Calibration of cells

Refractive index data are very useful for the quantitation of isotropic (liquid and cubic liquid crystal) phases, and for the calibration of cell thickness and nonflatness. Hovever, the analysis of birefringent phases using refractive index data has been found to be unreliable (9). A problem arises from the fact that the orientation of such phases relative to the direction of the light path, as veil as the system variables, influence refractive indices. In order to use refractive index data for quantitation, a phase must spontaneously orient in a reproducible fashion. Such orientation does occur in the case of fluid lamellar phases (as in short chain polyoxyethylene nonionic systems (7)), but viscous lamellar phases, hexagonal phases, and crystal phases do not orient to a sufficient degree. 

Due to the disadvantage of working with cells without liquid junctions, in practice the operational scale uses buffer solutions with known conventional pH for the calibration of cells with liquid junction [e.g., the convenient glass electrode (with the calomel or silver electrode, respectively, as reference)]. After calibration of the measuring cell (with a buffer of known conventional pH), the acidities of unknown samples can be measured in the same solvent. It is clear that for the standard buffers used, the conventional and the operational pH are identical. However, we cannot assume such an identity for the unknown samples. This is because the activities and the mobilities of the different ionic species might change the potential on the boundary with all liquid junctions (even without taking effect of the nonelectrolytes into account). 

Table 1 Reference solutions for calibration of cell constants...

Due to the disadvantage of working with cells without liquid junctions, in practice the operational scale uses buffer solutions with known conventional pH for the calibration of cells with liquid junction [e.g., the convenient glass electrode (with the calomel or silver electrode, respectively, as reference)]. After calibration of the measuring cell (with a buffer of known conventional pH), the... 

In this section we present a siunmary of the experimental method used to obtain information on the electrical conductivity of high temperature, high pressure aqueous electrolyte solutions. An excellent review of the techniques used up to 1985 has been done by Marshall and Frantz (Marshall and Frantz, 1987). The reader could refer to classical books on electrolytes to learn about the common practice on calibration of cells and measurement procedures using impedance bridges (Robinson and Stokes, 1965 Spiro, 1984). 

From the ventilation point of view, the fixed points -38.83 °C (triple-point of mercury), 0.010 °C (triple-point of water), 29.76 °C (melting point of gallium), and 156.60 °C (freezing point of indium) are of relevance. The triple-point of water is relatively simple to achieve and maintain with a triple-point apparatus. Some freezing point cells are covered in standards. In practical temperature calibration of measuring instruments, the lTS-90 fixed points are not used directly. 

Therefore, by measuring the cell emf, E, we can determine the pH. The value of E is established by calibrating the cell, which requires measuring E for a solution of known pH. 

In a separate set of experiments designed to follow the gas phase reactions of CHj-radicals with NO, CHj- radicals were generated by the thermal decomposition of azomethane, CHjN NCHj, at 980 °C. The CH3- radicals were subsequently allowed to react with themselves and with NO in a Knudsen cell that has been described previously [12]. Analysis of intermediates and products was again done by mass spectrometry, using the VIEMS. Calibration of the mass spectrometer with respect to CH,- radicals was carried out by introducing the products of azomethane decomposition directly into the high vacuum region of the instrument. 

Dunsmore, H. S. Midgley, D., The calibration of glass electrodes in cells with liquid junction, Anal. Chim. Acta 61, 115-122 (1972). 

It has been emphasized repeatedly that the individual activity coefficients cannot be measured experimentally. However, these values are required for a number of purposes, e.g. for calibration of ion-selective electrodes. Thus, a conventional scale of ionic activities must be defined on the basis of suitably selected standards. In addition, this definition must be consistent with the definition of the conventional activity scale for the oxonium ion, i.e. the definition of the practical pH scale. Similarly, the individual scales for the various ions must be mutually consistent, i.e. they must satisfy the relationship between the experimentally measurable mean activity of the electrolyte and the defined activities of the cation and anion in view of Eq. (1.1.11). Thus, by using galvanic cells without transport, e.g. a sodium-ion-selective glass electrode and a Cl -selective electrode in a NaCl solution, a series of (NaCl) is obtained from which the individual ion activity aNa+ is determined on the basis of the Bates-Guggenheim convention for acr (page 37). Table 6.1 lists three such standard solutions, where pNa = -logflNa+, etc. 

Type of cell Gas pressure (Torr) Calibration ratio (fiW/mm) Constant thermal power Variable thermal power... 

The 3He melting pressure thermometer has been chosen to extend the ITS 90 for several reasons, such as the good sensitivity over three temperature decades, except around the pressure minimum at 315.24 mK. On the other hand, such a minimum is a reference point in the calibration of the pressure transducer in fact, the pressure must be measured in situ since, below 315.24 mK, the entrance of the measurement cell is blocked by solid 3He. 

The gas pycnometer is based on the ideal gas law. A known quantity of gas (characterized by a determined temperature and pressure) is allowed to flow from a calibrated reference volume into a calibrated sample cell containing the solid. A second pressure reading is obtained, and the sample volume is calculated. 

Proper calibration of the DSC instruments is crucial. The basis of the enthalpy calibration is generally the enthalpy of fusion of a standard material [21,22], but electrical calibration is an alternative. A resistor is placed in or attached to the calorimeter cell and heat peaks are produced by electrical means just before and after a comparable effect caused by the sample. The different heat transfer conditions during calibration and measurement put limits on the improvement. DSCs are usually limited to temperatures from liquid nitrogen to 873 K, but recent instrumentation with maximum temperatures close to 1800 K is now commercially available. The accuracy of these instruments depends heavily on the instrumentation, on the calibration procedures, on the type of measurements to be performed, on the temperature regime and on the... 

Furthermore, in more recent studies high [Ca2+]mt signals are seen in only a few mitochondria within a given cell, and reports claiming very high [Ca2+]mt under physiological conditions are based on cells isolated by enzymatic dispersion. This, coupled with the uncertainty of calibration of luminescent and fluorescent Ca2+ indicators within the mitochondrial matrix, (for nuclei see Perez-Terzic et al 1997) should raise serious questions about the correct values of [Ca2+]mt. It is unfortunate that, with rare exceptions, very few available studies compare free with total mitochondrial Ca in the same cell type observed under the same condition. 

The calibration of the calorimetric unit P, leading to the calibration constant s (see chapter 9), can be made by the Joule effect, with a resistor inserted into the photochemical reactor cell. As justified shortly (equation 10.16), no calibration is required for the photoinert cell in unit R. 

The bulk density of the feedstock at ambient temperature and pressure should be measured prior to the design of a new screw, especially if it contains in-plant recycle resin. The measurement method is extremely simple and requires only a calibrated cell and a scale. A calibrated measuring cell with a volume of 500 cm can easily be constructed by welding a thin-walled metal pipe to a flat sheet of metal, as shown in Fig. 4.2. The bulk density is measured by filling the cell with feedstock, leveling the top with a steel ruler, and then weighing the cell contents. A more formal measurement technique was developed by ASTM as standard method D1895. 

The ISFET-based integrated coulometric sensor-actuator system was introduced in 1985 [154] in order to facilitate in situ calibration of ISFETs. The essential components of a prototype sensor based on this operational principle are shown in Fig. 4.20.B. The system was built by integrating a large noble-metal actuator electrode and a counter-electrode in a piece of silicon. A window in the actuator electrode was etched to receive the gate of the ISFET, which functioned as a pH indicator. The flow-through cell was constructed by sealing a silicon cover with an etched cavity of the chip. The system operation resembles that of a conventional coulometric titration system very closely. The sample was first injected into the cavity and the... 

While most appfications were performed in suspended cell cultures some authors showed that the application of NADH-dependent fluorescence monitoring is also possible in immobifized cell systems. Here the growth of Clostridium acetobutylicum and the Saccharomyces cerevisiae immobilized in different calcium alginate structures was studied. However, calibration of the culture fluorescence signal with the biomass concentration was not possible but qualitatively an increasing biomass also led to an increase in the fluorescence signals. 

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