ICP-optical

Induaively Coupled Plasma-Optical Emission Spectroscopy, ICP-Optical 633... 

Inductively Coupled Plasma-Optical (ICP-optical) methods and ICPMS are extremely sensitive elemental survey techniques that also are described in this volume. ICP methods, however, require a solution for analysis, so that the direct... 

The Inductively Coupled Plasma (ICP) has become the most popular source for multielement analysis via optical spectroscopy since the introduction of the first commercial instruments in 1974. About 6000 ICP-Optical Emission Spectrometry (ICP-OES) instruments are in operation throughout the world. 

ICP-Optical Inductively Coupled Plasma Optical Emission... 

Solid Sampling Atomic Absorption Spectrometry ICP Optical Emission Spectrometry ICP Mass Spectrometry... 

The chemical compositions of the samples were obtained by ICP in a Varian 715-ES ICP-Optical Emission Spectrometer. Powder X-ray diffraction was performed in a Philips X pert diffractometer using monochromatized CuKa. The crystallinity of the zeolites was obtained from the intensity of the most intense reflection at 23° 20 considering the parent HZ5 sample as 100% crystalline. Textural properties were obtained by nitrogen physisorption at -196°C in a Micromeritics ASAP 2000 equipment. Surface areas were calculated by the B.E.T. approach and the micropore volumes were derived from the corresponding /-plots. Prior to the adsorption measurements the samples were degassed at 400°C and vacuum overnight. 

The certification procedure for seven trace metals (Ba, Ca, Li, Mg, Mn, Na and Sr) in the certified reference material FEBS-1 (National Research Council Canada, Institute for National Measurement Standards, Ottawa, Canada) based on fish otolith matrix by isotope dilution - ICP-MS in comparison to ICP optical emission spectrometry and X-ray fluorescence analysis, is described by Sturgeon et al4X The isotope dilution technique is also employed for species analysis in biological systems,46 e.g., for the determination of mercury species in tuna material,54 or in aquatic systems using cold vapour ICP-MS.55... 

Inorganic pigments and lakes (organic dyes bonded to an inorganic support) can be recognized by the ratio of elements in their composition, making elemental analysis an important tool in their identification. EDS may facilitate an initial qualitative analysis, but quantitative analysis and the detection of trace elements are needed to identify the inorganic colorant components. Due to sample size restrictions, the methods that can be employed are limited. The techniques of inductively-coupled plasma mass spectrometry (ICP-MS), ICP-optical emission spectroscopy (ICP-OES), and laser ablation ICP-MS are described in the literature (56). 

This bias in lead analysis was observed for all the methods used by laboratories atomic absorption (flame and furnace), ICP (optical and MS), and other methods, as shown in Fig. 9. This bias was not observed for cadmium, and means of the different methods were very close to the reference value. 

Spray Chambers. Spray chambers [14] were designed mostly empirically for use with conventional pneumatic nebulizers during the development of ICP optical emission spectrometry. The main purpose of the spray chamber was thought to be to remove large droplets that would not have sufficient time to be completely vaporized during their 1- to 2-msec travel in the plasma, although what... 

Two different kinds of direct injection nebulizers are available commercially. The total consumption nebulizer was developed by Greenfield et al. [36] for ICP optical emission spectrometry. The concept for the Cetac direct injection nebulizer (DIN) was developed by Fassel, Houk, and coworkers [35,37]. It has a narrow sample-carrying capillary [30-50 xm inner diameter (i.d.), 0.5 to 1 m long] that extends slightly past the nebulizer gas tube. A second, auxiliary or makeup, nebulizer gas is introduced through another concentric tube outside the nebulizer gas tube. A gas displacement pump (up to 1500 psi) or HPLC pump is used to deliver the sample to the nebulizer through the long, narrow capillary. 

When compared with optical spectrometric techniques of elemental analysis, the techniques based on mass spectrometry provide an increase in sensitivity and in analytical working range of some orders of magnitude. For instance, the detection limits with ICP-MS are three orders of magnitude better than ICP-optical emission spectrometry (ICP-OES). Figure 1.45 shows the maximum sensitivity obtained for the different elements, using an ICP-MS coupling with a quadrupole. 

International Organization for Standardization ISO 10540-3, Animal and Vegetable Fats and Oils - Determination of Phosphorus Content - Part 3 Method Using Inductively Coupled Plasma (ICP) Optical Emission Spectroscopy (2002)... 

Fig. 98. ICP-optical emission spectrometer, (a) gas supply, (b) sampler, (c) peristallic pump, (d) nebulizer, (e) nebulization chamber, (f) hf generator, (g) ICP torch, (h) spectral apparatus, data acquisition, data processing.

Fig. 99. Volatilization of dry solution aliquots from a graphite boat evaporation system coupled to a simultaneous ICP optical emission spectrometer at different heating currents [34],...

To study the influence of chemical impurities on labelhng yields of DOTATATE, a solution of °Y or Lu was added to 50 mL of 0.4M sodium acetate containing 10 gg of DOTATATE and 50 mg/mL of ascorbic acid (pH4.5) to obtain a DOTATATE to radionuclide molar ratio of about 20. These solutions were spiked with varying quantities of metallic contaminants (e.g. Ca, Cu, Cd, Fe, Zn). The quantities of metal cations were adjusted to obtain metal to radiometal molar ratios ranging from 1 to 100. The concentration of each analyte was verified by ICP optical emission spectrometry. The reaction mixture was incubated at 95°C for 25 min. Each point was tested in duplicate. 

The cerium and titanium oxide contents were determined by inductively coupled plasma (ICP) optical emission spectroscopy (Perkin-Elmer Optima 3300DV) of dissolution of the ground catalysts in acid solutions. The composition of the powder samples and monolithic supports are shown in Tables la) and 2 respectively. 

Today, analyses of bulk fossil chemistry are largely conducted by inductively coupled plasma (ICP) atomic emission spectrometry (AES), ICP mass spectrometry (MS) or ICP optical emission spectrometry (OES) techniques (e.g. Rosenthal et al. 1999 DeVilliers et al. 2002 Green et al. 2003). These techniques permit rapid and precise (c. 1% for many elements) measurement of a number of chemical constituents simultaneously. ICP-MS offers higher sensitivities than AES and OES, enabling measurement of more elements and smaller sample sizes. 

At the end of the deposition process some of the support material was stuck to the side of the inner SS cup, while most of the powder (-70-95%) was freely tumbling. In order to collect the powder, the inner SS cup was simply removed and inverted onto a piece of weighing paper. The powder stuck to the side remained in the cup and was not used for the subsequent work. Precious metal loading was determined using a Thermo Jarrell Ash IRIS Inductively Coupled Plasma (ICP) Optical Emission Spectrometer using procedures described previously.[l]... 

Yttrium was found to be effective for signal compensation in the detection of boron and titanium in human blood using axial-view ICP optical emission spectrometry (Garavaglia et al. 2002). 

In general, detection limits with the KiP source are contparable to or better thait other atomic spectral procedures. Table lO-.f compares detection limits for Several of these methods. Note that more elements can be detected at levels of 10 ppb or less with plasma excitation than with other emission or absttrplion melhods. As we shall see in Chapter 11, the ICP coupled with mass spectrontetrie detection improves detection limits by two to live orders of magnitude for many elements and is thus strong competition for ICP optical emission spectroscopy. 

Figure 11-17 compares detection limits for iCPMS with those for ICP optical emission spectroscopy (ICP-OES) and those for electrothermal atomic absorption spectroscopy (ETA AS) for selected elements. These data arc typical for most other elements in the periodic table. Generally, detection limits with mass spectromeiric detection range from 0.02 to 0.7 ppb wilh the majority of elements in the range of 0.02 to 0.1 ppb. 

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