High trace contaminants, determination

The high-purity water thus produced typically has a conductance of about 0.5 x 10-6fi-1cm-1 (0.5juScm-1) and is suitable for use under the most stringent requirements. It will meet the purity required for trace-element determinations and for operations such as ion chromatography. It must however be borne in mind that such water can readily become contaminated from the vessels in which it is stored, and also by exposure to the atmosphere. For the determination of organic compounds the water should be stored in containers made of resistant glass (e.g. Pyrex), or ideally of fused silica, whereas for inorganic determinations the water is best stored in containers made from polythene or from polypropylene. 

It was generally agreed that any determinations of trace metals carried out on seawater prior to about 1975 are questionable, principally due to the adverse effects of contamination during sampling, which were then little understood and lead to artificially high results. It is only in the past few years that methods of adequate sensitivity have become available for true ultra-trace metal determinations in water. 

The analysis of tetramethylammonium hydroxide (TMAH) solutions manufactured by SACHEM Inc. of Cleburne, Texas, includes the determination of trace elements. These elements cause less-than-optimum performance of integrated circuit boards manufactured by SACHEM s customers that use these solutions in their processes. Alkali and alkaline earth metals (e.g., Li, Na, K, Mg, Ca, and Ba) can reduce the oxide breakdown voltage of the devices. In addition, transition and heavy metal elements (e.g., Ti, Cr, Mn, Fe, Co, Ni, Cu, Zn, Ag, Au, and Pb) can produce higher dark current. Doping elements (e.g., B, Al, Si, P, As, and Sn) can alter the operating characteristics of the devices. In SACHEM s quality control laboratory, ICP coupled to mass spectrometry is used to simultaneously analyze multiple trace elements in one sample in just 1 to 4 min. This ICP-MS instrument is a state-of-the-art instrument that can provide high throughput and low detection Emits at the parts per thousand level. Trace elemental determination at the parts per thousand level must be performed in a clean room so that trace elemental contamination from airborne particles can be minimized. 

There has been considerable interest in the determination of ions at trace levels as, for example, in applications need high-purity water as in semiconductor processing and the determination of trace anions in amine treated waters. For this investigation, we will define "trace" as determinations at or below 1 pg/1 (ppb) levels. The Semiconductor Equipment and Materials International (SEMI) recommended the use of IC for tracking trace ionic contaminants from 0.025 to 0.5 pg/1 [18]. In addition, the Electric Power Research Institute (EPRI) has established IC as the analytical technique for determining of trace level concentrations of sodium, chloride and sulfate down to 0.25 pg/1 in power plant water [19]. 

Today, as a direct solid-state analytical technique, dc GDMS is more frequently applied for multi-element determination of trace contaminants, mostly of high purity metallic bulk samples (or of alloys) especially for process control in industrial laboratories. The capability of GDMS in comparison to GD-OES (glow discharge optical emission spectrometry) is demonstrated in a round robin test for trace and ultratrace analysis on pure copper materials.17 All mass spectrometric laboratories in this round robin test used the GDMS VG 9000 as the instrument, but for several... 

Trace impurities in noble metal nanoclusters, used for the fabrication of highly oriented arrays on crystalline bacterial surface layers on a substrate for future nanoelectronic applications, can influence the material properties.25 Reliable and sensitive analytical methods are required for fast multi-element determination of trace contaminants in small amounts of high purity platinum or palladium nanoclusters, because the physical, electrical and chemical properties of nanoelectronic arrays (thin layered systems or bulk) can be influenced by impurities due to contamination during device production25 The results of impurities in platinum or palladium nanoclusters measured directly by LA-ICP-MS are compared in Figure 9.5. As a quantification procedure, the isotope dilution technique in solution based calibration was developed as discussed in Chapter 6. 

Reliable results on trace elements require precautions to avoid contamination. Concentrations of trace elements determined in lake water are often in ranges similar to those measured in the oceans the requirements for contamination-free sampling are thus similar (25, 26). Teflon-coated Go-Flo samplers were used. They were carefully cleaned with acid (0.01 M HN03) and high-... 

Possible contamination due to atmospheric dust and particle emission attributable to laboratory staff activities (smoking, use of cosmetics, etc.) can be avoided in trace analytical determinations at the pg/kg, pg/L, and pg/m ranges by working under clean-room conditions. A laminar-flow clean bench ensures that particles with a diameter >0.1 pm will be removed with an efficiency of 99.9% through high-efficiency, sub-... 

Zbinden, R, and Andrey, D. (1998). High pressure ashing—Determination of trace element contaminants in food matrices using a robust, routine analytical method for ICP-MS. Af. Spectrosc. 19(6), 214. 

TOF-SIMS can be applied to identify a variety of molecular fragments, originating from various molecular surface contaminations. It also can be used to determine metal trace concentrations at the surface. The use of an additional high current sputter ion source allows the fast erosion of the sample. By continuously probing the surface composition at the actual crater bottom by the analytical primary ion beam, multi element depth profiles in well defined surface areas can be determined. TOF-SIMS has become an indispensable analytical technique in modem microelectronics, in particular for elemental and molecular surface mapping and for multielement shallow depth profiling. 

There are a number of CRMs available for this group of elements in semm and urine (see Table 6.3). The most severe problems with the determination of these trace elements are contamination and loss. Therefore, strict protocols are necessary to prevent these problems. Contamination can be prevented by cleaning thoroughly all used utensils, and the use of highly purified chemicals. Loss is mostly due to exchange between the container walls and can be prevented by working at a pFI<2. 

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