Mass spectrometry samples INDEX

In the first step, we were able to separate this penta derivative by preparative H.P.L.C. and we subsequently treated it with an excess of propyleneimine in order to reach the required hexasubstituted compound. Under such conditions, we succeeded in preparing a N3P3(MeAz)g real sample (free of chlorine, as demonstrated by neutron activation analysis) identified by mass spectrometry (Fig. 32) and by P nmr (Fig. 33) (6 = — 36 ppm with 85 % HjPO as standard, to be compared with 8(N3P3Azg) = --37 ppm). The refractive index of this sample, n = 1.4825, appeared to be significantly far from Ratz s value. 

The samples were analyzed by capillary gas chromatography and gas chromatography/mass spectrometry (GC/MS). Identifications were verified by comparing the component s mass spectmm and experimental retention index (I) with that of an authentic reference standard. The retention system proposed by Kovats (12) was utilized. When standards were not available the identifications were considered tentative. 

There exist several different detectors suitable for detecting the analytes after the chromatographic separation. Some commercial detectors used in LC are ultraviolet (UV) detectors, fluorescence detektors, electrochemical detectors, refractive index (RI) detectors and mass spectrometry (MS) detectors. The choice of detector depends on the sample and the purpose of the analysis. 

Spectroscopic techniques are popular as a means of detection on chips. Examples include the determination of flavins and DNA by fluorescence. Spectrophotometric techniques are often used for biological samples . Mass spectrometry has also been used. Benetton et al. coupled electrospray ionisation MS to a chip while Sillon et al. developed a low cost mass spectrometer which incorporated the ionisation chamber, filter and detector on the chip. A fibre optic coupler has been developed as a detector. The dual optical fibre configuration (one transmitting, one receiving, (Eigure 10.5)) in the chip forms the microchannel as well as the detector itself and measures refractive index changes but can also be used to measure absorbance . 

The main purpose of the detector in a field-flow fractionation (FFF) system is to quantitatively determine particle number, volume, or mass concentrations in the FFF size-sorted fractions. Consequently, a number, volume, or mass dependent size distribution of the sample can be derived from detection systems applied to FFF [e.g., (UV-Vis) fluorescence, refractive index, inductively coupled plasma ionization mass spectrometry (ICPMS)]. Further, on-line light scattering detectors can provide additional size and molecular weight distributions of the sample. 

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