THE FREEZING POINTS OF HIGH PURITY METALS AS PRECISION TEMPERATURE STANDARDS: VI. THERMAL ANALYSES ON FIVE SAMPLES OF LEAD WITH PURITIES GREATER THAN 99.999+%
An investigation has been made of the freezing and melting temperatures of five samples of high purity lead (supplier's analyzed impurity contents < 0.7 to < 4 p.p.m.) including zone refined metal. Using the induced freezing technique, plateaux of essentially constant (< ±0.0001 °C) temperature with durations of over 1 hour are readily obtained on the cooling curves of these samples. A standard deviation in plateau temperature (liquidus point) of ±0.0001 °C was obtained from a series of 30 induced freezes on a particular sample. The pressure effect on the freezing temperature of lead was found to be 0.0080 °C for 1 atmosphere. A value of 327.426 °C (Int. 1948) was determined for the standard liquidus point of pure lead.The liquidus points of the samples were intercompared with a precision of about 0.0002 °C, and alloy melting ranges were examined following different types of freezing with and without overnight anneals near the solidus temperature. Alloy melting range parameters were found to be useful in the selection of the samples of highest purity and at the same time showed that an uncertainty of 0.002 °C in the above value of the liquidus point of pure lead may exist because of residual impurity contents in the purest samples that were examined.