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Quantifying Uncontrolled Landfill Gas Emissions from Two Florida ...

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2.2.3 Background Measurements<br />

Background methane concentration measurements were collected at Site #2 on February 25<br />

using the OP-TDLAS instrument. The measurements were collected at a location south of the<br />

control cell, upwind of the landfill cells at the site. The data collected were used to establish an<br />

average background methane concentration at the site.<br />

2.3 Total and Speciated Mercury Sampling<br />

During the February 2007 field campaign, the total mercury samples (THg) were collected using<br />

an iodated charcoal trap as a sorbent. A backup tube was also present to assess any breakthrough.<br />

The sorbent tube was heated to above the dew point of the gas stream to prevent condensation on<br />

the sorbent. Water vapor <strong>from</strong> the stream was collected and quantified using a silica gel<br />

impinger. A diaphragm air pump was used to pull sample through the train and collect the<br />

sample. The volume of gas sampled was monitored and quantified using a volatile organic<br />

sampling train (VOST) box. The sample flow rate was nominally 0.8 liters/minute for 37.5<br />

minutes, which equates to a total volume of approximately 30 liters.<br />

The traps were returned to the lab where the iodated carbon is leached of collected Hg using hotrefluxing<br />

HNO3/H2SO4 and then further oxidized by a 0.01 N BrCl solution. The digested and<br />

oxidized leachate sample was analyzed using the FGS-069 CVAFS total Hg analysis method<br />

(which served as the basis for U.S. EPA Method 1631, developed, authored, and validated by<br />

Frontier Geosciences).<br />

During the October 2007 field campaign, carbon tube samples taken <strong>from</strong> the landfills were<br />

analyzed by a modified SW-846 Method 7473, “Mercury in Solids and Solutions by Thermal<br />

Decomposition, Mercury Amalgamation, and Atomic Adsorption Spectroscopy” and CFR Part<br />

60 Method 30B, “Determination of Total Vapor Phase Mercury <strong>Emissions</strong> <strong>from</strong> Coal-Fired<br />

Combustion Sources Using Carbon Sorbent Tubes.” Samples were analyzed using a Lumex RA­<br />

915+ Zeeman spectrometer with a RP-M324 decomposition furnace attachment cell. No mercury<br />

amalgamation was necessary due to the sensitivity of the instrument. The iodated carbon samples<br />

were loaded into a quartz combustion boat and inserted into a decomposition furnace at 775 °C.<br />

The mercury species were converted to elemental mercury and detected by the Zeeman atomic<br />

adsorption spectrometer. The analyzer was calibrated using NIST certified HgCl2 standards <strong>from</strong><br />

SCP Sciences. Elemental mercury spiking of the carbon tubes was performed using an impinger<br />

containing a stannous chloride solution. The mercury standard was dispensed into the impinger<br />

and the elemental mercury is pulled through the glassware system onto the iodated carbon. The<br />

elemental mercury spike was used to assess the recovery the mercury <strong>from</strong> the carbon tubes.<br />

Dimethyl mercury (DMM) was sampled using a slightly different technique. A Carbotrap was<br />

used as a sorbent, with a backup tube to assess any breakthrough. A third iodated carbon trap<br />

was also present to collect any elemental mercury present. The sorbent tube was heated to a<br />

temperature above the dew point of the gas stream to prevent condensation on the sorbent. Water<br />

vapor <strong>from</strong> the stream was collected and quantified using a silica gel impinger. A diaphragm air<br />

pump was used to pull the sample through the train and collect the sample. The volume of gas<br />

sampled was monitored and quantified using a volatile organic sampling train (VOST) box. The<br />

sample flow rate was nominally 0.35 liters/minute for a total volume of approximately 0.5 liters.<br />

2-6

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