The Reston Chlorofluorocarbon Laboratory

Procedure for the Laboratory Analysis of Halocarbons

Gas Samples Water Samples

Dry the gas using Mg(ClO4)2.

 

Introduce the gas into a loop of known volume.

Introduce water into a stripping cell.

Measure the temperature and pressure of the gas.

Strip halocarbons with N2 Gas flow >40cc/min for 4 min.

Inject the gas through a trap of Mg(ClO4)2 and Ascarite (NaOH)to remove H2O, H2S and CO2(H2S interferes with the analysis of CFC-11).

Same as for gases

Trap the halocarbons on Porasil C and Porapak T at -30°C. At -30°C O2 and most of the very high N2O not trapped (N2O interferes with the analysis of CFC-12).

Same as for gases

Heat trap to 95°C to release halocarbons.

Same as for gases

Inject release halocarbons through a pre-column of Porasil C into a Column of Porasil C.

Same as for gases

Reverse the flow in the pre-column after about 40 sec. The reversal of flow vents out the highly retentive halocarbons and greatly reduces the time for the analysis.

Same as for gases

The halocarbons are separated in the column. Time required is 7 to 15 min.

Same as for gases

Halocarbons passed through an Electron Capture Detector (ECD) containing 63Ni. By beta (e-) radioactive decay (CFCs+e- = CFCs-), the CFCs- move to the cathode in the detector and produce a small current. The current is amplified.

Same as for gases

Integrator measures areas. Areas are converted to concentrations.

Same as for gases