Flow Analysis with Spectrophotometric and Luminometric Detection book cover

Flow Analysis with Spectrophotometric and Luminometric Detection

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.

Audience

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

Hardbound, 472 Pages

Published: January 2012

Imprint: Elsevier

ISBN: 978-0-12-385924-2

Reviews

  • "The book is clearly written and comprehensive. This monograph could be used as a textbook both for advanced courses and for experienced researchers in different fields who would like to obtain detailed information about flow techniques."--Anal Bioanal Chem, 2012, Volume 403
    "The aim [of this book] is to provide the reader with the most important basic aspects of flow techniques, according to the experience of the authors. In this sense, a detailed overview of the use of spectrophotometric and luminometric detection is presented with some details which may be scarcely found in other similar books. Some injection devices developed by the Brazilian Center for Nuclear Energy in Agriculture (CENA) are presented in detail. All the chapters end with an interesting and useful list of references. Summary The book is clearly written and comprehensive. This monograph could be used as a textbook both for advanced courses and for experienced researchers in different fields who would like to obtain detailed information about flow techniques."--Analytical and Bioanalytical Chemistry, (2012) 403:1465-1466


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

    3.1.1.1. Flow regime

    3.1.1.2. Composition of the flowing stream

    Tandem stream

    Mono-segmented stream

    3.1.1.3. Temporal variations in flow rates

    Constant flow

    Pulsating flow

    Sinusoidal flow

    Reversed flow

    Linearly-variable flow

    Intermittent flow

    Pulsed flow

    3.1.1.4. Alterations to the flow pattern

    3.1.2. Sample dispersion

    3.1.2.1. Dispersion inside a tubular reactor

    3.1.2.2. Dispersion inside a mixing chamber

    Improved mixing conditions

    High sample dispersion

    Exponential dilution

    Establishment of fluidized beads

    Manifold components behaving as mixing chambers

    3.1.2.3. Dispersion by confluent streams

    3.1.2.4. 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

    3.3.2.1. Peak height

    3.3.2.2. Peak area

    3.3.2.3. 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

    4.1.1.1. Losses of radiation

    Radiation losses at interfaces

    Radiation losses at the cuvette walls

    Radiation losses inside the sample

    Compensation of radiation losses

    4.1.1.2 The Lambert-Beer law

    4.1.1.3. Practical aspects of the Lambert-Beer law

    Concentration of the radiation absorbing species

    Monochromaticity of the radiation

    Sample homogeneity

    Chemical deviations

    Temperature

    Stray radiation

    4.1.1.4. Special strategies

    Dual-wavelength spectrophotometry

    Solid phase spectrophotometry

    4.1.2. Turbidimetry

    4.1.2.1. Losses of radiation

    4.1.2.2. Relationship between turbidance and analyte concentration

    4.1.2.3. Practical aspects

    Characteristics of the particles

    Monochromaticity of radiation

    Sample uniformity

    Chemical deviations (including co-precipitation)

    Rate of turbidity formation

    Stray radiation

    4.1.2.4. Special strategies

    4.1.2.5. 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

    4.2.3.1. Historical testimonies

    4.2.3.2. The two components of the Schlieren effect

    Poor mixing conditions

    Good mixing conditions

    4.2.3.3. Applications

    4.2.3.4. 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

    4.2.3.5. 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

    5.2.3.1. Dispersion parameters

    Temperature

    Sample viscosity

    Diffusion coefficient

    Composition of the sample and reagent solution

    Others

    5.2.3.2. 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

    5.3.3.1. Large sample volume

    5.3.3.2. 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

    5.4.3.1. Automated devices

    5.4.3.2. Devices with feedback mechanisms

    5.4.3.3.Trends

    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

    5.6.6.1. General figures of merit

    Accuracy

    Precision

    Selectivity

    Sensitivity

    Detection limit

    Dynamic range

    5.6.6.2. Figure of merit specific to flow based procedures

    Carryover

    Sampling rate

    Ruggedness

    Portability

    6. Instrumentation

    6.1. Fluid propulsion

    6.1.1. Peristaltic pumps

    6.1.2. Syringe (piston) pumps

    6.1.2.1. Use of large volume pistons (syringes)

    6.1.2.2. Use of small volume pistons

    6.1.3. Diaphragm pumps

    6.1.3.1. Solenoid pumps

    6.1.3.2. 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

    6.2.2.1. Sampler

    6.2.2.2. Time-based introduction

    6.2.2.3. Loop-based introduction

    6.2.2.4. Hydrodynamic injection

    6.2.2.5. Nested injection

    6.2.3. Reactors

    6.2.3.1. Coiled reactors / mixing coils

    6.2.3.2. Packed bed reactors

    6.2.3.3. Single bead string reactor

    6.2.3.4. Knitted (or knotted) reactors

    6.2.3.5. Reactor-like artefacts

    6.2.4. Accessories

    6.2.4.1. Connectors

    Connectors for linking tubes together

    Connectors for linking manifold tubes with other components

    6.2.4.2. Solution containers

    6.3. Detection and data processing

    6.3.1. Flow-cells

    6.3.1.1. Classical and Z-shaped flow-cells

    6.3.1.2. Spiral flow-cells

    6.3.1.3. 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

    7.1.1.1. Merging zones relying on different convergent carrier streams

    7.1.1.2. Merging zones relying on a single carrier stream

    7.1.1.3. Merging zones relying on an intermittent stream

    7.1.2. Applications

    7.1.2.1. Reduction of reagent consumption

    7.1.2.2. Matching the analytical signal with the dynamic concentration range

    7.1.2.3. Single point determinations incorporating blank determinations

    7.1.2.4. Speciation

    7.1.2.5. Reducing undesirable adsorption processes

    7.1.2.6. Sequential determinations

    7.1.2.7. Standard addition method

    7.2. Zone sampling

    7.2.1. Implementation

    7.2.2. Applications

    7.2.2.1. High sample dispersion

    7.2.2.2. Simultaneous determinations

    7.2.2.3. Variable dispersion

    7.2.2.4. Detailed study of dispersion

    7.3. Stream splitting

    7.3.1. Segmented flow analysis

    7.3.2.Unsegmented flow analysis

    7.3.2.1. Stream splitting / stream merging

    Expansion of the dynamic concentration range

    Differential kinetic analysis

    Simultaneous determinations

    7.3.2.2. 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

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