A modified Schlenk line for gas‐phase accelerating rate calorimetry capable of quantitatively sampling and safely handling hazardous gases

Abstract

AbstractThis paper reports a new method using a modified Schlenk line for quantitative charging and safe disposal of gases in a gas‐phase accelerating rate calorimetry (ARC) test. The modified Schlenk line is capable of accurately measuring the mass of gas(s) charged to the ARC bomb. The method conveniently allows loading a single gas or multiple gases for reaction. It also provides dosing (or shot addition) capability to add a gaseous sample for when the gas is too reactive to be preloaded with other components. The modified Schlenk line enables safely handling toxic and extremely reactive gaseous chemicals, including collecting gases for further characterization, and disposing the gaseous products and unreacted samples into neutralizing scrubbers after the ARC run. The modified Schlenk line can also be utilized to test solid, liquid, or gas/liquid/solid mixed phases under specific atmospheres. Additional capabilities of the assembly line include quick leak checking and easily removing unwanted air/moisture in the headspace of the bomb or impurities (residual solvents) in the sample before an ARC run, resulting in more reliable data. The utility of this method is demonstrated in the thermal evaluation of the chlorination of toluene with chlorine gas and the thermal stability study of a halogenated ethane.