Limit plasma mass spectrometry

The complex of the following destmctive and nondestmctive analytical methods was used for studying the composition of sponges inductively coupled plasma mass-spectrometry (ICP-MS), X-ray fluorescence (XRF), electron probe microanalysis (EPMA), and atomic absorption spectrometry (AAS). Techniques of sample preparation were developed for each method and their metrological characteristics were defined. Relative standard deviations for all the elements did not exceed 0.25 within detection limit. The accuracy of techniques elaborated was checked with the method of additions and control methods of analysis. 

Inductively coupled plasma-mass spectrometry (ICP-MS) is a multielement analytical method with detection limits which are, for many trace elements, including the rare earth elements, better than those of most conventional techniques. With increasing availability of ICP-MS instalments in geological laboratories this method has been established as the most prominent technique for the determination of a large number of minor and trace elements in geological samples. 

In modern times, most analyses are performed on an analytical instrument for, e.g., gas chromatography (GC), high-performance liquid chromatography (HPLC), ultra-violet/visible (UV) or infrared (IR) spectrophotometry, atomic absorption spectrometry, inductively coupled plasma mass spectrometry (ICP-MS), mass spectrometry. Each of these instruments has a limitation on the amount of an analyte that they can detect. This limitation can be expressed as the IDL, which may be defined as the smallest amount of an analyte that can be reliably detected or differentiated from the background on an instrument. 

ICP-MS (inductively coupled plasma mass spectrometry) is frequently used for determining ultratrace amounts of technetium [9]. In spite of the high cost of the equipment, this detection method is far superior to other radiometric methods as regards sensitivity. When a double focussing high-resolution system is used (HR-ICP-MS) and an ultrasonic nebulizer is introduced [10], the detection limit is in the order 0.002 mBq. The ICP-MS method has been successfully applied to the determination of environmental "Tc as well as to other long-lived radionuclides of neptunium and plutonium in the environment. 

The corrosion of antimony electrodes was also measured using ICP-MS (inductively coupled plasma mass spectrometry) for dissolved antimony in vivo [156], After the electrodes were inserted in the plasma, the antimony concentration showed a linear rise with time at a rate approximately of 94 j,g/L/h (r2 = 0.997). Although the projected antimony concentration is lower than the safe limit, accumulation of dissolved antimony and localized toxic effects in tissue may prevent the antimony electrode from long-term implantable applications. 

At present, inductively coupled plasma mass spectrometry provides a unique, powerful alternative for the determination of rare earths in natural samples [638,639]. Nevertheless, its application to the determination of rare earths at ultratrace concentration level in seawater is limited, because highly saline samples can cause both spectral interferences and matrix effects [640]. Therefore, a separation of the matrix components and preconcentration of the analytes are prerequisites. To achieve this goal, many preconcentration techniques have been used, including coprecipitation with... 

Michalke, B. (2005). Capillary electrophoresis-inductively coupled plasma-mass spectrometry a report on technical principles and problem solutions, potential, and limitations of this technology as well as on examples of application. Electrophoresis 26, 1584—1597. 

Soil samples were wet sieved into (a) 2-4 mm, (b) 1-2 mm, (c) 0.5-1 mm, (d) 250-500 i m, (e) 125-250 am, (f) 63-125 j,m and (g) <63 j.m fractions. A ferruginous/magnetic fraction (m) was also prepared from the 2-4 mm fraction. Soil fractions were crushed, digested with HNO3/HCI/HF/HCIO4 and then analysed by Inductively Coupled Plasma Optical Emission Spectrometry (ICP-OES) for Al, Ca, Cu, Fe, K, Mn, Na, P, S and Zn. Inductively Coupled Plasma Mass Spectrometry (ICP-MS) was used to determine Ag, As, Cd, Pb and Sb because of the lower detection limits by this method. The mineralogy of selected samples was determined by qualitative X-ray diffractometry. 

Cations were determined by high-resolution inductively coupled plasma-mass spectrometry (HR-ICPMS), relatively new analytical instrumentation with a large dynamic range and detection limits (DLs) in the low (1-50) parts per trillion (ppt) for most elements. The exceedingly low DLs allow for recognition of elemental variations that are not possible with traditional analytical methods for water. 

Early investigations on Mg isotope variations have been limited by an uncertainty of 1 to 2%o. Catanzaro and Murphy (1966) for instance concluded that terrestrial Mg isotope variations are restricted to a few %o. The introduction of multicoUector-inductively coupled-plasma mass spectrometry (MC-ICP-MS) increased the precision by one order of magnitude and has initiated a new search of natural isotope variations (Galy et al. 2001, 2002). These authors obtained an overall 4%c variation in 5 Mg. 

In 1C, the election-detection mode is the one based on conductivity measurements of solutions in which the ionic load of the eluent is low, either due to the use of eluents of low specific conductivity, or due to the chemical suppression of the eluent conductivity achieved by proper devices (see further). Nevertheless, there are applications in which this kind of detection is not applicable, e.g., for species with low specific conductivity or for species (metals) that can precipitate during the classical detection with suppression. Among the techniques that can be used as an alternative to conductometric detection, spectrophotometry, amperometry, and spectroscopy (atomic absorption, AA, atomic emission, AE) or spectrometry (inductively coupled plasma-mass spectrometry, ICP-MS, and MS) are those most widely used. Hence, the wide number of techniques available, together with the improvement of stationary phase technology, makes it possible to widen the spectrum of substances analyzable by 1C and to achieve extremely low detection limits. 

Figure 21-24 Flame, furnace, and inductively coupled plasma emission and inductively coupled plasma—mass spectrometry detection limils (ng/g = ppb) with instruments from GBC Scientific Equipment, Australia. [Flame, furnace. ICP from R. J. Gill. Am. Lab. November 1993, 24F. ICP-MS from T. T. Nham, Am. Lab. August 1998. 17A Data for Ct Br, and l are from reference 14.] Accurate quantitative analysis requires concentrations 10-100 times greater than the detection limit.

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). 

In the test method, the coal or coke to be analyzed is ashed under controlled conditions, digested by a mixture of aqua regia and hydrofluoric acid, and finally dissolved in 1% nitric acid. The concentration of individual trace elements is determined by either inductively coupled plasma-atomic emission spectrometry (ICPAES) or inductively coupled plasma-mass spectrometry (ICPMS). Selected elements that occur at concentrations below the detection limits of ICPAES can be analyzed quantitatively by graphite furnace atomic absorption spectrometry (GFAA). 

Inductively coupled plasma mass spectrometry has been used for the analysis of uranium. However, the technique suffers from spectral interferences and it has relatively poor detection limits. 

Inductively coupled plasma mass spectrometry is a relatively new technique for elemental analysis and has superior limits of detection over optical methods. Also, this technique has an order of magnitude better detection limit than that obtained by the conventional fluorometric method. Uranium has many stable and unstable isotopes but 238U has the largest percentage abundance (99.274%). 

Boomer and Powell [242] have developed an analytical technique using inductively coupled plasma mass spectrometry to estimate the concentration of uranium in a variety of environmental samples including soil. The lower limit for quantitation is 0.1 ng/ml. Calibration is linear from the low limit to 100 ng/ml. Precision, accuracy and a quality control protocol were established. Results are compared with those obtained by the conventional fluorometric method. 

The determination of 129I in low-level radioactive waste was accomplished by radioactive instrumental neutron activation analysis [3]. A different group reported the determination of both 129I and 127I by neutron activation analysis and inductively coupled plasma mass spectrometry [4]. The method was very rapid - a sample could be analysed in three minutes. However, interference from 129Xe resulted in limited sensitivity for 129I detection. 

Inductively coupled plasma-mass spectrometry (ICP-MS) is a powerful technique that uses an inductively coupled plasma as an ion source and a mass spectrometer as an ion analyzer. It can measure the presence of more than 75 elements in a single scan, and can achieve detection limits down to parts per trillion (ppt) levels for many elements—levels that are two or three orders of magnitude lower than those obtained by ICP-AES (Keeler 1991). It is more expensive than ICP-AES and requires more highly skilled technical operation. Aluminum levels in urine and saliva were detected down to 0.02 g/mL and in blood serum to 0.001 g/mL using ICP-MS (Ward 1989). Speciation studies have employed ICP-MS as a detector for aluminum in tissue fractions separated by size-exclusion chromatography (SEC) with detection limits of 0.04 g/g in femur, kidney and brain (Owen et al. 1994). 

IATA ICAP ICP ICP-AES ICP-MS ICV ID IDL IDW ISO International Air Transportation Association inductively coupled argon plasma inductively coupled plasma inductively coupled plasma-atomic emission spectrometry inductively coupled plasma-mass spectrometry initial calibration verification identification instrument detection limit investigation-derived waste International Standardization Organization... 

If the reference materials are pure substances and can be specified on the microscopic level, then they represent the unit amount of substance. Because there are no absolute pure substances the representation is in all cases an approximation. The degree of approximation is given by the accuracy of the contents of the main component. In case of pure elements, e.g. metals Fe, Cu, Zn the determination of the main component by coulometry is limited by an uncertainty of 0.01%. The determination of all impurities needs completeness and requires a great deal of analytical equipment. However, a combination of inductively coupled plasma-mass spectrometry (ICP-MS), atomic absorption spectrometry (AAS) and isotope dilution mass spectrometry (ID-MS) covering all elements of the periodic table allows a decrease of total uncertainty to 0.0032% (Cu, see Fig. 8). 

Shen et al. [262] evaluated indirectly coupled plasma mass spectrometry as an element detector for the supercritical fluid chromatography of organotin compounds in water. Detection limits of 0.04 and 0.047pg absolute were obtained, respectively, for tetrabutyltin and tetraphenyltin. 

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