Inductively coupled plasma mass spectrometry (ICP-MS) and its application in life sciences

Inductively-coupled plasma mass spectrometry (ICP-MS) has made much progress since its birth in the late 1990s. This paper will give a rather systematic overview on the use of this technique in new devices and technologies related to plasma source, sample-introducing device and detecting spectrometer etc. In this overview, an emphasis will be put on the evaluation of the ICP- MS technique in combination with a series of physical, chemical and biological techniques, such as laser ablation (LA), capillary electrophoresis (CE) and high performance liquid chromatograph (HPLC), along with their representative high accuracy and high sensitivity. Finally, comprehensive and fruitful applications of the ICP-MS and its combinative techniques in the detection of trace metallic elements and isotopes in complex biological and environmental samples will be revealed.

Analysis of Cu,Co,V and Zn in Coastal Waters of the East China Sea by Inductively Coupled Plasma Mass Spectrometry(ICP-MS)

In this study, a simple method for the simultaneous determination of trace metals(Cu, V, Co, Zn) in coastal seawater using the Mg(OH)2 coprecipitation inductively coupled plasma mass spectrometry(ICP-MS) was developed. This multi-element method enables the simultaneous extraction of four metals, particularly Co and V. The recoveries of Cu, Co, V and Zn after Mg(OH)2 coprecipitation were 73%, 96%, 94% and 92%, which means that our procedure was well-suited to the determination of these four trace metals. The detection limits were 3.81, 0.18, 6.09 and 1.91 nmol L-1, respectively. Then, applying this method to the simultaneous determination of these four metals in coastal water samples from the East China Sea revealed that the concentrations of Cu, Zn, Co and V were higher in bottom waters compared to water at other depths, and higher concentrations were generally observed at the Yangtze River estuary. Additionally, example vertical profiles of dissolved trace metal concentrations for the East China Sea in spring and autumn are compared. These findings indicate that Zn had the greatest seasonal variation followed by Cu, V and Co. For Zn and Co, the concentrations were higher during spring than during autumn. For Cu and V, the seasonal variation in the concentrations was opposite.

Determination of potassium content as principal components in pyrotechnic compositions used for fireworks and firecrackers based on inductively coupled plasma optical emission spectrometric approach （ICP-OES）

Inductively coupled plasma optical emission spectrometric approach（1CP-OES） is used to determine the potassium content as principal component in pyrotechnic compositions used for fireworks and firecrackers. Element of potassium is conunonly found in potassium nitrate and potassium perchlorate in pyrotechnic compositions in fireworks and firecrackers. Statistical analysis shows that potassium nitrate content in pyrotechnics is between 10% to 60% and the potassium perchlorate content is between 20% to 70%,which counted in the content of potassium element is between 4% to 23%. Concept of this method： considering the weight of the sample is 400rag,constant volume is 1L and the concentration of potassium is between 10 mg/L to 90 mg/L in sample solution, the determination scope of the method for the potassium content would be between 1% to 23%.Further experiments proved that the fitting correlation coefficient of potassium calibration curve is 0.9997 or higher, recovery is 89.15%-100.23%.The allowable differential value is 0.4% between two single tests under repeatable conditions. This method can completely satisfy the requirements of the fireworks and firecrackers industry with high accuracy and good precision.

Determination of magnesium and aluminum content as principal components in pyrotechnic compositions used for fireworks and firecrackers based on inductively coupled plasma optical emission spectrometric approach （ICP-OES）

Inductively coupled plasma optical emission spectrometric approach（ICP-OES）is used to determine the magnesium and aluminum content as principal components in pyrotechnic compositions used for fireworks and firecrackers. Elements of magnesium and aluminum are commonly found in aluminum powder or magnesium-aluminum alloy powder in pyrotechnic compositions in fireworks and firecrackers. Statistical analysis shows that the magnesium content in pyrotechnics is between 8% to 30% and the aluminum content is between 8% to 35%（roughly）.Concept of this method： suppose the weight of the sample is 400rag,constant volume is IL and the concentlation of magnesium and aluminum is between 12mg/L to 160mg/L in sample solution, the determination scope of the method for magnesium and aluminum content would be between 3% to 40%.Further experiments proved that the fitting correlation coefficient of the magnesium calibration curve is 0.9999 or higher, recovery is 101.01% -101.96%.The fitting correlation coefficient of the aluminum calibration curve is 0.9999 or higher, recovery is 99.36%-103.07%. The allowable differential value is 0.4% between two single tests under repeatable conditions. This method can completely satisfy the requirements of the fireworks and firecrackers industry with high accuracy and good precision.

Quantification of trace amounts of impurities in high purity cobalt by high resolution inductively coupled plasma mass spectrometry

A An analytical method using high resolution inductively coupled plasma mass spectrometry （HR-ICP-MS） for rapid simultaneous determination of 24 elements （Be, Mg, A1, Ti, V, Cr, Mn, Fe, Ni, Cu, Zn, Ga, Ge, As, Se, Mo, Ag, Cd, Sn Sb, Ba, Pt, Au, and Pb） in high purity cobalt was described. Sample digestions were performed in closed microwave vessels using HNO3 and HCI. The matrix effects because of the presence of excess HCI and Co were evaluated. The usefulness of high mass resolution for overcoming some spectral interference was demonstrated. The optimum conditions for the determination were tested and discussed. The standard addition method was employed for quantitative analysis. The detection limits were 0.016-1.50 ].tg·g^-1, the recovery ratios were 92.2%-111.2%, and the RSD was less than 3.6%. The method was accurate, quick, and convenient. It was applied to the determination of trace impurities in high purity cobalt with satisfactory results.

Microstructure, Hardness and Corrosion Resistance of ZrN Films Prepared by Inductively Coupled Plasma Enhanced RF Magnetron Sputtering

ZrN fihns were deposited on Si（111） and M2 steel by inductively coupled plasma （ICP）-enhanced RF magnetron sputtering. The effect of ICP power on the microstructure, mechanical properties and corrosion resistance of ZrN films was investigated. When the ICP power is below 300 W, the ZrN films show a columnar structure. With the increase of ICP power, the texture coefficient （To） of the （111） plane, the nanohardness and elastic modulus of the films increase and reach the maximum at a power of 300 W. As the ICP Power exceeds 300 W, the films exhibit a ZrN and ZrNx mixed crystal structure without columnar grain while the nanohardness and elastic modulus of the films decrease. All the ZrN coated samples show a higher corrosion resistance than that of the bare M2 steel substrate in 3.5% NaCl electrolyte. The nanohardness and elastic modulus mostly depend on the crystalline structure and Tc of ZrN（111）.

Experimental Study of the Influence of Process Pressure and Gas Composition on GaAs Etching Characteristics in Cl_2/BCl_3-Based Inductively Coupled Plasma

A study of Cl2/BCl3-based inductively coupled plasma （ICP） was conducted using thick photoresist mask for anisotropic etching of 50μm diameter holes in a GaAs wafer at a relatively high average etching rate for etching depths of more than 150μm. Plasma etch characteristics with ICP process pressure and the percentage of BCI3 were studied in greater detail at a constant ICP coil/bias power. The measured peak-to-peak voltage as a function of pressure was used to estimate the minimum energy of the ions bombarding the substrate. The process pressure was found to have a substantial influence on the energy of heavy ions. Various ion species in plasma showed minimum energy variation from 1.85 eV to 7.5 eV in the pressure range of 20 mTorr to 50 mTorr. The effect of pressure and the percentage of BCl3 on the etching rate and surface smoothness of the bottom surface of the etched hole were studied for a fixed total flow rate. The etching rate was found to decrease with the percentage of BCl3, whereas the addition of BCl3 resulted in anisotropic holes with a smooth veil free bottom surface at a pressure of 30 mTorr and 42% BC13. In addition, variation of the etching yield with pressure and etching depth were also investigated.

Determination of trace elements in high purity nickel by high resolution inductively coupled plasma mass spectrometry

The contents ofMg, Al, Si, Ti, Cr, Mn, Fe, Co, Cu, Ga, As, Se, Cd, Sb, Pb and Bi in high purity nickel were determined by high resolution inductively coupled plasma mass spectrometry （HR-ICP-MS）. The sample was dissolved in HNO3 and HCI by microwave digestion. Most of the spectral interferences could be avoided by measuring in the high resolution mode. The matrix effects because of the presence of excess HC1 and nickel were evaluated. Correction for matrix effects was made using Sc, Rh and T1 as internal standards. The optimum conditions for the determination were tested and discussed. The detection limits range from 0.012 to 1.76 ~tg/g depending on the type of elements. The applicability of the proposed method is also validated by the analysis of high purity nickel reference material （NIST SRM 671）. The relative standard deviation （RSD） is less than 3.3%. Results for determination of trace elements in high purity nickel were presented.

Spheroidization of silica powders by radio frequency inductively coupled plasma with Ar–H2 and Ar–N2 as the sheath gases at atmospheric pressure

Amorphous spherical silica powders were prepared by inductively coupled thermal plasma treatment at a radio frequency of 36.2 MHz. The effects of the added content of hydrogen and nitrogen into argon(serving as the sheath gas), as well as the carrier gas flow rate, on the spheroidization rate of silica powders, were investigated. The prepared silica powders before and after plasma treatment were examined by scanning electron microscopy, X-ray diffraction, and laser granulometric analysis. Results indicated that the average size of the silica particles increased, and the transformation of crystals into the amorphous state occurred after plasma treatment. Discharge image processing was employed to analyze the effect of the plasma temperature field on the spheroidization rate. The spheroidization rate of the silica powder increased with the increase of the hydrogen content in the sheath gas. On the other hand, the spheroidization rate of the silica power first increased and then decreased with the increase of the nitrogen content in the sheath gas. Moreover, the amorphous content increased with the increase of the spheroidization rate of the silica powder.

Ion Density Distribution in an Inductively Coupled Plasma Chamber

The ion density distribution in the reaction chamber was diagnosed by a Langmuir probe. The rules of the ion density distribution were obtained under the pressures of 9 Pa, 13 Pa, 27 Pa and 53 Pa in the reaction chamber, different radio-frequency powers and different positions. The result indicates that the ion density decreases as the pressure increases, and increases as the power decreases. The ion density of axial position z =0 achieves 5.8×1010 on the center of coil under the power of 200 w and pressure of 9 Pa in the reaction chamber.

Modeling Approach and Analysis of the Structural Parameters of an Inductively Coupled Plasma Etcher Based on a Regression Orthogonal Design

The geometry of an inductively coupled plasma （ICP） etcher is usually considered to be an important factor for determining both plasma and process uniformity over a large wafer. During the past few decades, these parameters were determined by the ＂trial and error＂ method, resulting in wastes of time and funds. In this paper, a new approach of regression orthogonal design with plasma simulation experiments is proposed to investigate the sensitivity of the structural parameters on the uniformity of plasma characteristics. The tool for simulating plasma is CFD-ACE＋, which is commercial multi-physical modeling software that has been proven to be accurate for plasma simulation. The simulated experimental results are analyzed to get a regression equation on three structural parameters. Through this equation, engineers can compute the uniformity of the electron number density rapidly without modeling by CFD-ACE＋. An optimization performed at the end produces good results.

Surface Modification of Nanometre Silicon Carbide Powder with Polystyrene by Inductively Coupled Plasma

An investigation was made into polystyrene （PS） grafted onto nanometre silicon carbide （SIC） particles. In our experiment, the grafting polymerization reaction was induced by a radio frequency （RF） inductively coupled plasma （ICP） treatment of the nanometre powder. FTIR （Fourier transform infrared spectrum） and XPS （X-ray photoelectron spectroscopy） results reveal that PS is grafted onto the surface of silicon carbide powder. An analysis is presented on the effectiveness of this approach as a function of plasma operating variables including the plasma treating power, treating time, and grafting reaction temperature and time.

The determination of 52 elements in marine geological samples by an inductively coupled plasma optical emission spectrometry and an inductively coupled plasma mass spectrometry with a high-pressure closed digestion method

An improved analytical method to determine the content of 52 major, minor and trace elements in marine geological samples, using a HF-HCl-HNO_3 acid system with a high-pressure closed digestion method（HPCD）, is studied by an inductively coupled plasma optical emission spectrometry（ICP-OES） and an inductively coupled plasma mass spectrometry（ICP-MS）. The operating parameters of the instruments are optimized, and the optimal analytical parameters are determined. The influences of optical spectrum and mass spectrum interferences, digestion methods and acid systems on the analytical results are investigated. The optimal spectral lines and isotopes are chosen, and internal standard element of rhodium is selected to compensate for matrix effects and analytical signals drifting. Compared with the methods of an electric heating plate digestion and a microwave digestion, a high-pressure closed digestion method is optimized with less acid, complete digestion,less damage for digestion process. The marine geological samples are dissolved completely by a HF-HCl-HNO_3 system, the relative error（RE） for the analytical results are all less than 6.0%. The method detection limits are 2–40μg/g by the ICP-OES, and 6–80 ng/g by ICP-MS. The methods are used to determine the marine sediment reference materials（GBW07309, GBW07311, GBW07313）, rock reference materials（GBW07103, GBW07104,GBW07105）, and cobalt-rich crust reference materials（GBW07337, GBW07338, GBW07339）, the obtained analytical results are in agreement with the certified values, and both of the relative standard deviation（RSD） and the relative error（RE） are less than 6.0%. The analytical method meets the requirements for determining 52 elements contents of bulk marine geological samples.

Quantification of Trace Amounts of Impurities in High Purity Cobalt by High Resolution Inductively Coupled Plasma Mass Spectrometry

An analytical method using high resolution inductively coupled plasma mass spectrometry （HR-ICP-MS） for rapid simultaneous determination of Be, Mg, Al, Ti, V, Cr, Mn, Fe, Ni, Cu, Zn, Ga, Ge, As, Se, Mo, Ag, Cd, Sn, Sb, Ba, Pt, Au and Pb in high purity cobalt was described. Sample digestions were performed in closed microwave vessels using HNO3 and HCl. The matrix effects due to the presence of excess HCl and Co were evaluated. The usefulness of high mass resolution for overcoming some spectral interference was demonstrated. The optimum conditions for the determination was tested and discussed. Correction for matrix effects, Sc, Rh and Bi were used as internal standards. The detection limits is 0.003-0.57 μg/g, the recovery ratio is 92.2%-111.2%, and the RSD is less than 3.6%. The method is accurate, quick and convenient. It has been applied to the determination of trace impurities in high purity cobalt with satisfactory results.

Determination of micro yttrium in an ytterbium matrix by inductively coupled plasma atomic emission spectrometry and wavelet transform

In the determination of trace yttrium (Y) in an ytterbium (Yb) matrix byinductively coupled plasma atomic emission spectrometry (ICP-AES), the most prominent line ofyttrium, Y 371.030 nm line, suffers from strong interference due to an emission line of ytterbium.In mis work, a method based on wavelet transform was proposed for the spectral interferencecorrection. Haar wavelet was selected as the mother wavelet. The discrete detail after the thirddecomposition, D3, was chosen for quantitative analysis based on the consideration of bothseparation degree and peak height. The linear correlation coefficient between the height of the leftpositive peak in D3 and the concentration of Y was calculated to be 0.9926. Six synthetic sampleswere analyzed, and the recovery for yttrium varied from 96.3 percent to 110.0 percent. The amountsof yttrium in three ytterbium metal samples were determined by the proposed approach with an averagerelative standard deviation (RSD) of 2.5 percent, and the detection limit for yttrium was 0.016percent. This novel correction technique is fast and convenient, since neither complicated modelassumption nor time-consuming iteration is required. Furthermore, it is not affected by thewavelength drift inherent in monochromators that will severely reduce the accuracy of resultsobtained by some chemometric methods.

Frequency dependence of plasma characteristics at different pressures in cylindrical inductively coupled plasma source

The effects of driving frequency on plasma parameters and electron heating efficiency are studied in cylindrical inductively coupled plasma(ICP) source. Measurements are made in an Ar discharge for driving frequency at 13.56/2 MHz, and pressures of 0.4-1.2 Pa. In 13.56 MHz discharge, higher electron density(n_e) and higher electron temperature(T_e) are observed in comparison with 2 MHz discharge at 0.6-1.2 Pa. However, slightly higher n_e and T_e are observed in 2 MHz discharge at 0.4 Pa. This observation is explained by enhanced electron heating efficiency due to the resonance between the oscillation of 2 MHz electromagnetic field and electron-neutral collision process at 0.4 Pa. It is also found that the variation of T_edistribution is different in 13.56 and 2 MHz discharge.For ICP at 13.56 MHz, T_eshows an edge-high profile at 0.4-1.2 Pa. For 2 MHz discharge, T_e remains an edge-high distribution at 0.4-0.8 Pa. However, the distribution pattern involves into a center-high profile at 0.9-1.2 Pa. The spatial profiles of n_e remain a center-high shape in both 13.56 and 2 MHz discharges, which indicates the nonlocal kinetics at low pressures. Better uniformity could be achieved by using 2 MHz discharge. The effects of gas pressure on plasma parameters are also examined. An increase in gas pressure necessitates the rise of n_e in both 13.56 and 2 MHz discharges. Meanwhile, T_e drops when gas pressure increases and shows a flatter distribution at higher pressure.