CCD-1型平面光栅电弧直读发射光谱仪测定化探样品中铅锡钼铜银锌的方法研究

2017年三月我单位购进湖北地质中心实验室王鹤龄研发专利技术,将原来WP-1米平面光栅摄谱仪改造为CCD-1型平面光栅电弧直读发射光谱仪。CCD-1型平面光栅电弧直读发射光谱仪是对WP-1米平面光栅摄谱仪改造升级后,成为一款高性能全谱直读光谱仪。我们在原有CCD-1平面光栅电弧直读发射光谱仪测定硼锡银钼基础上,通过多次方法实验,研究出一次摄谱同时测定铅锡钼铜银锌六项元素的分析方法。六个元素测定的检出限Pb 1.56 Sn 0.42 Mo0.21 Cu 0.87Ag 0.012 Zn 7.95(RSD﹪ n=12)1.25﹪~7.43﹪,测定结果经验证准确度精密度检出限和合格率各项指标满足地质矿产实验室管理规范的要求。     

基于深孔改进电极发射光谱法同时测定地球化学样品中微量银、锡、硼

采用深孔改进电极,一米平面光栅交流电弧摄谱法同时测定地球化学样品中微量银、锡、硼的含量。以三氧化二铝、硫酸钾、氟化钠和碳粉作缓冲剂,锗作内标。方法检出限为:银0.015μg/g、锡0.32μg/g、硼1.0μg/g,相对标准偏差(RSD)为5.8%~7.5%。实验用国家一级标准物质进行验证,方法的测定值与标准值相符。     

改造的平面光栅直读光谱仪在测定化探样品中银硼锡元素的应用

平面光栅摄谱仪是地球化学普查样品中,测定银、硼、锡等元素常用的仪器.为提高分析效率和质量,2015年我单位将二米平面光栅摄谱仪改造为CCD-Ⅰ型平面光栅直读光谱仪.改造后的仪器检测限为Ag:0.013μg/g,Sn:0.43μg/g,B:0.71μg/g.精密度(RSD%,n=12)均小于10%,测定国家一级标准物质结果与标准值相符,完全满足地球化学普查样品中银、硼、锡等元素的分析要求.     

电弧直读光谱仪的开发与应用

介绍一种国内首创的电弧直读光谱仪。该仪器由交/直流电弧激发光源、凹面光栅分光系统、光电倍增管接收器及智能测控系统所组成。研制成功地质样品专用的"交流电弧直读光谱仪"和高纯金属专用的"直流电弧直读光谱仪"可取代1m或2m光栅摄谱仪,省去了光谱相板、洗相及译谱等繁琐的操作程序。在优化的分析条件下,可直接对粉末状地球化学样品及高纯金属氧化物中的多种微量元素同时进行直读光谱测定,具有灵敏、准确、快速的特点,各项技术指标符合所属领域的"国家标准"及"行业规范"的要求。现已有多家使用单位采用"交流电弧直读光谱仪"分析了十几万件地球化学样品中的银、锡和硼等元素,取得了良好的应用效果。     

直接滴加液体缓冲剂CCD-I型交流电弧直读发射光谱法测定土壤中银锡

以氟化铵为液体缓冲剂,采用直接固体进样,使用CCD-I型交流电弧直读发射光谱法同时测定土壤中的Ag、Sn,其检出限为Ag 0.035μg/g,Sn 0.52μg/g。免去称样及与粉末缓冲剂混合磨匀的过程,缩短流程,快速简便。滴加氟化铵作缓冲剂,使Sn难挥发元素快速蒸发,增强检测信号强度,增加灵敏度。     

直接滴加液体缓冲剂CCD-I型交流电弧直读发射光谱法测定土壤中银锡

以氟化铵为液体缓冲剂,采用直接固体进样,使用CCD-I型交流电弧直读发射光谱法同时测定土壤中的Ag、Sn,其检出限为Ag 0.035μg/g,Sn 0.52μg/g。免去称样及与粉末缓冲剂混合磨匀的过程,缩短流程,快速简便。滴加氟化铵作缓冲剂,使Sn难挥发元素快速蒸发,增强检测信号强度,增加灵敏度。     

直接滴加液体缓冲剂CCD-I型交流电弧直读发射光谱法测定土壤中银锡

以氟化铵为液体缓冲剂,采用直接固体进样,使用CCD-I型交流电弧直读发射光谱法同时测定土壤中的Ag、Sn,其检出限为Ag 0.035μg/g,Sn 0.52μg/g。免去称样及与粉末缓冲剂混合磨匀的过程,缩短流程,快速简便。滴加氟化铵作缓冲剂,使Sn难挥发元素快速蒸发,增强检测信号强度,增加灵敏度。     

发射光谱光电直读法测定高纯铝中的微量杂质

发射光谱光电直读(简称“光电法”)直接分析固体样品,具有快速、准确、多元素同时测定等优点,但以往的方法,灵敏度都比较低。鹿岛次郎等报导,光电法直接测定高纯铝固体样品中的Fe、Si和Cu时,它们的分析含量范围分别为0.001—1.5％,0.001—2.0％和0.001—1.0％,当它们的含量低于0.01时,分析精度(相对均方偏差)为10％.美国利用1.5米或20米光栅光电直读光谱仪分析上述含量元素时,所得的工作曲线形状是非线性的。     

聚光科技推出高分辨率电弧全谱直读光谱仪

<正>聚光科技正式对外发布直读光谱仪家族的最新成员:E5000A型高分辨率电弧直读光谱仪,与E5000共用同一技术平台,把原有2 400 L/mm的光栅更换为3 600 L/mm,增大光谱仪色散,分辨率提高了30%,光谱半高全宽达到18pm。在样品分析过程中,能有效的避免元素间干扰,使     

DCP直读光谱测定地质样品中痕量稀土元素

地质样品中痕量稀土元素的测定,已有不少报导。本文主要采用P507萃取树脂分离和富集稀土元素,以DOP为光源,用中阶梯光栅直读光谱仪进行痕量稀土元素测定。本实验提出了一套可供选用的最     

非平衡等离子体放电模式及反应器结构对氨气分解制氢的影响

在常压下研究了不同等离子体放电模式及反应器结构对氨分解制氢反应的影响.实验中调节反应器结构分别产生了介质阻挡放电和交流弧放电两种放电模式.通过对两种放电模式的放电图像、电压-电流波形和氨分解过程中等离子体区活性物种的发射光谱(OES)研究发现,与介质阻挡放电相比,交流弧放电为局部强放电,具有更高的电源效率和电子密度.因此,在介质阻挡放电中氨气分子大部分通过生成电子激发态物种NH3*,再与载能电子碰撞断裂N―H键进行氨分解反应;而在交流弧放电中载能电子具有更高的平均电子能量,可直接断裂氨气分子的N―H键生成NH2和NH等高活性物种,促进氨分解反应的进行.结果表明,交流弧放电的氨分解效果要明显优于介质阻挡放电.在交流弧放电模式下不同类型反应器对氨气分解转化率由高到低的顺序为:管-管管-板针-板板-板.在输入功率为30 W,气隙间距为6 mm时,管-管交流弧放电的氨气转化率达到60%左右,而板-板介质阻挡放电的氨气转化率仅为4%.     

Investigation of Electrode Phenomena in an Innovative Thermal Plasma Process for Glass Melting

A multi-phase alternating current (AC) arc has been applied to glass melting technology. The large volume discharge produced by a stable multi-phase AC arc is preferable to melt the granulated glass materials. The discharge behavior and the high-temperature region of the plasma can be controlled by the electrode configurations. In this study, the spatial characteristics of the arc discharge were examined by image analysis of high-speed camera. Results show arc existence area is related with electrode configuration. This study provides the useful information of efficient particle treatment in the preferred electrode configuration. However, the electrode erosion is one of the most considerable issues to be solved. The combination of high-speed video camera and band-pass filters was introduced to measure the electrode temperature to investigate the erosion mechanism of the multi-phase AC arc. The dynamic behavior of the electrode vapors in the arc was investigated by using the same high-speed camera system. Results show the tungsten electrode mainly evaporates at the anodic period during AC cycle.     

Characteristics of Multi-Phase Alternating Current Arc for Glass In-Flight Melting

An innovative in-flight melting technology with multi-phase AC arc was developed for glass industry. The enthalpy probe and high speed video camera were used to characterize the temperature, velocity, and discharge behavior of multi-phase AC arc. The effects of input power and sheath gas flow rate on arc and melting behavior were investigated. Results show that the temperature and velocity on arc center are increased with input power or sheath gas flow increase. The fluctuation of luminance area ratio and coefficient of variation reflects the change of arc discharge behavior. High temperature of plasma enhances the melting of granulated raw particles during in-flight heating treatment. The shrinkage of particle and the volatilization degree of Na₂O increase under a larger flow rate of sheath gas. The characterized arc behavior agrees with the melting behavior of glass raw materials, which can provide valuable guidelines for the process control of glass melting.     

High Speed Video Camera and Electrical Signal Analyses of Arcs Behavior in a 3-Phase AC Arc Plasma Torch

A 3-phase AC plasma torch has been developed and aims at overcoming some limits of the classical DC torches in terms of efficiency, cost and reliability. However, the arc behavior in 3-phase plasma torch remains poorly explored. This paper is dedicated to the high speed video camera at 100,000 frames per second and electrical signal analyses of arcs behavior in a 3-phase AC arc plasma torch. First, a reference case at 150 A, in nitrogen as working gas, has been deeply analyzed. Afterwards, a parametric study based on current and inter-electrode gap has been carried out. Results show that only one arc can exist at a given time and arcs rotate by switching from a pair of electrodes to another one, following the maximal electrical gap potential. However, a particular “abnormal” arc behavior was sometimes observed. Indeed, the arc motion within the inter-electrode gap increases the heat exchange and stabilizes the 3-phase discharge whereas the system is unbalanced when the arc is in the periphery. The analysis highlights that the arc motion is strongly influenced by the electrode jet velocity and repulsive Lorentz forces. The parametric study shows that the current increases both jet velocity and arc discharge stability. Elsewhere, the increase of the inter-electrode gap can also stabilizes the electrical 3-phase arc discharge. Furthermore, the correlation between arc motion and current waveform is highlighted. This work is likely to open the way toward a better understanding of 3-phase discharges in the perspective of their further optimization.     

Problems and optimization of sampling,storage, and sample preparation in the determination of the trace element composition of human saliva

Experimental results are reported on the effect of the procedure of sampling, storage conditions, and sample preparation of saliva on the concentrations of trace elements determined by atomic emission digital spectrography of liquid samples with spectrum excitation from their dry residues in an AC arc at a tip of a carbon electrode. Recommendations on the optimization of the stages of sampling, storage, and preparation of saliva samples are given.     

交流放电法合成多种形态的碳纳米管

碳纳米管的发现［１］引起了科学界的广泛重视,人们对于这种新型材料在纳米导线、高强纤维、超导等方面的应用寄予厚望．目前,合成碳纳米管的方法主要是采用不等径石墨棒直流放电,在阴极上得到含有碳纳米管的沉积物［２］．对于碳纳米管的应用,有关的理论研究［３］及...     

A Comparison Between MHD Modeling and Experimental Results in a 3-Phase AC Arc Plasma Torch: Influence of the Electrode Tip Geometry

Arc behavior in 3-Phase AC plasma technology remains poorly explored. This system noticeably differs from the classical DC plasma torches and aims to overcome certain limitations, such as efficiency, equipment cost and reliability. A MHD model of a 3-Phase AC plasma torch was recently developed at Mines-ParisTech. The model does not include the electrodes in the computational domain. In parallel, experiments were conducted using a high-speed video camera shooting 100,000 frames per second. In this paper, the comparison between MHD modeling and experimental results shows that the arc behavior is in line with the results from the MHD model. Particularly, the strong influences of both the electrode jets and Lorentz forces on the arc motion are confirmed. However, some differences between experimental and numerical electrical waveforms are observed and particularly in the current–voltage phase shift. A new model was then developed by integrating the electrodes into the computational domain and adjusting the electrode tip geometry. With this simulation, we were able to reproduce the phase shift, power and voltage values with a good accuracy showing the strong influence of electrode tip geometry on the 3-Phase arc plasma discharge.     

交流电弧中共存稀土元素对光谱线强度影响的研究

本工作较系统地研究了在交流电弧中不同量的共存稀土元素镝、钬，饵，铥和镱对某些被测稀土元素光谱线强度的影响。用交流电弧激发溶液干渣样品，其样品是在固定量的被测元素溶液中各自分别加入不同量的共存元素镝、钬、铒、铥和镱，摄谱后测量各被测元素的光谱线强度对共存元素在溶液中各个不同浓度作关系曲线。     

Fe-C纳米微粒的透射电镜观察与选区电子衍射分析

利用透射电镜观察和选区电子衍射分析研究了在18kPa的Ar气氛中通过交流电弧法制备的Fe -C纳米微粒。结果表明微粒主要为两种类型 :一类是FeC合金微粒 ,另一类是具有氧化层结构的Fe微粒 ,不同粒径的微粒类呈现不同聚集特性。