techniques for approximating the international temperature ... - BIPM
techniques for approximating the international temperature ... - BIPM
techniques for approximating the international temperature ... - BIPM
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37<br />
with a repeat calibration after clipping about 1 cm of wire from <strong>the</strong> hot junction to avoid<br />
effects of contamination.<br />
Reliable freezing points cannot be obtained with this method because some material<br />
from <strong>the</strong> <strong>the</strong>rmoelements dissolves in <strong>the</strong> molten bridge, changing its freezing <strong>temperature</strong><br />
by an indeterminate amount and producing a freezing transition with a rapidly changing<br />
<strong>temperature</strong>.<br />
The melting <strong>temperature</strong> of palladium is influenced by dissolved oxygen; in an<br />
oxygen-free atmosphere <strong>the</strong> melting <strong>temperature</strong> is 1554.8 °C and in air is about 1553.5 °C<br />
[Jones and Hall (1979), Coates et al. (1983), Bed<strong>for</strong>d (1972a), Jones (1988)]. With a<br />
platinum bridge on a <strong>the</strong>rmocouple with a pure platinum <strong>the</strong>rmoelement, ei<strong>the</strong>r <strong>the</strong> bridge<br />
frequently breaks or <strong>the</strong> platinum <strong>the</strong>rmoelement melts near, and be<strong>for</strong>e, <strong>the</strong> bridge itself,<br />
depending upon <strong>the</strong> degree of <strong>temperature</strong> uni<strong>for</strong>mity. The platinum point is best used with<br />
double alloy noble metal <strong>the</strong>rmocouples or with refractory metal <strong>the</strong>rmocouples.<br />
The accuracy of <strong>the</strong> procedure is mainly limited by <strong>the</strong> contamination of <strong>the</strong> metal<br />
bridge by <strong>the</strong> <strong>the</strong>rmocouple wire, and by <strong>the</strong> furnace's tendency to raise <strong>the</strong> <strong>temperature</strong> of<br />
<strong>the</strong> <strong>the</strong>rmocouple legs, weakly opposed by <strong>the</strong> latent heat absorbed by <strong>the</strong> melting bridge,<br />
above <strong>the</strong> melting point. With Pt10Rh/Pt <strong>the</strong>rmocouples it is possible to obtain a<br />
reproducibility (1 standard deviation) of about ± 2 µV between two test runs at <strong>the</strong> gold point,<br />
about ± 4 µV at <strong>the</strong> palladium point, and about ± 8 µV at <strong>the</strong> platinum point. A detailed<br />
description of <strong>the</strong> use of <strong>the</strong> wire-bridge method in an interlaboratory intercomparison is<br />
given by Crovini et al. (1987).<br />
3.3.3 Miniature Fixed Points <strong>for</strong> Thermocouple Calibrations<br />
Tischler and Koremblit (1982) have devised a modification of metal-fixed-pointcalibrations<br />
<strong>for</strong> <strong>the</strong>rmocouples using miniature ingots that has some of <strong>the</strong> advantages of<br />
both regular fixed points and <strong>the</strong> wire-bridge method. It can provide calibrations that in many<br />
cases are as accurate as <strong>the</strong> <strong>the</strong>rmocouples <strong>the</strong>mselves and can also provide <strong>the</strong> possibility<br />
of in-situ calibration. The technique has been applied successfully with In, Sn, Cd, Pb, In,<br />
Sb, AI, Ag, Au, Cu. A small crucible (volume - 0.1 cm3, mass - 0.3 g) machined from 6 mm<br />
diameter graphite rod to <strong>the</strong> shape shown in Fig. 3.4 is filled with a pure metal ingot (mass of<br />
metal from 0.5 to 2 g). A hole is drilled through <strong>the</strong> graphite below <strong>the</strong> ingot chamber and<br />
ano<strong>the</strong>r through <strong>the</strong> graphite lid. One leg of <strong>the</strong> <strong>the</strong>rmocouple can be inserted into each hole<br />
without touching <strong>the</strong> metal ingot. This completes <strong>the</strong> electric circuit, prevents contamination<br />
of <strong>the</strong> metal ingot, and permits repeated use of <strong>the</strong> crucible with <strong>the</strong> same <strong>the</strong>rmocouple or<br />
<strong>the</strong> exchange of <strong>the</strong>rmocouples.