bluuebunny/crossref_metadata_2025 huggingface dataset:
Refinement and evaluation of an automated mass spectrometer for nitrogen isotope analysis by the Rittenberg technique
Authors: Mulvaney R. L. , Liu Y. P.
Published: March 2007

An apparatus designed to automatically perform hypobromite oxidations of ammonium salt samples for nitrogen isotope analyses with a mass spectrometer was modified to improve performance and reduce analysis time. As modified, reference N2 is admitted to the mass spectrometer between samples from a dedicated inlet manifold, for calibration at the same pressure as that of the preceding sample. Analyses can be performed on samples containing 10 μg to 1 mg of
N (or more), at a rate of up to 350 samples/day. When operated with a double‐collector mass spectrometer, the standard deviation at the natural abundance level (10 analyses, 50‐150 μg N) was <0.0001 atom % 15N. Very little memory was observed when natural abundance samples (0.366 atom % 15N) were analysed. following samples containing 40 atom % 15N. Analyses in the
range, 0.2 to 1 atom % 15N (50‐150 μg N), were in good
agreement with manual Rittenberg analyses (1 mg N) using a dual‐inlet system, and precision was comparable. For enrichments of 2 to 20 atom % 15N, automated analyses were slightly lower than manual analyses, which was attributed to outgassing of N2 from the plastic microplate used to contain samples.
The expanding role of robotics in the clinical laboratory
Authors: Ozawa K. , Schnipeslky P. , Pardue H. L. , Place J. , Truchaud A.
Published: March 2007

This paper provides an in‐depth description of the current
applications of robotics in clinical laboratories. The trends and
impact of the use of robotics in clinical chemistry in the forseeable
future are also discussed.
Measuring the effects of laboratoryautomation: The power of empiricallyderived models
Authors: Fitzgerald Gerry , Swanson Jim
Published: March 2007

Laboratory data systems are automated for a variety of scientific
and management reasons. A key part to maintaining these systems
is to regularly assess the impact that automation has had on the
laboratory and the organization as a whole. Smith Kline Beecham
R&D is using a number of different types of measurement, as well
as a number of different tools, for measuring how automated
laboratory systems are affecting the workflow and information flow
in the laboratory. This targeted programme of metrics has increased
management confidence in laboratory automation efforts, helped
anticipate data processing bottlenecks, and highlighted end‐user
support needs.
Jumping into the 20th century before it istoo late: is laboratory robotics still in itsinfancy?
Authors: Weinstein David B. , France Dennis S.
Published: March 2007

Successful management of laboratory robotic automation programmes
in the environment of research and drug discovery within
the pharmaceutical industry may perhaps be best compared to a chef
preparing the perfect hollandaise sauce. All the ingredients must be
available at the same time and be of highest quality for the right
price. However, if components are not added in the right quantities
and in the proper order, no amount of whipping together by the
product champion will create the best product. In the past,
managerial scepticism surrounding useful implementation of cost‐effective,
high‐throughput robotic systems often placed these
‘modern toys’ at low priorities for research development laboratories.
Management now recognizes the unique contributions of
robotics in the research environment. Although the scientific director
must still play the role of product champion, new questions are
being proposed and new commitments are being made to bring the
potential of robotic automation to every laboratory where repetitive
functions can benefit from new applications. Research laboratory
directors have become both the key ingredient, as well as the rate‐limiting
determinant in the development of new applications.
Having fulfilled the promise of robotic automation to release
talented personnel, the challenge now is for the ‘end users’, the bench
scientists, to be provided with opportunities to invest the time and
effort required for future applications and new career functions.
Quality control in the year 2000
Authors: Schade Bernd
Published: March 2007

‘Just‐in‐time’ production is a prerequisite for a company to meet the
challenges of competition. Manufacturing cycles have been so successfully optimized that release time now has become a significant factor. A vision for a major quality‐control (QC) contribution to profitability in this decade seems to be the just‐in‐time release. Benefits will go beyond cost savings for lower inventory. The earlier detection of problems will reduce rejections and scrap. In addition, problem analysis and problem‐solving will be easier.

To achieve just‐in‐time release, advanced automated systems like robots will become the workhorses in QC for high volume pharmaceutical production. The requirements for these systems are extremely high in terms of quality, reliability and ruggedness. Crucial for the success might be advances in use of microelectronics for error checks, system recording, trouble shooting, etc. as well as creative new approaches (for example the use of redundant assay
systems).
Quantities and units for centrifugation inthe clinical laboratory
Authors: Lauritzen M.
Published: March 2007

The centrifuge is widely used in clinical laboratories for the
separation of components. For example in laboratories performing
biochemical analyses on body fluids it is routinely used to separate
blood cells from plasma, to separate sediment from urine, to
measure the volume fraction of erythrocytes in blood (the
haematocrit), and to separate bound from free components in protein
binding and immunoprocedures. Less routinely, centrifugation is
used for separation of lipoproteins in reference procedures for their
measurement, separation of cellular components, and separation of
DNA fragments. Various quantities are used for the description
and the calculation of the separation processes at centrifugation.
The aim of this document is to provide manufacturers and users of
centrifuges with a list of quantities and units for centrifugation
consistent with the International System of Units, SI, and
standards of the International Organization for Standardization (ISO).
Simultaneous multiwavelength study of thereaction of phenolphthalein with sodium hydroxide
Authors: Tam K. Y. , Chau F. T.
Published: March 2007

A photodiode array (PDA) spectrophotometer was used to study the
fading reaction of phenolpthalein in dilute sodium hydroxide
solution. The principal component analysis (PCA) method was
employed to identify the number of light absorbing species in the
kinetics system. The target factor analysis (TFA) procedure,
coupled with the Broyden‐Fletcher‐Goldfard‐Shanno (BFGS)
optimization method, was applied to the observed data to deduce the
rate constants and the concentration‐time profile of the reaction. The
internal referencing method was shown to be essential in improving
the quality of data obtained by a single beam PDA
spectrophotomer.
Sequential automatic on‐line determinationof aquiculture nutrients: phosphate and nitrate
Authors: Linares P. , de Castro M. D. Luque , Valcárcel M.
Published: March 2007

A continuous‐flow method for the determination of nitrate and
phosphate in water is proposed. The method is based on insertion of
reagents and sample solutions into a single channel through a
programmable switching valve. The method depends upon heteropolyacid
with phosphate and on the modified Griess reaction for
nitrate, and permits the determination of in the range 1‐20 μg/ml and between 5 and 100 μg/ml, the achievable
sampling frequency being 45/hour. The two analytes can be
determined in N/P ratios between 0.25 and 100. The method has
been applied to the determination of nitrate and phosphate in the
sea‐water used in fish farms.
An automatic system for crystal growthstudies at constant supersaturation
Authors: March J. G. , Costa-Bauzá A. , Grases F. , Söhnel O.
Published: March 2007

An automatic system for growing crystals from seeded supersaturated
solutions at constant supersaturation is described. Control of
burettes and data acquisition are controlled by computer. The
system was tested with a study of the calcium oxalate kinetics of
crystal growth.
Integrated laboratory information system ina large hospital laboratory in Singapore
Authors: Jacob Edward , Tan It-Koon , Chua Kim-Seng , Lim See-Heng
Published: March 2007

This paper describes an integrated approach to the computerization
of all major disciplines of laboratory medicine and pathology.
Installed in the Department of Pathology, Singapore General
Hospital (SGH), the computer system discussed comprises a
RISC‐based Data General Aviion 6200 computer and Meditech
MAGIC software. The system has been interfaced with the
hospital host IBM computer and supports patient information
transfer, result reporting, phlebotomy management, and compilation
of laboratory and financial management reports. The main
functions of the system include: on‐line and off‐line acquisition of
patient information and test data; preparation of single/combined/cumulative reports; transmission of reports within and between
laboratories; instantaneous provision of data in response to
telephone enquiries; calculations of quality control/workload/productivity statistics and indices; and generation of billing lists.
The computer enables reports to be provided on patient tests results
in individual wards, at various specialist out‐patient clinics, and in
the Accident and Emergency Department of the SGH through the
IBM mainframe, as well as to remote printers installed at several
other major hospitals.

The use of the MAGIC integrated laboratory information
system has resulted in a significant increase in laboratory efficiency
and productivity.
The role of atomic fluorescence spectrometry in the automatic environmental monitoring of trace element analysis
Authors: Stockwell P. B. , Corns W. T.
Published: March 2007

Considerable attention has been drawn to the environmental levels of mercury, arsenic, selenium and antimony in the last decade. Legislative and environmental pressure has forced levels to be lowered and this has created an additional burden for analytical chemists. Not only does an analysis have to reach lower detection levels, but it also has to be seen to be correct. Atomic fluorescence detection, especially when coupled to vapour generation techniques, offers both sensitivity and specificity.

Developments in the design of specified atomic fluorescence detectors for mercury, for the hydride‐forming elements and also for cadmium, are described in this paper. Each of these systems is capable of analysing samples in the part per trillion (ppt) range reliably and economically. Several analytical applications are described.
An automated GC/MS system for the analysis of volatile and semi‐volatile organic compounds in water
Authors: Vickers Allen K. , Wright Lowell M.
Published: March 2007

This paper describes a GC/MS system capable of performing Volatile Organic Analysis on liquids, solids, and air. When combined with a syringe auto‐injector, the system is completely automated for both volatile and semi‐volatile analyses. An OI Analytical Model 4551 Vial Multisampler and an OI Analytical DPM‐16 Multisampler are interfaced and then connected to an OI Analytical Model 4560 Sample Concentrator, an HP Model 5971 MSD, an HP Model 7673 Auto‐Injector, and an HP Model 5890 Series II GC to form a multi‐tasking GC/MS system. This system is shown to allow greater versatility in the laboratory.
Flow injection analysis of water. Part 1: Automatic preconcentration determination of sulphate, ammonia and iron(II)/iron(III)
Authors: Cosano J. S. , de Castro M. D. Luque , Valcárcel M.
Published: March 2007

This paper describes a simple flow‐injection (FI) manifold for the determination of a variety of species in industrial water. The chemical systems involved in the determination of ammonia (formation of Indophenol Blue), sulfate (precipitation with Ba(II)), and iron (complexation with 1,10‐phenanthroline with the help of a prior redox reaction for speciation) were selected so that a common manifold could be used for the sequential determination of batches of each analyte. A microcolumn of a suitable ion exchange material was used for on‐line preconcentration of each analyte prior to injection; linear ranges for the determination of the analytes at the ng/ml levels were obtained with good reproducibility. The manifold and methods are ready for full automation.
Flow injection analysis of water. Part 2: Integrated system for automatic multideterrnination
Authors: Cosano J. S. , de Castro M. D. Luque , Valcárcel M.
Published: March 2007

This paper describes an integrated flow injection (FI) system for the determination of ammonia, sulphate and Fe(II)/Fe(III) which can work unattended for long periods. The system was designed for the determination of individual analytes in long series of samples. Each batch of samples requires manual selection of parameters and units, such as wavelength for monitoring, preconcentration column, loops and switching of three valves to select the carrier, reagents and eluent. The system then works automatically.
Criteria for the assessment of analyser practicability
Authors: Biosca C. , Galimany R.
Published: March 2007

This article lists the theoretical criteria that need to be considered to assess the practicability of an automatic analyser. Two essential sets of criteria should be taken into account when selecting an automatic analyser: ‘reliability’ and ‘practicability’. Practibility covers the features that provide information about the suitability of an analyser for specific working conditions.

These practibility criteria are classsified in this article and include the environment; work organization; versatility and flexibility; safely controls; staff training; maintenance and operational costs.
A PC‐based titrator for flow gradient titrations
Authors: Fuhrmann B. , Spohn U.
Published: March 2007

This paper describes a PC (personal computer) based titrator which was developed for gradient flow titrations. Concentration gradients were generated electrolytically or volumetrically in small tubes. Complete titration curves can be recorded on‐line and evaluated automatically. The titrator can be used with all liquid flow detectors with low axial dispersion. The titrator was evaluated for the titration of thiosulphate with electrogenerated triiodide and for the titration of ammonia with electrogenerated hypobromite after continuous gas dialytic separation of ammonia from the sample solution.
Systematic top‐down approach to clinical chemistry
Authors: Pardue Harry L. , Truchaud Alain , Ozawa Kyoichi , Place John , Schnipelsky Paul
Published: March 2007

This paper introduces a systematic approach to organizing the discipline of clinical chemistry. The approach is called a top‐down, systems approach because it starts at the top with the most general concepts and works down through less general concepts to the most specific details and techniques. The hypothesis is that the discipline can be organized into hierarchical levels of functional processes and operational approaches to those processes. The functional processes represent what clinical scientists do; the operatinal approaches represent how they do it. Because functional processes change little, if at all, with time, they are used to develop a stable infrastructure or framework for the discipline. That infrastructure is then used to organize and understand operational approaches that tend to change rapidly with time in response to technological advances. The paper begins with the most general functional processes and then uses selected examples of the more general functions to illustrate lower hierarchical levels or functional processes and operational approaches.
Signal‐to‐noise optimization and evaluation of a home‐made visible diode‐array spectrophotometer
Authors: Raimundo, Ivo M. , Pasquini Celio
Published: March 2007

This paper describes a simple low‐cost multichannel visible spectrophotometer built with an RL512G EGG‐Reticon photodiode array. A symmetric Czerny‐Turner optical design was employed; instrument control was via a single‐board microcomputer based on the 8085 Intel microprocessor. Spectral intensity data are stored in the single‐board′s RAM and then transferred to an IBM‐AT 3865X compatible microcomputer through a RS‐232C interface. This external microcomputer processes the data to recover transmittance, absorbance or relative intensity of the spectra. The signal‐to‐noise ratio and dynamic range were improved by using variable integration times, which increase during the same scan; and by the use of either weighted or unweighted sliding average of consecutive diodes. The instrument is suitable for automatic methods requiring quasi‐simultaneous multiwavelength detections, such as multivariative calibration and flow‐injection gradient scan techniques.
Development of fully‐automated synthesissystems
Authors: Sugawara Tohru , Kato Shinji , Okamoto Shigeha
Published: March 2007

This paper describes the development of fully‐automated synthesis systems for preparing and isolating various kinds of pharmaceutical
compounds. The systems are versatile, and are able to perform
most of the chemical reactions currently used in organic chemistry,
with the exception of hydrogenation which requires high pressure.
An additional benefit is the very user‐friendly software.
Unsegmented flow approach for on‐linemonitoring of pH, conductivity, dissolvedoxygen and determination of nitrite andammonia in aquaculture
Authors: Ariza A. C. , Linares P. , de Castro M. D. Luque , Valcárcel M.
Published: March 2007

A fully automated flow system for on‐line monitoring of
analytes/parameters of interest in aquaculture is described. The
approach has been optimized for the photometric determination of
nitrite and ammonia and the continuous monitoring of pH,
conductivity and dissolved oxygen, but these analytes/parameters
are readily changeable as required. The system has been tested by
monitoring these species in the input and output sea water streams
of tanks at a fish breeding farm and also by monitoring water
containing high concentrations of fish feed.
Increasing the biosafety of analyticalsystems in the clinical laboratory
Authors: Truchaud A. , Schnipelsky P. , Pardue H. L. , Place J. , Ozawa K.
Published: March 2007

Biosafety is an important part of the know‐how of all clinical
laboratory professionals. Biosafely must have high priority in the
design and use of analytical systems. Attention should be focused
on reducing the handling of biological specimens, reducing
biohazards to laboratory personnel, and on improving the labelling
and containment of biohazardous materials. In this paper, biosafety
issues are discussed in relation to the design of analytical systems,
their use and maintenance.
Key issues for establishing a roboticslaboratory in the pharmaceutical industry
Authors: Conder Steve
Published: March 2007

The Analytical Research and Development Department of
Bristol‐Myers Squibb has a laboratory dedicated to robotic analysis
of solid dose forms. It consists of eight individuals responsible for
nine robotic systems. The laboratory is dedicated to the support of
Phase III stability studies that require dissolution, potency, content.
uniformity and Karl Fischer moisture assays. The group performs
about 15000 assays a year for approximately six long‐term stability
programs. The key issues for success were personnel selection,
methods development (methods transfer), routine assay support,
documentation, validation, training and support services. This
paper discusses the establishment of the laboratory and the future
issues important to continued success.
Use of a robotic station for full automation of thedetermination of organic matter in soil and fertilizers
Authors: Torres P. , García-Mesa J. A. , de Castro M. D. Luque
Published: March 2007

A fully automatic method for the determination of organic matter
has been implemented using a robotic station. The overall process
involves weighing, dilution, oxidation in very harsh working
conditions (K2Cr2O7 + concentrated H2SO4) dilution, centrifugation
and photometric monitoring of the Cr(III) formed.
Batches of six samples are manipulated by the robot, which also
calibrates and delivers the results of the sample determination, both
in soil and fertilizers, as percentages of organic matter which require
slightly different sample treatment. The precision and validation
of the method have been established using both types of samples
and the results obtained compare well with those of the method
used for routine analysis in official agricultural laboratories.
Automated synthesis ofradiopharmaceuticals for PET: anapparatus for [1‐11C]labelled aldoses
Authors: Nishimura Shintaro , Yajima Kazuyoshi , Harada Norihiro , Ogawa Yasuhiro , Hayashi Nobuyoshi
Published: March 2007

This paper describes an instrumentation system for positron
emission tomography (PET). A variety of [1‐11C]labelled
aldoses, such as [1‐11C]‐D‐glucose, and galactose by a modification
of the Kiliani‐Fischer method have been produced. The instrumentation
is fully automatic and consists of a synthesis system and
control system. The synthesis system has the following functions:
supplying reagents; performing reactions; purifying 11C labelled
aldose; and preparing an injectable solution of 11C labelled aldose.
These operations are performed by the control system in a remote
control room. In a preliminary, hot experiment an injectable solution
of [1‐11C]‐D‐glucose was obtained. In addition, the operator is
exposed to minimal radiation. The radioactivity of [1‐11C]‐Dglucose
was 47 MBq, and the preparation time was 49 min.
Automated synthesis of radiopharmaceuticals for positron emissiontomography: an apparatus for labelling with [11C] methyl iodide (MIASA)
Authors: Cork D. G. , Yamato H. , Yajima K. , Hayashi N. , Sugawara T. , Kato S.
Published: March 2007

A fully automated apparatus for the routine synthesis and
formulation of short‐lived 11C (t1/2 = 20 min) labelled radiopharmaceuticals
for positron emission tomography (PET) has
been developed. [11C]Carbon dioxide is converted to [11C]methyl
iodide, which can be used to label a wide variety of substrates by
methylation at C, N, O, or S electron rich centres. The apparatus,
MIASA (methyl iodide automated synthesis apparatus), was
designed to operate as part of an automated labelling system in a
shielded ‘hot’ laboratory. The apparatus was designed without the
size constraints of typical instrumentation used in hot cells, although
it is compact where necessary. Ample use of indicators and sensors,
together with compact design of the reaction flasks for small dead
space and efficient evaporation, led to good reliability and
performance. The design of the hardware and software is described
in this paper, together with a preparation of 3‐N‐[11C]methylspiperone
as a sterile injectable solution in physiological saline.
Use of artificial intelligence in analytical systems for the clinical laboratory
Authors: Place John F. , Truchaud Alain , Ozawa Kyoichi , Pardue Harry , Schnipelsky Paul
Published: March 2007

The incorporation of information‐processing technology into analytical systems in the form of standard computing software has recently been advanced by the introduction of artificial intelligence (AI), both as expert systems and as neural networks.

This paper considers the role of software in system operation, control and automation, and attempts to define intelligence. AI is characterized by its ability to deal with incomplete and imprecise information and to accumulate knowledge. Expert systems, building on standard computing techniques, depend heavily on the domain experts and knowledge engineers that have programmed them to represent the real world. Neural networks are intended to emulate the pattern‐recognition and parallel processing capabilities of the human brain and are taught rather than programmed. The future may lie in a combination of the recognition ability of the neural network and the rationalization capability of the expert system.

In the second part of the paper, examples are given of applications of AI in stand‐alone systems for knowledge engineering and medical diagnosis and in embedded systems for failure detection, image analysis, user interfacing, natural language processing, robotics and machine learning, as related to clinical laboratories.

It is concluded that AI constitutes a collective form of intellectual propery, and that there is a need for better documentation, evaluation and regulation of the systems already being used in clinical laboratories.
Automation in the pharmaceutical analysis laboratory: a centralized/decentralizedapproach
Authors: Scypinski Stephen , Nelson Linda , Sadlowski Theodore
Published: March 2007

It has been over 10 years since robots have appeared in the pharmaceutical analysis laboratory. In the early days, it was common for one selected individual to be responsible for the programming, usage and maintenance of the robots(s). However, the increasing use of robotics has prompted the formation of robotics
‘laboratories’ and/or ‘groups’. This is especially true when
multiple robotic systems and applications are involved.

Over the past several years at ISLAR, many champions of robotics have given presentations on the setup and usage of robotics within their organizations. These managers have described both the ‘centralized’ and ‘decentralized’ approaches to the implementation of robotics. In the centralized system, a single group is charged with all aspects of the robotic project, including justification, purchase, validation, use and maintenance. Under such an
arrangement, samples are usually given to the robotics group for analysis. In contrast, a totally decentralized approach to robotics would have units interspersed throughout the organization, with each individual group responsible for their respective unit(s), in
much the same way as liquid chromatographs are considered.

At Hoffmann‐La Roche, aspects of both the centralized and decentralized approaches to robotics are used which make our combined system the ‘best of both worlds’. This paper describes the Roche philosophy towards robotics and highlights the advantages to the system used.
Moving up the automation S‐curve: The role of the laboratory automation supportfunction in successful pharmaceutical R&D
Authors: Maddux Randy J.
Published: March 2007

The political and economic climate that exists today is a challenging
one for the pharmaceutical industry. To effectively compete in today′s marketplace, companies must discover and develop truly innovative medicines. The R&D organizations within these companies are under increasing pressure to hold down costs while accomplishing this mission. In this environment of level head count and operating budgets, it is imperative that laboratory management uses resources in the most effective, efficient ways possible. Investment in laboratory automation is a proven tool for doing just that.

This paper looks at the strategy and tactics behind the formation and evolution of a central automation/laboratory technology support function at the Glaxo Research Institute. Staffing of the function is explained, along with operating strategy and alignment with
the scientific client base. Using the S‐curve model of technological progress, both the realized and potential impact on successful R&D automation and laboratory technology development are assessed.
A Hadamard transform UV absorption detection for high performance liquidchromatography. Part I. Preliminary experiments
Authors: Brayan J. G. , Malcolme-Lawes D. J. , Mew C. D. , Xie S.
Published: March 2007

The principles and design of a Hadamard transform UV absorbance detector for liquid chromatography are outlined, and some spectra of aromatic compounds passing through its flow cell are presented. This approach could be valuable in providing a
low‐cost multi‐wavelength detection method for liquid chromatography.
Automated synthesis of radiopharmaceuticals for positron emissiontomography: an apparatus for [1‐11C] labeled carboxylic acid
Authors: Yajima Kazuyoshi , Yamazaki Hiroyoshi , Kawashima Hidefumi , Ino Sento , Hayashi Nobuyoshi , Miyake Yoshihiro
Published: March 2007

A fully automated apparatus for the synthesis and formulation of short‐lived 11C (t1/2 = 20 min)‐labeled carboxylic acids for
positron emission tomograpy (PET) has been developed. Injectable solutions of [1‐11C]acetic acid, [1‐11C]octanoic acid and [1‐11C]palmitic acid wilh radioactivities of 6.36‐8.29 GBq, 0.070‐1.43 GBq and 0.42‐0.89 GBq were obtained. The preparation time was under 40 min after the end of bombardment.
An automatic washing function means that labeled compound of the same or different kinds can be produced several times a day without any maintenance of the system. The control system is sited away from the ‘hot laboratory’, so operator exposure to radiation is minimized.
Integration of laboratory and process testing data
Authors: Tyszkiewicz Michael
Published: March 2007

The author describes ACS Inc.′s Pro‐LIMS system which
integrates laboratory and process procedures. The system has been
shown to be an important toolfor quality assurance in the process
manufacturing industry.
A new approach to mixing techniques for enhanced performance in automated sample preparation
Authors: Qian François , Vérette Eric , El-Sayed Atika
Published: March 2007

In the automation of sample dilution or derivatization, the
performance of the mixing technique employed when adding solvents or reagents to samples is critical. This paper presents a newly developed mixing method, based on conventional aspiration and dispensing of liquid techniques, but which considerably improves the precision of mixing. The paper discusses the results of a comparison of the technique with other methods and describes the application of the technique to several different types of sample solutions, including a highly concentrated glucose solution. The
mixing technique was performed on a Gilson XL Sampling Injector, with a 1/25 dilution of a paraben solution in 2 ml vials to give relative standard deviations of 0.2 to 0.3% (N =10).
The speciation of copper (II)/ethylenediamine/oxalate system by evolving factor analysis
Authors: Ren Shouxin , Gao Ling
Published: March 2007

Principal component analysis and evolving factor analysis were
applied to the study of the speciation of Cu (II)/ethylenediamine/ oxalate. Two programs were designed, based on mathematical algorithms. Error functions were calculated for evaluating the number of species. Submatrix analysis plots were constructed to
estimate the species present in the system. The method should prove
useful in studies of complex systems in environmental samples.
The electronic NOSE and its application to the manufacture of food products
Authors: Hodgins Diana , Sirnmonds Derek
Published: March 2007

The Electronic NOSE (Neotronics Olfactory Sensing Equipment)
is an instrument which mimics the human olfactory sensory system.
It analyses complex vapours and produces a simple output. In the food industry there are numerous examples where the aroma from the raw ingredients through to the final product are important. These aromas are currently analysed using human sensory panels
or analytical equipment such as gas chromatography/mass spectroscopy (GC/MS).

The Electronic NOSE described in this paper was not developed to replace the GC/MS or the sensory panel but to provide an instrumental measure of aroma quality which would be related to and complement the current methodology. The Electronic NOSE is a robust system which can detect complex vapours at levels similar to the human, which means typically in the parts per billion range. The system produces an output which can be easily related to sensory data and is easy to interpret by a non‐skilled operator. No part of this system reacts with the sample under test.
Upgrade of a semi‐automatic flow injection analysis system to a fully automatic one by means of a resident program
Authors: Prodromidis M. I. , Tsibiris A. B. , Karayannis M. I.
Published: March 2007

The program and the arrangement for a versatile, computer‐controlled
flow injection analysis system is described. A resident program (which can be run simultaneously and complementary to any other program) controls (on/off, speed, direction) a pump and a pneumatic valve (emptying and filling position). The system was
designed to be simple and flexible for both research and routine work.
Stabilized filter‐supported bilayer lipid membranes (BLMs) for automated flow monitoring of compounds of clinical, pharmaceutical, environmental and industrial interest
Authors: Nikolelis Dimitrios P. , Siontorou Christina G.
Published: March 2007

This paper describes the results of analytical applications of electrochemical biosensors based on bilayer lipid membranes (BLMs) for the automated rapid and sensitive flow monitoring of substrates of hydrolytic enzymes, antigens and triazine herbicides. BLMs, composed of mixtures of egg phosphatidylcholine (egg PC) and dipalmitoylphosphatidic acid (DPPA), were supported on ultrafiltration membranes (glass microfibre or polycarbonate filters) which were found to enhance their stability for flow experiments. The proteins (enzymes, antibodies) were incorporated into a floating lipid matrix at an air‐electrolyte interface, and then a casting procedure was used to deliver the lipid onto the filter supports for BLM formation. Injections of the analyte were made into flowing streams of the carrier electrolyte solution and a current transient signal was obtained with a magnitude related to the analyte concentration. Substrates of hydrolytic enzyme reactions (acetylcholine, urea and penicillin) could be determined at the micromolar level with a maximum rate of 220 samples/h, whereas antigens (thyroxin) and triazine herbicides (simazine, atrazine and propazine) could be monitored at the nanomolar level in less than 2 min. The time of appearance of the transient response obtained for herbicides was increased to the order of simazine, atrazine and propazine which has permitted analysis of these triazines in mixtures.
Evaluation of the Dimension XL clinical chemistry system
Authors: Neelkantan Neel V. , Mizzer John P. , Weinacht Jack , Thompson David R. , Sener Bulent , Stille Diane K. , Zhao Wei G. , Miller David
Published: March 2007

The analytical performance of the Dimension XL clinical chemical system was evaluated. The XL is the latest addition to the Dimension family of instruments; it is a random access analyser with a throughput up to 740 tests/hour. Regression analysis of method comparison studies with Dimension AR yielded slopes of 0.93 to 1.03 and correlation coefficients ≥0.96 for 28 assays. Excellent precision performance was also observed. New instrument features of the XL are discussed.
Optimization of control parameters of a hot cold controller by means of Simplex type methods
Authors: Porte C. , Caron-Poussin M. , Carot S. , Couriol C. , Moreno M. Martin , Delacroix A.
Published: March 2007

This paper describes a hot/cold controller for regulating crystallization operations. The system was identified with a common method (the Broida method) and the parameters were obtained by the Ziegler‐Nichols method. The paper shows that this empirical method will only allow a qualitative approach to regulation and that, in some instances, the parameters obtained are unreliable and therefore cannot be used to cancel variations between the set point and the actual values. Optimization methods were used to determine the regulation parameters and solve this identcation problem. It was found that the weighted centroid method was the best one.
An automated system for liquid‐liquid extraction in monosegmented flow analysis
Authors: Facchin Ileana , Rohwedder Jarbas J. R. , Pasquini Celio
Published: March 2007

An automated system to perform liquid‐liquid extraction in monosegmented flow analysis is described. The system is controlled by a microcomputer that can track the localization of the aqueous monosegmented sample in the manifold. Optical switches are employed to sense the gas‐liquid interface of the air bubbles that define the monosegment. The logical level changes, generated by the switches, are flagged by the computer through a home‐made interface that also contains the analogue‐to‐digital converter for signal acquisition. The sequence of operations, necessary for a single extraction or for concentration of the analyte in the organic phase, is triggered by these logical transitions. The system was evaluated for extraction of Cd(II), Cu(II) and Zn(II) and concentration of Cd(II) from aqueous solutions at pH 9.9 (NH3/NH4Cl buffer) into chloroform containing PAN (1‐(2‐pyridylazo)‐2‐naphthol) . The results show a mean repeatability of 3% (rsd) for a 2.0 mg l-1 Cd(II) solution and a linear increase of the concentration factor for a 0.5mg l-1 Cd(II) solution observed for up to nine extraction cycles.
An automatic system for determining the effects of temperature on the hysteresis curves of ion‐selective electrodes
Authors: Magalhães Júlia M. C. S. , Machado Adélio A. S. C.
Published: March 2007

This paper describes an automatic system which measures the effect of temperature variations on the response of ion‐selective electrodes (hysteresis curves). The system is managed by a computer program which plots hysteresis curves following a pre‐established temperature cycle, from setting and controlling the temperature of the water‐bath, to acquiring the response potentials of up to five electrodes after temperature stabilization.
Flow injection analysis of iron in rain water with thiocyanate and surfactant
Authors: Tripathi A. N. , ehikhalikar S. , Patel K. S.
Published: March 2007

This paper explains a new procedure for flow injection analysis (FIA) determination of iron in rain water based on the colour reaction of Fe3+ with thiocyanate ions in the presence of the cationic surfactant cetylpyridinium chloride (CPC). The value of apparent molar absorptivity of the complex in terms of iron is (2.00) x 104 l mole-1 cm-1 at an absorption maximum of 490 nm. The detection limit of the method is 8 ppb Fe. The sample throughput is 90 samples/h at a flow rate of 4.0 ml/min. The reaction mechanism, optimization of FIA variables, and effect of various types of surfactant are described. None of the tested anions and cations interfered with the determination of iron. The method was used for the quantification and flux determination of iron in rain water.
Semi‐automatic determination of elemental sulphur in rubber
Authors: Saraswathi K. , Vijayalakshmi K. , Prameela P.
Published: March 2007

Electro‐active elemental sulphur dissolved in hydrazine hydrate solvent was studied by d.c. polarography, cyclic voltammetry and millicoulometry in sodium acetate, ammonium tartrate and sodium phosphate buffers in an aqueous medium. The method, which uses a mercury electrode, is highly sensitive with less interference than other polarographic methods. The method was extended to the determination of sulphur in pressure rubber tubing. This paper also suggests a mechanism of electrode reaction.
Distinction and quantification of carry‐over and sample interaction in gas segmented continuous flow analysis
Authors: Zhang Jia-Zhong
Published: March 2007

The formulae for calculation of carry‐over and sample interaction are derived for the first time in this study. A scheme proposed by Thiers et al. (two samples of low concentration followed by a high concentration sample and low concentration sample) is verified and recommended for the determination of the carry‐over coeffcient. The derivation demonstrates that both widely used schemes of a high concentration sample followed by two low concentration samples, and a low concentration sample followed by two high concentration samples actually measure the sum of the carry‐over coeffcient and sample interaction coefficient. A scheme of three low concentration samples followed by a high concentration sample is proposed and verified for determination of the sample interaction coeffcient. Experimental results indicate that carry‐over is a strong function of cycle time and a weak function of ratio of sample time to wash time. Sample dispersion is found to be a function of sample time. Fitted equations can be used to predict the carry‐over, absorbance and dispersion given sample times, and wash times for an analytical system. Results clearly show the important role of intersample air segmentation in reducing carry‐over, sample interaction and dispersion.
Flow injection analysis of nitrogen dioxide using a galvanic detector
Authors: Liu Shan-jun , Shen Han-xi , Feng Jian-xing , Tubino M.
Published: March 2007

A flow injection configuration (FIA) based on a galvanic detector for the determination of nitrogen dioxide is described. The gaseous sample is directly injected into a gaseous carrier. The sample is transported toward the detector. The steady state measurements are not required to obtain the reproducible peak signals. The features of FIA are compared with that of continuous flow monitoring application. The flow injection system is simple, rapid and capable of detecting NO2 in the range of 1‐500 ppm (v/v). The measuring range and sensitivity of the galvanic detector in FIA depend on the sample volume. A relative standard deviation is 2.4% (n = 10) for 200 ppm (v/v) of nitrogen dioxide. The sampling frequency is about 24 h-1
Automation of a spectrophotometric method for measuring L ‐carnitine in human blood serum
Authors: Galan Amparo , Padros Anna , Arambarri Marta , Martin Silvia
Published: March 2007

A spectrometric method for the determination of L‐carnitine has been developed based on the reaction of the 5,5′ dithiobis‐(2‐nitrobenzoic) acid (DTNB) and adapted to a Technicon RA‐2000 automatic analyser Química Farmacéutica Bayer, S.A.). The detection limit of the method is 13.2μmol/l, with a measurement interval ranging from 30 to 320 μmoll1. Imprecision and accuracy are good even at levels close to the detection limit (coeffcient of variation of 5.4% for within‐run imprecision for a concentration of 35μmol/l). A good correlation was observed between the method studied and the radiometric method. The method evaluated has suffcient analytical sensitivity to diagnose carnitine deficiencies. The short time period required for sample processing (30 samples in 40min), the simple methodology and apparatus, the ease of personnel training and the low cost of the reagents make this method a good alternative to the classical radiometric method for evaluating serum L‐carnitine in clinical laboratories without radioactive installations.
LIS–lnterlink—connecting laboratory information systems to remote primary health–care centres via the Internet
Authors: Clark Barry , Wachowiak Bartosz , Crawford Ewan W. , Jakubowski Zenon , Kabata Janusz
Published: March 2007

A pilot study was performed to evaluate the feasibility of using the Internet to securely deliver patient laboratory results, and the system has subsequently gone into routine use in Poland. The system went from design to pilot and then to live implementation within a four‐month period, resulting in the LIS‐Interlink software product. Test results are retrieved at regular intervals from the BioLinkTM LIS (Laboratory Information System), encrypted and transferred to a secure area on the Web server. The primary health‐care centres dial into the Internet using a local‐cell service provided by Polish Telecom (TP), obtain a TCP/IP address using the TP DHCP server, and perform HTTP ‘get’ and ‘post’ operations to obtain the files by secure handshaking. The data are then automatically inserted into a local SQL database (with optional printing of incoming reports)for cumulative reporting and searching functions. The local database is fully multi‐user and can be accessed from different clinics within the centres by a variety of networking protocols.
Planning and establishment of a high throughput screening site
Authors: Tomlinson Julie J. , Butler Brent T. , Frezza Joan , Harris Cole O. , Smith Albert A. , Knight W. Blaine
Published: March 2007

In 1996 and 1997, Glaxo Wellcome′s US Research division planned and established their second generation research strategy. An important aspect of the strategy entailed development of two automated screening sites in Biochemistry in Research Triangle Park, NC. Development of the new operations required many decisions to be made very quickly, including automated process design, system selection and site preparation. Descriptions of the decision made in the development of one of the screening sites are presented in this paper.
Available options for doing more with less: laboraory automation as one tool in the arsenal
Authors: Scypinski Stephen , Baiano John , Sadlowski Theodore
Published: March 2007

Projects that require analytical support can evolve from a number of different situations, for example new molecular entities from drug discovery; process changes; packaging changes; site changes; line extensions; and inlicensed projects and compounds. Laboratory automation has been shown to provide a viable and practical solution to assisting in analytical development. However, it is not always the most logical answer. A truly flexible and responsive analytical unit will make a decision on a case‐by‐case basis, when faced with a new project, whether it is best to: automate some or all aspects/testing involved; contract out to a reputable and approved contract research organization (CRO); hire temporary help; use available in‐house resources; use a combination of the options shown above (for example to evaluate the complexity of the new project versus what the in‐house resources are currently working on). The paper discusses the advantages and disadvantages of the various options with respect to providing analytical support and suggests optionsfor the most effective use of resources. The role of automation as one of the important tools in the arsenal of these options is highlighted.
Laboratory automation —some perspectives on the challenges in the implementation of the technology in pharmaceutical development
Authors: North Nigel , Smith Simon
Published: March 2007

The intensifying pressure on reducing the development time for new pharmaceutical products is resulting in an increasing need for laboratory automation. A key element for the successful implementation of robotics for drug product analysis is the establishment of a reliable process for interaction of the automation team with its various customers, for example development product team and manufacturing group. The reduction of cycle time for product development appears to be resulting in more stability studies to support NDA/MAA filings for several reasons. Key clinical information may not be available before initiation of the stability studies and simultaneous world‐wide development may result in an increase in the number of product strength and pack options.
Placing and preserving priorities: projects, productivity, progress and people
Authors: Babiak John
Published: March 2007

High throughput screening (HTS) involves using automated equipment to test a large number of samples against a defined molecular target to identify a reasonable number of active molecules in a timely fashion. Major factors which can influence priorities for the limited resources of the HTS group are projects, productivity, progress and people. The challenge to the HTS group is to provide excellent and timely screening services, but still devote efforts to new technologies and personnel development. This article explains why these factors are so important.