Diagnostics of laser-induced plasma on carbon-based polymer material using atomic and molecular emission spectra

Time-integrated optical emission analysis of laser-induced plasma on Teflon is presented.Plasma was induced under atmospheric pressure air using transversely excited atmospheric CO_(2) laser pulses.Teflon is a C-based polymer that is,among other things,interesting as a substrate for laser-induced breakdown spectroscopy analysis of liquid samples.This study aimed to determine the optimal experimental conditions for obtaining neutral and ionized C spectral lines and C2 and CN molecular band emission suitable for spectrochemical purposes.Evaluation of plasma parameters was done using several spectroscopic techniques.Stark profiles of appropriate C ionic lines were used to determine electron number density.The ratio of the integral intensity of ionic-to-atomic C spectral lines was used to determine the ionization temperature.A spectral emission of C2 Swan and CN violet bands system was used to determine the temperature of the colder,peripheral parts of plasma.We critically analyzed the use of molecular emission bands as a tool for plasma diagnostics and suggested methods for possible improvements.

CORRECTION OF WING INTERFERENCE WITH KALMAN FILTERING IN INDUCTIVELY COUPLED PLASMA ATOMIC EMISSION SPECTROMETRY

A Kalman filter was developed for correction of wing interference in ICP-AES.Modeling wing interference theoretically instead of experimentally, the filter can compensate the shift in wavelength position in scans, and therefore reduce the effect of the interference on detection limit.

A Perspective of Laser Sampling for Inductively Coupled Plasma-Atomic Emission Spectro metry for Rock and Mineral Analysis

The development of laser sampling for optical emission spectrometry is reviewed . Advantages and limitations of pulsed laser sampling are compared with those of continuous laser sampling . A novel method of laser sampling of liquid samples for inductively coupled plasma -atomic emission spectrometry has been proposed , and its analytical performance investigated.Experimental results showed that,as a method of sample introduction , laser vaporization of liquid samples enjoyed certain advantages , e.g.,much higher sensitivity, much lower detection limit and reduced sample volume , over solution nebulization . A perspective of the application of laser sampling-inductively coupled plasma - actomic emission spectrometry for rock and mineral analysis is estimated as well.

Quantitative Determination of Density of Ground State Atomic Oxygen from Both TALIF and Emission Spectroscopy in Hot Air Plasma Generated by Microwave Resonant Cavity

Two experimental techniques have been used to quantify the atomic oxygen density in the case of hot air plasma generated by a microwave （MW） resonant cavity. The latter operates at a frequency of 2.45 GHz inside a cell of gas conditioning at a pressure of 600 mbar, an injected air flow of 12 L/min and an input MW power of 1 kW. The first technique is based on the standard two photon absorption laser induced fluorescence （TALIF） using xenon for calibration but applied for the first time in the present post discharge hot air plasma column having a temperature of about 4500 K near the axis of the nozzle. The second diagnostic technique is an actinometry method based on optical emission spectroscopy （OES）. In this case, we compared the spectra intensities of a specific atomic oxygen line （844 nm） and the closest wavelength xenon line （823 nm）. The two lines need to be collected under absolutely the same spectroscopic parameters. The xenon emission is due to the addition of a small proportion of xenon （1% Xe） of this chemically inert gas inside the air while a further small quantity of H2 （2~） is also added in the mixture in order to collect OH（A- X） and NH（A-X） spectra without noise. The latter molecular spectra are required to estimate gas and excitation temperatures. Optical emission spectroscopy measurements, at for instance the position z=12 mm on the axis plasma column that leads to a gas measured temperature equal to 3500 K, an excitation temperature of about 9500 K and an atomic oxygen density 2.09× 1017＋ 0.2×1017 cm-3. This is in very good agreement with the TALIF measurement, which is equal to 2.0×101T cm-3.

Diagnostics of Argon Inductively Coupled Plasma and Dielectric Barrier Discharge Plasma by Optical Emission Spectroscopy

An experimental setup was built up to carry out radio frequency (RF) inductively coupled plasma (ICP) and dielectric barrier discharge (DBD), and to depict the optical emission spectra (OES) of the discharges. OES from argon ICP and DBD plasmas in visible and near ultraviolet region were measured. For argon ICP, the higher RF power input (higher than 500 W for our machine), the higher degree of argon plasma ionization. But that doesn't mean a higher mean electron energy. With the increase in the power input, the mean electron energy increases slightly, whereas the density of electron increases apparently On the contrary, argon DBD discharge behaves in the manner of a pulsed DC discharge on optical emission spectroscopy and V-I characteristics. DBD current is composed of a series of pulses equally spaced in temporal domain. The Kinetics of DBD emission strength is mainly governed by the frequency of the current pulse.

A Study on the Determination of Copper by Microwave Induced Plasma Atomic Emission Spectrometry (MIP-AES)

The determination of copper by MIP-AES was investigated in detail. Aqueous samples were introduced from an ultrasonic nebulizer and the solvent was removed by a desolvation device before introduction of the aerosol into the MIP. The desolvation system consisted of a condenser associated with a concentrated H2SO4 absorption cell. Various experimental conditions and interferences from easily ionised elements (EIEs) were also studied and some practical samples were analyzed.

Optical Emission Spectroscopic Measurement of Hydroxyl Radicals in Air Discharge with Atomized Water

Effects of discharge mode, voltage applied, size of the nozzle discharge electrode and flow rate of water on the generation of hydroxyl radical were investigated in air discharge with atomized water, by using optical emission spectroscopy （OES）. Water was injected into the discharge region through the discharge nozzle electrode, and a large amount of fine water drops, formed and distributed in the discharge region, corona discharge was more effective to generate were observed. It was found that negative DC the hydroxyl radicals in comparison to positive DC corona discharge or negative pulsed discharge. A larger outer diameter of the nozzle electrode or a stronger electric field is beneficial for hydroxyl-radical generation. Moreover, there is a critical value in the flow rate of atomized water against the discharge voltage. Below this critical value, hydroxyl-radical generation increases with the increase in flow rate of the water, while above this value, it decreases. In addition, it is observed that OES from the discharge is mainly in the ultraviolet domain. The results are helpful in the study of the mechanism and application of plasma in pollution-control in either air or water.

Optical Emission Spectroscopic Studies of ICP Ar Plasma

The ion line of 434.8 nm and atom line of 419.8 nm of Ar plasma produced by an inductively coupled plasma （ICP） were measured by optical emission spectroscopy and the influences from the working gas pressure, radio-frequency （RF） power and different positions in the discharge chamber on the line intensities were investigated in this study. It was found that the intensity of Ar atom line increased firstly and then saturated with the increase of the pressure. The line intensity of Ar^＋, on the other hand, reached a maximum value and then decreased along with the pressure. The intensity of the line in an RF discharge also demonstrated a jumping mode and a hysteresis phenomenon with the RF power. When the RF power increased to 400 W, the discharge jumped from the E-mode to the H-mode where the line intensity of Ar atom demonstrated a sudden increase, while the intensity of Ar^＋ ion only changed slightly. If the RF power decreased from a high value, e.g., 1000 W, the discharge would jump from the H-mode back to the E-mode at a power of 300 W. At this time the intensities of Ar and Ar^＋ lines would also decrease sharply. It was also noticed in this paper that the intensity of the ion line depended on the detective location in the chamber, namely at the bottom of the chamber the line was more intense than that in the middle of the chamber, but less intense than at the top, which is considered to be related to the capacitance coupling ability of the ICP plasma in different discharge areas.

Measurements of Absolute Atomic Nitrogen Density by Two-Photon Absorption Laser-Induced Fluorescence Spectroscopy in Hot Air Plasma Generated by Microwave Resonant Cavity

For the first time, absolute densities of atomic nitrogen in its ground state (N4S) have been measured in hot dry and humid air plasma columns under post-discharge regime. The determination of space-resolved absolute densities leads to obtain the dissociation degrees of molecular nitrogen in the plasma. The hot plasmas are generated inside an upstream gas-conditioning cell at 600 mbar when the air gas flow is directly injected at 10 slm in a microwave resonant cavity (2.45 GHz, 1 kW) placed in the downstream side. Density measurements based on laser induced fluorescence spectroscopy with two-photon excitation (TALIF), are more particularly performed along the radial and axial positions of the plasma column. Calibration of TALIF signals is performed in situ (i.e. in the same gas-conditioning cell but without plasma) using an air gas mixture containing krypton. Optical emission spectroscopy is considered to estimate the rotational gas temperature by adding a small amount of H2 in dry air to better detect OH (A-X) spectra. The rotational temperatures in humid air plasma column (50% of humidity) are larger than those of dry air plasma column by practically 30% near the nozzle of resonant cavity on the axis of the plasma column. This is partly due to attachment heating processes initiated by water vapor. A maximum of the measured absolute nitrogen density is also observed near the nozzle which is also larger for humid air plasma column. The obtained dissociation degrees of molecular nitrogen in both dry and humid air plasma along the air plasma column are lower than the cases where only thermodynamic equilibrium is assumed. This is characteristic of the absence of chemical and energetic equilibria not yet reached in the air plasma column dominated by recombination processes.

Elemental Content in Brown Rice by Inductively Coupled Plasma Atomic Emission Spectroscopy Reveals the Evolution of Asian Cultivated Rice

The phylogenetic relationship for classification traits and eight mineral elements in brown rice （Oryza sativa L.） from Yunnan Province in China was carried out using microwave assisted digestion followed by inductively coupled plasma atomic emission spectroscopy, and the analytical procedures were carefully controlled and validated. In general, the results show that the mean levels of K, Ca, Mg, Fe and Cu in brown rice for 789 accessions of rice landraces was distinctly lower than that of improved cultivars. They further demonstrate that Ca plays an important role in the differentiation of subspecies indica-japonica, especially to enhance adaptation of cold stress, and that five mineral elements in brown rice enhance the eurytopicity from landrace to improved cultivar. Hierarchical cluster analysis, using average linkage from SPSS software based on eight mineral elements in brown rice, showed that Yunnan rice could be grouped into rice landrace and improved cultivar, with the rice landrace being further clustered into five subgroups, and that, interestingly, purple rice does not cluster with either of the groups. Our present data confirm that indica is the closest relative of late rice and white rice, and that they constitute rice landraces together, whereas japonica is the closest relatives of non-nuda, early-mid and glutinous rice. It is further shown that japonica, non-nuda, early-mid, glutinous, white and red rice might be more primitive than indica, nuda, late, non-glutinous and purple rice, respectively.

Effect of Low-Frequency Power on Etching Characteristics of 6H-SiC in C4F8/Ar Dual-Frequency Capacitively Coupled Plasma

Dry etching of 6H silicon carbide （6H-SiC） wafers in a C4Fs/Ar dual-frequency capacitively coupled plasma （DF-CCP） was investigated. Atomic force microscopy （AFM） and X-ray photoelectron spectroscopy （XPS） were used to measure the SiC surface structure and compositions, respectively. Optical emission spectroscopy （OES） was used to measure the relative concentration of F radicals in the plasma. It was found that the roughness of the etched SiC surface and the etching rate are directly related to the power of low-frequency （LF） source. At lower LF power, a smaller surface roughness and a lower etching rate are obtained due to weak bombardment of low energy ions on the SiC wafers. At higher LF power the etching rate can be efficiently increased, but the surface roughness increases too. Compared with other plasma dry etching methods, the DF-CCP can effectively inhibit CχFγ films＇ deposition, and reduce surface residues.

Investigation of Capacitively Coupled Argon Plasma Driven by Dual-Frequency with Different Frequency Configurations

Low pressure argon dual-frequency （DF） capacitively coupled plasma （CCP） is generated by using different frequency configurations, such as 13.56/2, 27/2, 41/2, and 60/2 MHz. Characteristics of the plasma are investigated by using a floating double electrical probe and optical emission spectroscopy （OES）. It is shown that in the DF-CCPs, the electron temperature Te decreases with the increase in exciting frequency, while the onset of 2 MHz induces a sudden increase in Te and the electron density increases basically with the increase in low frequency （LF） power. The intensity of 750.4 nm emission line increases with the LF power in the case of 13.56/2 MHz, while different tendencies of line intensity with the LF power appear for other configurations. The reason for this is also discussed.

The Study of the Impact of Mercury Sample Magnetization Prior to Detection by Emission Spectroscopy

Experimental investigations were conducted in this study to explore the effect of magnetization on water sample properties and to envisage whether the effect is beneficial for mercury detection in a sample of water or not. Subjecting the water sample to 0.3 Tesla magnetic field for 14 hours led to instantaneous effects on the examined water properties, where a reduction in the values of pH （7%） and interfacial tension （0.2%） was observed, whereas an increase （8%） in water electrical conductivity was recorded. Similar behaviours with slight changes in trend were observed after storing the samples for six days, which indicates a creation of permanent effects. Other experiments were conducted to explore the impact of magnetizing water sample containing inorganic mercury prior to detection by emission spectroscopy. Samples were prepared with different mercury concentrations and derivatized by using tin chloride （SnCI2）. The generated mercury vapour species were transported with aid of carrier gas into a dielectric barrier discharge plasma atomizer, in which the mercury signal at 253.65 nm was recorded. The results have shown 3.5%-7.5% increase in the signal intensities recorded for the magnetized samples, mostly attributed to a reduction in the sample surface tension and other reasons, which facilitates analyte derivatization.

Diagnosis of a low pressure capacitively coupled argon plasma by using a simple collisional-radiative model

This paper proposes a simple collisional-radiative model to characterise capacitively coupled argon plasmas driven by conventional radio frequency in combination with optical emission spectroscopy and Langmuir probe measurements. Two major processes are considered in this model, electron-impact excitation and the spontaneous radiative decay. The diffusion loss term, which is found to be important for the two metastable states （4s[3/2]2, 4s＇[1/2]0）, is also taken into account. Behaviours of representative metastable and radiative states are discussed. Two emission lines （located at 696.5 nm and 750.4 nm） are selected and intensities are measured to obtain populated densities of the corresponding radiative states in the argon plasma. The calculated results agree well with that measured by Langmuir probe, indicating that the current model combined with optical emission spectroscopy is a candidate tool for electron density and temperature measurement in radio frequency capacitively coupled discharges.

Comparison of heating mechanisms of argon helicon plasma in different wave modes with and without blue core

In this work,we investigated the discharge characteristics and heating mechanisms of argon helicon plasma in different wave coupled modes with and without blue core.Spatially resolved spectroscopy and emission intensity of argon atom and ion lines were measured via local optical emission spectroscopy,and electron density was measured experimentally by an RFcompensated Langmuir probe.The relation between the emission intensity and the electron density was obtained and the wavenumbers of helicon and’Trivelpiece-Gould’(TG)waves were calculated by solving the dispersion relation in wave modes.The results show that at least two distinct wave coupled modes appear in argon helicon plasma at increasing RF power,i.e.blue core(or BC)mode with a significant bright core of blue lights and a normal wave(NW)mode without blue core.The emission intensity of atom line 750.5 nm(lArⅠ750.5nm)is related to the electron density and tends to be saturated in wave coupled modes due to the neutral depletion,while the intensity of ion line 480.6 nm(IArⅡ480.6nm)is a function of the electron density and temperature,and increases dramatically as the RF power is increased.Theoretical analysis shows that TG waves are strongly damped at the plasma edge in NW and/or BC modes,while helicon waves are the dominant mechanism of power deposition or central heating of electrons in both modes.The formation of BC column mainly depends on the enhanced central electron heating by helicon waves rather than TG waves since the excitation of TG waves would be suppressed in this special anti-resonance region.

电感耦合等离子体发射光谱法测定土壤中有效磷的不确定度评价

为准确测定土壤中有效磷的含量,采用电感耦合等离子体光谱仪进行测定,并对测定过程中相关因素引起的不确定度进行评定。整个实验过程中不确定度来源主要包括以下5个方面:(1)样品称量时引入的不确定度u(m);(2)加入浸提液时浸提液体积V引入的不确定度u(V);(3)标准溶液配置时引入的不确定度u(C_(s));(4)标准曲线拟合引入的不确定度u(C0);(5)样品测量重复性引入的不确定度u(R)。结果表明,样品测量重复性、标准溶液配置、标准曲线拟合在整个实验中引入的不确定度影响较大。因此,在实际样品测定过程中,一定要注意对结果有影响的不确定度因素,加强质量控制,使结果准确可靠。

电感耦合等离子体发射光谱法测定石灰岩中游离二氧化硅

建立电感耦合等离子体发射光谱(ICP-AES)法和粉末压片制样-X射线荧光光谱(XRF)法联合测定石灰岩中游离二氧化硅含量。准确称取经105℃烘干2 h的石灰岩样品0.1000 g,置于30 mL聚四氟乙烯坩埚中,加入8m L浓磷酸,置于300℃电热板上沸腾20 min,冷却后定容在100 mL容量瓶中,静置12 h。采用ICP-AES测定溶解在溶液中的二氧化硅含量,采用XRF测定石灰岩中二氧化硅总含量,用总的二氧化硅含量减去溶液中二氧化硅的含量就得出了游离二氧化硅的含量。经4种标准物质验证,游离二氧化硅含量分析结果与标准值满足规范中相对误差允许限的要求。该方法操作步骤更为简便,分析速度快,低含量游离二氧化硅结果准确度高,适用于批量石灰岩样品中游离二氧化硅含量分析。

ICP-AES法和原子荧光法检测硫熏处理对山药中重金属的影响

目的:研究硫黄熏蒸对山药中重金属含量的影响,为评估硫黄熏蒸的安全性及山药加工工艺提供科学依据。方法:选取13批不同产地的硫黄对山药进行熏蒸处理,使用微波消解法对样品进行前处理,并通过电感耦合等离子体原子发射光谱法与原子荧光光谱分析法定量分析硫黄及熏蒸前后山药中汞(Hg)、砷(As)、铜(Cu)、镉(Cd)和铅(Pb)的含量。结果:13批硫黄中Pb、As、Hg含量偏高。硫黄熏蒸后,山药中Pb含量普遍上升,且部分样品中As、Hg和Cu含量亦有增加。结论:硫黄熏蒸可能导致重金属元素从硫黄迁移到山药中,因此应制定严格的硫黄熏蒸工艺规范,确保山药的安全性和质量,减少对人体健康的潜在风险。

电感耦合等离子体发射光谱法测定蒙脱石中钛含量

本研究建立了电感耦合等离子体发射光谱法(ICP-OES)测定蒙脱石中钛(Ti)元素含量的检测方法。实验结果表明该方法线性关系良好,相关系数(r)大于0.999;钛元素的检出限和定量限分别为0.0965和0.318 mg·kg^(-1);精密度和重复性的相对标准偏差(RSD)分别为0.676%和2.29%,加标回收率为99.69%。以上结果说明该方法检出限低,精密度和准确度高,是检测蒙脱石以及类似矿物样品钛元素的理想分析方法。

线叶金雀花茶中矿物质元素含量测定及饮用安全性分析

分析线叶金雀花茶的饮用安全性,为其加工和质量控制提供参考。采用电感耦合等离子体发射光谱法(inductively coupled plasma-atomic emission spectroscopy,ICP-AES)测定线叶金雀花茶中的钾、钙、钠、镁、磷、铁、锌、锰、铜、砷、铅、镉12种矿物质元素含量,并研究基于冲泡时间和冲泡次数对矿物质元素溶出率的影响,探讨其饮用安全性。结果表明:中国、南非2种不同产地的样品中矿物质元素含量排序均为钾>钠>钙>镁>磷>铁>锰>锌>铜,波兰样品中矿物质元素的含量排序为钠>钾>钙>镁>磷>铁>锰>锌>铜,砷、铅、镉在三种样品中均未检出,三种样品中铁元素含量差异显著(P<0.05),除铁元素外,南非和波兰的线叶金雀花茶中矿物质元素的含量无显著差异(P>0.05)。通过对矿物质元素的溶出特性进行探讨,线叶金雀花茶可在90℃、冲泡5 min条件下,冲泡2次;在此条件下,人体通过饮用线叶金雀花茶摄入过量钙、磷、铁、锌、铜、锰、砷、铅、镉元素的风险较低。鉴于矿物质元素摄入量的可获得性和可承受性,线叶金雀花茶能补充少量的矿物质元素,是一种良好的饮品原料。