Detector Deviations

Following the determination of the radiometric calibration of a detector, an additional step is required to achieve its calibration for the erythema response (CIE). Due to manufacturing limitations, the spectral sensitivity of broadband detectors deviates form the CIE biological action spectrum. Therefore, die requirement for a correction factor to enable the simulation of the CIE weighted irradiance by any of those commercial... 

It follows that for a truly linear detector, r = 1, and the proximity of (r) to unity will indicate the extent to which the response of the detector deviates from true linearity. The response of some detectors having different values for (r) are shown as curves relating the detector output (V) to solute... 

It was found that that in the case of soft beta and X-ray radiation the IPs behave as an ideal gas counter with the 100% absorption efficiency if they are exposed in the middle of exposure range ( 10 to 10 photons/ pixel area) and that the relative uncertainty in measured intensity is determined primarily by the quantum fluctuations of the incident radiation (1). The thermal neutron absorption efficiency of the present available Gd doped IP-Neutron Detectors (IP-NDs) was found to be 53% and 69%, depending on the thicknes of the doped phosphor layer ( 85pm and 135 pm respectively). No substantial deviation in the IP response with the spatial variation over the surface of the IP was found, when irradiated by the homogeneous field of X-rays or neutrons and deviations were dominated by the incident radiation statistics (1). 

In addition, the mirrors are adjustable, so that unimportant areas can be ignored. Light re-emmited from the surfaee is detected, and the detector signal is transmitted to a computer programmed with acceptable deviation levels for comparison with a reference component. Tolerance levels can vary for different areas of the same test piece they may, for example, be higher on a ground section than on adjacent unmachined areas. 

Periodical verification" enables, by annual measurements on the particular flaw detector itself, to detect any non acceptable deviation of characteristics. These verifications are also performed at the delivery of the flaw detector, or at the occasion of repair. 

Precision The precision of a gas chromatographic analysis includes contributions from sampling, sample preparation, and the instrument. The relative standard deviation due to the gas chromatographic portion of the analysis is typically 1-5%, although it can be significantly higher. The principal limitations to precision are detector noise and the reproducibility of injection volumes. In quantitative work, the use of an internal standard compensates for any variability in injection volumes. 

To the analytical chemist, a standard deviation31 is a logical figure of merit for the comparison of detectors. We shall merely introduce the important subject of counting errors (10.2) here. For present purposes, it suffices to know that these errors are predictable, and that they set a lower limit to the standard deviation in an analytical method that depends upon measuring the intensity of an x-ray beam by an integrating detector. 

The top and the bottom x-ray detector each contain a multiplier phototube coated with phosphor. This tube compares the intensity of the x-ray beam entering the detector with that of the light from the reference standard, a discharge lamp. The reference beam is part of a circuit that maintains the x-ray source at constant intensity. The deviation wedge comes to rest when the intensities of the transmitted x-ray beams stand in a predetermined ratio. At this point, the unbalance in the servo system has been compensated, and the position of the deviation wedge consequently indicates the thickness of the strip. In 1955, this application was made fully automatic that is, the unbalance (or error signal) just mentioned was used to readjust tandem cold reduction mills of the United States Steel Corporation. Automatic control proved significantly more effective than manual control. 

Notes. (1) Krypton-filled detector. (2) Tungsten content 0.0240 gram of tungsten per gram of solution. (3) Each determination complete and independent except that aliquots of the same solution were used for an entire series. (4) sa is the standard deviation, as usually defined, for a single determination. 

The mixing time will be that required for the mixture composition to come within a specified deviation from the equilibrium value and this will be dependent upon the way in which the tracer is added and the location of the detector. It may therefore be desirable to record the tracer concentration at several locations, and to define the variance... 

ECD = electron capture detector GC = gas chromatography HPLC = high-performance liquid chromatography MC = microcoulometric detector MS = mass spectrometry NICI = negative ion chemical ionization RSD = relative standard deviation SPE = solid phase extraction... 

Deviating from the setup discussed earlier, the y-ray beam can also be consistently collimated by structures other than the absorber holder. If this is the entrance window of the detector, the counter should have a lead shield, and the absorber must be sufficiently large to prevent radiation from passing by. For Mossbauer scattering experiments, the same arguments have to be considered. 

Assay sensitivity is defined here as the concentration of analyte that inhibits the observed absorbance by 50% or the IC50. The lower limit of detection (LLD) is the lowest analyte concentration that elicits a detector response significantly different from the detector response in the absence of analyte. In some cases, the LLD is defined as three standard deviations from the mean of the zero analyte control. In other cases, the LLD is defined empirically by determining the lowest concentration of analyte that can be measured with a given degree of accuracy. Readers are referred to Grotjan and Keel for a simplified explanation and to Rodbard for the complete mathematics on the determination of LLD. 

A linear dependence between detector response and the amount of sample entering the detector is expected for phosphorus and is generally found. Deviations from the predicted detector response are more common with sulfur-containing than phosphorus-containing compounds (171,173). The detector response in the sulfur aK>de can be described by equation (3.17)... 

Extracolumn dispersion is a major problem for the packed fused silica capillary columns with internal diameters less than 0.35 mm. Peak standeunl deviations will be in the submicroliter range and extensive equipment modification is required for operation under optimum conditions. A reasonable compromise is to esploy injection voluMs of a few hundred nanoliters or less with detector volumes of a similar or preferably smaller size. This demands considerable ingenuity on behalf of the analyst since, as... 

Deviation refractometers are the most commonly used. This version of the DRI measures the deflection in the location of a light beam on the surface of a photodiode by the difference in refractive index between the polymer solution and pure solvent. The Fresnel-type refractometers operate on the principle that the intensity of light reflected from a glass-liquid interface is dependent on the incident angle and the RI difference between the two phases. The deviation and Fresnel detectors typically have cell volumes of 5 to 10 pi, detection limits of about 5 x 10-6 refractive index units (RIU), and a range of 10 7 to 10 3 RIU.156 The deflection-type DRI is relatively insensitive to the buildup of contaminants on the sample cell and is therefore of special utility in laboratories that process large numbers of samples, such as industrial laboratories. 

In the above-described measurement, which we call the absolute method, all pumps have equal speeds (rpm) owing to interconnection to the same drive-shaft. In order to express, if required, a deviation registered for the analyte concentration, one must calibrate with a standard by varying its rpm (B) with respect to that of the titrant (A) a B/A rpm ratio greater than unity means a proportionally lower concentration and vice versa. In general, the absolute method serves to control a sample stream with nearly constant analyte concentration as a sensor one uses not only electroanalytical but often also optical detectors. However, with considerably varying analyte concentrations the differential method is more attractive its principle is that in the set-up in Fig. 5.15 and with the sensor adjusted to a fixed and most sensitive set-point, the rpm of the sample stream (C) is varied with respect to that of the titrant (A) by a feedback control (see Fig. 5.3a) from the sensor via a regulator towards the... 

With the new VME/UNIX control system on the polarised hot-neutron normal-beam diffractometer D3 at ILL, each measurement cycle for both peak and background intensities lasts 2 s, and the (+)/(-) counting-time fractions are defined with a 1 MHz clock. There are two detector scalers and two monitor scalers ((+) and (-) states). In Table 1, we compare the flipping ratio measured for the strong 200 and the weak 600 Bragg peak reflections of a CoFe sample. As expected, the standard deviation cr (if) is improved in the case of the strong reflection (16%). 

Chromatographic system (See Chromatography <621 >.) The liquid chromatograph is equipped with a 230 nm detector and a 4.6 mm x 30 cm column that contains packing L7. The flow rate is about 2 mL/min. Chromatograph the Resolution solution and the Standard preparation, and record the peak responses as directed under Procedure the resolution, R, between the dibutyl phthalate and miconazole peaks is not less than 5, the tailing factor for the miconazole peak is not more than 1.3, and the relative standard deviation for replicate injections of the Standard preparation is not more than 2%. The relative retention times are about 0.7 for dibutyl phthalate and 1 for miconazole. 

Chromatographic system. (Follow the method described in the general procedure <621 >.) The gas chromatograph is equipped with a flame ionization detector and a 1.2 m x 2 mm column packed with 3% phase G32 on support S1A. The injection port, detector, and column temperatures are maintained at about 250, 300, and 250 °C, respectively, and helium is used as the carrier gas, flowing at rate of about 50 mL/min. The relative retention times for cholestane and miconazole nitrate are about 0.44 and 1, respectively. Chromatograph the Standard preparation, and record the peak responses as directed for procedure The resolution, R, between cholestane and miconazole nitrate is not less than 2 and the relative standard deviation of replicate injections is not more than 3%. 

Guo et al. [53] developed a gas chromatographic method for the analysis of miconazole nitrate in creams and injections. The conditions were flame ionization detector, stationary phase of 5% SE 30 support of Chromosorb W (AS-DMCS, 80—100 mesh) packed column 3 m x 3 mm column temperature 275 °C injection temperature 290 °C and diisooctyl sebacate and internal standard. The average recoveries for creams and injections were 97.7 and 101.4%, respectively. The relative standard deviations were 2.2 and 1.3%, respectively. 

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