Sample ion pairs

Flowing FS-MMLLE with on-line hyphenation to FtPLC has also been investigated. Sandahl et al. were the first to interface FS-MMLLE with reversed-phase HPLC for the on-line extraction of methyl-thiophanate in natural water, obtaining an LOD of 0.5 pg L-1.89 Also, a parallel FS-SLM and FS-MMLLE design was coupled on-line to reverse-phase HPLC for the extraction of methyl-thiophanate (by MMLLE) and its metabolites (by SLM) in natural water.90 In addition, on-line coupling of FS-MMLLE and normal-phase HPLC has been successfully applied in the determination of vinclozolin (Ee =118 and LOD = 1 pg I. ) in surface water91 and of in-sample ion-paired cationic surfactants (Ee > 250 and LOD = 0.7-5 ug L-1) in river water and wastewater samples.92... 

In reversed-phase IPC, maximum k values are obtained at intermediate values of pH, where the sample compounds are completely ionized and ion-pair formation is at a maximum. As the pH of the mobile phase is lowered, sample anions begin to form the un-ionized acids HA, leading to a smaller number of sample ion pairs in the stationary phase. Adds are usually separated at a pH of 7-9, whereas bases are separated at a pH of 1-6. 

For chromium speciation with ICP-DRC-MS analysis, ammonia was selected as the reaction gas. Airborne Cr(VI) was separated from Cr(III) using a silica gel determination of ultratrace quantities of Cr(VI) was possible using preconcentration via complexation and ICP-DRC-MS. For aqueous samples, ion pair reversed phase HPLC was applied. ... 

An alternative way of eliminating water in the RPLC eluent is to introduce an SPE trapping column after the LC column (88, 99). After a post-column addition of water (to prevent breakthrough of the less retained compounds), the fraction that elutes from the RPLC column is trapped on to a short-column which is usually packed with polymeric sorbent. This system can use mobile phases containing salts, buffers or ion-pair reagents which can not be introduced directly into the GC unit. This system has been successfully applied, for example, to the analysis of polycyclic aromatic hydrocarbons (PAHs) in water samples (99). 

A sensitive determination of alkanesulfonates combines RP-HPLC with an on-line derivatization procedure using fluorescent ion pairs followed by an online sandwich-type phase separation with chloroform as the solvent. The ion pairs are detected by fluorescence. With l-cyano-[2-(2-trimethylammonio)-ethyl]benz(/)isoindole as a fluorescent cationic dye a quantification limit for anionic surfactants including alkanesulfonates of less than 1 pg/L per compound for a 2.5-L water sample is established [30,31]. 

To determine secondary alkanesulfonates in sewage wastewaters, solid phase extraction (SPE) and a single-step procedure which combines elution and injection port derivatization for analysis with GC-MS were developed [36]. Again a tetrabutylammonium ion pair reagent was employed both to elute the secondary alkanesulfonates as their ion pairs from CI8-bonded silica disks and to derivatize sulfonate ion pairs under GC injection port conditions. Secondary alkanesulfonates were effectively recovered from samples of raw sewage (>92%) and from primary (>98%) and secondary (>85%) effluents. No... 

Factors may be classified as quantitative when they take particular values, e.g. concentration or temperature, or qualitative when their presence or absence is of interest. As mentioned previously, for an LC-MS experiment the factors could include the composition of the mobile phase employed, its pH and flow rate [3], the nature and concentration of any mobile-phase additive, e.g. buffer or ion-pair reagent, the make-up of the solution in which the sample is injected [4], the ionization technique, spray voltage for electrospray, nebulizer temperature for APCI, nebulizing gas pressure, mass spectrometer source temperature, cone voltage in the mass spectrometer source, and the nature and pressure of gas in the collision cell if MS-MS is employed. For quantification, the assessment of results is likely to be on the basis of the selectivity and sensitivity of the analysis, i.e. the chromatographic separation and the maximum production of molecular species or product ions if MS-MS is employed. 

Direct measurement of adsorptive stripping voltaimnetric peaks using HMDE 0.60 V and accumulation potential of -0.40V Dilution in phosphate buffer and water, analyzed in Vis region Ion pair formation with octadecyltrimethylammonium bromide at pH 5.6, extraction of ion pair into n-butanol Sample solution mixed with 1 M HCl, ethanol and purification on Sephadex DEAE 25 gel, gel beads are filtered off, packed into 1 nun cell and absorbance measured... 

Figure 4.27 Flow chart for coluwi selection based on sample type (m - molecular weight). PLC precipitation-liquid chromatography SEC = size-exclusion chromatography lEC - ion-exchange chromatography HIC hydrophobic interaction chromatography LSC liquid-solid chromatography RPC - reversed-phase liquid chromatography BPC (polar) bonded-phase chromatography and IPC - ion-pair chromatography.

An inductively coupled plasma formed by passing argon through a quartz torch is widely used for the mass spectroscopic analysis of metal compounds separated by online HPLC.6 Samples are nebulized on introduction into the interface. Plasma impact evaporates solvent, and atomizes and ionizes the analyte. Applications include separation of organoarsenic compounds on ion-pairing F4PLC and vanadium species on cation exchange. 

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