Flow Analysis with Spectrophotometric and Luminometric Detection

Flow Analysis with Spectrophotometric and Luminometric Detection

1st Edition - December 15, 2011

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  • Authors: Elias Ayres Guidetti Zagatto, Claudio Oliveira, Alan Townshend, Paul Worsfold
  • Hardcover ISBN: 9780123859242
  • eBook ISBN: 9780123859259

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With the ever increasing number of samples to be assayed in agronomical laboratories and servicing stations, fertilizer and food industries, sugar factories, water treatment plants, biomedical laboratories, drug quality control, and environmental research, the interest for automated chemical analysis has been increasing.In this context, flow analysis is very attractive, as they the flow-based procedures are characterized by enhanced analytical figures of merit. Moreover, the flow analysers do not usually require sophisticated and expensive instrumentation, are amenable to full automation and to miniaturization, and are well suited for in situ analyses.The tendency to carry out traditional methods of analysis in the flow analyser has becoming more pronounced, especially in relation to large-scale routine analyses. The technology of solution handling has become more and more improved, leading to enhanced strategies for chemical assays. Consequently, different modalities of flow analysis (e.g. SFA, FIA, SIA) have been conceived, developed and applied to solve real problems. Most of the flow-based analytical procedures presently in use, however, do not exploit the full potential of flow analysis.The main object of the book is then to provide a scientific basis and to familiarise a wide community of researchers, students, technicians, etc with the uses of flow analysis. Emphasis is given to spectrophotometric and luminometric detection, in relation to agronomical, geological, industrial, pharmaceutical and environmental applications.The book includes historical and theoretical aspects, recent achievements in instrumentation, guidelines for methodology implementation, and applications. It serves also as an applications-oriented text book.

Key Features

  • Detailed historical and theoretical background
  • Various modes of operation
  • Spectrophotometric and luminometric detection
  • Strategies for solution handling
  • Large number of applications


Researchers, students, consultants and practitioners in flow analysis, spectrophotometry, luminescence, flow injection analysis, sequential injection analysis and segmented flow analysis.

Table of Contents

  • 1. Introduction

    1.1. General

    1.2. The advent of Flow Analysis

    1.3. The development of Flow Analysis

    1.4. Main features of Flow Analysis

    1.4.1. Sample insertion

    1.4.2. Sample dispersion

    1.4.3. Reproducible timing

    1.4.4. Other attractive features

    Transient analytical signal

    Low susceptibility to biased results

    Improved system design

      1. Aims and scope of the monograph

    Appendix 1.1. Important monographs related to Flow Analysis

    Appendix 1.2. Journal Special Issues dedicated to Conferences on Flow Analysis

    2. Historical view

    2.1. Early developments

    2.2. Segmented flow analysis

    2.3. Flow injection analysis

    2.4. Sequential injection analysis

    2.4.1. Bead injection analysis

    2.4.2. Lab-on-valve

    2.5. Multi-commuted flow analysis

    2.5.1. Multi-syringe flow injection analysis

    2.5.2. Multi-pumping flow analysis

    2.6. Other flow systems

    2.7. Commutation in flow analysis

    2.8. Flow pattern

    2.9. Instrument characteristics

    2.10. Trends

    3. Fundamentals

    3.1. The flowing sample

    3.1.1. Flow pattern Flow regime Composition of the flowing stream

    Tandem stream

    Mono-segmented stream Temporal variations in flow rates

    Constant flow

    Pulsating flow

    Sinusoidal flow

    Reversed flow

    Linearly-variable flow

    Intermittent flow

    Pulsed flow Alterations to the flow pattern

    3.1.2. Sample dispersion Dispersion inside a tubular reactor Dispersion inside a mixing chamber

    Improved mixing conditions

    High sample dispersion

    Exponential dilution

    Establishment of fluidized beads

    Manifold components behaving as mixing chambers Dispersion by confluent streams Practical indices for expressing sample dispersion

    The volumetric fraction.

    Experimental determination

    Practical situations

    Worked examples

    3.1.3. Visualisation of the dispersing sample zone

    3.2. System configurations

    3.2.1. Single-line flow systems

    3.2.2. Confluence flow systems

    3.3. The detector response

    3.3.1. Flat peaks

    3.3.2. Bell shaped peaks Peak height Peak area Peak width

    3.3.3. Gathering the calibration model

    4. Interaction of radiation with the flowing sample

    4.1. Fundamentals

    4.1.1. UV-Visible spectrophotometry Losses of radiation

    Radiation losses at interfaces

    Radiation losses at the cuvette walls

    Radiation losses inside the sample

    Compensation of radiation losses The Lambert-Beer law Practical aspects of the Lambert-Beer law

    Concentration of the radiation absorbing species

    Monochromaticity of the radiation

    Sample homogeneity

    Chemical deviations


    Stray radiation Special strategies

    Dual-wavelength spectrophotometry

    Solid phase spectrophotometry

    4.1.2. Turbidimetry Losses of radiation Relationship between turbidance and analyte concentration Practical aspects

    Characteristics of the particles

    Monochromaticity of radiation

    Sample uniformity

    Chemical deviations (including co-precipitation)

    Rate of turbidity formation

    Stray radiation Special strategies Final remarks

    4.1.3. Nephelometry

    4.1.4. Fluorimetry and phosphorimetry

    4.1.5. Chemiluminescence and bioluminescence

    4.2. The Schlieren effect

    4.2.1. Physical principles

    4.2.2. Occurrence

    4.2.3. The Schlieren effect in flow analysis Historical testimonies The two components of the Schlieren effect

    Poor mixing conditions

    Good mixing conditions Applications Emergence

    Differences between sample and carrier solutions

    Pulsed sample inlet into the flow cell

    Pulsed addition of merging streams

    Exploitation of intermittent streams

    Addition / removal of manifold components Minimizing the Schlieren effect

    Improvement of system design

    Subtraction of monitored signals

    4.3. Presence of immiscible phases

    5. Flow Analysers

    5.1. The segmented flow analyser

    5.1.1. Characteristics

    5.1.2. Sample dispersion

    5.1.3. Controlling sample dispersion

    5.2. The flow injection analyser

    5.2.1. Characteristics

    5.2.2. Sample dispersion

    5.2.3. Controlling sample dispersion Dispersion parameters


    Sample viscosity

    Diffusion coefficient

    Composition of the sample and reagent solution

    Others Dispersion parameters – system geometry

    Sample volume

    Injection mode

    Dimensions of the analytical path

    Tubing inner diameter

    Flow rate

    Confluent stream additions

    Site of confluence stream addition

    Artefacts in the analytical path

    5.3. The sequential injection analyser

    5.3.1. Characteristics

    5.3.2. Sample dispersion

    5.3.3. Controlling sample dispersion Large sample volume Limited sample dispersion

    5.4. The multi-commuted flow analyser

    5.4.1. Characteristics

    5.4.2. sample dispersion

    5.4.3. Discretely actuated devices Automated devices Devices with feedback mechanisms

    5.5. Other flow analysers

    5.5.1. The mono-segmented flow analyser

    5.5.2. The discontinuous flow analyser

    5.3.3. The Lab-on-Valve and Lab-on-Chip flow analysers

    5.6. Describing the flow analyser

    5.6.1. Establishment of the flowing stream

    5.6.2. Sample introduction

    5.6.3. Manifold characteristics

    5.6.4. Sample processing

    5.6.5. Detection

    5.6.6. Performance of the flow system General figures of merit





    Detection limit

    Dynamic range Figure of merit specific to flow based procedures


    Sampling rate



    6. Instrumentation

    6.1. Fluid propulsion

    6.1.1. Peristaltic pumps

    6.1.2. Syringe (piston) pumps Use of large volume pistons (syringes) Use of small volume pistons

    6.1.3. Diaphragm pumps Solenoid pumps Piezoelectric pumps

    6.1.4. Gas pressurized reservoirs

    6.1.5. Osmotic pumps

    6.1.6. Gravity

    6.2. sample handling

    6.2.1. Tubes

    6.2.2. Sample introduction Sampler Time-based introduction Loop-based introduction Hydrodynamic injection Nested injection

    6.2.3. Reactors Coiled reactors / mixing coils Packed bed reactors Single bead string reactor Knitted (or knotted) reactors Reactor-like artefacts

    6.2.4. Accessories Connectors

    Connectors for linking tubes together

    Connectors for linking manifold tubes with other components Solution containers

    6.3. Detection and data processing

    6.3.1. Flow-cells Classical and Z-shaped flow-cells Spiral flow-cells Long optical path length flow-cells

    6.3.2. Detectors

    6.3.3. System control, data acquisition and data treatment

    6.4. Miniaturisation of the flow system

    7. Special strategies for flow manipulation

    7.1. Merging zones

    7.1.1. Implementation Merging zones relying on different convergent carrier streams Merging zones relying on a single carrier stream Merging zones relying on an intermittent stream

    7.1.2. Applications Reduction of reagent consumption Matching the analytical signal with the dynamic concentration range Single point determinations incorporating blank determinations Speciation Reducing undesirable adsorption processes Sequential determinations Standard addition method

    7.2. Zone sampling

    7.2.1. Implementation

    7.2.2. Applications High sample dispersion Simultaneous determinations Variable dispersion Detailed study of dispersion

    7.3. Stream splitting

    7.3.1. Segmented flow analysis

    7.3.2.Unsegmented flow analysis Stream splitting / stream merging

    Expansion of the dynamic concentration range

    Differential kinetic analysis

    Simultaneous determinations Stream splitting without stream merging

    7.3.3. Sample removal from the analytical path

    7.4. Zone splitting

    7.4.1. Implementation

    7.4.2. Applications

    7.5. Sample incubation: zone trapping (general) and sample stopping

    7.6.Prior assay

    7.7. Multi-detection (with a single detector)

    8. Sample handling

Product details

  • No. of pages: 472
  • Language: English
  • Copyright: © Elsevier 2012
  • Published: December 15, 2011
  • Imprint: Elsevier
  • Hardcover ISBN: 9780123859242
  • eBook ISBN: 9780123859259

About the Authors

Elias Ayres Guidetti Zagatto

Affiliations and Expertise

CENA, University of São Paulo, Brazil Universidade de Sao Paulo, Centro de Energia Nuclear na Agricultura, Brazil

Claudio Oliveira

Affiliations and Expertise

University of Maringa, Brazil

Alan Townshend

Alan Townshend holds B.Sc., Ph.D.and D.Sc degrees from the University of Birmingham, where he lectured in analytical chemistry from 1964 to 1980. He moved to the University of Hull in 1980, where he introduced both analytical chemistry and toxicology as degree subjects. He became Professor of Analytical Chemistry in 1984 and later held the G. F. Grant Chair of Chemistry and served as Dean. He became Director of the institute for Chemistry in Industry in c.2000 and retired from the University in 2004. He has published five books and edited numerous others. He has also published more than 300 scientific papers, his main interests initially being flame spectroscopy and, from about 1978 onwards, analytical applications of chemiluminescence and of immobilised reagents (especially enzymes), and flow injection analysis. Professor Townshend was a senior editor of Analytica Chimica Acta (Elsevier) until 2006 and of the Dictionary of Analytical Reagents (Chapman and Hall, 1993). He has been an Editor of all three editions of the Encyclopedia of Analytical Science. He was President of the Analytical Division of the Royal Society of Chemistry (RSC) in 1996-98 and has served on several of its committees. He was an active member of the Analytical Chemistry Division of the International Union of Pure and Applied Chemistry for many years. He also was a member of the Council of the Analytical Chemistry Division of the Federation of European Chemical Societies for four years. His interests in forensic science and toxicology led to appointments to bodies governing the competence of forensic scientists and the verification of anti-doping tests in horse racing. He also served on the Chemistry panels of the Higher Education Council’s Research Assessment and Teaching Quality exercises. After retirement, Emeritus Professor Townshend successfully completed a part-time BA course in Archaeology (2006 – 13) at the University of Hull. He is now involved in genealogy with help from the University of the Third Age (U3A) and also organises wine appreciation meetings for the local U3A branch.

Affiliations and Expertise

University of Hull, Department of Chemistry, UK

Paul Worsfold

Paul Worsfold is Professor of Analytical Chemistry in the School of Geography, Earth and Environmental Sciences at the University of Plymouth. He obtained his BSc at Loughborough University of Technology in 1976 and his PhD in Analytical Chemistry at the University of Toronto in 1980. This was followed by positions at the Technical University of Denmark, Sheffield City Polytechnic and the University of Hull. He was awarded a DSc in 1998, was President of the RSC Analytical Division (2004-06), a Governor of IGER (BBSRC research institute; 2000-06), chair of the Division of Analytical Chemistry of EuCheMS (2011-2016) and Editor of the journal Analytica Chimica Acta (1990-2018). He has received the Royal Society of Chemistry SAC Silver Medal, the Society of Chemical Industry H.E. Armstrong Endowed Lectureship, the C.B. Huggins Endowed Lectureship from Acadia University, Canada, the Royal Society of Chemistry Theophilus Redwood Endowed Lectureship and the Japanese Association for Flow Injection Analysis Honour Award. Professor Worsfold has more than 370 publications including nearly 250 original research papers and supervised 61 PhD completions. His research interests are in the broad areas of Analytical Chemistry and Environmental Chemistry. Specific themes include flow injection analysis (FIA), techniques for the determination of phosphorus and trace metal species in natural waters and the design and deployment of instrumentation for studying environmental processes and biogeochemical cycles.

Affiliations and Expertise

University of Plymouth, UK.

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