Fixed-cell instruments

With fixed-cell instruments, samples must be loaded directly into the calorimetric chamber, and the need for a metal pan or batch cell is eliminated. Such a system... 

Whereas most fixed-cell instruments are power-compensation instruments (because it is possible to place heaters on the base of cells that are not removable), batch-cell instruments are available as either power-compensation or heat-flux designs. One design of a heat-flux, batch-cell instrument is the micro-DSC in (Setaram). The instrument consists of a calorimetric block into which two channels are machined. One channel holds the sample cell, the other holds the reference cell. At the bottom of each channel, between the cell and the block, is a plane-surfaced transducer. The transducers provide a thermal pathway between the cells and the block and are used to maintain the cells at a temperature identical to that of the block. The electrical signal produced by the transducer on the sample side is proportional to the heat evolved or absorbed by the sample. The temperature of the calorimetric block is maintained by a precisely thermostated circulating liquid. The liquid is raised in temperature by a separate heater and is cooled by a supply of circulating water. The precise control of the temperature of the circulating liquid allows scan rates of just 0.001°C min-1 to be attained and ensures that the calorimetric block is insulated from the surrounding environment. 

Biological autofluorescence in mammalian cells due to flavin coenzymes (FAD and FMN absorption, 450 nm emission, 515 nm) and reduced pyridine nucleotides (NADH absorption, 340 nm emission, 460 nm) can be problematic in the detection of fluorescence probes in tissues and cells. Fixation with aldehydes, particularly glutaraldehyde, can result in high levels of autofluorescence. This can be minimized in fixed cells by washing with 0.1% sodium borohydride in phosphate-buffered saline (5) prior to antibody incubation. Problems due to autofluorescence can be minimized by selecting probes and optical filters that maximize the fluorescence signal relative to the autofluorescence. Other factors that limit IF include the performance of the detection instrument (i.e. how well the microscope has been calibrated and set), the specificity of the antibodies, and the specimen preparation. 

Irrespective of whether an instrument employs fixed cells or batch cells, some design considerations are common to all HSDSC instruments. To measure accurately small powers, it is necessary to ensure good baseline stability throughout the course of an experiment. This is usually achieved by maintaining very accurate control of the calorimetric block temperature and ensuring that the properties of the sample and reference cells, such as geometry, cell volume, local environment, thermal conductivity and conduction pathways, and heating rate, are identical. 

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. 

Visual methods have been virtually displaced for most determinations by methods depending upon the use of photoelectric cells (filter photometers or absorptiometers, and spectrophotometers), thus leading to reduction of the experimental errors of colorimetric determinations. The so-called photoelectric colorimeter is a comparatively inexpensive instrument, and should be available in every laboratory. The use of spectrophotometers has enabled determinations to be extended into the ultraviolet region of the spectrum, whilst the use of chart recorders means that the analyst is not limited to working at a single fixed wavelength. 

This procedure has the great advantage that some potential sources of error are eliminated. The measurements do not depend upon accurate wavelength positions as they are made with respect to the spectrum itself and any cell errors are avoided by using the same fixed-path-length cell. Also, by employing this measured ratio any variations in the source intensity, the instrument optics or sensitivity are eliminated. 

The conductance of a solution is the inverse of its resistance, and conductance has units of ohms 1 or mohs. The higher the conductance of a solution, the lower is its electrical resistance. A conductivity meter and conductivity cell are used to determine the effective resistance of a solution. The conductivity cell consists of a pair of platinized platinum electrodes with an area of approximately 1.0 cm2 with spacers designed to hold the electrodes rigidly parallel and at a fixed distance from each other. The cell can be standardized with solutions of known conductivity to obtain the cell constant, k so that the instrument response R... 

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