Fisons System

Application developed by using a Fisons GC 8000 chi omatogi aph where the two columns were installed and coupled via a moving capillary stream switching (MCSS) system. The chi omatogi aph was equiped with a flame-ionization detector on the MCSS system outlet and a Flame-photometric detector on the main column outlet, and a split/splitless injector. 

Electrospray (ES) mass spectrometry was carried out with a Fisons platform quadrupole mass specfrometer coupled fo a VG Masslynx data system. The samples were introduced into the source by direct injection via a valve loop system. Loop injection was accomplished with a Rheodyne 7125 injector valve, placing a 10-pl loop in the acetoni-trile/water stream. 

Table 5.3 sets out the advantages and disadvantages of the batch and continuous flow techniques. The introduction of continuous-flow hydride/vapour-generation has substantially advanced the value and acceptance of the technique for trace elemental analysis. Appfied Research Laboratories (now part of Fisons Elemental), P.S. Analytical and Varian have all introduced continuous-flow hydride/vapour-generation systems, whilst Perkin Ehner has used the flow injection modification to automate the techniques with their instrumentation. 

The specific surface area (ssa) of the solids (m g ) obtained after hydrolysis and drying at various temperatures was measured routinely by multi-point BET method at 77K by N2 adsorption in a Fisons Sorptomatic 1900 system. From these isotherms the BET ssa s were determined and the corresponding pore size distribution was also found. Typical results including the adsorption-desorption isotherms as well as the corresponding pore size distributions are shown in Fig.2... 

For TGA, a Setaram TGA-DTA 92 apparatus was used. Alternatively, a home-built apparatus was employed for TPD-MS. GC analysis was on a Chrompack CP-Sil-5 column, eventually coupled to a Fisons mass spectrometer. ESR spectra were recorded with a Bruker ESP-300 and a TE104 cavity at temperatures between 130 and 300 K. N2 sorption experiments were performed with an Omnisorp-100 instrument. The t-plot method was applied for the analysis of the pore volume. Solid state NMR spectra were recorded using a Bruker MSL 400 spectrometer at a resonance frequency of 100.61 MHz. Cross polarization was optimized with glycine as a reference. For the measurement of liquid samples, a Bruker AMX 300 system was used, operating at 300.13 and 75.47 MHz for iH and C, respectively. 

The experimental apparatus required to perform UK experiments is relatively simple (Figure 1). The two isotopic feeds are routed via a four-way valve to either a vent or the reactor. Their flow rates are set as closely as possible using standard mass flow controllers. The pressures of the two gas streams are then equalised using a differential pressure transducer and fine needle valve at the vent outlet. The reactor effluent is monitored continuously by a quadmpole mass spectrometer (Fisons Instruments GasLab 300) via a capillary sampling system. 

Fisons introduced the first DPI with the capsule-based Spinhaler . This was followed by a number of other capsule devices and then by unit dose blisters and multidose systems. DPIs are very diverse in their design and operation, since each product manufacturer has developed their own proprietary devices for their own drugs. 

Confirmation of peak identity was accomplished through the use of a Fisons (Danvers, MA) VO Platform II mass spectrometer connected to a VG Mass Lynx data system. The system was operated in the negative ion electrospray mode. The ion source temperature was set at 150°C while the cone voltage was -20V The ID LC conditions were identical to those obtained off-line except that a Varian W12 HPLC (Fernando, CA) was used along with a Varian 9050 UV-Vis detector... 

A total of 100 p of the sample is allowed to equilibrate with 300 mbar of CO2 of known content for 10 hr at 25°C in a VG ISOPREP-18 H2O-CO2 equilibration system (Fisons Instruments, Inc., 32 Conunerce Center, Danvers, MA 019 ). At the end of the equilibration, the CO2 is allowed to expand into a VG PRISM gas-isotope-ratio mass spectrometer system (Fisons Instruments, Inc.) for abundance measurement (Wong et al., 1987). 

Fisons original biological and chemical records system was set up in 1973 on a remote ICL computer and was subject to the hardware and software limitations of the time. Results were recorded by biologists on datasheets and largely in free format. Some codes were added by information scientists before the data was sent for input. Chemical structures were stored as Wiswesser Line Notations (WLN). 

We had previously organised a number of ORAC training courses, conducted by the experts at Leeds, and these served as OSAC courses for many of our chemists. However, we backed them up with a series of short OSAC courses aimed at explaining the conventions used in our file and one or two traps for the unwary. We have no systematic data but anecdotal evidence suggests that the system has been very well accepted by Fisons chemists. 

The authors acknowledge the collaboration between Polyma Laboratories, Thomal Sdences Division (now Rheometric Scimtific) and Fisons (the STA-MS System) and with BioRad (the TGA and STA-FTIR systmns). In particular the he of David Compton, Paul Nicholas and Paul Larc is gratdiilly acknowledged. 

Coft fison of primary system controt and protection actions... 

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