SILOXANES (TD-GC-MS)

60 Northland Road, Unit 1 • Waterloo, ON N2V 2B8 • +1 519 886 6910

Determination of Siloxanes in Municipal Landfill and Digester Gas

by Thermal Desorption Gas Chromatography Mass Spectrometry

Source of Siloxanes
Siloxanes are a family of man-made compounds that contain silicon (Si), oxygen
(O) and methyl (CH3) groups. They can either be found in cyclic or linear formations.
Siloxanes are found in numerous commercial products, such as hair products,
cosmetics, deodorants, defoamers, food additives, windshield and dry cleaning
fluids, and municipal waste-water sludge. Many of these products ultimately
end up in landfills. The biological breakdown of organic matter in the absense of
oxygen (anaerobic digestion) produces biogas. Siloxanes are released into landfill
water leachate or biogas through this decomposition process.
Cyclic Formation

Environmental Fate & Concerns

Siloxanes entering landfill water leachate (aquatic environment) will quickly
degrade, evaporate, or bind to organic rich particulates, thus limiting their
availability and toxicity to organisms. However, due to the volatility and
widespread use of lower molecular weight siloxanes, a significant portion of
the siloxanes orginally present in landfills are found in the biogas. Siloxanes
are not believed to contribute to air pollution or impact the ozone layer. In the Linear Formation
environment (water, soil, air), siloxanes ultimately degrade to inorganic silica,
water and carbon dioxide.

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Commercial Concerns - Biogas Combustion

Since biogas normally contains significant amounts of methane, it is used as an
energy or heating source. During combustion of biogas containing siloxanes,
silicon is released. This silicon combines with free oxygen to form white
mineral deposits on surfaces mostly composed of silicates (SixOy), along with
other elements such as calcium, sulfur, zinc, and phosphorus. These deposits
can accumulate to several millimeters in thickness, damaging engine pistons,
cylinder heads and turbine blades by causing pitting and abrasive wear, and
these deposits can foul post combustion catalysts. This damage leads to
efficiency losses or the requirement for complete engine overhauls at 5,000
hours or less of operation.

Sampling & Analysis

A major obstacle to understanding the levels of cyclic D(x) (most commonly x = 3 to 6) and linear L(x) (most commonly x = 2
to 5) structured siloxanes in biogas has been the difficulty in accurate measurement. The most widely used collection method,
impinger collection into methanol, suffers from accuracy and sensitivity problems, as well as being very labour and time intensive.
Alternatively, collection into canisters has resulted in siloxane losses on canister surfaces, especially for the heavier cyclic compounds,
and problems with preparation of standards.
Due to the limitations of both impinger and canister sampling procedures discussed above, ALS Environmental’s Waterloo
laboratory has developed a method for collection of siloxanes on thermal desorption sorbent tubes folled by thermal desorption
gas chromatography mass spectrometry analysis. Collection of siloxanes on TD tubes overcomes the limitations/problems of other
sampling techniques for siloxanes providing rapid and simple collection, as well as sensitive and accurate analysis.

Other Compounds of Concern in Biogas

Municipal landfill biogas can also contain other offensive components at elevated concentrations including: methane (45-70%),
carbon dioxide (30-45%), nitrogen (<10%), hydrogen (<1%), hydrogen sulfide (<1%), oxygen (<3%), and water vapour (<4%).

Complete Air Quality Testing Capabilities at ALS Environmental

In addition to analysis of silxanes, the ALS Environmental laboratory network offers analysis of the other biogas hydrocarbons and
fixed gases listed above, plus complete analysis of VOCs using canisters or thermal desorption tubes (EPA TO-15 & EPA TO-17 methods),
compressed breathing gas to CSA standards and a comprehensive list of organic and inorganic chemicals by NIOSH/OSHA industrial
hygiene methods.

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