Adsorbants solid phase extraction

Solid-Phase Extractions In a solid-phase extraction the sample is passed through a cartridge containing solid particulates that serve as the adsorbent material. For liquid samples the solid adsorbent is isolated in either a disk cartridge or a column (Figure 7.17). The choice of adsorbent is determined by the properties of the species being retained and the matrix in which it is found. Representative solid adsorbents... 

Selected Adsorbents for Solid-Phase Extraction of Liquid Samples... 

In a solid-phase extraction the analytes are first extracted from their solution matrix into a solid adsorbent. After washing to remove impurities, the analytes are removed from the adsorbent with a suitable solvent. Alternatively, the extraction can be carried out using a Soxhlet extractor. 

A solid-phase extraction in which the solid adsorbent is coated on a fused-silica fiber held within a syringe needle. 

The solid phase extraction cartridge (SPEC) is another somewhat vainglorious name given to a short inert plastic tube packed with an adsorbent, usually a reversed phase or an ion exchange resin. The particle size of the packing is often significantly larger than that used... 

A cleanup procedure is usually carried out to remove co-extracted matrix components that may interfere in the chromatographic analysis or be detrimental to the analytical instrument. The cleanup procedure is dependent on the nature of the analyte, the type of sample to be analyzed, and the selectivity and sensitivity of the analytical instrument used in the analysis. Preliminary purification of the sample extracts prior to chromatographic separation involves liquid-liquid partitioning and/or solid-phase extraction (SPE) using charcoal/Celite, Elorisil, carbon black, silica, or aminopropyl-silica based adsorbents or gel permeation chromatography (GPC). 

Fig. 18.1 Systems used to absorb aroma compounds from samples for analytical purposes, a Traps loaded with various adsorbents [4]. b Solid-phase extraction (disk in a holder assembly) [5]. c Solid-phase microextraction (coated needle inserted in sample) [5]. d Twister (1 -cm length) [4]. (Courtesy of GERSTEL GmbH and Co. KG)...

A fourth conclusion, based on the advantages of the use of solid adsorbents, is the gradual replacement of solvent extractions with solid phase extractions. The movement toward this replacement is already evidenced by the commercial availability of several different cartridges of bonded phases and high-surface-area synthetic polymers. 

Figure 28-16 shows steps in the solid-phase extraction of 10 ng/mL of steroids from urine. First, a syringe containing 1 mL of C 8-silica is conditioned with 2 mL of methanol to remove adsorbed organic material (Figure 28-16a). Then the column is washed with 2 mL of water. When the 10-mL urine sample is applied, nonpolar components adhere to the C18-silica, and polar components pass through (Figure 28-16b). The column is then rinsed with 4 mL of 25 mM borate buffer at pH 8 to remove polar substances (Figure 28-16c). Then rinses with 4 mL of 40 vol% methanol/60% water and 4 mL of 20% acetone/80% water remove less polar substances (Figure 28-l6d). Finally, elution with two 0.5-mL aliquots of 73% methanol/27% water washes the steroids from the column (Figure 28-16e).

Besides solid-phase extraction, column chromatography is also often used for cleanup and purification of polyphenolics from plant material. Ionic adsorbants (polyvinylpyrrolidone or PVP, polyamides, and Sephadex LH-20) and Amberlite XAD-2 resin have been used to isolate and purify polyphenolics from crude extracts. For the separation of polyphenolics from plant material, column chromatography using Sephadex LH-20, a gel-filtration matrix, is often used with various eluting solvents (Park and Lee, 1996). The most widely used solvents for column chromatography are aqueous methanol and aqueous ethanol. 

Solvent extraction in combination with TD-GC-FID gives the opportunity to concentrate the extract directly on the adsorbent tube (solid phase extraction) by injection of the sample extract and purge off the solvent with for example, helium. Methanol extracts of house dust can be concentrated on adsorbent tubes by injecting up to 50 jllI and analyze the tubes by TD-GC (Kofoed-Sorensen and Clausen, 2004). 

The selection of adsorbent packing material is based on the polarity of pollutants to be analyzed. The nonpolar hydrophobic adsorbents retain the nonpolar analytes and allow the polar substances to pass through the column. The hydrophilic adsorbents adsorb the polar components, allowing the nonpolar materials to pass through. Various stationary phases for solid phase extraction are listed below in Table 1.5.1. 

Solid-phase extractions (SPE), in which DOM is selectively concentrated on a solid-phase extractant such as XAD-2 resin or Ci8 adsorbent. In these methods, both inorganic solutes and water are removed concurrently, and a suitable solvent is used to desorb the concentrated, desalted DOM from the solid-phase extractant. In principle, all inorganic solutes may be removed by SPE. 

After several decades of research, fundamental aspects of the chemical composition and structure of marine organic matter remain elusive. Advances in the chemical characterization of marine organic matter are, in large part, dependent on the development of quantitative methods for its concentration and isolation from seawater. Each of the major methods currently used for the isolation of marine DOM recovers around one-third of the DOM in seawater (solid-phase extractions, using XAD resins or C18 adsorbents, and ultrafiltration). A coupled reverse osmosis-electrodi-alysis method has recently been used to recover an average of 75% 12% of marine DOM from 16 seawater samples however, the method has emerged too recently to have been well tested at this time. 

Analytes may accumulate in the sorption phase either by adsorption onto the surface of solid sorbent materials or by absorption in absorbent liquids or polymers that behave like subcooled liquids.The advantage of solid adsorbents is the potential to select materials with a high affinity and selectivity for target analytes. However, the sorption capacity of adsorbents is usually limited, and the description of adsorption/desorption kinetics of analytes to adsorbents is complex. Typically, the adsorbent materials used in passive samplers are similar to those used in solid-phase extraction techniques. 

A promising solid-phase extraction adsorbent for metals and more particularly As is nanometer Ti02 material and immobilized nanometer Ti02.70,71 Both As(III) and As(V), or As(III) alone, were quantitatively absorbed on immobilized nanometer TiOz depending on the pH (for LODs, see Table 7.2). 

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