bluuebunny/crossref_metadata_2025 huggingface dataset:
An improved automated immunoassay for C‐reactive protein on the Dimension® clinical chemistry system
Authors: Wei Tie Q. , Kramer Steve , Chu Victor P. , Hudson Dave , Kilgore Daniel , Salyer Sue , Parker Grace , Eyberger Amy , Arentzen Rene , Koiv Heikki
Published: March 2007

Recent clinical data indicate that the measurement of the concentration of C‐reactive protein (CRP) requires a higher sensitivity and wider dynamic range than most of the current methods can offer. Our goal was to develop a totally automated and highly sensitive CRP assay with an extended range on the Dimension® clinical chemistry system based on particle‐enhanced turbidimetric‐immunoassay (PETIA) technology. The improved method was optimized and compared to the Binding Site′s radial immunodiffusion assay using disease state specimens to minimize interference. Assay performance was assessed on the Dimension® system in a 12‐instrument inter‐laboratory comparison study. A split‐sample comparison (n = 622) was performed between the improved CRP method on the Dimension® system and the N Latex CRP mono method on the Behring Nephelometer, using a number of reagent and calibrator lots on multiple instruments. The method was also referenced to the standard material, CRM470, provided by the International Federation of Clinical Chemistry (IFCC). The improved CRP method was linear to 265.1mg/l with a detection limit between 0.2 and 0.5mg/l. The method detects antigen excess from the upper assay limit to 2000mg/l, thereby allowing users to retest the sample with dilution. Calibration was stable for 60 days. The within‐run reproducibility (CV) was less than 5.1% and total reproducibility ranged from 1.1 to 6.7% between 3.3 and 265.4mg/l CRP. Linear regression analysis of the results on the improved Dimension® method (DM) versus the Behring Nephelometer (BN) yielded the following equation: DM = 0.99 × BN − 0.37; r = 0.992. Minimal interference was observed from sera of patients with elevated IgM, IgG and IgA. The recovery of the IFCC standard was within 100 ± 7 % across multiple lots of reagent and calibrator. The improved CRP method provided a sensitive, accurate and rapid approach to quantify CRP in serum and plasma on the Dimension® clinical chemistry system. The ability to detect antigen excess eliminated reporting falsely low results caused by the ‘prozone effect’.
Managing laboratory automation: integration and informatics in drug discovery
Authors: Manly Charles J.
Published: March 2007

Drug discovery today requires the focused use of laboratory automation and other resources in combinatorial chemistry and high‐throughput screening (HTS). The ultimate value of both combinatorial chemistry and HTS technologies and the lasting impact they will have on the drug discovery process is a chapter that remains to be written. Central to their success and impact is how well they are integrated with each other and with the rest of the drug discovery processes‐informatics is key to this success. This presentation focuses on informatics and the integration of the disciplines of combinatorial chemistry and HTS in modern drug discovery. Examples from experiences at Neurogen from the last five years are described.
Measurement of blood acetoacetate and β‐hydroxybutyrate in an automatic analyser
Authors: Galán Amparo , Hernández Josém. , Jimenez Orlando
Published: March 2007

g‐hydroxybutyrate and acetoacetate as well as lactate and pyruvate are intermediary metabolites normally present in blood. The g‐hydroxybutyrate/acetoacetate ratio is an expression of the mitochondrial oxido‐reduction state. This ketone body ratio can provide a clue to diagnosis and metabolic status in congenital errors of the electron transport chain and pyruvate metabolism. The standardization of these analytical procedures improves the interpretation of the results helping in the difficult diagnosis of mitochondrial diseases in children. This study describes an adaptation to a Dimension R 2 L (Dade Behring, Newark, Delaware, USA) automatic analyser for a method to measure blood ketone bodies (g‐hydroxybutyrate and acetoacetate). The method allows the metabolites to be measured directly in nondeproteinized plasma (fluoride/ethylenediaminetetraacetic acid). This adaptation simplifies the analytical procedure and limits the turnaround time to 20 minutes. With a sample volume of 200 μ l metabolite concentrations ranging from 12 to 1300 μ molL−1 of g‐hydroxybutyrate and from 10 to 450 μ molL−1 of acetoacetate may be measured with a reliable analytical response.
Evaluation of use of the optional unit QA‐810V for the determination of five‐part leukocyte differentials
Authors: Tsuda Izumi , Takubo Takayuki , Kamitani Tomio , Tatsumi Noriyuki
Published: March 2007

The newly developed QA‐810V is an optional unit for the determination of five‐part white blood cell differentials. It can be used together with the same manufacturer′s haematology analyser which has been used in relatively small‐sized laboratories. The present study evaluates the basic performance of the QA‐810V and the MEK‐8118 haematology analyser using routinely obtained blood specimens treated with ethylenedioaminetetraacetic acid‐2K. In this evaluation, reproducibility was good and little carryover was found. Accurate measurements were possible for up to 24h of storage. Storage at 4°C yielded more stable measurements of complete blood counts and five‐part differentials than storage at room temperature. A good correlation between findings with the MEK‐8118 haematology analyser and those with the SE‐9000 haematology analyser was found for complete blood counts. The leukocyte differential obtained with the QA‐810V correlated well with eye counts, with r > 0.9 for percentages of neutrophils, lymphocytes and eosinophils. Scattergrams obtained with the QA‐810V reflected the presence of abnormal cells. The performance of the QA‐810V was excellent and it can improve the quality of testing in clinical laboratories.
Expediting the formulation development process with the aid of automated dissolution in analytical research and development
Authors: Sadowitz Jon P.
Published: March 2007

The development of drugs in the generic pharmaceutical industry is a highly competitive arena of companies vying for few drug products that are coming off patent. Companies that have been successful in this arena are those that have met or surpassed the critical timeline associated with trial formulation development, analytical method development, and submission batch manufacturing and testing. Barr Laboratories Inc., has been successful in the generic pharmaceutical industry for several reasons, one of which includes automation. The analytical research and development at Barr has employed the use of automated dissolution early in the lifecycle of a potential product. This approach has dramatically reduced the ‘time to market’ on average for a number of products. The key to this approach is the network infrastructure of the formulation and analytical research and development departments. At Barr, the cooperative ability to work and communicate together has driven the departments to streamline and matrix their work efforts and optimize resources and time. The discussion will reference how Barr has been successful with automation and gives a case study of products that have moved with rapid pace through the development cycle
Optimizing production of serially diluted compounds and distribution to multiple targets
Authors: Harris Cole O. , Schweiker Stephanie L.
Published: March 2007

The need for a multiple‐target compound selectivity programme led to the establishment of a single robotic system that produces a compound′s serial dilution and its distribution to multiple replicate assay plates. A Genesis RSP 150 integrated into a Zymate Laboratory Automation System XP produced the serial dilutions, and the subsequent replicate assay plates were produced quickly and accurately by an efficient use of the carousels and rapid plate. Currently, this process allows for the production of over 200 serial dilution assay plates in a workday.
Laboratory 2000 ‐ The challenge of achieving efficiency and compliance
Authors: Potter John A.
Published: March 2007

Significant advances within the field of laboratory automation and instrumentation have greatly benefited the pharmaceutical industry in its quest to discover, develop and monitor the quality of its products. Necessitated by the need for efficiency and greater productivity, faster and more cost‐effective means of analyses exist in the form of devices made up of complex electromechanical components, all logically controlled and most with the capability to interface with sophisticated information systems. This benefit does come with a price, a greater responsibility to ensure data quality while complying with increased regulatory requirements. Commitment to this responsibility presents a substantial challenge to scientists and managers throughout the industry. Due diligence must be demonstrated. A comprehensive evaluation of every laboratory system utilized, a solid plan of action for correcting any known deficiencies including upgrades or complete replacement, and an accurate monitoring procedure with the ability to measure progress are all absolute necessities to ensure success. Crossfunctional team effott and communication must transpire with full managerial support. Vendors need to be audited, made aware of any functional or quality inadequacies they possess as well as the pharmaceutical industry′s expectation for these shortcomings to be rapidly corrected. Suppliers of these systems should also be encouraged to provide complete ‘off‐the‐shelf solutions’ to eliminate the need for in‐house customization. The requirements for regulatory compliance in today′s electronic environment have been well publicized. The players involved are not only listening, but also taking the necessary steps to retain and improve efficiency without sacrificing quality. With the proper measures, planning and action, a highly automated, cost‐effective and compliant laboratory operation can become a reality.
Computational chemistry, data mining, high‐throughput synthesis and screening ‐ informatics and integration in drug discovery
Authors: Manly Charles J.
Published: March 2007

Drug discovery today includes considerable focus of laboratory automation and other resources on both combinatorial chemistry and high‐throughput screening, and computational chemistry has been a part of pharmaceutical research for many years. The real benefit of these technologies is beyond the exploitation of each individually. Only recently have significant efforts focused on effectively integrating these and other discovery disciplines to realize their larger potential. This technical note will describe one example of these integration efforts.
Integrating automation and LC/MS for drug discovery bioanalysis
Authors: Rossi David T.
Published: March 2007

A novel, integrated approach for automated sample handling in drug discovery bioanalysis is described. The process includes aspects of animal study design, biological sample collection, sample processing and high‐throughput APILC/MS operating in under multiple reaction monitoring (MRM). A semi‐automated 96‐well liquid—liquid extraction technique for biological fluid sample preparation was developed and used in conjunction with the integrated sample‐handling approach. One plate of samples could be prepared within 1.5 h compared with 4 h for a manual approach, and the resulting 96‐well plate of extracts was directly compatible with the LC/MS. Feasibility studies for the development of the process included sample collection map generation and information management, sample collection formatting, evaluation of alternative dilution schemes for high‐concentration samples, choice of biological fluid, and evaluating the capabilities of the two liquid‐handling workstations. Numerous comparisons between the new approach and conventional sample‐handling approaches gave equivalent drug‐quantitation results for several example compounds. This new sampling process has approximately doubled the efficiency (as measured by studies assayed per month) of drug discovery bioanalysis in our laboratory. The approach was also used in conjunction with time‐of‐flight mass spectrometry instrumentation (LC/TOF/MS) to quantify and characterize the disposition of simultaneously dosed example drug compounds in the rat. Likely strategies for future automated sample preparation workstations are described.
Solvent effect modelling of isocyanuric products synthesis by chemometric methods
Authors: Havet Jean-Louis , Billiau-Loreau Myriam , Porte Catherine , Delacroix Alain
Published: March 2007

Chemometric tools were used to generate the modelling of solvent e¡ects on the N‐alkylation of an isocyanuric acid salt. The method proceeded from a central composite design applied on the Carlson solvent classification using principal components analysis. The selectivity of the reaction was studied from the production of different substituted isocyanuric derivatives. Response graphs were obtained for each compound and used to devise a strategy for solvent selection. The prediction models were validated and used to search for the best selectivity for the reaction system. The solvent most often selected as the best for the reaction is the N,N‐dimethylformamide.
Low‐cost virtual instrumentation system of an energy‐dispersive X‐ray spectrometer for a scanning electron microscope
Authors: Lei Junfeng , Zeng Libo , Liu Ronggui , Liu Juntang , Zhang Zelan , Hu Jiming
Published: March 2007

The paper describes an energy‐dispersive X‐ray spectrometer for a scanning electron microscope (SEM‐EDXS). It was constructed using the new architecture of a virtual instrument (VI), which is low‐cost, space‐saving, fast and flexible way to develop the instrument. Computer‐aided teaching (CAT) was used to develop the instrument and operation rather than a traditional instrument technique. The VI was designed using the object‐oriented program language C++ and compact programmable logical devices (CPLD). These include spectra collection and processing, quantitative analysis and X‐ray‐intensity distribution analysis. The procedure is described in detail. The VI system gives an e¡ective and user‐friendly human interface for the whole analytical task. Some examples are described.
Monte Carlo simulation for the prediction of precision of absorbance measurements with a miniature CCD spectrometer
Authors: Tsaousoglou E. P. , Bolis S. D. , Efstathiou C. E.
Published: March 2007

The precision characteristics of the absorbance measurements obtained with a low‐cost miniature spectrometer incorporating an array detector were evaluated. Uncertainties in absorbance measurements were due to a combination of non‐uniform light intensity and detector response over the wavelength range examined (350‐850 nm), in conjunction with the digitization of the intensity indications and the intrinsic noise of the detecting elements. The precision characteristics are presented as contour plots displaying the expected RSD% of absorbances on the absorbance versus wavelength plane. The minimum RSD% for the spectrometer configuration tested was observed within the 0.2‐1.5 absorbance units and 500‐750 nm wavelength range. Without invoking signal enhancement features of the data‐acquisition program (scan average, higher integration times, smoothing based on averaging the signal detected by adjacent pixels), the attainable precision within this range was 0.4‐0.8%. A computer program based on Monte Carlo simulations was developed for the prediction of absorbance precision characteristics under various conditions of measurements.
High‐resolution laboratory lysimeter for automated sampling of tracers through a 0.5 m soil block
Authors: Johnson A. , Mathews T. J. , Matthews G. P. , Patel D. , Worsfold P. J. , Andrew K. N.
Published: March 2007

A computer‐controlled, automated sample collection from a 0.5‐m lysimeter, designed to give superior temporal and spatial resolution for monitoring the movement of chemical tracers through a large undisturbed soil block, is described. The soil block, 0.520.520.5 m, was monitored for saturation using eight time domain reflectometry probes. Rainfall was applied at approximately 1600 ml hm1 using a 12212 array of 23‐gauge (0.318 mm internal diameter) hypodermic needles. Soil leachates were collected at the base of the soil block using a machined aluminium collection plate with a 10210 grid of funnels that passed leachates to sample collection palettes. Sample collection was automated using a personal computer equipped with National Instruments LabVIEW™ software and linked to sensors for palette tracking. The automation of the lysimeter allowed sample collection and storage over a user‐defined period with no human interaction. As an example of the use of the automated lysimeter, results show the distribution of phosphate within the soil. The eluted phosphate showed an initial and secondary peak, and only emerged from preferential flow channels.
Development of a photometric system for continuous flow analysis
Authors: Randhawa S. S. , Bansod Baban K. S. , Singh Anirudh K. , Chand G. , Ganju A. K.
Published: March 2007

Most chemical analyses carried out in a clinical laboratory are colorimetric. An improved photometric system is described where a tungsten lamp is the light source, a photo‐diode is the detector and a microcontroller 8051 is used for processing and displaying absorbances. The performance characteristics of the instrument are reported. The parameters investigated are photometric linearity, precision and instrumental drift.
Is combinatorial chemistry on the right track for drug discovery?
Authors: Wildonger Richard A. , Deegan Tracy L. , Lee John W.
Published: March 2007

Critical to the effective implementation of high throughput methods of synthesis is the necessity for a significant supporting level of automation. There are a number of critical issues associated with the successful introduction, and supporting role, of automation of small molecule chemical synthesis. Clearly there are needs for automation to increase drug candidate synthesis throughput. Automation of repetitive and laborious tasks associated with the synthesis process can release skilled chemists to apply their talents to the more challenging investigational aspects of developing new synthetic protocols. This provides continuity in the compound supply pipeline and ensures an optimal use of the automated platform for compound production. The very high fidelity of performing repetitive processes that can be managed through automation also removes some of the limitations and errors associated with more fallible human operators. This can include very difficult tasks associated with tracking data, and general information and inventory management. Taken collectively, these attributes associated with automation can lead to greater efficiencies, throughputs and improved allocation of human resources with concomitant reductions in costs associated with current day and future drug discovery. In our library development/synthesis paradigm, we feel that automation support must be invoked early in the process and that this automation support must continue throughout the project.
LabVIEW‐based sequential‐injection analysis system for the determination of trace metals by square‐wave anodic and adsorptive stripping voltammetry on mercury‐film electrodes
Authors: Economou Anastasios , Voulgaropoulos Anastasios
Published: March 2007

The development of a dedicated automated sequential‐injection analysis apparatus for anodic stripping voltammetry (ASV) and adsorptive stripping voltammetry (AdSV) is reported. The instrument comprised a peristaltic pump, a multiposition selector valve and a home‐made potentiostat and used a mercury‐film electrode as the working electrodes in a thin‐layer electrochemical detector. Programming of the experimental sequence was performed in LabVIEW 5.1. The sequence of operations included formation of the mercury film, electrolytic or adsorptive accumulation of the analyte on the electrode surface, recording of the voltammetric current‐potential response, and cleaning of the electrode. The stripping step was carried out by applying a square‐wave (SW) potential‐time excitation signal to the working electrode. The instrument allowed unattended operation since multiple‐step sequences could be readily implemented through the purpose‐built software. The utility of the analyser was tested for the determination of copper(II), cadmium(II), lead(II) and zinc(II) by SWASV and of nickel(II), cobalt(II) and uranium(VI) by SWAdSV.
A compact automated microprocessor–based stopped–flow analyser
Authors: Koupparis Michael A. , Walczak Ken M. , Malmstadt Howard V.
Published: March 2007

Erratumdx.doi.org/10.1155/S1463924680000466
Automation in urinalysis: evaluation of three urine test strip analysers
Authors: Bonini Pierangelo , Sanguini Lucilla C. , Grossi Laura , Ceriotti Ferruccio , Murone Michelangelo
Published: March 2007

A clinical laboratory evaluation was conducted on the Clinitek Auto 2000, the Super Aution Analyzer and the Urotron RL9 for the determination of glucose, protein, pH, blood, ketone‐bodies and bilirubin.

Precision of the systems was tested using three commercial control urine materials, and reported as the percentage of times the instrument repeats a certain value. Good repeatability was obtained with all the instruments.

Accuracy of the systems was evaluated by comparison with quantitative procedures, and to check agreement between methods yielding semi‐quantitative and quantitative results, ranges of acceptability were defined, based on the criteria reported in a previous paper [2]. It was then found that 87.5 to 98.9% of results from the Urotron RL9 and the Clinitek Auto 2000 were acceptable. With the Super Aution Analyzer the level of agreement was apparently lower because of the higher number of concentration steps used by this instrument.
Acquisition and analysis of GFAAS data
Authors: Adams M. J. , Ewen G. J. , Shand C. A.
Published: March 2007

Since its inception as an analytical technique some 30 years ago atomic absorption spectrometry has become a firmly established method for the analysis of trace metals. Graphite furnace atomic absorption spectrometry provides the analyst with the capability of analysis of solutions containing µg l-1 levels of the analyte, but, because of the transient nature of the signals, a sophisticated approach to the data aquisition and handling of data is required. Most modern commercial graphite furnace atomic absorption spectrometers have built in microprocessors for this purpose but they often have limited capability for extensible user programs and limited data storage facilities. In this communication we describe the use of an Apple IIe microcomputer for the acquisition of data from a Pye Unicam SP9 graphite furnace atomic absorption spectrometer. Details of the interface which utilizes an in‐house designed AD converter, and an overview of the Pascal and assembler programs employed are given. The system allows the user to record, store and dump the graphical display of the furnace signalsfor all analyses performed. Files containing details of peak height, and area are formatted on an eight‐column spreadsheet. Details of sample type, concentrations of standards, dilutions and replication are entered from the keyboard. The calibration graph is constructed using a moving quadratic fit routine and the concentrations of the analyte in unknown solutions calculated. In addition to this, greater processing power and integration of the data into other analytical schemes can be achieved by exporting the data to other software packages and computers. Details of data transfer between the Apple IIe and an Amstrad PC 1512 are given. Some examples of the use of the system in the development of an analytical methodfor silver in plant material are given.
General principles for the classification of analysers
Authors: Haeckel R.
Published: March 2007

The IUPAC Commission on Automation and New Technologies has developed a scheme for the classification of analytical systems. The classification scheme is reported in this paper.
Control of optics in random access analysers
Authors: Truchaud A.
Published: March 2007

The technology behind random access analysers involves flexible optical systems which can measure absorbances for one reaction at different scheduled times, and for several reactions performed simultaneously at different wavelengths. Optics control involves light sources (continuous and flash mode), indexing of monochromatic filters, injection‐moulded plastic cuvettes, optical fibres, and polychromatic analysis.
Immunoturbidimetric determination of serum transferrin on a Kone Progress autoanalyser
Authors: Cynober Luc , Le Boucher Jacques , Giboudeau Jacqueline
Published: March 2007

The Kone Progress, a multiparametric discrete analyser, was used
to determine serum transferrin with a kit supplied by Kone. Assays
recommended by the French Society of Clinical Chemistry were
performed in order to assess the suitability of the test. Repeatability
was assessed using serum pools with low (L), medium (M) and
high (H) concentrations of transferrin. The coeffcients of
variation (CV) were 5.4, 3.2 and 2.0% respectively for 30
determinations (within‐batch). Reproducibility on 15 consecutive
days (between‐batch) was also satisfactory (CV for L = 7.3%, M =
6.3% and H = 3.8%). There was no serum‐to‐serum
contamination. Results correlated closely with those obtained using
radial immunodiffusion (RID) (r = 0.942) and total iron‐binding
capacity (r = 0.954)for 90 determinations.

Transferrin measurement by immunoturbidimetry on the Kone
Progress emerges as a well‐suited, rapid and inexpensive
alternative to other time‐consuming (RID) and sophisticated (laser
immunonephelemeter) techniques.
Towards properly controlled analyticalmeasurement methods
Authors: Hangos K. M. , Leisztner L.
Published: March 2007

It is of great practical importance to develop simple methods for the
automatic detection ofthe controlled state of the analytical method
being applied. The key point is to find quantities that greatly affect
the quality of the analytical results and that can be easily estimated
during the measurement process from the measured data. The
signal‐to‐noise ratio has proved to be such a quantity in gas
chromatographic methods. The statistical properties of the
estimation of the signal‐to‐noise ratio from gas chromatographic
data have been investigated. The suggested practical method for
estimating the signal‐to‐noise ratio proved to be biased from a
mathematical statistical point of view, but the bias is usually not
greater than 10%. It has been shown by practical examples that the
signal‐to‐noise ratio affects the quality of the analytical results and
it is easy to estimate its value from practical data.
A simple flow‐injection method for thedetermination of blood glucose using aTechnicon immobilized enzyme coil
Authors: Gizurarson Sveinbjörn
Published: March 2007

The applicability of a single‐channel flow‐injection system with
immobilized enzyme coil (Technicon) and UV detection to the
determination of glucose is described. The method was used for a
pure glucose solution and for serum. The detection limit was 0.10
mM, the rate of determination was 20‐40 per hour and the
precision was satisfactory. The system is very simple and practical
when many analysis are to be determined periodically.
Data acquisition system for chemical kineticstudies
Authors: Zhu Yu-zhen , Zhou Xin , Zang Xiang-sheng
Published: March 2007

A microcomputer‐interfaced data acquisition system for chemical
kinetics (interfacing with laboratory analogue instruments) has
been developed. Analogue signals from instruments used in kinetics
experiments are amplifed by a wide‐range adjustable high‐gain
operational amplifier and smoothed by an op‐based filter, and then
digitized at rates of up to 104 samples per channel by an ADC
0816 digitizer. The ADC data transfer and manipulation routine
was written in Assembler code and in high‐level language; the
graphics package and data treatment package is in Basic. For the
various sampling speeds, all of the program can be written using
Basic‐Assembler or completely in Assembler if a high sampling
rate is needed. Several numerical treatment methods for chemical
kinetics have been utilized to smooth the data from experiments.

The computer‐interfaced system for second‐order chemical kinetic
studies was applied to the determination of the rate constant of the
saponification of ethyl acetate at 35°C. For this specific problem,
an averaging treatment was used which can be called an interval
method. The use of this method avoids the diffcully of measuring
the starting time of the reaction. Two groups of experimental data
and results were used to evaluate the systems performance. All of the
results obtained are in agreement with the reference value.
Comparison of seven serum assays on fourautomatic analysers
Authors: Sacchetti Lucia , Cerasuolo Dionigio , Besozzi Marco , D′Agostino Antonio , Franzini Carlo , Salvatore Francesco
Published: March 2007

Serum enzyme assays used on four different analysers (Hitachi 737,
Hitachi 705, Cobas‐bio and RA‐2X) were compared by determining
the activity of seven different enzymes (AST, ALT, LD, ALP,
GGT, CK and AMS). Performance checks (quality control
procedure) and replications (the study of the total analytic
imprecision and of its components) were conducted and the methods
were compared by linear regression analysis with statistical
inference on the curves following the protocols of the National
Committee for Clinical Laboratory Standards (NCCLS: PSEP‐
2, PSEP‐3, PSEP‐4). The correlation coefficients between the
methods (r = 0.991‐0.999), together with the other statistical
parameters, indicated that the methods are well correlated on all the
instruments. The total imprecision was good for all analytes, except
ALT. Among the instruments tested, the RA‐2X gave more
variable results, although the total imprecision was acceptable.

There was no relevant carry‐over effect. The evaluation of performance claims indicated that the expected error did not
substantially affect the results at the level of clinical decisions.
Computer‐based automation of concentration measurementswith ion‐selective electrodes
Authors: Ibañez josé A. , Victoria L. , Barzanallana Rafael M.
Published: March 2007

An integrated computer system consisting of an expandable
ionanalyzer and a PC has been used to automate concentration
measurements with ion‐selective electrodes (ISEs). The ionanalyzer
determines ionic concentrations using a reference electrode
coupled with an ISE. The measurements and calibrations are
carried out in a thermostated sample changer equipped with a flow
cell. The data obtained by the ionanalyzer are sent via a standard
RS 232‐C interface to a microcomputer. In this paper, we describe
the automatic data acquisition system and the subsequent processing
of the measurements. One program (Transorion) automatically
collects the measurements carried out by the ionanalyzer, giving a
real‐time graphic representation of the measurement on the
computer screen. A second program (Graforion) facilitates the
management of the data stored by the first program, and listing and
graphics of these can be obtained on the printer/plotter. The method
has been used to study continuous concentration changes in an
aqueous solution of potassium iodide.
Evaluation of the Hitachi 717 analyser
Authors: Biosca Carmen , Antoja Felipe , Sierra Cristina , Douezi Helene , Macià Magda , Alsina María-Jesús , Galimany Román
Published: March 2007

The selective multitest Boehringer Mannheim Hitachi 717 analyser
was evaluated according to the guidelines of the Comisión de
Instrumentación de la Sociedad Española de Química Clinica and
the European Committee for Clinical Laboratory Standards. The
evaluation was performed in two steps: examination of the
analytical units and evaluation in routine operation.

The evaluation of the analytical units included a photometric study:
the inaccuracy is acceptable for 340 and 405 nm; the imprecision
ranges from 0.12 to 0.95% at 340 nm and from 0.30 to 0.73 at 405
nm, the linearity shows some dispersion at low absorbance for
NADH at 340 nm, the drift is negligible, the imprecision of the
pipette delivery system increases when the sample pipette operates
with 3 μl, the reagent pipette imprecision is acceptable and the
temperature control system is good.

Under routine working conditions, seven determinations were
studied: glucose, creatinine, iron, total protein, AST, ALP and
calcium. The within‐run imprecision (CV) ranged from 0.6% for
total protein and AST to 6.9% for iron. The between run
imprecision ranged from 2.4% for glucose to 9.7% for iron. Some
contamination was found in the carry‐over study. The relative
inaccuracy is good for all the constituents assayed.
Determination of inorganic phosphorus inserum: Evaluation of three methods appliedto the Technicon RA‐1000 analyzer
Authors: Rubino L. , Catapano V. , Guerra G.
Published: March 2007

We have evaluated three analytical methods for determining
inorganic phosphorus in serum applied to the Technicon RA‐I000
analyzer: a fully enzymatic colorimetric method based on the
specific system purine nucleoside phosphorylase/xanthine oxidase
coupled to an indicator colorimetric reaction similar to the Trinder
reaction; a chemical method involving the direct UV measurement
of the phosphomolybdate complex; and a chemical method with
reduction of the phosphomolybdate complex to molybdenum blue.
Experiments were performed to assess within‐run and between‐day
precision, linearity, interference and correlation. The best performance
characteristics were shown by the enzymatic colorimetric
method and the phosphomolybdate UV method.
Evaluation of an automatic gaschromatographic system for the identification of bacterial infective agents
Authors: Arcelloni C. , Griffini A. , Paroni R. , Bonini P. A.
Published: March 2007

The potential clinical application of gas chromatography to
microbial identifcation was evaluated. A completely automated
system, the MIS (Microbial Identification System; Hewlett‐
Packard) can analyse and identify pure strains by comparison of
their cellular fatty acids patterns (C9‐C20) with the reference
parameters stored in a library. Three hundred and sixty‐seven
strains were tested, comparing the gas chromatographic results
with those obtained by the traditional microbiological methods in
the bacteriology laboratory of our Institute. A standardized
extractive procedure was followed to obtain the fatty acid methyl
esters (FAMEs), but some modifications to the recommended
procedure were introduced in the bacterial growth procedures:
colonies harvested not only from the recommended growth media but
also from selective media routinely used in the bacteriology
laboratory were successfully examined. These modifications did not
influence the results but improved the ease for the user; good
agreement with the comparison method was observed as far as
identifications of genus and species are concerned for 238 cases.
The major advantages of this computerized system are a reduction
in the time required to obtain the final results, the elimination of
human errors by using the autosampler and a better inter‐laboratory
comparability of results owing to a higher degree of objectivity. On
the other hand, the limited throughput of MIS (only 40 samples in
24 h) prevents its use in a large routine laboratory; this technology
is appropriate in emergency cases, in taxonomic studies and as a
confirmatory method.
Multicentre evaluation of the Monarch (IL)clinical chemistry analyser
Authors: Ceriotti Ferruccio , Guagnellini Emma , Zoppi Francesco , Montalbetti Norberto , Okely Carlo , Bonini Pierangelo
Published: March 2007

A multicentre evaluation of the Monarch centrifugal analyser is
reported. Precision, linearity and accuracy were assessed by
comparison with routine methods. Calibration stability, photometric
and dispensing accuracy, and carry‐over related to samples
and reagents were also evaluated. The overall performance of the
instrument was good, showing an excellent photometric and
dispensing accuracy, absence of sample‐dependent carry‐over, and almost
negligible reagent carry‐over. Good precision, linearity and
correlation with routine methods were found for the parameters
tested. The instrument is reliable and is now used as the routine
clinical chemistry analyser in two of the three laboratories taking
part in the evaluation.
Computer‐controlled apparatus forautomated development of continuous flow methods
Authors: Wentzell Peter D. , Hatton Michael J. , Shiundu Paul M. , Ree Ronald M. , Wade Adrian P. , Betteridge D. , Sly Timothy J.
Published: March 2007

An automated apparatus to assist in the development of analytical
continuous flow methods is described. The system is capable of
controlling and monitoring a variety of pumps, valves, and
detectors through an IBM PC‐AT compatible computer. System
components consist of two types of peristaltic pumps (including a
multiple pump unit), syringe pumps, electrically and pneumatically
actuated valves, and an assortment of spectrophotometric and
electrochemical detectors. Details of the interface circuitry are given
where appropriate. To demonstrate the utility of the system, an
automatically generated response surface is presented for the flow
injection determination of iron(II) by its reaction with
1,10‐phenanthroline.
Calibration in process monitoring by usingunsegmented continuous‐flow systems
Authors: de Castro M. D. Luque , Valcárcel M.
Published: March 2007

An overview is presented of the different aspects of the role of
analytical chemistry in process monitoring and control. On‐line
monitoring is currently the most attractive option in this area,
especially with unsegmented‐flow techniques. In addition to
allowing automation of these systems, the variety of ways in which
calibration and recalibration can be performed allows their
adaptation to any situation by using extremely simple, home‐made
manifolds. The most relevant designs are presented and critically
discussed in this paper.
Determination of specific proteins by the FIA principle
Authors: Andersen Ib
Published: March 2007

The following analytes have been investigated: urine albumin (u‐albumin), plasma‐transferrin (p‐transferrin), p‐haptoglobin, p‐IgG, p‐IgA, p‐IgM, and p‐orosomucoid. An unmodified commercial analytical system FIA Star (Tecator) with a two‐channel injector (40 μl) was used. The prediluted plasma samples and antibodies are allowed to react for 33 s before the change in turbidity is measured as a Peak maximum at 405 nm. The optimal concentrations of calibrators and antibodies have been determined to secure antibody excess. Response time (i.e. delay between aspiration of a sample and presentation of the result in absorption units) is 75 s. Automatic print‐out of the absorbance profile and movement of the sample rack further accounted for 21 s per sample, so the throughput is reduced to 75 determinations per 2 h. Results are available within an hour, compared to two‐12 days with the present methods (electroimmunoassays). Parallel analyses with established methods/analysers show excellent agreement for u‐albumin, p‐transferrin and p‐haptoglobin. For p‐IgG, p‐IgA and p‐IgM the reaction time of 33 s is insufficient because their relative molecular masses (i.e. the size of the molecules) are so high, 150.000‐971.000. Five minutes is a more adequate reaction time, which makes a serial analyser such as FIA Star unsuitable for larger workloads of samples of immunoglobulins. The plasma concentration of Orosomucoid is low, resulting in high sample blanks. It is therefore recommended that the reaction is followed kinetically if a serial analyser is used.
State of the art in on‐line techniques coupled to flow injection analysis FIA/on‐line‐ a critical review
Authors: Puchades R. , Maquieira A. , Atienza J. , Herrero M. A.
Published: March 2007

Flow injection analysis (FIA) has emerged as an increasingly used laboratory tool in chemical analysis. Employment of the technique for on‐line sample treatment and on‐line measurement in chemical process control is a growing trend. This article reviews the recent applications of FlA. Most papers refer to on‐line sample treatment. Although FIA is very well suited to continuous on‐line process monitoring, few examples have been found in this areamost of them have been applied to water treatment or fermentation processes.
Device for data‐acquisition from transient signals: kinetic considerations
Authors: Sampedro A. Sanchez , Vives S. Sagrado , Calatayud J. Martinez
Published: March 2007

This paper reports on the evaluation and testing of a home‐made device. Data‐acquisition, treatment of transient signals and the hardware and software involved are discussed. Some practical aspects are developed in order to power the autonomy of procedures using the device. Kinetic and multi‐signal calculations are considered in order to cover the actual tendencies in continuous‐flow analysis. Somepractical advantages versus the use of classical chart recorders or commercial computerized‐instrument devices are pointed out.
Automatic system for the determination of boron in ceramic frits
Authors: Más F. , Estela J. M. , Cerdà V. , Ochandio E.
Published: March 2007

An automatic system for the potentiometric determination of boron
in ceramic frits was developed. The system includes a personal computer for instrumental control, data acquisition and processing, which allows up to 13 samples to be analysed sequentially with no human intervention.

The system performance was tested on the titration of standard solutions, which it carried out with low errors and RSD. It was subsequently applied to the determination of the B203 content in various types of ceramic frits with good results.
Computer‐assisted automated synthesis.III. Synthesis of substituted N‐(carboxyalkyl) amino‐acid tert‐butyl ester derivatives
Authors: Hayashi Nobuyoshi , Sugawara Tohru , Kato Shinji
Published: March 2007

A versatile automated synthesis apparatus, equipped with a chemical artificial intelligence, was developed to prepare and isolate a wide variety of compounds. The apparatus was to the synthesis of substituted N‐(carboxyalkyl)amino‐acids. The apparatus [1,2] is composed of units for performing various tasks,for example reagent
supply, reaction, purification and separation, each linked to a control system. All synthetic processes, including washing and drying of the apparatus after each synthetic run, were automatically performed from the mixing of the reactants to the isolation of the products as powders or crystals. The reaction of an amino‐acid tertbutyl ester acetic acid salt with a 2‐keto acid sodium salt produces an unstable intermediate, Schiff base, which is reduced with sodum cyanoborohydride to give a substituted N‐(carboxyalkyl)aminoacid tert‐butyl ester sodium salt. The equilibrium and the consecutive reactions were controlled by adding sodium cyanoborohydride using the artificial intelligence software, which contained novel kinetic equations [3] and substituent effects [4].

Substitued N‐(carboxyalkyl)amino‐acid tert‐butyl esters, 90 derivatives, were automatically synthesized using the computerassisted automated synthesis apparatus. The syntheses were performed unattended 24 hours a day, except for supplying the raw
materials, reagents and solvents. The apparatus is extremely valuable for synthesizing many derivatives of a particular compound. The configurations of the products were determined by circular dichroism measurements.
Construction and evaluation of an automated flow injection‐stopped flowanalyser for multipoint reaction rate spectrophotometric methods. Determinationof ammonia nitrogen, creatinine and phosphate
Authors: Georgiou Constantinos A. , Koupparis Michael A.
Published: March 2007

The construction and evaluation of a fully automated Flow Injection‐Stopped Flow (FI‐SF) spectrophotometric analyser is described. A microcomputer (Rockwell AIM 65) is used to control the analyser (sample injection, stop and start of the pump) through a suitable interface. Data acquisition is achieved using a 12 bit ADC card and a suitable subroutine in 6502 assembly language, allowing data sampling at a frequency of 7.5 kHz. The measurement interface and software were evaluated using a voltage ramp generator. A precision of 0.02‐1.1% RSD (N =10) was obtained for voltage ramps in the range of 1‐37 mVs-1. The FI‐SF analyser was evaluated in routine analysis by developing FI‐SF kinetic spectrophotometric methods for the determination of ammonia nitrogen (20‐250 ppm, 0.4‐2.5% RSD) based on the
Berthelot reaction, creatinine (20‐220 ppm, 0.9‐3.6% RSD) based on the Jaffé reaction, and phosphate (5‐30 ppm, 1.0‐3.3% RSD) based on the phosphomolybdenum blue reaction. The reaction rate is measured by linear fitting of multiple absorbance readings vs time. Algorithms for automated estimation of the residence time, the linear range of the reaction curve, and data treatment are presented.
IFCC recommendation: The theory of reference values. Part 4. Control of analytical variation in the production, transfer and application of reference values
Authors: Solberg Helge Erik , Stamm D.
Published: March 2007

This paper is the fourth in a series of Recommendations on the Theory of Reference Values. The others cover:

Part 1. The Concept of Reference Values [1].

Part 2. Selection of Individuals for the Production of Reference Values [2].

Part 3. Preparation of Individuals and Collection of Specimens for the Production of Reference Values [3].

Part 5. Statistical Treatment of Collected Reference Values. Determination of Reference Limits [4].

Part 6. Presentation of Observed Values Related to Reference Values [5].

A Guide to the Documents is currently in preparation.

The Expert Panel of Theory of Reference Values (EPTRV) was created in 1970 by the Committee on Standards (at present: Scientific Division) of the International Federation of Clinical Chemistry (IFCC). Its task was to develop a nomenclature and recommend procedures for the production of reference values and their treatment, and presentation of observed values in relation to reference data.

The first document in the above‐mentioned series describes the subject of reference values and defines various terms. It would be best to read it for a thorough understanding of the present document.
The applications of a commercial gas/liquidseparator coupled with an inductivelycoupled plasma mass spectrometer
Authors: Hitchen Peter , Hutton Robert , Tye Christopher
Published: March 2007

A commercially available hydride generator, with a novel
membrane gas‐liquid separator, has been coupled to a new ICPMS
instrument which itself features many unique design
considerations. Little or no optimization of the mass spectrometer or
ionization source was required to obtain excellent analytical data;
and a variety of matrices have been analysed.

The elements As and Se are usually used to demonstrate the
effectiveness of a hydride generation system, and these are of
particular importance, bearing in mind potential Ar molecular
overlaps with isotopes of interest. The flexibility of the hydride
generation ICP‐MS system is highlighted, with the inclusion of
analytical figures of merit for the elements Sn, Sb, Ge and Hg, as
well as As and Se. Data obtained by ‘standard’ pneumatic
nebulization on the ICP‐MS is compared with that obtained with
the hydride generator for all of the elements.

Improvements of between 50 and 100 times were gained in
measurements of three sigma detection limits for all elements in the
determinations, including Hg. Measurements were made on several
isotopes for particular elements, and the data is included for the
purposes of comparison. Stabilities of between 1 and 2.5% were
obtained for 0.5 ppb solutions over 10 min measurement periods, all
data is presented without using an internal standard.

Finally, analytical data from seawater standards, spiked with low
levels of As and Se and calibrated against aqueous standards,
demonstrate excellent recoveries. This is of particular interest
bearing in mind the well‐documented molecular interferences from
high chloride matrices on As and Se analysis.