Sample
Preparation and Introduction for Atomic Spectroscopy
McCrone
Group
850 Pasquinelli Drive,Westmont, Illinois 60559
630-887-7100
8:30am Workshop Registration
9:00
am
Atomic
Spectrometry: Overview and New Developments
Dr. Jon Carnahan, Northern Illinois
University
9:45
am
Metals Digestions Made Easy (Hot
Block)
Les Orr, Environmental Express, Inc.
10:20
am Break & visit vendors
10:50
am
A “How-To” Practical Approach to
Microwave Digestion
Elaine Hasty, CEM Corp.
11:25
am
Better, Faster,
Stable-er Standards Preparation
Dr. Tom Rettburg, VHG Labs, Inc.
12
noon Lunch (provided) & visit Vendors
1:00
pm
The Role of the
Nebulizer in ICP Sample Introduction
Dr. Geoff Coleman, Meinhard Glass
Products
1:35
pm
Laser Ablation Fundamentals, Techniques and
Applications
Mike Colucci, New Wave Research
2:10
pm Break & visit Vendors
2:40
pm
Temperature Controlled Spray Chambers and Specialty Torches
Jerry Dulude, Glass Expansion, Inc.
3:15
pm
Specialized Introduction Techniques for Liquid and Solid Samples
Using
ICP-AES and ICP-MS Detection
Dr. Fred Smith, CETAC Technologies
3:50
pm Q&A Closing
A workbook of the presentation slides will be provided to all attendees.
Use PDF
File for Registration
Abstracts
Atomic
Spectrometry: Overview and New Developments
Jon W. Carnahan, Adam E. Dill, Courtney, A.
Cherok
Northern Illinois University
Department of Chemistry and Biochemistry
DeKalb, IL 60115
Reliability, robustness,
and the ability to generate easily understood data are desirable characteristics
atomic spectrometry possesses. In terms of scientific instrumentation, these
techniques are quite mature. Nevertheless, they account for a large fraction of
the chemical analyses done in today’s laboratories.
Atomic spectrometric
techniques have undergone some fascinating improvements in recent years. Many
of the improvements are a function of improved atom/ion reservoirs, sample
introduction approaches, primary sources, and photon (or ion) optics. Improvements
in atom/ion reservoirs and sample introduction have led to more sensitive and
stable detection.
Currently, many new forms
of atomic spectrometry are being developed in order to meet the demand for new
methods of chemical analysis. Many of the forms of atomic spectrometry being
developed contain different types of atom/ion reservoirs and sample introduction
methods to solve problems that some more developed instrumentation may be unable
to solve, such as surface/depth analysis or more sensitive and selective
detection of specific elements. Although some of these forms of atomic
spectroscopy are relatively new, many of them have led to some promising
improvements for specific applications.
In this talk, an overview
of atomic spectrometric techniques, including electrothermal, flame, plasma,
arc, and glow discharge methods will be presented.
Metals Digestions Made Easy
Les Orr, Environmental Express, Inc.
For the past four decades
or so, significant progress has been made with instrumentation for the
determination of metals. But the digestion procedure for dissolution has
remained relatively the same. As MDL’s decreased, labs experienced
contamination on a scale that previously went undetected.
Technology has finally
caught up to the prep lab, incorporating equipment that benefits the digestion
procedure by eliminating many of the chances for contamination. Corrosion-free
materials and disposable “glassware” is only the start of the benefits.
As a natural progression,
automation has occurred thus reducing safety, labor and more QC concerns for the
lab. Now the instruments for detection are capable of reaching the levels
intended for “real world” samples.
A “How-To”
Practical Approach to Microwave Digestion
Elaine Hasty, CEM Corporation
This presentation will
focus on the practical aspects of pressurized digestion and dissolution for
organic and inorganic sample types. Included will be an overview of reagent
choices and temperature programs appropriate for various sample matrices. The
various approaches to control – temperature, pressure, single reference vessel
or all vessel control will be outlined along with their pros and cons.
A straightforward approach
to method development for unknown samples will be presented with clear and
concise guidelines given for various types of samples.
Better, Faster,
Stable-er Standards Preparation
Thomas Rettberg, Ph.D.
VHG labs
276 Abby Rd
Manchester, NH 03103
Advancements in technology
have not reduced the fundamental basis of most instrumental techniques--the need
for a current calibration created using calibration standards. Optical and mass
spectrometric techniques for “metal group” determinations have developed over
time to be increasingly multi-element, commonly at lower concentrations, more
likely to include non-metals or problematic elements; such as mercury, and tend
to involve more direct analysis of complex matrices. One aim of this talk will
be to cover some of the interdependencies associated with preparing appropriate
and stable calibration standards for these situations.
Increased throughput is
also a key objective of most laboratories. It is important to understand that
the solution matrix (whether aqueous and organic) for blanks and standards be
well-suited for shortened uptake and rinse times coupled with long sample batch
duration. General guidelines for determining the best stock standard to use,
the meaning of traceability, and expiration of certification will also be
discussed.
The Role of
the Nebulizer in ICP Sample Introduction
Dr. Geoff Coleman,
Meinhard Glass Products
The role of the
nebulizer is to convert an ostensibly homogeneous sample solution to an aerosol
for efficient and reproducible transport to the plasma where it will be rapidly
and reproducibly desolvated, vaporized, dissociated, then excited and/or
ionized. Each of those processes has an impact on its successor. If the
processes are not highly reproducible in time, space and completeness, the
analytical signal cannot be reproducible either. Since the rate of evaporation
of solvent from a droplet is a function of the surface area to volume ratio, the
smaller the droplet, the faster and more completely it will desolvate then
vaporize, dissociate, and undergo excitation and/or ionization. Studies show
that little signal is derived from droplets larger than 5 um; most comes from
droplets that are 3 um or less, in diameter. Unfortunately, the nebulizers which
produce the smallest droplet sizes are limited in their applicability for other
reasons.
The fact is, no
nebulizer does everything well; each has its strengths and weaknesses; each is
better suited to particular set of circumstances whether it is a matter of cost,
convenience, robustness, ease of use, stability, reproducibility, the size of
the aerosol it produces, as well as other criteria that might apply. We will
briefly look at how nebulizers work, what is available, some strengths and
weaknesses of each design, and where each is most useful.
Laser
Ablation Fundamentals, Techniques and Applications
Mike Colucci, New Wave Research
Laser ablation ICP-AES and
ICP-MS has been a rapidly evolving analytical tool since the early 1980’s. The
fundamental 1064nm wavelength of a Nd-YAG laser is stepped down by harmonic
generation to produce 266nm, 213nm and 193nm wavelengths suitable for ablation
of solid materials and introduction of the generated aerosol into an ICP source
for trace element and isotope analysis. Transmissive materials, such as high
purity quartz and fused silica, require deep UV wavelengths (213-193nm) for
effective coupling, whereas opaque materials such as metals and plastics ablate
efficiently at the 266nm wavelength.
The laser ablation systems
are equipped with a beam delivery system that enables the laser to be focused
upon a sample surface at a range of spot sizes at the micron scale. Laser
ablation is an attractive alternative to solution analysis due to 1) virtually
no sample preparation, 2) high spatial resolution, 3) high transport efficiency,
and 4) it is a microdestructive technique. Application areas currently
utilizing laser ablation include, but are not limited to: Geological Sciences,
Forensic Sciences, Life Sciences, etc. Product lines span the UV spectrum from
266nm to 193nm laser ablation systems. Software and hardware capabilities allow
complete automation for a range of experiment types.
Temperature Controlled Spray Chambers and Specialty Torches
Jerry Dulude, Glass Expansion, Inc., Pocasset,
MA
Typically, the only time an
ICP analyst is concerned with spray chamber temperature is for the analysis of
volatile organic solvents that require a chilled chamber to maintain the
plasma. Otherwise, it is assumed that 1) room temperature is ideal for all
aqueous applications, 2) the spray chamber is at room temperature, and 3) room
temperature is constant. All of these assumptions will be refuted in this
paper. It will be demonstrated that spray chamber temperature is as critical a
parameter as nebulizer gas flow or RF power and can be appropriately adjusted to
optimize an ICP method. The effects of spray chamber temperature will be
examined with respect to intensity, detection limits, plasma robustness, and the
degree of suppression.
The standard (i.e. that
which is shipped with the instrument) ICP torch is assumed to be ideal for all
applications. In reality, specialized torches provide superior performance for
specific applications. Specialized torches are available and will be described
for applications such as the analysis of brines, engine oils, and semi-conductor
solvents.
Specialized Introduction Techniques for Liquid and Solid Samples
Using ICP-AES
and ICP-MS Detection
Dr. Fred
Smith, CETAC Technologies, 14306 Industrial Road, Omaha, NE 68144.
This presentation is comprised of two parts, with the first concerning
liquid sample introduction and the second direct solid sampling with little or
no sample preparation.
Specialized liquid sample introduction techniques for ICP-AES and ICP-MS
may be used for a number of reasons. These reasons can include enhanced analyte
signal, reduction of sample matrix interferences, the introduction of very low
volume (< 1mL) samples, and shorter analysis times. A variety of techniques
will be described, including ultrasonic nebulization, membrane desolvation,
inert low-flow nebulizers, hydride generation, and discrete sampling.
Direct solid sampling can avoid a number of problems with acid digestion
of a solid: difficulty of digesting certain solids (ex. ceramics, polymers),
contamination from impurities in mineral acids, and loss of element distribution
information. The technique of laser ablation will be described, with details of
typical laser wavelengths, applications, and methods of calibration.