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.     

交流电弧直读光谱法快速测定地球化学样品中的银、锡、硼、钼、铅

采用国内首创的交流电弧直读光谱仪,以交流电弧为激发光源、凹面光栅分光、光电倍增管接收、智能测控系统快速数据采集及处理,可取代传统1米或2米光栅摄谱仪的相板记录方式及洗相、译谱等繁琐的操作程序。在优化的实验条件下,对粉末状地球化学样品中的银、锡、硼、钼、铅,进行交流电弧直读光谱法测定,检出限分别为0.012,0.24,1.65,0.20,1.30μg/g,精密度和准确度均可满足行业规范的要求,其测定值与ICP-MS和ICP-AES的分析结果相符。     

固体进样-CCD光电直读发射光谱法测定地球化学样品中微量银、硼和锡

CCD技术能有效提高仪器分辨率和灵敏度,在获得样品全谱信息的同时能够完整展示待测元素蒸发行为,对于测定地球化学样品中微量银、硼、锡有着重要作用,同时固体进样技术是环境友好型技术,对环境污染较少。基于CCD全谱单色器技术用WP-1型平面光栅摄谱仪进行改造升级成为CCD-1型光电直读发射光谱仪,替代了感光相板摄谱、显影、定影、译谱等过程,节约了材料和试剂,建立了固体进样-CCD光电直读发射光谱法测定地球化学样品中微量银、硼和锡的分析方法,以焦硫酸钾、氟化钠、氧化铝、碳和二氧化锗的混合物作为光谱缓冲剂,样品与光谱缓冲剂1:1比例混匀后在下电极中压实,通过对下电极开侧孔的方式有效解决了摄谱过程中冒样的问题,同时对上电极规格选择问题进行了讨论,研究优化了激发电流和曝光时间,确定在预燃阶段选择激发电流为5A,持续3s,在激发阶段选择激发电流为14A,持续35s,利用自带SpecDirect软件可准确校正干扰谱线,自动扣除背景,并能实时观察样品基线波动。选用合成硅酸盐光谱分析标准物质绘制校准曲线,分析了6种国家一级标准物质,结果表明：该方法银、硼和锡的检出限（3s）分别为0.01、0.55、0.12 mg/kg,上述3种元素的测定值与标准值相符,相对标准偏差（n=12）依次为2.43%-8.67%, 5.79%-9.35%, 5.25%-8.70%,方法各项指标均满足《地质矿产实验室测试质量管理规范》（DZ/T0130.4-2006）的要求。     

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。     

高纯钼中痕量杂质元素的光谱分析

使用国产仪器、设备及材料,对钼中痕量杂质元素的光谱分析中各主要条件进行了试验与研究。确定直流电弧阳极激发,一次同时测定钠、镁、铝、铁、钴、镍、锰、铜、钛、钒、铬、硅、铅、铋、锡、锑、镉十七个杂质元素。测定下限为0.1～3ppm,测定下限总量为17.3ppm,单次测定标准偏差4.5～20%。实验部分1.仪器设备、材料及试剂光谱仪—WPG-100型平面光栅摄谱仪,一级光谱倒数线色散为8埃/毫米。光源—半导体硅整流设备GZH5-18型。电极—光谱纯石墨电极φ6毫米。     

纯氧化钕中14个稀土元素的光谱测定

在轻稀土元素中,钕的应用较为广泛。在光谱分析中普遍应用氩-氧控制气氛直流电弧粉末法测定稀土元素氧化物中稀土元素杂质。测定下限比一般直流电弧法改善1—2个数量级,手续相对比化学光谱法简便。本文采用碳粉为缓冲剂、大色散光谱仪,一次摄谱测定14个稀土元素。测定下限达0.00x—0.0x%,部份元素可达0.000x%;变异系数为4.5—25%。与国外同类仪器所测水平相当。仪器及工作条件GE-340型平面光栅摄谱仪,三透镜照明系统,波段中心7670埃;气氛:氩:氧=4:1,流量5升/分;光源:直流电弧阳极激发,230伏,     

《国内外分析仪器与产品介绍》(八)

(通信处: 产品名称二米平面光栅摄谱仪 表1北京光学仪器厂部分产品介绍北京通县西门北京光学仪器厂经济部何存兴.电话9526901一355,电报82凡4)型号WSP一1主要用途用于钢铁、有色金属、地质矿产、环保、卫生等样品的定性、半定量和定量发射光谱分析高频等离子体平面光栅摄谱仪WP一ZL 主要技术指标焦距f=1800 mm光栅:1200条/mm一级色散率:4,5入/mm一级复盖波长:1080凡(2 40m州宽)主机指标同上ICP激发方式:自激式激发功率:3.5 kVA 参考价格阮)包括交直流电弧发生器28600元包括ICP光源和交直流电弧49100兀巧0平面光栅摄谱仪WP一075用于微…     

用0.5米平面光栅摄谱仪测定低含量锡

为了发挥小仪器的效能,我们试验了用0.5米平面光栅摄谱仪测定低含量锡。采用正交设计选择了主要摄谱条件。测定下限为0.003%。对锡含量为0.134%和0.011%的试样进行7次测定,相对标准偏差分别为7%和8%。用本法测定管理样以及与其它方法结果对照,结果基本吻合。一、仪器及工作条件WSP-2型0.5米平面光栅摄谱仪。三透镜     

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     

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。     

高压覆膜制样-X射线荧光光谱法测定多金属矿中的多种元素

采用新的制样技术——高压(1800 kN)覆膜(3.6μm Polyester Film)制样,波长色散X射线荧光光谱测定多金属矿中19种组分。该制样技术对高硅锌矿石GBW07237(SiO282.95%),不加黏结剂,也能制出理想的样片。测定结果显示1800 kN制备样品多数组分的灵敏度、精密度和检出限较400 kN制备的样品有所改善。15个多金属矿标准物质建立校准曲线,使用Rh Kα的瑞利散射线作内标测定Cu、Pb、Zn、As和Rh Kα的康普顿散射线作内标测定Sb、Ag、Sn、Bi、Mo及经验系数法校正基体效应。Cu、Pb、Zn、Mn、As、Sb、Ag、Sn、Bi、Mo的测定结果与化学法相符,可同时分析其中的Cd、S、Fe、SiO2、Al2O3、MgO、CaO、Na2O、K2O等成分。实现了固体直接进样测定多金属矿中的多种元素。高压覆膜制样技术是制样技术的突破,国内外尚未见报道。     

Atomic emission spectrochemical analysis of human tissues

A procedure is developed for atomic emission spectrochemical analysis of human organs. The spectra in partially incinerated tissue samples are excited in an ac electric arc and registered by a photodiode array MAES. The developed procedure was used to analyze samples of liver and kidney extracted from corps for the concentration of ten microelements, Fe, Mg, Mn, Cu, Mo, Pb, Ni, Cd, Sn, and Ag. The mean arithmetical values and concentration ranges for these elements in 14 samples were calculated. The presented data are compared with the published ones for other regions over the world.     

The Study of Determining As,Sb, Bi in Geological Samples With ICP-AES

The three elements,As,Sb,Bi, the same as Ag,Au,Cu, Hg, Mo, Pb, Sn, W,Zn,are important indicated elements in looking for gold mine, which are usually determined by atomic fluorescent spectrometer (AFS). Since the conditions of their hydride generation are different and the contents among them have no proportion relation, they can't be determined simultaneously. And because the dynamic range of AFS is narrow,the samples must be diluted or weighed again if the content of a certain element is too high or low.     

Spektrographische Bestimmung von Verunreinigungen in Mo(VI)-oxid mit Tetra?thylammoniumjodidpuffer

Zusammenfassung Eine direkte spektrographische Methode zur Bestimmung von As, Te, Sb, Pb, Sn, Bi, Cd, Ag, W, Ti, Fe, Cu und Zn in Mo(VI)-oxid durch Anwendung eines neuen thermochemischen Reagenses — Tetraäthylammoniumjodid (TEAI) — wurde entwickelt. Der TEAI-Puffer gewährleistet eine vollständigere Trennung der zu bestimmenden Elemente von der Matrix und eine höhere Empfindlichkeit im Vergleich zum bisher verwendeten Graphitpulver. Durch Anwendung eines inhomogenen Magnetfeldes bzw. durch Zufuhr von KJ oder ZnO wird eine weitere nachträgliche Erhöhung der Empfindlichkeit bei der Bestimmung der meisten Verunreinigungen erzielt. Das Verfahren zeichnet sich durch gute Reproduzierbarkeit und Genauigkeit aus.

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Direct spectrographic determination of impurities in Mo(VI) oxide using a tetraethylammonium iodide buffer

A direct spectrographic method for the determination of As, Te, Sb, Pb, Sn, Bi, Cd, Ag, W, Ti, Fe, Cu and Zn in Mo(VI) oxide has been developed by using a new thermochemical agent, tetraethylammonium iodide (TEAI). The TEAI-Buffer ensures a complete separation of the elements to be determined from the matrix and a higher sensitivity by comparison with the graphite powder commonly used in practice. A higher sensitivity for most impurities has further been achieved by using an inhomogeneous magnetic field or by adding KI or ZnO, respectively. Main advantage of the method is its good reproducibility and precision.

     

Major elements as possible factors of trace element urban pedochemical anomalies

The relationship between real total contents of the major elements Na, Mg, Al, Si, P, S, K, Ca, Ti, Fe and the trace elements Ag, As, B, Ba, Co, Cr, Cu, Mn, Mo, Ni, Pb, Sb, Se, Sn, V, U, Zn in topsoil from the central part of Vilnius is analysed. The amounts of most elements were determined by energy-dispersive X-ray fluorescence, while amounts of Ag, B, Co were measured by optical atomic emission spectrophotometry. Two factors were distinguished according to major elements: anthropogenic (A) including Ca, Mg, Fe, P, S and clayey (C) including K, Al, Ti. Boron, Mn, Cr and U are significantly correlated with members of both factors, Sb with none of them and other trace elements either with all (Cu, Zn, Pb, Se, Ba, Ni, Co) or with separate (V, Ag, Sn, Mo, As) members of the A-factor. Only B, Mn, Cr, U (partly their additive index Z1) are influenced by the C-factor, while twelve other trace elements (also their additive index Z2) are influenced by the A-factor. The additive index Z of all 17 elements is also affected by the A-factor. Four groups of sites have been distinguished according to normal or higher contents of both factors. The majority of trace element anomalies are related to the sites affected by the A-factor.     

直接稀释进样-电感耦合等离子体原子发射光谱法同时测定原油中20种元素

原油样品(2.0g)用稀释剂航空煤油稀释至20.0g后,直接进样供电感耦合等离子体原子发射光谱法测定其中银、铝、硼、钡、钙、镉、铬、铜、铁、镁、锰、钼、钠、镍、铅、硅、锡、钛、钒和锌等20种元素的含量。在优化的试验条件下,20种元素的检出限(3S/N)在0.1～3mg·kg-1之间。方法用于分析原油样品,所得测定值的相对标准偏差(n=6)在1.24%～6.23%之间,回收率在80%～105%之间。     

Schnellbestimmung von Cu, Ag und Pd in PbSn-Verzinnungsb?dern durch Atomabsorptions-Spektroskopie

Zusammenfassung Eine Absorptionsmethode zur direkten Bestimmung von Cu, Ag und Pd in Pb-Sn-Legierungen wurde erarbeitet. Für die Bestimmung vorteilhafte Absorptionslinien (Cu 324,7 nm, Ag 338,3 nm und Pd 276,3 nm) wurden ermittelt und auf diesen intermetallische Interferenzen von 0–500 ppm Cu, Ag und Pd sowie von 10000ppm Pb und Sn gemessen. 1g der Legierung wird in 10 ml HNO₃ (D 1,52) und 2 ml 50 % HF gelöst. Die Lösung wird in einer Acetylen-Luft-Flamme analysiert. Die Methode erlaubt Gehalte bis zu 3·10^–4 % Cu, 5·10^–4 % Ag und 8·10^–4% Pd (zweifache Blindwerthöhe) mit ausreichender Genauigkeit zu bestimmen.

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Rapid determination of Cu, Ag and Pd in PbSn-tinning baths by atomic-absorption spectroscopy

An atomic absorption method for direct determination of Cu, Ag and Pd in Pb-Sn-alloys has been developed. For the determination favourable absorption lines (Cu 324.7 nm, Ag 338.3 nm and Pd 276.3 nm) were found out. Intermetallic interferences of 0–500 ppm of Cu, Ag and Pd as also 10000 ppm of Pb and Sn were measured on these lines. 1 g of the alloy is dissolved in 10 ml HNO₃ (d 1.52) and 2 ml of 50 % HF. The solution is analyzed in an acetylene-air flame. This method allows the analyzing of contents up to 3×10^–4 % Cu, 5·10^–4% Ag and 8×10^–4% Pd (twofold blank) with sufficient precision.

     

Direct determination of trace elements in tungsten products using an inductively coupled plasma optical emission charge coupled device detector spectrometer

An echelle inductively coupled plasma optical emission spectrometer equipped with a segmented array of charge coupled device detectors was used for the direct determination of trace impurities in tungsten products. No sample preparation was necessary. The multicomponent spectral fitting software provided by the instrument was used for the correction of spectral interference and background. The detection limits of the trace elements Al, As, Bi, Ca, Cd, Co, Cr, Cu, Fe, K, Mg, Mn, Mo, Ni, P, Pb, Sb, Sn, Ti and V in tungsten matrix were obtained under optimized operating conditions. The accuracy of the proposed method was assessed using three National Reference Materials. As a result of their ultra-trace concentrations in the reference materials, As, Pb and Sn could not be determined satisfactorily. The concentrations found for the other elements agreed quite well with those of the certified values of the reference materials.     

Direct solid atomic emission spectrometric analysis of metal samples by an argon microwave plasma torch coupled to spark ablation

Spark ablation has been combined to microwave plasma torch atomic emission spectrometry for the direct analysis of compact metallic samples. The material is ablated by a medium voltage spark (450 V, 370 Hz) in a point-to-plane configuration and swept into a 100-W, 2.45-GHz argon microwave discharge. The microwave plasma is observed end-on and the radiation analysed with a polychromator. The detection limits for Fe, Ni, Pb and Sn in brass, Cr, Cu, Ni, Mn, Mo, Si and V in steel and Cu, Fe, Mg, Mn, Si and Zn in aluminium with the microwave plasma torch in the case of measurements with a polychromator are in the μg/g range and by a factor of up to 20 higher than those obtained with spark ablation coupled to inductively coupled plasma atomic emission spectrometry using a high resolution sequential spectrometer. The stability of the emission signal depends on the element studied and relative standard deviations usually are between 0.5 and 3.5%. In the case of low-alloy steels, the linearity and the precision of the calibration could be improved by internal standardisation. Several elements (Cr, Cu, Ni, Si and V) could be determined in a steel sample (BAS SS 410/1) with high accuracy and precision.