Determination of the Halogen Elements in Aqueous, Organic, and Solid Samples Using ICP-OES Oct 1, 2006 By: Garry Kunselman, Peter Brown, Craig Seeley, Arthur Reed

Accurate determination of trace Cl, Br, and I is important in industries such as petrochemical refining, chemical manufacturing, biomedical and nutritional supplement manufacturing, and environmental analysis. Until recently, it was thought that the halogen elements could not be determined effectively by inductively coupled plasma–optical emission spectroscopy (ICP-OES); however, with recent advances in spectrometer and detector design, these elements are now readily determined. In fact, ICP-OES offers many advantages for the measurement of Cl, Br, and I. These include ease-of-use and the ability to test for other elements simultaneously, along with good sensitivity, precision, and accuracy. This article describes the measurement of chlorine in tissue and oil samples as well as the measurement of bromine in plastics and electronic materials where the solids were sampled using laser ablation.

Exploring the Next Generation of Mass Spectrometer for Metal Analysis: Time-of-Flight Oct 1, 2006 By: Christine Rivera, Andrew "Flynn" Saint, William Balsanek

Although inductively coupled plasma–mass spectrometry (ICP-MS) has rapidly attained acceptance as the choice in trace metal analysis, most commercially available instruments are equipped with quadrupole-based mass analyzers. Quadrupole mass spectrometers have been available commercially for ICP since the early 1980s. Modifications and advances in these types of instruments predominantly have been in the sample introduction and ion optic areas, leaving the quadrupole mass spectrometer untouched.

Elemental Analysis of Edible Oils and Fats by ICP-OES Oct 1, 2006 By: D. Ardelt, P. Ivanov, O. Schulz

The analysis of edible oils and fats by inductively coupled plasma–optical emission spectroscopy (ICP-OES) utilizing direct injection after dilution with kerosene is described. Sample preparation was performed according to EN ISO 661 (1) and ISO 10540-3 (2). The accuracy was investigated using the AOCS reference sample, "Trace Metals in Soybean Oil" (3) and by spike recovery measurements using commercial sunflower oil. The analysis requirements for sensitivity, precision, and accuracy were met. This article includes line selection, detection limits, and accuracy studies.

Multiline Analysis: A Key Technique to Enhance Analytical Reliability in ICP-AES Oct 1, 2006 By: Jean Michel Mermet, Agnès Cosnier, Emmanuel Fretel, Sébastien Vélasquez, Alexandre Grigoriev, Cendrine Dubuisson

Interactive dedicated tools have been developed to facilitate the use of multiline analysis in inductively coupled plasma–atomic emission spectroscopy (ICP-AES) with emphases on multiline selection and on statistics for rejection of possible outliers. The aim is to take full benefit of the available information when using a charge-coupled device (CCD) detector–based instrument and to enhance the accuracy of the results. Determination of Cu in steel will be used to illustrate the potential of the tools.

Optimization of a High Sample Throughput Method for the Determination of Trace Nutrients in Agricultural Soil Samples Using ICP-OES Oct 1, 2006 By: Cynthia P. Bosnak, Dennis Yates, Robert Thomas

The use of fertilizers is important to increase crop yields in soils that are being used for agricultural purposes. However, in order to maximize plant growth, it is also absolutely essential to know how the crops are using the nutrients in the soil. This process is commonly referred to as a fertility management program, where many soil samples are taken over a predefined area of the land and analyzed for various components such as pH, organic matter, and trace element nutrients. This article describes how a soil testing laboratory in the midwest has developed a method to analyze up to 3500 soil samples per day for 11 trace metals, using inductively coupled plasma–optical emission spectroscopy. It will focus on the soil sampling procedure together with the sample preparation requirements for this high workload environment. The instrumental analytical procedure will be described in greater detail, particularly how the measurement protocol and sampling process are optimized to cope with such extreme..

Analysis of Nitrogen, Other Nutrient Elements, and Toxic Elements in Fertilizers Using ICP Spectroscopy Oct 1, 2006 By: Matthew Cassap

Fertilizers are used to provide major plant nutrients (N, P, and K), secondary plant nutrients (Ca, S, and Mg), and micronutrients such as B, Mn, Fe, Cu, Zn, Mo, and Se. Accurate determination of the composition of fertilizers is essential so that the correct dose can be applied to the soil. An insufficient application of a fertilizer can result in poor crop yield, and an excessive application can result in environmental damage such as eutrophication by dissolved phosphates and nitrates entering water courses or land contamination from nonnutrient elements within the fertilizers. Inductively coupled plasma (ICP) spectroscopy offers cost-effective analysis of fertilizers because of its multielement capabilities. Complex torch designs and sparging systems have been employed in the past to determine nitrogen by ICP spectroscopy, but these additions to ICP instrumentation are costly and prolong analysis time.

In drug discovery, determining information about the extent of metabolism and the elucidation of metabolite structures is a vital step for lead optimization and drug scaffold refinement. The identification and characterization of metabolites plays an important role in both the drug discovery and development phases, as unsuitable pharmacokinetics (bioavailability and drug distribution), toxicity, and adverse drug reactions might be linked to metabolic instability. Historically, metabolite identification was carried out after a compound had been chosen for drug development. However, to reduce candidate failures attributed to toxicity effects, many pharmaceutical companies now conduct these experiments in the earliest phases of candidate drug selection.

With electron ionization (EI) used in most gas chromatography–mass spectrometry (GC–MS) applications, the molecular ion typically is broken apart into multiple fragment ions during the EI process.

Detrimental health effects of a group of brominated flame retardants, polybrominated diphenyl ethers (PBDEs), have been recognized recently, but only after their wide usage and consequently, global dispersal. Of the possible 209 PBDE congeners, 39 (varying in degree of bromination from mono to deca) have been identified previously in the three common technical mixtures. Additional congeners, presumably debromination products of the fully brominated decabromodiphenyl ether (BDE-209), also have been reported in biotic and abiotic environments. However, costly analytical standards are needed to confirm their identification. In addition, the most widely used identification approach, electron ionization (EI) mass spectrometry (MS), primarily produces spectra indicating only homologue grouping (for example, hepta-BDE). Without specific compound identification, full assessment of toxicological consequences of PBDE burdens is impeded. It has been reported previously that electron-capture negative ionization (ECNI),..