ICPAE emission mass spectrometry

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). 

Ultraviolet-visible (UV-Vis) spectrophotometric detectors are used to monitor chromatographic separations. However, this type of detection offers very little specificity. Element specific detectors are much more useful and important. Atomic absorption spectrometry (AAS), inductively coupled plasma-atomic emission spectroscopy (ICPAES) and inductively coupled plasma-mass spectrometry (ICP-MS) are often used in current studies. The highest sensitivity is achieved by graphite furnace-AAS and ICP-MS. The former is used off-line while the latter is coupled to the chromatographic column and is used on-line . 

These methods include X-ray fluorescence spectrometry (XRF), inductively coupled plasma mass spectrometry (ICPMS), inductively coupled plasma atomic emission spectrometry (ICPAES), and atomic absorption spectrometry (AAS) (Welz and Sperling 1999) the respective detection limits of these methods are summarized in Table 19.1. Also listed are the detection limits for the metallochromic ligand complexes separated by reverse phase-high-per-formance liquid chromatography (RP-HPLC). These ligands include 4-(2-pyridyla-... 

Detection limits are presented for 61 elements by ten analytical determinative methods FAAS flame atomic absorption spectrometry ETAAS electrothermal atomization atomic absorption spectrometry HGAAS hydride generation atomic absorption spectrometry including CVAAS cold vapor atomic absorption spectrometry for Hg ICPAES(PN) inductively coupled plasma atomic emission spectrometry utilizing a pneumatic nebulizer ICPAES(USN) inductively coupled plasma atomic emission spectrometry utilizing an ultrasonic nebulizer ICPMS inductively coupled plasma mass spectrometry Voltammetry TXRF total reflection X-ray fluorescence spectrometry INAA instrumental activation neutron analysis RNAA radiochemical separation neutron activation analysis also defined in list of acronyms. 

A very recent volume edited by Berthed (2002) is on countercurrent chromatography - the support-free liquid stationary phase. Ebdon et al. (1987) review directly coupled liquid chromatogramphy-atomic spectroscopy. The review by Uden (1995) on element-specific chromatographic detection by atomic absorption, plasma atomic emission and plasma mass spectrometry covers the principles and applications of contemporary methods of element selective chromatographic detection utilizing AA, AES and MS. Flame and furnace are considered for GC and HPLC, while MIP emission is considered for GC and ICPAES for HPLC. Combinations of GC and HPLC with both MIPAES and ICPAES are covered and supercritical fluid chromatographic (SFC) and field flow fractionation (FFF) are also considered. 

GFAAS graphite furnace atomic absorption spectrometry ICPAES inductively coupled plasma atomic emission spectrometry ICPMS inductively coupled plasma mass spectrometry INAA instrumental neutron activation analysis... 

Direct determination after dilution with water can be used for the determination of tin in canned fruit juices [102]. For biological media, samples are decomposed by a nitric-perchloric acid mixture and analyzed after dilution by a standard addition technique. Tin hydride reduced by a sodium borohydride and trichloracetic acid solution are introduced into ICPAES after separation of liquid and excess hydrogen by an improved gas-liquid separator. Emission intensity is measured at 189.989 nm. The detection limit is 30 pg/mL [103]. Lower detection limits can be achieved by using ICPAES-mass spectrometry, [104]. 

We consider the determination of the concentration of elements in various materials studied in agricultural and environmental applications, by the use of the following methods atomic absorption spectroscopy (AAS) using a flame (FAAS) or a graphite furnace (GFAAS) as an atom cell inductively coupled plasma atomic emission spectroscopy (ICPAES) inductively coupled plasma mass spectrometry (ICPMS) and X-ray fluorescence (XRF). The analytical characteristics of the methods as normally practised are compared with the requirements of fitness for purpose in the examination of soils and sediments, waters, dusts and air particulates, and animal and plant tissue. However, there are numerous specialized techniques that cannot be included here. 

Determination of uranium in soil samples can be carried out by nondestructive analysis (NDA) methods that do not require separation of uranium (needed for alpha spectrometry or TIMS) or even digestion of the soil for analysis by ICPMS, ICPAES, or some other spectroscopic methods. These NDA methods can be divided into passive techniques that utilize the natural radioactive mission (gamma and x-ray) of the uranium and progeny radionuclides or active methods where neutrons or electromagnetic radiation are used to excite the uranium and the resultant emissions (gamma, x-rays, or neutrons) are monitored. In many cases, sample preparation is simpler for these nondestructive methods but the requiranent of a neutron source (from a nuclear reactor in many cases) or a radioactive source (x-ray or gamma) and relatively complex calibration and data interpretation procedures make the use of these techniques competitive only in some applications. In addition, the detection limits are usually inferior to the mass spectrometric techniques and the isotopic composition is not readily obtainable. 

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