Remote,real-time,on-line monitoring of high-temperature samples by noninvasive open-path laser plasma spectrometry

A remote detection system based on optical emission spectrometry of laser-induced plasmas has been developed to record spectra in the visible region from samples placed at remote distances from the excitation source. Unlike from fiber-optic-based systems, light collection is performed remotely as well. Laboratory-scale experiments have shown the possibility of performing real-time analysis of samples placed remotely. The application in the noninvasive analysis of hot samples (at 1,200 degrees C) has been demonstrated as well, allowing the dynamic monitoring of selective elemental migration.     

Old stones, new science

Museum collections include many French medieval limestone sculptures of unknown origin. To localize the source of their stone, the composition of samples from such sculptures has been determined by neutron activation analysis (INAA). Using multivariate statistics, we compared their compositional profiles with groups of samples from French monuments and from quarries known to medieval craftsmen. This process has suggested a provenance for some sculptures and allowed us to assign others to a region or a quarry that provided stone for their production.     

Determination of iron,cobalt, nickel,manganese, zinc,copper, cadmium and lead in human hair by inductively coupled plasma-atomic emission spectrometry

A method was standardized for the dissolution of hair samples and analysis was carried out by inductively coupled plasma atomic emission spectrometry (ICP-AES). Hair samples were brought into solution by using a mixture of nitric acid and hydrogen peroxide. Various parameters that influence the sample preparation, namely temperature, digestion time and ratio of acid mixture were studied and standardized. The optimized method has been employed to digest standard reference materials and hair samples of residents of India, collected from different age groups and sex, and analyzed for Fe, Co, Ni, Mn, Zn, Cu, Cd and Pb. The values agree for most of the metals with the data reported for human hair samples of residents of India. The NIES CRM Human Hair No. 5 and IAEA Reference Hair HH-1 certified reference materials were used in order to verify the accuracy of the method and the results were in excellent agreement with the certified values.     

Instrumental neutron activation determination of Pt,Ru, Ir,Sc, Cr,Fe, Co,La, Ce,Nd, Sm,Yb, Lu,Hf and Ta employing CIRUS reactor as a thermal neutron source

An accurate and simple method has been developed for the determination of Pt, Ru, Ir and other elements employing instrumental neutron activation analysis (INAA). Nondestructive analysis has been carried out for the determination of these elements in different rock samples such as Dolerite, Dyke Dolerite, Country Basalt, Hyaloclastite, Trachyte, Ijolite, Spillite, Diorite and Lamprophyre from various locations like Daman, Tapti, Murud, Talasari, Ranala and Bassein in Maharashtra state. High flux provided by the CIRUS reactor (1×10¹³ n cm^?2s^?1) has been used for thermal neutron bombardment followed by radioassaying of the (n,γ) products on a HPGe detector coupled to a PC-based MCA unit.     

Radioisotope x-ray fluorescence analysis of ancient pottery from Tel Kouzama site in Damascus, Syria

The radioisotope X-ray fluorescence method has been utilized in the analysis of thirty nine archaeological pottery fragment samples from Tel Kouzama site, Damascus city, Syria. The samples were irradiated by a 109Cd radioisotope source (-9 10(8) Bq) for 1000 s. 17 chemical elements were determined. These elemental concentrations have been processed using two multivariate statistical methods, cluster and factor analysis in order to determine similarities and correlation between the various samples. Factor analysis confirms that samples were correctly classified by cluster analysis. These two methods suggest that samples can be considered to be manufactured using four different sources of raw material.     

Simultaneous estimation of copper, zinc, cadmium and mercury in biological material by neutron activation analysis

Simultaneous determination of copper, zinc, cadmium and mercury with high sensitivity is possible by neutron activation analysis. After irradiation, the samples are digested and an initial separation of the four elements made by means of an ion-exchange resin. The elements in the separated fractions are then treated to give radio-chemical purity, precipitated, and their activities measured. A purely instrumental technique for the analysis of zinc in samples of biological material is also described. The samples are irradiated for a week and after the activity has decayed for about three months it is measured on a gamma-spectrometer.     

FAAS法连续分析测试电池锌粉中镁铁铜铅锰

提出了运用FAAS法连续分析测试电池锌粉中Mg、Fe、Cu、Pb、Mn的含量,给出了Mg、Fe、Cu、Pb、Mn最佳测定条件及线性范围,在测定中对样品中的干扰因素进行了综合考虑.方法具有很好的灵敏度和重现性,步骤简单、操作容易、干扰少.测定样品Mg、Fe、Cu、Pb、Mn含量的相对标准偏差均小于1.0%（n=10）.标准加入回收率均在97.0%-101.5%（n=6）范围内.适用于电池锌粉中Mg、Fe、Cu、Pb、Mn的含量控制分析和样品系统分析.     

Determination of Zn, B, Fe, Mg, Ca, Na and Si in anisette samples by inductively coupled plasma atomic emission spectrometry

A comparative study of several digestion methods of anisette samples has been carried out. Two dry ashing (DA) treatments as well as four wet ashing (WA) procedures using different mixtures of acids were applied for the sample mineralisation before analysis. Once the anisette samples were mineralised, the contents of Zn, B, Fe, Mg, Ca, Na and Si were determined by inductively coupled plasma-atomic emission spectrometry (ICP-AES). Each method has been studied statistically and also attending to their feasibility. After performing the optimisation of the different treatments tested, it was concluded that one wet ashing method employing a HNO₃:H₂O₂ (10:1) mixture was the most suitable. This method was applied to the analysis of anisette samples. Na, Ca, Mg and Si were present in concentrations up to 215 mg l⁻¹ for Na, 11.6 for Mg, 6.2 for Ca and 5.1 for Si. Fe and B concentrations were not higher than 0.12 mg l⁻¹ and lower for Zn.     

X-ray fluorescence analysis for the study of fragments pottery excavated at Tell Jendares site, Syria, employing multivariate statistical analysis

X-ray fluorescence analysis study of 44 archaeological pottery samples collected from Tell Jendares site north-west of Syria has been carried out. Four samples of the total previous investigated samples were obtained from the kiln found on Tell Jendares site. Seventeen different chemical elements were determined. The XRF results have been processed using two multivariate statistical cluster and factor analysis methods in order to determine the similarities and correlation between the selected samples based on their elemental composition. The methodology successfully separates the samples where three distinct chemical groups were discerned.     

The simultaneous determination of Th,Pu, Ra isotopes, 210Pb, 55Fe, 32Si and 14C in marine suspended phases

An efficient and systematic chemical procedure for the simultaneous measurement of Th, Pu, Ra isotopes, ²¹⁰Pb, ⁵⁵Fe, ³²Si and ¹⁴C in the same sample has been developed. This method has been applied successfully to the measurement of these isotopes in oceanic particulate samples collected from several tons of sea water. This procedure should find application in the analysis of geochemical samples.     

Provenance studies of pottery fragments from medieval Cairo, Egypt

In the analysis of archeological pottery fragments, instrumental neutron activation analysis has been utilized to establish the elemental concentrations of up to 37 chemical elements for each of 53 archeological pottery samples from medieval Cairo, Egypt, and one additional sample of Chinese porcelain. These elemental concentrations have been utilized in a statistical analysis procedure in order to determine similarities and correlations between the various samples. Multivariate analyses have been used to quantitatively determine these interrelationships. This methodology successfully separated the Egyptian samples into two broad categories: (1) polychrome decorated ceramic ware and (2) monochrome celadon ware. In addition the methodology successfully identified the one unique sample of Chinese porcelain. Several samples appeared to be either a mixture of categories or outliers in the data set and were not attributable to any distinct category.     

Rapid,automatic, high capacity dumas determination of nitrogen

Chemical and physical processes which take place in the Carlo Erba ANA 1400 automatic nitrogen analyzer were investigated. The instrument and its sampler were modified. Several drums with samples can be stacked upon each other for automatic analysis.About 100 analyses can be carried out in a working day, and the instrument can be loaded with further 100 or more samples for automatic analysis overnight.One analysis takes 5 min and the analyst can present a result within less than 10 min after that he has obtained the specimen for analysis. A minimum of labor is required. The instrument does clean work, requires very little laboratory space, and causes no environmental hazards.A series of 20 analyses of pure organic nitrogen-containing compounds gave a standard deviation from theory of 0.08% N. Examples of nitrogen determinations in mineral oils are reported. A cyclone mill, Retsch ZM1 was found to grind 200 g of grains, hay, peat, and other materials of agricultural interest in about 1 min to a powder, fine enough for analysis with the ANA. Examples of such analyses are reported.The method can favorably replace the Kjeldahl method in many instances of industrial, agricultural, and food analysis.     

Quantitative determination of inorganic minor cations in sodium-, calcium-, magnesium-matrix simulated samples by capillary electrophoresis

The analysis of ammonium, alkali and alkaline-earth trace cations (0.5 ppm) in samples with a calcium, sodium or magnesium matrix (500 ppm) has been achieved using 10 mM imidazole (pH 4.5) electrolyte to which a complexing agent (15-crown-5, oxalic acid or dipicolinic acid) has been specifically added in order to decrease the electrophoretic mobility of the matrix cation and thus to allow the separation of higher mobility cations at sub-ppm concentrations. The influence of several experimental parameters (complexing agent concentration, buffer pH and temperature) have been studied in order to optimize the separation. The complexing agent concentration appears to be the main parameter governing the selectivity of the cations during the analysis of matrix samples. In optimized conditions, we have checked that the separation between minor inorganic cations is not significantly altered by an increase in the matrix cation concentration. As the concentration of the matrix cation increases, the migration times of minor cations remain unchanged even for a 1000 ppm concentration of the matrix cation. Finally, these optimized buffers allow the quantitation of minor cations down to 0.05% (w/w) for calcium- or magnesium- matrix simulated samples and 0.2% (w/w) for sodium-matrix simulated samples.     

Simultaneous oxygen,carbon, nitrogen,sulfur and silicon determination in coal by proton induced gamma-ray analysis

The technique of gamma-ray analysis of light elements (GRALE) is extended to measure the concentration of carbon, nitrogen, oxygen, sulfur and silicon in coal samples. The composition of the sample is determined by analyzing the spectrum of gamma rays emitted following inelastic scattering of protons bombarding the target. A large volume lithium drifted germanium detector is used as a gamma-ray detector in this work. Coal samples are irradiated with 9.5 MeV protons in a helium atmosphere for 1000 sec. Results with standard coal samples indicate that the method has an accuracy of ∼5% of the concentration of each element and a precision of ∼4% for elements constituting at least 1% of the coal by weight.     

Determination of Al, Ba, Ca, Cu, Fe, K, Mg, Mn, Na, Sr and Zn in red wine samples by inductively coupled plasma optical emission spectroscopy: Evaluation of preliminary sample treatments

A comparative study of sample treatment for removing the organic matter (mainly alcohol) to analyse red wine samples for metal content (Al, Ba, Ca, Cu, Fe, K, Mg, Mn, Na, Sr and Zn) from ICP-OES has been carried out. Thus, three procedures have been assayed before metal analysis: Dry ashing (DA), wet ashing (WA) and the removal of alcohol by evaporation (AR). The obtained results showed that the three methods lead to unbiased recoveries close to 100%. However, the uncertainty of AR method was about twice of the remainder ones. From practical considerations, the DA procedure was considered more suitable for determining metal elements in wine samples by ICP-OES.     

Simultanbestimmung von Si, Mn, P, Cu, Al, Ni, Cr, Mo, V, Ti, Co und As in St?hlen mit ICP-AES

Summary A universal method for quantitative analysis of twelve elements in low-alloy steels is described. The samples are digested in a mixture of sulfuric-/nitric acid/ammonium peroxodisulfate. Si, Mn, P, Cu, Al, Ni, Cr, Mo, V, Ti, Co, As are determined in solution by ICP-AES. The procedure was tested with NBS and BCS reference samples. The analytical results are in good agreement with the certified values. With slight modifications, the method is applicable to the analysis of high-alloy steel samples.     

血清和血清外泌体的蛋白质组分析及其在肝内胆管癌中的应用

外泌体是由各种类型细胞在正常或非正常生理情况下分泌释放至细胞外且携带多种生物活性分子的细胞外囊泡,在细胞间通讯和免疫应答等生物过程中发挥着重要作用。肝内胆管癌是一种胆道上皮恶性肿瘤,早期无明显临床症状且生存率较低,目前常用的诊断手段包括依赖于影像设备的诊断方式和灵敏度及特异性较低的诊断标志物等,这些手段的不足对发展新的特异性标志物提出了需求。该文对血清中的外泌体进行了分离和表征,并采用液相色谱-质谱技术针对健康组与肝内胆管癌患者组的血清样本和血清外泌体样本进行了无标记定量蛋白质组学分析,分别从两种类型样本中鉴定并筛选到271和430种可信蛋白质。基于血清样本和血清外泌体样本的可信蛋白质定量表达值进行多维统计分析都能将健康组与肝内胆管癌患者组良好地区分开。对血清样本中鉴定到的蛋白质进行差异蛋白质筛选,肝内胆管癌患者组相对于健康组有15个上调和8个下调蛋白质;对血清外泌体样本中鉴定到的蛋白质进行差异蛋白质筛选,肝内胆管癌患者组相对于健康组有33个上调和18个下调蛋白质;基于两种样本筛选到的差异蛋白质中仅有4个是重复的,且基于血清外泌体样本的51个差异蛋白质中有35个蛋白质属于外泌体蛋白质数据库。针对差异蛋白质进行生物学信息分析,与差异蛋白质相关的分子功能、生物过程和信号通路主要涉及天然免疫反应、炎症反应和凝血等过程。该研究为发现肝内胆管癌的潜在生物标志物和探究肝内胆管癌的发生、发展和转移等过程提供了参考和借鉴价值。此外,通过比较研究发现血清外泌体样本能够获得较多的差异蛋白质和生物学信息,证明了外泌体作为组学分析样本的价值和应用潜力。     

Instrumental neutron activation determination of Pt, Ru, Ir, Sc, Cr, Fe, Co, La, Ce, Nd, Sm, Yb, Lu, Hf and Ta employing CIRUS reactor as a thermal neutron source

An accurate and simple method has been developed for the determination of Pt, Ru, Ir and other elements employing instrumental neutron activation analysis (INAA). Nondestructive analysis has been carried out for the determination of these elements in different rock samples such as Dolerite, Dyke Dolerite, Country Basalt, Hyaloclastite, Trachyte, Ijolite, Spillite, Diorite and Lamprophyre from various locations like Daman, Tapti, Murud, Talasari, Ranala and Bassein in Maharashtra state. High flux provided by the CIRUS reactor (1×10¹³ n cm^–2s^–1) has been used for thermal neutron bombardment followed by radioassaying of the (n,) products on a HPGe detector coupled to a PC-based MCA unit.     

The determination of cadmium,copper, iron,lead and zinc in aerosols by atomic-absorption spectrometry

The determination of five elements in filter papers loaded with air particulate matter has been investigated. After a wet destruction of about 10 cm² of filter material by a standard procedure, analysis was carried out with a flame atomic absorption method for zinc and a flameless procedure for Cd, Cu, Fe and Pb. Furnace program parameters for each of the elements in different acid solutions are reported. The interferences of some common anions and the most abundant cations in aerosol material are described. For some urban and industrial samples, the results are compared with those obtained by energy-dispersive x-ray fluorescence. Accuracy was checked against standard samples.     

用改进的因子分析-光度法同时测定含有锗钼钨锡的混合物体系

本文通过模拟纯谱及非零截距的引入,改进了因子分析-光度法。用该法探讨了以对硝基苯基荧光酮及溴代十六烷基三甲铵作为试剂的多元络合物体系同时测定锗、钼、钨、锡的最佳条件。实验证实用该法测定合成样品及钢样,结果满意。