Simultaneous flow-injection analysis of three components with on-line dialyzers in series. Determination of sodium, potassium and chloride in blood serum

A fast and reliable fully automated three-component flow-injection procedure for the simultaneous determination of sodium, potassium and chloride in blood serum is described. A single sample injection (100-mul blood serum) is directed to two different channels by using two dialyzers in series. To avoid interferences and blocking of the fine jet of the atomizer, sodium and potassium are dialyzed by the first dialyzer before measurement by AES with a flame photometer. A second dialyzer in series is used to eliminate interferences and for automated dilution before the dialyzed chloride is measured by UV/VIS spectrophotometry at 485 nm. The results obtained for the sodium, potassium and chloride in blood serum at a sampling rate of 106 samples per hour compared well with data obtained by standard methods.     

厌食症患儿血微量元素分析

为探讨患儿厌食与血微量元素之间的关系,用等离子体原子发射光谱法测定了厌食症患儿与正常对照组血微量元素锌、铁、铜、钙、镁含量。结果表明,厌食症组患儿血清锌明显低于对照组（P〈0．001）,而铁与对照组相比差异明显（P〈0．05）,而两组血铜、钙、镁比较差异均无统计学意义（P〉0．005）。提示厌食症患儿与血微量元素缺乏密切相关,要重视儿童营养,强调科学、合理的喂养方法和良好的生活习惯。     

Evaluation of atomic fluorescence, absorption and emission techniques for the determination of mercury

Summary Atomic fluorescence (AFS), absorption (AAS) and emission (AES) systems were evaluated for the determination of inorganic mercury. Identical vapour generation and amalgamation procedures were used to permit direct comparison of the performance of a commercial long-path AAS instrument to laboratory constructed non-dispersive AFS as well as He-MIP based AES instruments. Instrumental noise-limited detection limits (LOD) were 0.94, 2.4, 2.8 pg for AAS, AES and AFS techniques, respectively. Methodological LOD's were found to be blank controlled and similar for all three instruments, viz. 9, 25 and 16 pg for AAS, AFS and AES, respectively. All three systems produced accurate results at the low ng/l concentration, as verified by the analysis of a certified river water reference material (NRCC ORMS-1).     

Analysis of fragrance compounds in blood samples of mice by gas chromatography, mass spectrometry, GC/FTIR and GC/AES after inhalation of sandalwood oil.

After inhalation experiments with sandalwood oil and the pure fragrance compounds coumarin and alpha-terpineol, substances were detected and measured in the blood samples of test animals (mice) using gas chromatography/mass spectrometry (GC/MS) (MID) in connection with GC/FTIR (SWC), GC/AES (carbon and oxygen trace) and flame ionization detection/gas chromatography. Using tiglinic acid benzyl ester as the internal standard the following concentrations in serum could be found: alpha-santalol 6.1 ng/mL, beta-santalol 5.3 ng/mL and alpha-santalene 0.5 ng/mL. In separate inhalation experiments with coumarin and with alpha-terpineol the corresponding concentrations were 7.7 ng/mL and 6.9 ng/mL, respectively.     

Thermoluminescence study,including the effect of heating rate,and chemical characterization of Amarnath stone collected from Amarnath Holy Cave

This paper reports TL glow curve analysis and evaluation of kinetic parameter for Amarnath stone collected from Amarnath Holy Cave. TL was recorded with different heating rates (3.3, 4, 6.7, 8, and 10 ° s^?1). The samples gave good TL peaks at 310, 314, 308, 323, and 327 °C for the different heating rates. The corresponding activation energy (E) values were calculated. The peaks were indicative of second-order kinetics. Samples were characterized by XRD analysis. Inductively coupled plasma activated emission spectroscopic (ICP–AES) analysis was performed to determine percentages of elements in the natural mineral. Results from ICP–AES and XRF (X-ray fluorescence spectroscopy) studies were compared.     

Comparative composition analysis of SiOx and SiNx thin films by AES,EDX and RBS

The chemical composition of thin films in SiO_x and SiN_x systems (“SIPOS”) have been analyzed by comparative AES, EDX, and RBS of the same samples to assess the extent of possible errors introduced by the “weak points” of each method. These exist for EDX in the necessity of a thickness correction, for AES in a possible composition dependence of the sensitivity factors, and for RBS in the low sensitivity in detecting light elements. Linear correlations between the data obtained by RBS and EDX have been revealed over the whole range of x. Therefore, EDX can be calibrated by appropriate standards of pure SiO₂ or Si₃N₄ films. For AES analysis a calibration curve is needed. Using RBS data for calibration the content of the light components O and N might be slightly overestimated by this method.     

Microdetermination of silicon in blood, serum, urine, and milk using furnace atomic absorption spectrometry

A simple, direct microanalytical method for quantitative determination of silicon in human whole blood, serum, urine, and milk by furnace atomic absorption technique has been developed. The method employs standard additions and combines the inherent specificity and simplicity of atomic absorption analysis with the greatly increased sensitivity possible with a heated graphite tube atomizer for the determination of silicon in microliter samples. The sensitivity of the method is 1.3 ng. The method is suitable for the direct analysis of silicon with no sample preparation other than dilution with deionized water, thereby minimizing contamination due to sample preparation. The relative standard deviation for 10 μl of blood (1:1), serum (1:1), urine (1:7), and milk (1:1) was 3.45% or less.     

电感耦合等离子体原子发射光谱法测定电镀铬溶液中铜、铁、铝及镍元素的含量

研究了ICP-AES法测定电镀铬溶液中杂质元素铜、铁、铝、镍含量的方法,对仪器的工作条件、分析线选择、基体影响、共存元素干扰、酸量的影响等进行了试验论证,通过与化学分析方法比较,结果表明方法快速、简便、准确、可靠,完全满足分析要求。     

Characterization of the stoichiometry of coevaporated FeSix films by AES, EDX, RBS, and electron microscopy

The composition of FeSi_x films on Si coevaporated from separate sources of Fe and Si was analyzed comparatively by AES, EDX, RBS, and electron microscopy. Cross-checks between EDX and RBS reveal systematic errors originating from the spectra background subtraction in RBS and from the thickness correction of the EDX signals. PCA (principal component analysis) assisted AES was successfully applied to the characterization of different Si bonding states in nonstoichiometric FeSi_x films. For the growth of β-FeSi₂ films by means of molecular beam epitaxy (MBE) the adjustment of the atomic beam intensities is reported in order to illustrate the capabilities of the various techniques.     

Summary of ISO/TC 201 Standard: ISO 29081: 2010, surface chemical analysis—Auger electron spectroscopy—reporting of methods used for charge control and charge correction

This international standard specifies the minimum amount of information required for describing the methods of charge control and charge correction in measurements of Auger electron transitions from insulating specimens by electron‐stimulated AES to be reported with the analytical results. Information is provided in an Annex on methods that have been found useful for charge control prior to or during AES analysis. The Annex also includes a summary table of methods or approaches, ordered by simplicity of approach. A similar international standard has been published for XPS (ISO 19318: 2003(E), Surface chemical analysis—XPS—reporting of methods used for charge control and charge correction. Copyright © 2010 John Wiley & Sons, Ltd.     

Integrated multi-sensor chip with photocured polymer membranes containing copolymerised plasticizer for direct pH, potassium, sodium and chloride ions determination in blood serum

An analytical system based on a sensor array with ion-selective field effect transistors (ISFETs) monolithically integrated in one chip covered with photocured polymer membranes containing copolymerised plasticizer and a sequential injection analysis (SIA) is shown to offer an automation of the analysis of blood serum components. For sequential injection system a custom made dual channel flow cell for the sensor array was developed. Optimisation of ion-sensitive membrane characteristics and calibration solution compositions were carried out. The system was used to analyze sodium, potassium, chloride ion contents in blood serum samples. The precision of the ion determination in samples was typical for potentiometic method with standard deviation of about 3-5%.     

Oberflächenanalyse — Neue Wege zur Untersuchung von Eigenschaften metallischer Werkstoffe

It is shown, how modern methods in surface analysis can be used for the determination of properties, especially in the field of high-purity metals research. After a brief review of the most important techniques (AES, ESCA, SIMS, ISS) for surface and in-depth analysis, some examples from the work of the author with AES on brittle fracture, grain boundary segregation, surface segregation, diffusion, and analysis of thin films demonstrate different problems in application.     

Establishing a protocol for trace element determinations in serum samples from healthy elderly population in São Paulo city, SP, Brazil

Summary In this study a protocol for blood serum analysis was defined and the concentrations for Br, Ca, Cl, Fe, Na, Rb, Se and Zn were obtained by instrumental neutron activation analysis. Blood samples were collected from healthy elderly volunteers who were selected based on the SENIEUR protocol. Contamination of blood by the collection procedure was also evaluated and found negligible. The serum was separated by centrifugation, then freeze-dried and analyzed. Most of results obtained were within the acceptable value ranges used by physicians for normal population. The certified reference material, NIST SRM 1566b Oyster Tissue was analyzed for quality control.     

Using of Fractional Separation for the Analysis of MoO<Subscript>3</Subscript> by Atomic Emission Spectrometry with Inductively Coupled Plasma and Electrothermal Vaporization

The introduction of various forms of molybdenum into an inductively coupled plasma was studied in the vaporization of solutions from a graphite tube. A temperature program is selected that enables the separated vaporization of analytes and molybdenum (matrix) for atomic emission spectrometry with inductively coupled plasma and electrothermal vapoization (ETV–ICP–AES) analysis. The limits of detection for analytes in the ETV–ICP–AES analysis of molybdenum trioxide are evaluated using the fractional separation of analytes and the matrix.     

Higher detectability method for the analysis of nucleosides,putative tumor biomarkers,in blood serum samples by CE‐UV with reversed EOF

The development and validation of methodologies for the analysis of biological samples is of outcome importance in order to obtain trustworthy results. This work reports a novel CE‐UV method for the assessment of nucleosides, putative tumor biomarkers, in blood serum. The separation of seven nucleosides within c.a. 20 min has been achieved with: BGE 30 mmol/L borate at pH 9.90, 50 mmol/L CTAB, and 10% methanol; V = –10 kV; T = 20°C; and capillary dimensions of 56 cm × 50 μm. The sample plug was concentrated by a modified large volume sample stacking strategy that provided better detectability. Validation showed that the method is suitable for bioanalytical purposes and initial applications in serum samples from healthy subjects are also presented. Finally, statistical methods were applied to verify the effect of characteristics such as age, smoking habits, and alcohol consumption on nucleoside concentrations in blood serum. Univariate statistical analysis tests emphasized the need for age matching, which was confirmed by PCA‐DA and PLS‐DA. Cancer history in the nearby family may also interfere in nucleoside levels in blood serum, since adenosine concentrations were statistically higher for volunteers who declared having diseased relatives.     

Theoretical Auger electron spectra of polymers by density functional theory calculations using model dimers

We propose a new approach for analysis of Auger electron spectra (AES) of polymers by density functional theory (DFT) calculations with the Slater's transition-state concept. Simulated AES and X-ray photoelectron spectra (XPS) of four polymers [(CH2CH2)n (PE), (CH2CH(CH3))n (PP), (CH2CH(OCH3))n (PVME), and (CH2CH(COCH3))n (PVMK)] by DFT calculations using model dimers are in a good accordance with the experimental ones. The experimental AES of the polymers can be classified in each range of 1s-2p2p, 1s-2s2p, and 1s-2s2s transitions for C KVV and O KVV spectra, and in individual contributions of the functional groups from the theoretical analysis.     

Size-based analysis of incinerator fly ash using gravitational SPLITT fractionation, sedimentation field-flow fractionation, and inductively coupled plasma-atomic emission spectroscopy

Fly ash has been regarded as hazardous because of its high adsorption of toxic organic and/or inorganic pollutants. Fly ash is also known to have broad distributions of different chemical and physical properties, such as size and density. In this study, fly ash emitted from a solid waste incinerator was pre-fractionated into six sub-populations by use of gravitational SPLITT fractionation (GSF). The GSF fractions were then analyzed by sedimentation field-flow fractionation (SdFFF) and ICP–AES. SdFFF analysis showed the fly ash has a broad size distribution ranging from a few nanometers up to about 50 µm. SdFFF results were confirmed by electron microscopy. Inductively coupled plasma–atomic emission spectroscopy (ICP–AES) analysis of the GSF fractions showed the fly-ash particles contain a variety of inorganic elements including Ca, Si, Mg, Fe, and Pb. The most abundant in fly ash was Ca, followed by Si then Mg. No correlations were found between trace element concentration and particle size.     

A critical comparison of on-line coupling IC-ICP-(AES, MS) with competing analytical methods for ultra trace analysis of microelectronic materials

On-line coupling of ion chromatography and atomic spectrometry (IC-ICP-(AES, MS)) are compared to so-called reference methods and other competing methods for ultra trace characterization of solid microelectronic materials. The comparison is based on analytical data gained for well characterized samples by a number of different laboratories. The matrices used for comparison are Mo, Mo-oxide, MoSi_x, W, W-oxide, WSi_x, metallic As, red P and Re. The analyte elements accessible by IC-ICP-(AES, MS) and with reference values for at least one other method are Ag, Al, Ba, Ca, Cd, Cr, Co, Cu, Fe, K, Mg, Mn, Na, Ni, Ti, Tl, Th, U and Zn. The agreement of results of IC-ICP-(AES, MS) with those of isotope dilution mass spectrometry (IDMS) and radiochemical activation analyses (RNAA) shows good accuracy for most elements and some contamination problems with ubiquitous elements. A correlation of IC-ICP-(AES, MS) and GDMS results is undoubtful, but the discrepancies are rather high. As further technique ETV-ICP-MS is compared, whose results are in reasonable agreement with IC-ICP-(AES, MS). Details on some new applications as well as of some new methodological enhancements of on-line coupling IC-ICP(AES, MS) for the matrices As and P were included.     

Examples for the improvements in AES depth profiling of multilayer thin film systems by application of factor analysis data evaluation

Factor analysis has proved to be a powerful tool for the full exploitation of the chemical information included in the peak shapes and peak positions of spectra measured by AES depth profiling. Due to its ability to extract the number of independent chemical components, their spectra and their depth distributions, its information content exceeds the one of the usual peak-to-peak height evaluation of AES depth profile data. Using modern software with a graphically interactive user interface the analyst is put into a position, where he can work with Factor Analysis on a physically intuitive level despite of all the matrix algebra mathematics which it is based upon. The progress brought about by Factor Analysis to AES depth profiles of thin films is demonstrated by the analysis of two thin film systems. The first one is a Pt/Ti metallisation used as bottom electrode for ferroelectric thin films, the second one is a multilayer system where a Ti silicide formation of buried Ti/Si bilayers has been induced. Both examples show that Factor Analysis evaluation of AES depth profile data is capable to give access to stoichiometry information and to reveal interfacial layer phases, information which is hardly obtained from the conventional peak-to-peak height data evaluation.