Library



Brammer Standard Company is proud to offer a very helpful book,

Automatic Atomic-Emission-Spectroscopy
by Karl Slickers, Dipl.Ing. Second Edition, 1993 ISBN 3-9803333-1-0

This 500 page book, together with many drawings, graphs, and tables, is specifically written for users and those people who choose to use spectrochemical analysis in a routine application.

It provides detailed and thorough information regarding various techniques such as glow discharge, ICP, DC Plasma, and arc and spark for the analysis of liquids, powders, and metals for process control, QC and environmental protection. For those techniques, it is the most detailed reference guide on the market.



Contents

Chapter Title
1 Prefaces
2 Fields of application for AES
3 Chemical analysis with spectrometers
4 Physical fundamentals of AES
5 Samples
6 Spectrometer design
7 Calibration and evaluation
8 Spectrometer methods and applications for routine analysis
9 Design of spectrometer rooms
10 Further application examples
11 References
12 Key word index
13 Contributions from spectrometer manufacturers
14 Advertisements


1. Prefaces

1.1 Preface to the first German edition published in 1977
1.2 Preface to the first English edition published in 1981
1.3 Preface to the second German edition published in 1992
1.4 Preface to the second English edition
1.5 Introducing the author

2. Fields of application for AES

3. Chemical analysis with spectrometers - spectrochemical analyses

3.1 Economic aspects of spectrometers
3.11 Operating personnel and training
3.12 Spectrometer reliability and down time
3.2 Quality assurance and product liability

4. Physical fundamentals of AES

4.1 Short introduction and historical review
4.2 Atomic structure
4.3 Atomic excitation
4.31 Excitation with thermal energy
4.32 Excitation with electrical energy
4.33 Excitation with optical energy
4.34 Energy - Wavelength - Temperature
4.4 Spectra
4.41 Atomic or line spectra
4.42 Molecule or band spectra
4.43 Continua
4.44 Width and displacement of spectral lines
4.45 Self-absorption and self-reversal
4.5 Electromagnetic radiation and wavelength ranges
4.51 Wavelength units
4.52 Wavelength atlases
4.6 Comparison of AES, AAS and AFS

5. Samples

5.1 Types of samples (definitions)
5.11 Calibration samples
5.12 Recalibration samples
5.13 Check samples
5.2 Sampling from melts
5.3 Preparation of metal samples
5.31 Mechanical preparation of samples from metal melts
5.32 Preparation of samples from semifinished products
5.321 Mechanical preparation (with chip removal)
5.322 Briquetting technique
5.323 Remelting techniques
5.3231 Electric arc furnace remelting method
5.3232 Remelting technique with inductive heating
5.4 Preparation of powders, nonconductors, minerals and similar substances
5.41 Sample preparation without fusion
5.42 Sample preparation with fusion
5.421 Fusion in a muffle furnace
5.422 Fusion with inductive heating
5.423 Fusion with gas flame
5.5 Sample preparation for liquids (solutions)

6. Spectrometer design

6.1 Energy and radiation sources
6.11 Flames and plasmas to which the sample is introduced
6.111 Chemical flames
6.112 Electrical plasmas
6.1121 Direct current plasma, DCP
6.1122 Loaded-line microwave plasma, LLMP
6.1123 Microwave-induced plasma, MIP
6.1124 Inductively coupled plasma, ICP
6.113 Sample introduction to flames and plasmas
6.1131 Liquid sample introduction
6.11311 Sample introduction using pneumatic nebulisers
6.11312 Sample introduction using hydraulic high-pressure nebulisers, HHPN
6.11313 Sample introduction using ultrasonic nebulisers, USN
6.11314 Nebuliser or spray chamber
6.11315 Argon humidifier
6.11316 Aerosol dryer
6.1132 Solid sample introduction
6.11321 Direct solids introduction
6.113211 Introduction into the ICP by means of a graphite crucible
6.113212 Powder introduction to ICP using vortex entrainment device
6.113213 Introduction to ICP using a suspension
6.11322 Indirect introduction of solid substances
6.113221 Introduction using electro-erosion, ELE
6.113222 Introduction using electrothermal vaporization, ETV
6.113223 Introduction using laser erosion
6.1133 Gas sample introduction
6.11331 Introduction direct and from a chromatograph
6.11332 Introduction from a hydride system
6.12 Electrical discharges in which the sample is at least one electrode (gas discharges)
6.121 Arc discharges, AD
6.122 Spark discharges, SD
6.123 Discharges at negative pressure, glow discharges
6.1231 Hollow cathode glow discharges, HCL (Hollow Cathode Lamp)
6.1232 Flat cathode glow, GDL (Glow Discharge Lamp)
6.13 Laser
6.2 Spectrometer optics
6.21 Radiation guidance from radiation source to spectrometer entrance slit - entrance optics
6.211 Direct radiation guidance
6.212 Indirect radiation guidance with lenses or mirrors
6.213 Indirect radiation guidance with lightguides
6.2131 Design and analysis possibilities with lightguides
6.214 Notes on the region in front of the entrance slit
6.22 Spectral dispersion
6.221 Spectral dispersion using a filter
6.222 Spectral dispersion using a prism
6.223 Spectral dispersion using a slit
6.224 Spectral dispersion using a grating
6.23 Spectrometer optics configurations
6.231 Spectrometer optics with a prism
6.232 Spectrometer optics with plane transmission grating
6.233 Spectrometer optics with plane reflection grating
6.234 Spectrometer optics with Rowland concave grating
6.235 Spectrometer optics with echelle grating
6.236 Characteristics of spectral dispersion with spectrometer optics
6.24 Spectrum detection
6.241 Monochromator
6.242 Polychomator
6.243 Combined monochromator/s and polychromator/s, "Monopoly"
6.244 Image Dissector echelle Spectrometer, IDES
6.25 Radiation guidance from exit slit to radiation receiver - exit optics
6.26 Additions to spectrometer optics using a Rowland concave grating
6.27 Photoelectric radiation measurement
6.28 Measurements of photoelectric current
6.281 Integrator circuit
6.2811 Estimating photoelectric currents in ICP and SDAR
6.282 Analogue/digital converters
6.2821 Dynamic integration
6.283 Measurement system design and description of functions
6.2831 Preamplifier
6.29 Computer control of a spectrometer
6.291 Spark generator (energy source) control
6.292 Argon supply control for spectrometers with SDAR
6.293 HV attenuator control
6.294 Monochromator control

7. Calibration and evaluation

7.1 General notes on numbers
7.2 Statistics in spectrometry
7.3 Working procedure
7.31 Sample parameters
7.32 Spectrometer parameters
7.33 Analytical lines
7.34 Resolution of measurement ranges
7.35 Capability of the spectrometer as a "radiation measuring machine"
7.4 Explanatory notes on calibration
7.41 Approximation of calibration curves using a polygon with n steps
7.42 Calibration of curve approximation with single and multiple polynomials of the nth degree
7.43 Approximation accuracy
7.5 Referral to a reference
7.51 Ratio method
7.52 Global calibration with SDAR
7.6 Data on calibration curves
7.61 Precision (ADS and RSD)
7.62 Equivalent concentration of spectral background (BEC) and detection limit (LOD)
7.63 Accuracy(SR)
7.631 Spectral Interference
7.632 Inter-element effect
7.633 Background correction
7.64 Taking account of the state of calibration; recalibration
7.7 Evaluation of measurement values of analytical data
7.71 Further processing of analytical data
7.711 Questions on further processing of analytical data
7.8 Comparison of spectrochemical analyses and chemical analyses
7.81 Accuracy of spectrometer calibration curves
7.82 Accuracy of production control chemical analyses
7.83 Round Robin investigations

8. Spectrometer methods and applications for routine analysis

8.1 Spectrometers with Rotrode, with spark discharges in air
8.11 Analysis of aqueous solutions
8.12 Analysis of active substances in oils
8.13 Analysis of abrasion products in machine oils and hydraulic liquids
8.14 Accessories for spectrometers with Rotrode for oil analysis
8.15 Hints on maintenance of spectrometers with Rotrode for oil analyses
8.16 Multirode or Ashing Rotrode
8.2 Mobile spectrometers with arc and spark discharges for on-site metal identification
8.21 Efficiency of mobile, in-plant AE spectrometers
8.22 Criteria for in-plant use
8.23 In-plant use
8.231 Rapid sorting of alloy materials
8.232 Identity testing
8.233 Approximate analysis and quality determination
8.24 Maintenance hints for mobile in-plant spectrometers with ADA
8.25 Metal analysis with mobile in-plant spectrometers with SDAR
8.251 Carbon determination in steel using lightguides
8.26 Maintenance hints for mobile in-plant spectrometers with SDAR
8.27 Automation of in-plant spectrometers
8.3 Spectrometers with spark discharges in argon
8.31 Some comparisons of spark discharges in air (SDA) and argon (SDAR)
8.32 Types of discharge with SDAR
8.33 Effect of oxygen and hydrogen on SDAR
8.34 The effect of oxygen and hydrogen on SDAR
8.35 Processes in the burn spot
8.36 Burn-off curves
8.37 Energy source (spark generator) for SDAR
8.371 HRRS
8.372 HEPS
8.373 SREPS
8.38 Monitoring the sparking process: SATEUS, SETEME
8.39 Effect of sample temperature
8.310 Radiation guidance to the optics
8.311 Summary of interference and pseudo-interference with SDAR
8.312 Variations in spark intensity against time - SAFT
8.3121 Determination of precious metals in lead collectors using SDAR with SAFT
8.313 Assessment criteria for spectrometers with SDAR for metal analysis
8.3131 Spectrometer parameters
8.3132 Precision
8.3133 Global calibration and accuracy
8.3134 Longtime stability
8.3135 Detection limit and background equivalent
8.3136 Contamination
8.3137 Machine operating times
8.3138 Sample sizes and machining
8.3139 Operating costs
8.31310 Spectrometer availability
8.31311 External operating conditions
8.31312 Ease of operation
8.31313 Commissioning time and costs: operator training
8.314 Metal analysis with SDAR
8.3141 Concentration ranges for important metals
8.3142 Gas analysis in metals
8.3143 Carbon analysis in steel
8.3144 Analysis of base concentration
8.3145 PIM = Peak Integration Method
8.3146 MAMA = Multiple Analytical Measurement Application
8.3147 Analysis of metal samples with small dimensions
8.3148 Analysis of coatings
8.3149 Analysis of (metal) powders
8.315 Analysis of nonconductive samples
8.3151 Trace analysis in oxides
8.3152 Analysis of slags and similar substances
8.316 Analytical quality control for spectrometers with SDAR before calibration
8.317 Hints on maintenance of spectrometers with SDAR for metal analysis
8.318 Information on servicing for analysis checks
8.319 Automation of spectrometers with SDAR
8.4 AE spectrometers with inductively coupled plasma (ICP)
8.41 Equipment assessment criteria for AE spectrometers with ICP
8.411 Energy Source (generator), radiation source (torch) and sample feed
8.412 Radiation off-take
8.413 Optics
8.42 Analysis assessment criteria for AE spectrometers with ICP
8.421 Precision
8.422 Accuracy
8.423 Detection limit and background equivalent
8.424 Longtime stability
8.425 Contamination
8.426 Machine operating times
8.427 Operating costs
8.428 Availability
8.429 External operating conditions
8.4210 Ease of operation
8.4211 Commissioning time and costs: operator training
8.43 Applications with AES-ICP
8.431 Analysis of liquids and solutions
8.432 Analysis of oils, and comparison with AES-SDA-Rotrode
8.433 Analysis of solids
8.4331 Analysis of suspensions
8.4332 Analysis with direct introduction and directly-coupled introduction by electrothermal vaporization ETV
8.4333 Analysis with indirect sample introduction by spark erosion ELE
8.5 Maintenance hints for AE spectrometers with ICP

9. Design of spectrometer rooms

9.1 Transport, installation and commissioning of spectrometers
9.11 Example of installation instructions for a spectrometer with ICP
9.12 Example of a check list for installation instructions for a spectrometer with ICP
9.2 Safety hints for spectrometer operation
9.3 Necessary and useful aids and consumables
9.4 Purification of argon
9.41 Purification of argon/hydrogen mixtures
9.5 Transmission of analytical and associated data
9.51 Questions on transmission of analytical and associated data

10. Further application examples

10.1 Trace analysis in pure copper using the globular arc
10.2 Trace analysis in ferrous metals with the hot hollow cathode lamp HHCL
10.3 Precious metal analysis by glow discharge lamp GDL
10.4 Analysis of ores, slags, cements, and similar substances using a tape machine
10.5 Trace analysis in geological samples with packed (cup) electrode
10.6 Analysis of aqueous solutions by flame
10.7 Analysis of aqueous solutions and oils using the loaded line microwave plasma LLMP

11. References

12. Key word index

12.1 Abbreviations

13. Contributions from spectrometer manufacturers

14. Advertisements