Removing Residual Thermal Stress
Vacuum sealing of ampules in borosilicate glass tubing is best accomplished using a hand torch which uses natural
gas (or propane) and oxygen. Hydrogen/oxygen flames are not recommended for borosilicate glass seals. When a
hydrogen flame is used to flame anneal the finished ampule, the flame temperature is too hot and will result in residual
thermal stress in the ampule. As air mixes with the hydrogen flame, temperatures above the strain and annealing point
will result. Tests have shown that using a hydrogen flame will result in the thermal stress line being relocated into the
ampule body rather than removing the strain. Flame annealing of the finished borosilicate ampule should be
accomplished by using the following technique. Immediately after sealing, remove the oxygen from the torch flame and
begin heating uniformly around the seal area using a gas only flame. This flame annealing process should also include
the area 10 to 20 mm from the sealed end. During sealing operations, the most severe thermal stress accumulates in
this 10 to 20 mm region. Continue annealing the ampule until a thin carbon black deposit appears on the surface of the
glass. Do not set the hot seal on a cold bench top, etc., instead, prop the ampoule on a heat resistant material in a
draft free location to cool. (See Glass Strain and Annealing)
.

Hydrogen/oxygen flames are generally required for quartz glass seals. Because of the low coefficient of expansion of
the quartz, residual strain in the quartz seal is not as severe and flame annealing is not generally required.


Quartz Sample Tubes
Prepare the quartz sample tube
by making a small indent in the
tube body. Insert a solid quartz
plug (rests on indent) after
loading sample. Evacuate. Heat
and collapse the quartz sample
tube onto the solid plug. With
care a vacuum tight seal can be
obtained. Remove the entire
sample tube from the vacuum
system. The sample bulb can be
removed from the tube top by
using a wet saw.
The finished tube will look similar
to this. Ideally, the mass of glass
where the seal has been made
will not be overly thick.
8.
7.
Explosion Hazards
In some cases, it will be necessary to freeze the material within the ampule to reduce the vapor pressure during
sealing operations. Care must be taken to eliminate the possibility of condensing liquid oxygen into the ampule.
(See Cryogenics and the Scientific Glassblower)
. Additionally, frozen aqueous solutions will expand and crack
ampules.
Almost any material sealed into a closed ampule will expand when warmed to room temperature or heated in an
oven. With a known quantity of material, calculate the vapor pressure vs.temperature of the material inside during
subsequent processes. Do not exceed the Maximum Allowable Internal Pressure (MAIP)
rating of the glass
ampule. Remember that the MAIP ratings are given for clean, abrasion and stress free glass tubes. The vacuum
seal will become the weakest part of the completed ampule. The seal shape, uniformity, and your ability to
remove thermal stress from the seal is important when considering the integrity of the finished ampule.
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