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14 Spectroscopy 27(7)
July 2012
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42 Spectroscopy 25(10)
Oc tober 2010
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July 2012
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Spectrometers for Elemental Spectrochemical Analysis, Part III: Arc/Spark Optical Emission Spectrometers
The author discusses arc/spark optical emission spectrometers. The basic modules of spectrometer systems have already been discussed in Part I of this series (1).
Volker Thomsen
f the arc/spark optical emission spectrometers in service today, 99% are used for the routine spectrochemical analysis of metals. Alloys of iron, aluminum, and copper together make up about 80% of this total. The remaining applications concern alloys of nickel, cobalt, zinc, titanium, magnesium, and the lead/tin/solder group. Refractories, precious metals, steel-making slags and geological materials, and other exotic materials account for the remaining 1% (2,3).
XPS Surface Characterization of Disposable Laboratory Gloves and the Transfer of Glove Components to Other Surfaces
Surface contamination on analytical samples or other handled materials can come from sources such as human hands, inappropriate packaging materials, airborne dust fallout, contaminated sample handling tools, or contaminated sample holders. An often overlooked source of contamination is disposable laboratory gloves, which are frequently worn for the purpose of protecting handled materials from fingerprints and other contaminants present on bare fingers. However, the gloves themselves may be a source of potential contamination transfer equal to or even greater than bare fingers. This study shows how X-ray photoelectron spectroscopy (XPS) can be used to determine the contaminants present on laboratory gloves and also evaluate the type and amount of contamination transfer from gloves to other surfaces.
Brian R. Strohmeier, John D. Piasecki, and Alexander Plasencia
Arc/Spark Excitation
we then seek to explain it. Ions created by EI and CI have been examined for decades, and our understanding is advanced, underpinning the discussion in this column. For ESI and MALDI, despite the broad applicability of the methods, our understanding of the ionic environments in those sources has not yet advanced to an analogous level of detail.
Electrical discharge excitation sources were developed in the latter part of the 19th entury. The first two decades of the 20th century saw considerable development in direct current, alternating current, and high voltage excitation sources. In the arc/spark spectrometer, the excitation is produced by the energy of the electrical discharge between the sample and the electrode. The resulting plasma temperatures effectively remove sample material (called ablation) and excite the constituent atoms. Today, this electrical discharge typically is carried out in an argon atmosphere, although all early instruments were run in air. For this type of spectrometer using electrical excitation, the sample must be electrically conductive. Therefore, this instrumentation is very popular in the metals industry. The Spark Stand and Arc/Spark Source: A diagram of a typical spark stand (electrode and sample geometry) is shown in Figure 1. It illustrates the conventional point-to-plane configuration (electrode to sample). The electrode typically is made of tungsten, although graphite electrodes have been used in the past with nonferrous materials.
The Fundamentals
An elementary fact about chemical reactions is that their rate depends on the temperature of the system. For many reactions, the reaction rate increases with an increase in temperature, and that dependence is shown by the classical Arrhenius rate equation. In short, the Arrhenius rate equation expresses the rate constant k of a reaction on the temperature T: k = Ae-E(act)/RT [1]
In this equation, A is the pre-exponential factor, R is the universal gas constant, and E(act) is the activation energy for the
The spark stand in modern instrumentation is flushed with argon to prevent oxidation effects and allow transmission of UV wavelengths absorbed by oxygen. A very basic electrical circuit diagram used to provide the discharge is shown in Figure 2, where V is a voltage source, S is a switch, C a capacitor, L an inductor, and R is a resistor. When the switch is closed the capacitor is charged to the voltage V. When the switch is opened, the electrical energy stored in the capacitor is released through the inductor and resistor, producing a discharge across the spark gap. Several comments must be made concerning the basic electrical circuit of Figure 2: The voltage in the circuit is generally between about 400 and 1000 V. This is not enough to cross (breakdown) the 34 mm spark gap. A much higher voltage, on the order of 10,000 V, is required. This is provided by an ignitor circuit (similar to the ignition coil of an automobile), whose sole function is to bridge the gap. Once this short path has been ionized, the lower voltage is sufficient for a continued discharge. In modern spark excitation sources, the discharge is unidirectional, from the electrode to the sample. To prevent an oscillating discharge as would occur normally in the circuit of Figure 2, a diode D is included across the capacitor. (A diode is an electrical circuit component that only permits a current to flow in only one direction.) The switch S is opened and closed electronically many times per second. This is referred to as the frequency of the discharge. The spark gap generally is referred to as the analytical gap in arc/spark spectrometry. The 500015,000 K plasma temperatures generated in this region is where the analytical
isposable elastic gloves are ubiquitous in scientific laboratories and are also widely used in many industries while handling critical surfaces. Disposable gloves are typically made from nitrile or latex rubber and offer their users protection from various aqueous acids and bases, biological and medical fluids, organic solvents, and other potentially harmful substances. A second major use of disposable gloves is to protect manufactured products and analytical samples from contamination caused by the transfer of skin cells, oils, salts, cosmetics, hand lotions, or other residues resulting from contact with bare hands. However, disposable gloves can also be an overlooked potential source of contamination on handled surfaces. In addition to the primary polymer structure, many types of common laboratory gloves also contain a variety of inorganic salt additives in the glove formulation. For example, zinc oxide is often added as an accelerator and calcium nitrate is used as a coagulant (1). Post-forming processes such as chlorination are often used to oxidize the outer glove surface to reduce surface tackiness (2). Silicone-containing mold-release agents that allow powder-free gloves to be
easily stripped from the glove formers during fabrication may be present on glove surfaces. Silicones are leachable and can be easily transferred to any object they contact (2). Furthermore, the inner surfaces of disposable gloves may have various polymeric surface coatings for improved donning properties or other specialized uses (2). These inner coatings or bulk glove components may permeate the glove material and segregate to the outer glove surface after exposure to certain solvents. Contact with solvents during rinsing of items being held may also transfer glove components to the surfaces of those items. Contamination resulting from surface residues on gloves can adversely affect materials used in industries in which surface cleanliness is essential for optimum product performance and can also interfere with sample analyses depending on the specificity and sensitivity of the analytical technique being used. Therefore, it is important to know if the various components within a particular glove material are leached out by certain solvents or if manufacturing residues present on the surfaces of gloves are easily transferred to other materials.
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Long-path gas cells
PIKEs long-path IR gas cells are designed for analysis of air contaminants, pure gases, and gas mixtures. According to the company, the fixedpath cells range from 2.4 m to 20 m, and the variable model can be adjusted from 1 m to 16 m. All of the cells reportedly mount rigidly to the baseplate of an FT-IR spectrometer.
News Spectrum
Jens Frisvad Receives Thought Leader Award
Agilent Technologies (Santa Clara, California) has announced the recipient of its latest Thought Leader award: Dr. Jens Frisvad from the Center for Microbial Biotechnology in the department of systems biology at the Technical University of Denmark (Lyngby, Denmark). The center is working to create a targeted metabolomics approach for thousands of compounds produced by Aspergillus, Penicillium, and Fusarium fungi. Scientists will use mutable internal standards to calibrate changes in both chromatographic retention and mass spectrometry (MS) sensitivity to compare extracts over many years. The award will provide the laboratory with use of a liquid chromatographyquadrupole time-of-flight (LCQTOF) MS system for discovery metabolomics, as well as an LCtriple-quadrupole (QQQ) MS system for target screening. Agilent will be supporting research in food safety, specifically the metabolomics of mycotoxins (toxins made by mold). Frisvad commented, Our research is aimed at showing the impact that analysis of LCQTOF and LC QQQ data can have on understanding the metabolomics of mycotoxins. We are extremely pleased that Agilent is helping us continue this important food-safety research. Mike McMullen, president of Agilents chemical analysis group, said, Our support of the work being done at the center for microbial biotechnology closely aligns with a major initiative at Agilent: providing tools and methods that help test the global food supply. By providing instruments to Dr. Frisvad and his team, we continue Agilents long history of helping create innovative ways to improve food safety.
PIKE Technologies,
Madison, WI; www.piketech.com
Andor Technology,
South Windsor, CT; www.andor.com
Coated filters
Coated filters from Optometrics are designed with ion-assisted deposition of refractory oxides and soft-coated filter capabilities. According to the company, the coatings remain stable and survive 300 C for long periods of time. Applications reportedly include fluorescence, analytical instrumentation, laser techniques, environmental monitoring, and imaging systems. Optometrics, Ayer, MA; www.optometrics.com
Raman analyzers
The ProRaman-L series Raman spectrometers from Enwave Optronics are designed to provide measurement capability down to low parts-per-million levels. According to the company, the instruments are suitable for process analytical method developments and other measurements requiring high sensitivity and high speed analysis. Enwave Optronics, Inc., Irvine, CA; www.enwaveopt.com
> Calendar
Miniature spectrometer
B&W Teks Exemplar miniature spectrometer features on-board data processing that includes averaging, smoothing, and automatic dark subtraction. According to the company, the instrument provides data transfer of 900 spectra/s, trigger delay of 14 ns, and gate jitter of 1 ns. B&W Tek, Newark, DE; www.bwtek.com/product/spectrometer/exemplar.html
The McCrone Micronising mill from Glen Creston is designed to reduce solid samples to micrometer sizes suitable for X-ray diffraction, X-ray fluorescence, infrared spectroscopy, and atomic absorption analysis. According to the company, the mills cylinder-grinding action produces linear contact blows and planar shearing, resulting in a short grinding time with little sample loss, even particle size distribution, and minimal crystal lattice disturbance. McCrone, London, England; www.mccrone.co.uk.
Glass Expansion,
Pocasset, MA; www.geicp.com
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2014 HIGHLIGHTS
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Annual Salary Survey Published in March Spectroscopys annual survey of spectroscopists salaries and employment issues measures the changes in compensation packages for spectroscopists. This popular annual analysis documents how the industrys bottom line affects the paychecks of spectroscopists, and provides a general outlook on employment conditions for the next year. Buyers Guide and Industry Trends 2014-2015 Published in August The annual Buyers Guide and Industry Trends issue is the most comprehensive resource for any spectroscopist looking for the latest spectroscopy-related suppliers, products or services, organized in categories specic to their needs. This issue also features cutting-edge market research and analysis from a leading independent consulting rm, exploring each technology area of this dynamic market. The Buyers Guide and Industry Trends issue continues to be a trusted and valued resource among the most inuential buyers in the industry. Corporate Capabilities 2014 Published in December This unique advertorial and application notebook publication presents you with an excellent opportunity to provide more than 26,000 of your best prospects with detailed information about your company and products.
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