E detectors

In this mode, ions are formed continuously in the ion source (a), but the electrostatic accelerating potential is applied in pulses (b). Thus, a sample of ions is drawn into the drift region (c) with more ions formed in the source. As shown in Figure 26.1, the ions separate according to m/z values (d) and arrive at the detector (e), the ions of largest m/z arriving last. 

Because two detectors are connected simultaneously in GC/MS, it is possible to rule out a detector problem if the erratic result occurs on both detectors (e.g., MS, FID). A poor result at one detector could be associated with a postcolumn splitter or a leak in the transfer line. Once the problem is isolated, the instrument manual is usually a valuable source for information on possible fixes. 

The most widely used molecular weight characterization method has been GPC, which separates compounds based on hydrodynamic volume. State-of-the-art GPC instruments are equipped with a concentration detector (e.g., differential refractometer, UV, and/or IR) in combination with viscosity or light scattering. A viscosity detector provides in-line solution viscosity data at each elution volume, which in combination with a concentration measurement can be converted to specific viscosity. Since the polymer concentration at each elution volume is quite dilute, the specific viscosity is considered a reasonable approximation for the dilute solution s intrinsic viscosity. The plot of log[r]]M versus elution volume (where [) ] is the intrinsic viscosity) provides a universal calibration curve from which absolute molecular weights of a variety of polymers can be obtained. Unfortunately, many reported analyses for phenolic oligomers and resins are simply based on polystyrene standards and only provide relative molecular weights instead of absolute numbers. 

This chapter will concentrate on the very high quality detectors that are needed in scientific imagers and spectrographs, and other applications that require high sensitivity, such as acquisition and guiding, adaptive optics and interferometry. We limit our discussion to focal plane arrays - large two-dimensional arrays of pixels - as opposed to single pixel detectors (e.g., avalanche photodiodes). 

On the other hand, if only specific GC detectors, e.g. the electron capture, nitrogen-phosphorus or flame photometric detectors, are tested, the argument of lack of GC method sensitivity is not acceptable. In most cases mass spectrometric detectors provide the sensitivity and selectivity needed. Unfortunately, tandem mass spectrometry (MS/MS) or MS" detectors for GC are still not widely used in official laboratories, and therefore these techniques are not always accepted for enforcement methods. 

KBr) databases. Quantitative analysis by GC-FUR is complicated by many uncertainties associated with both the chromatography and spectroscopy [196]. Bulk property detectors (e.g. TCD, FID, etc.) can be used for quantitative analysis when mixture components are known, but provide little structural information for unknown mixture components. Both integrated absorbance and Gram-Schmidt vector methods have been used for the quantitative analysis of mixture components in GC-FTIR. 

The main detectors used in AES today are photomultiplier tubes (PMTs), photodiode arrays (PDAs), charge-coupled devices (CCDs), and vidicons, image dissectors, and charge-injection detectors (CIDs). An innovative CCD detector for AES has been described [147]. New developments are the array detector AES. With modem multichannel echelle spectral analysers it is possible to analyse any luminous event (flash, spark, laser-induced plasma, discharge) instantly. Considering the complexity of emission spectra, the importance of spectral resolution cannot be overemphasised. Table 8.25 shows some typical spectral emission lines of some common elements. Atomic plasma emission sources can act as chromatographic detectors, e.g. GC-AED (see Chapter 4). 

HPLC-PDA-MS) are already being used. Although HPLC-NMR-MS provides a very powerful approach for compositional and structural analysis, it by no means represents the limit of what is possible in terms of hyphenation. On-line extraction and the attachment of multiple detectors (e.g. IR, F) make the technique even more powerful. Other analytical laboratories such as TG-DTA-DSC-FTIR, TD-CT/Py/GC-MS/FTIR and HPLC-UV/NMR/IR/MS have been put to work, but do not represent practical solutions for routine polymer/additive analysis. 

ECD (1) Electron-capture detector (2) Electrochemical detector E-SEM, ESEM Environmental scanning electron microscopy... 

Figure 6. Plan of the target preparation facilities consisting of UHV preparation chamber (a), (reactive) ion etching chamber (b), ion etching gun (c), laser (d), photon detector (e), transfer arms (f), Auger system for surface analysis (g), sample manipulator and annealing facility (h), load lock and optical microscope for viewing sample (i), evaporator (j), transmission diffractometer (k), and vacuum tank for main spectrometer (1).

Information density (storage density) Da = Ma / a Dv = Mv/v bit/cm2 bit/cm3 Static detectors, e.g., photographic plate a, v spatial storage unit... 

Information capacity (channel capacity) C = Mpot/1 bit/s Dynamic detectors, e.g., photomultiplier t time... 

Peter R. Bratt, Impurity Germanium and Silicon Infrared Detectors E.H. Pulley, InSb Submillimeter Photoconductive Detectors... 

While most other techniques use a limited amount of detectors (e.g., silica for visible, photomultipliers for UV) and MIR has a small number, NIR uses many types of semiconductors for detectors. The original PbS detectors are still one of the largest used in NIR, however, indium gallium arsenide (InGaAs), indium arsenide (InAs), indium antimonide (InSb), and lead selenide (PbSe) are among the semiconductor combinations used, both cooled and ambient. 

Fig. 7.18. Instrumental arrangement for the measurement of total reflection x-ray fluorescence. The x-rays from the source (A) are allowed to impinge on the sample mounted on a reflector plate (B). Most of the incident radiation bounces off the sample (C), but some results in the production of XRF (D), which is measured by the detector (E).

FIA star 5010 Modular, semi- or fully automatic operation. May be operated with process controller microprocessor. Can be set up in various combinations with 5017 sampler and superflow software which is designed to run on IBM PC/XT computer 60-180 samples h Dialysis for in-line sample preparation and in-line solvent extraction.Thermostat to speed up reactions. Spectrophotometer (400-700nm) or photometer can be connected to any flow through detector, e.g. UV/visible, inductively coupled plasma, atomic absorption spectrometer and ion-selective electrodes... 

Non-specific sum parameter analysis [12,13], which is still used today, failed [14,15] in the analyses of some of these compounds. Chromatographic methods in combination with non-substance specific detectors, e.g. colorimetric and photometric [5] or with substance specific detectors such as IR (infrared spectroscopy), NMR (nuclear magnetic resonance spectroscopy) or MS (mass spectrometry), are applied increasingly nowadays. 

Nowadays, forward geometry instruments are often constructed to be used in combination with an (optional) array detector, e.g., the JEOL HX-110 (EB), the Thermo Finnigan MAT 900 (EB) and the Micromass Autospec (EBE) instruments can be equipped in that way. The array detector is then located at the focus plane of the magnet, but different from the Mattauch-Herzog design it only covers a comparatively small m/z range simultaneously (Chap. 4.8). 

Manufacturers publish their product s performance characteristics as specifications, which are often used by the customer for comparison during the selection process. Table 1 shows the specifications of an Agilent 1100 Series Quaternary Pump, which is quite representative of other high-end analytical pumps. Note pulsation is particularly detrimental to the performance of flow-sensitive detectors (e.g., mass spectrometer, refractive index detector). Differences in dwell volumes and composition accuracy between HPLC systems might cause problems during method transfers. 

CE instrumentation is quite simple (see Chapter 3). A core instrument utilizes a high-voltage power supply (capable of voltages in excess of 30,000 V), capillaries (approximately 25—lOOpm I.D.), buffers to complete the circuit (e.g., citrate, phosphate, or acetate), and a detector (e.g., UV-visible). CE provides simplicity of method development, reliability, speed, and versatility. It is a valuable technique because it can separate compounds that have traditionally been difficult to handle by HPLC. Furthermore, it can be automated for quantitative analysis. CE can play an important role in process analytical technology (PAT). For example, an on-line CE system can completely automate the sampling, sample preparation, and analysis of proteins or other species that can be separated by CE. 

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