An automated activation analysis system

An automated delayed neutron counting and instrumental neutron activation analysis system has been developed at Los Alamos National Laboratory's Omega West Reactor (OWR) to analyze samples for uranium and 31 additional elements with a maximum throughput of 400 samples per day. The system and its mode of operation for a large reconnaissance survey will be described.     

An automated solid sample analysis system

Summary An automated solid sampling analysis system (SSAS) consisting of a powder sampler, an integrated microbalance, a transport and handling system for the sample boat, a microcontrolling unit for all necessary steps and an appropriate AAS instrument is described in detail and its potential for routine metal determination in various materials is demonstrated.     

An automated electrokinetic continuous sample introduction system for microfluidic chip-based capillary electrophoresis

An automated and continuous sample introduction system for microfluidic chip-based capillary electrophoresis (CE) was developed in this work. An efficient world-to-chip interface for chip-based CE separation was produced by horizontally connecting a Z-shaped fused silica capillary sampling probe to the sample loading channel of a crossed-channel chip. The sample presentation system was composed of an array of bottom-slotted sample vials filled alternately with samples and working electrolyte, horizontally positioned on a programmable linearly moving platform. On moving the array from one vial to the next, and scanning the probe, which was fixed with a platinum electrode on its tip, through the slots of the vials, a series of samples, each followed by a flow of working electrolyte was continuously introduced electrokinetically from the off-chip vials into the sample loading channel of the chip. The performance of the system was demonstrated in the separation and determination of FITC-labeled arginine and phenylalanine with LIF detection, by continuously introducing a train of different samples. Employing 4.5 kV sampling voltage (1000 V cm(-1) field strength) for 30 s and 1.8 kV separation voltage (400 V cm(-1) field strength) for 70 s, throughputs of 36 h(-1) were achieved with <1.0% carryover and 4.6, 3.2 and 4.0% RSD for arginine, FITC and phenylalanine, respectively (n = 11). Net sample consumption was only 240 nL for each sample.     

An automated activation analysis data acquisition system

An automated neutron activation analysis data acquisition system has been assembled from commercially available equipment. The modifications of the components needed to make this into a working system are described in the text. The main components of the data acquisition system are a sample changer, a Ge(Li) detector, a magnetic tape deck and a minicomputer based multichannel analyzer. The sample changer has a 200-sample capacity and can handle both solid and liquid samples. Software for controlling the data acquisition system is flexible, yet simple to use. The system has operated reliably for a year and has sharply reduced the effort needed for data acquisition.     

Optimization of parameters of a system for continuous activation analysis of liquids

Mathematical considerations on the optimization of the flow and mechanical parameters of a system for continuous analysis of liquids are presented. The system in question contains a pump, an activation vessel placed in the vicinity of a neutron generator target, a pipeline and a vessel for the measurement of the induced activity. The following parameters of the system were taken into consideration: volumes of the activation and measurement vessels, position of the activation vessel with respect to the neutron generator target, shape of the activation vessel, and flow rate of the pumped fluid. The system is adapted for continuous and interrupted mode of operation of the neutron generator. The results of the theoretical considerations were verified in practice with the use of the above system and the reaction¹⁶O (n, p)¹⁶N. The agreement of theory and experiment was proved.     

An unsegmented extraction system for flow injection analysis

In the system described, the two phases are fed into a module containing a PTFE membrane so that no segmentation takes place, i.e., each phase is fed to only on one dise of the membrane. The groove depth on the “aqueous” side of the membrane is 0.4 mm and on the “organic” side 0.8 mm. This latter groove is filled with a porous support of polyethylene. Caffeine, sodium dodecyl sulphate and sodium dioctylsulphosuccinate samples (40—500 μl) were injected into an aqueous carrier stream which was merged and mixed with an aqueous reagent before it was fed into the module. The maximum extraction efficiency varied with the flow rate but was in the range 8–18% and was obtained by injecting sample volumes larger than 400 μl. By injecting 40 μl of sample, the efficiency dropped by a factor of 1.5–7, depending on the character of the analyte. The system is suitable for coarse liquid-liquid extraction of concentrated samples because neither segmentation nor separation of the phases is required.     

Photometry in a continuous flow system

Summary Sulphate in various environmental samples was determined by measuring the optical absorbance upon reaction with the barium(II) dimethylsulphonazo(III) complex. The measurement took place in a flow-through system. Interferences from phosphate, metal ions and others were eliminated. The results of a turbidimetric measurement, a spectrophotometric measurement with thorin, an automatic titration and the proposed method are compared. The latter allows the determination of sulphate in the range of 1.4–60 mol·l^–1. The standard deviation is 0.3–0.6 mol·l^–1, depending on the type of sample (water) analysed. A determination takes 1.5min.

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Photometric in einem DurchflußsystemBestimmung von Sulphat mit Dimethylsulfonazo(III) in Umweltmaterial mit Hilfe eines Durchflußsystems

Zusammenfassung Sulfat wurde in verschiedenen Umweltproben durch Messung der Extinktion nach Reaktion mit dem Barium(II)-dimethylsulfonazo(III)-komplex im Durchflußsystem bestimmt. Störungen von Phosphat, Metallionen, u.a. wurden beseitigt. Die Ergebnisse einer turbidimetrischen, einer photometrischen, einer automatischen Titration und der vorgeschlagenen Methode werden verglichen. Die Methode ermöglicht die Sulfatbestimmung im Bereich von 1,4–60 mol·l^–1. Die Standardabweichung beträgt 0,3–0,6 mol· l^–1 je nach Typ des Probematerials (Wasser). Eine Bestimmung erfordert 1,5min.

     

Titrimetry in a continuous flow system

Summary Sulphate in the range of 5–2000 mol · l^–1 is automatically titrated with Ba(II) in a device with an optical detection which is able to correct automatically for dilution and turbidities. The flow-through system contains 80% v/v ethanol; the indicator is dimethyl sulfonazo(III). Above a concentration level of about 20 mol · l^–1 SO ₄ ^2– the standard deviation is less than 5% rel. The titration time is negligibly small as compared to the sampling time.

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Titrimetrie im DurchflußsystemI. Apparatur und Sulfatbestimmung

Zusammenfassung Sulfat wird im Bereich von 5–2000 mol · l^–1 automatisch mit Ba(II) mit einem Gerät mit optischer Detektion titriert, das automatisch für Verdünnung und Trübung korrigieren kann. Das Durchflußsystem enthält 80% v/v Äthanol; Indicator ist Dimethylsulfonazo(III). Die Standardabweichung für Proben mit einem Sulfatgehalt höher als 20 mol · l^–1 ist niedriger als 5% rel. Die Titrationsdauer ist vernachlässigbar im Vergleich mit der Zeit für die Probennahme.

     

Camdas: An automated conformational analysis system using molecular dynamics

We present an automated conformational analysis program, CAMDAS (Conformational Analyzer with Molecular Dynamics And Sampling). CAMDAS performs molecular dynamics (MD) calculations for a target molecule and samples conformers from the trajectory of the MD. The program then evaluates the similarities between each of the sampled conformers in terms of the root- mean-square deviations of the atomic positions, clusters similar conformers, and finally prints out the clustered conformers. This MD-based conformational analysis is a broadly used method, and CAMDAS is intended to provide a convenient framework for the method. CAMDAS has the ability to find the representative conformers automatically from an arbitrarily given structure of the molecule. The accuracy of the program was examined using N- acetylalanine-N-methylamide, and the obtained result was consistent with that of the systematic search method. In the test calculation of cyclodecane, CAMDAS could identify most of the known conformers and their conformational enantiomers by examining only 5000 conformers. In addition, the potential-scaled method, which we have developed previously as an accelerating technique for MD, could find two additional conformers of cyclodecane that have not been reported. CAMDAS presents a convenient way to find the energetically possible conformers of a molecule, which is needed especially in the early stage of drug design.     

An improved HPLC system for the analysis of photosynthetic pigments

Summary A high performance liquid chromatography system for the analysis of photosynthetic pigments is presented. The method employs an octadecylsilica stationary phase, a programmed quaternary mobile phase consisting of mixtures of methanol, acetonitrile, water and hexane, and a photodiode array detector. Carotenoids and chlorophylls are rapidly analysed in a single chromatographic separation. Thecis-trans isomers of most carotenoids are separated by this method.     

An automated gamma-ray counting system for fast neutron activation analysis

An automated gamma-ray counting system was designed and built for use in counting long-lived nuclides (T>hr) produced during analysis by fast neutron activation. The system is mechanically simple, vet interfaced to sophisticated control and counting equipment for completely automated counting.     

An automatic data acquisition and handling system for activation analysis

An automatic measurement and data handling system for activation analysis is described. The system comprises five automatic -spectrometers with sample changers, a central computer with four workstations and two communication networks, one to connect the gamma-spectrometers with the central computer and another to provide communication from the workstations to the central computer. The software comprises programs for control of the -spectrometers, communication between the different units, data handling and storage, interpretation of -spectra, calculation of element concentrations and creating reports.     

A continuous liquid-liquid extraction system coupled on-line with capillary gas chromatography for environmental and ecotoxicological analysis

The applicability of a liquid-liquid extraction system which is coupled on-line with a capillary gas chromatograph was studied for environmental and ecotoxicological analyses. The optimized and automated system was used for the determination of apolar and rather non-volatile organic compounds in aqueous samples. Relevant aspects of sample introduction, phase separation and selection of extraction solvent are discussed. Three routine-tipe applications are described, viz. an improved method for the determination of hexachlorocyclohexanes in ground water and the determination of the so-called NCC-ether and ACC-ether in ecotoxicological studies. Depending on the application studied, the concentration levels varied from 0.1 to 6000 μg/I, using ECD and/or FID detection. Typical coefficients of variation obtained with the total extraction–GC procedure were 2–25%. The system was found to be rugged, it saves time compared with set-ups involving off-line liquid-liquid extraction and considerably reduces the manual work load.     

An image analysis system for thin-layer chromatography quantification and its validation

Quantitation of thin-layer chromatography (TLC) using image analysis is attractive for its low cost and convenience. The image analysis is investigated by designing a digital imaging system with simple equipment, developing an image analysis software based on our algorithm, and validated the system in the TLC quantitative assay of cichoric acid present in Echinacea purpurea (L.) Moench. TLC used a polyamide thin-layer plate with chloroform-methanol formic acid-water (3:6:1:1) as the mobile phase and 3% (m/v) aqueous aluminum chloride solution as the visualization reagent. Images are acquired with a standard digital camera under a UV viewing lamp (365 nm) in a dark room. The three-dimensional gray scale digital image dataset (x, y, gray) is reduced to two-dimensional dataset (distance, accumulative gray) and then plotted as a curve. The area under the peak corresponding to the cichoric acid spot is integrated and used for quantitation. The whole method was validated by the assay tests of detection limit, calibration curve, repeatability, reproducibility, and recovery. The results showed that our digital imaging method and image analysis algorithm were applicable for the quantification of TLC. The whole method is convenient, efficient, and moderately accurate for the quantitative assay of cichoric acid present in Echinacea purpurea (L.) Moench.     

Experimental comparison of flow-injection analysis and air-segmented continuous flow analysis

A miniature continuous flow analyzer that can be configured for either air-segmented continuous flow analysis (c.f.a.) or flow-injection analysis (f.i.a.) was used to compare the performance of the two techniques in terms of sampling rates, samples and reagent consumption factors and analtical precision. Details of simply dye dispersion experiments and spectrophotometric chloride determinations are presented. Chloride determinations at rates of up to 360 determinations per hour could be achieved with either technique; sample and reagent consumption was less for the air-segmented flow system than for flow-injection systems equipped with either coiled open tubular reactors (0.05 cm i.d.) or single-bead-string reactors. The advantages of single-bead-string reactors for determinations by merging-zones f.i.a. are demonstrated. The c.f.a. and f.i.a. techniques are shown to be complementary, and the relative merits of each for various applications are discussed.     

An adaptive strategy for selecting representative calibration samples in the continuous wavelet domain for near-infrared spectral analysis

Sample selection is often used to improve the cost-effectiveness of near-infrared (NIR) spectral analysis. When raw NIR spectra are used, however, it is not easy to select appropriate samples, because of background interference and noise. In this paper, a novel adaptive strategy based on selection of representative NIR spectra in the continuous wavelet transform (CWT) domain is described. After pretreatment with the CWT, an extension of the Kennard–Stone (EKS) algorithm was used to adaptively select the most representative NIR spectra, which were then submitted to expensive chemical measurement and multivariate calibration. With the samples selected, a PLS model was finally built for prediction. It is of great interest to find that selection of representative samples in the CWT domain, rather than raw spectra, not only effectively eliminates background interference and noise but also further reduces the number of samples required for a good calibration, resulting in a high-quality regression model that is similar to the model obtained by use of all the samples. The results indicate that the proposed method can effectively enhance the cost-effectiveness of NIR spectral analysis. The strategy proposed here can also be applied to different analytical data for multivariate calibration.     

Investigation of turbomixers in continuous flow analysis

This paper describes an investigation of turbomixers as replacements for mixing coils in FIA. The turbomixer is a device that will efficiently mix three streams simultaneously. Although the traditional FIA gradient is not produced, the data shows that the reproducibility of a turbomixer continuous flow system is comparable to a standard FIA system.