VOC Laboratory and Sample Collection Proceedures

In-Situ Oxidative Technologies, Inc. T:\\\\Isotec\\\\JOBS\\\\LAB-STUD\\\\2011 SL VOC-PAH Lab Procedures.doc 1 Procedure for the Laboratory Treatability Study ISOTECSM performs a bench-scale laboratory treatability study to achieve the following objectives: ? Evaluate the effectiveness of the ISOTECSM oxidative process on a representative site-specific soil-slurry sample (Soil-slurry test). The soil-slurry sample is prepared by combining composited soil samples with site groundwater samples in a 2:1 ratio. ? For each ISOTEC catalyst under evaluation, determine the amount of catalyst/oxidant mix (reagent) required to oxidize the measured site contaminants (i.e. site-specific stoichiometry per catalyst); Typical bench scale study procedures are outlined below. The study consists of establishing initial conditions, setting up experimental control, conducting the experiments through application of various catalysts and oxidants, and then submitting the treated samples for analysis. Please note that this bench study includes VOC analysis for all test samples and total organic carbon (TOC), iron and manganese analysis for initial samples. If analysis for other parameters is required (such as PAHs, TPH or TAL metals), it can be performed at an additional cost. Initial Conditions Initial untreated/baseline conditions of soil, soil-slurry, and groundwater are established prior to initiating the experiment. Initial groundwater samples are analyzed for iron and manganese. Initial soil samples are analyzed for iron, manganese and total organic carbon (TOC). The initial soil-slurry samples are analyzed for VOCs. Experimental Control Experimental control samples (Control) are set up the same way as all other experimental samples during the study to document the following: ? reduction in contaminant concentrations due to sample dilution by reagent volumes injected, and ? reduction in contaminant concentrations due to volatilization caused by room temperature test conditions. Control sample is set up in a treatment reactor but is injected with distilled water instead of reagents. The volume of distilled water injected is identical to the volumes of reagent injected into treatment reactors. Control sample will remain at and is subject to the same conditions as all other treatment and monitoring reactors. Soil-Slurry Test Experimental Setup ISOTECSM soil-slurry test is designed to simulate the condition of saturated/ unsaturated zones at the site. Because contaminants tend to bind to aquifer matrix in the subsurface, they are not as readily degradable as the dissolved phase contaminants in groundwater. Furthermore, soil organic matter tends to impart a scavenging effect on the oxidizing agent leading to competition. However, an increase in the amount of reagent supply into the treated samples overcomes the solid binding force and achieves significant contaminant destruction. Soil-slurry test experiment is performed in multiple pairs of 120 ml sealed batch reactors. Soil-slurry mix is prepared from a two to one ratio by weight (2:1 w/w) of soil and groundwater. Soil-slurry is introduced into each reactor, leaving enough headspace for predetermined reagent volumes to be injected. The reactors are sealed with screw-top caps fitted with Teflon®-lined rubber septa to facilitate reagent injections. In-Situ Oxidative Technologies, Inc. T:\\\\Isotec\\\\JOBS\\\\LAB-STUD\\\\2011 SL VOC-PAH Lab Procedures.doc 2 Each pair receives a different volume of the reagent to test low, medium and high dosages. Similar to groundwater test, one reactor of each pair serves as the “treatment reactor” while the other serves as the “monitoring reactor”. Both reactors of each pair will receive identical reagent doses. Treatment reactor is not opened or sampled until the end of the experiment. Monitoring reactor is used to monitor the extent of the oxidation reaction of the pair, by periodically extracting small samples for oxidizer analysis. Distilled water is used to equalize the total volume of reagent used between multiple reactors pairs. The reactor pair which receives only distilled water will serve as control. Experimental Quenching Following the last application of reagent, all reactors remain undisturbed at room temperature for a minimum of 24 hours (2 weeks for persulfate) or until the oxidizer is completely consumed as determined by laboratory analysis. Treatment effectiveness is evaluated by calculating the percent VOC/ PAH reduction in each treatment reactor relative to the control reactors. Sample Collection and Analysis Following sample quenching, final values of pH are determined from the monitoring reactors. Samples are submitted to a New Jersey certified laboratory (Integrated Analytical Laboratories, LLC of Randolph, NJ) for contaminant analysis. Samples will be analyzed using EPA 624/8260 for VOCs, EPA 625/8270 for PAH, EPA 6010/6020/200.8/7000 series for iron and manganese, and EPA 415.1 for TOC. The samples will include: ? “Initial” groundwater samples for iron, and manganese analysis. ? “Initial” soil samples for iron, manganese, and TOC analysis. ? “Initial” soil-slurry samples for VOC analysis. ? “Control” soil-slurry samples for VOC analysis. ? “Treatment” low, medium and high dosage soil-slurry samples for VOC analysis. In-Situ Oxidative Technologies, Inc. T:\\\\Isotec\\\\JOBS\\\\LAB-STUD\\\\2011 SL VOC-PAH Lab Procedures.doc 3 ISOTECSM Laboratory Study Sample Collection In order to perform an ISOTEC lab study, a representative soil and/or groundwater sample must be collected from an area of concern at the site exhibiting the highest detected levels of contaminants. Please purge the well prior to groundwater sampling. Field and trip blanks are not required. For soil samples, please collect a representative soil sample or a composite. A summary of the sample containers required for the laboratory study is provided below. Please contact ISOTEC for sample requirements other than those listed below. ***Please ensure zero head space in 1 liter jars *** Container Type No. Matrix Preservative 1 liter, amber glass* 6 Groundwater Ice only Zip lock bags placed in clean paint cans 1 (10 lbs) Soil Ice only For testing both modified Fenton’s as well as catalyzed persulfate, double the above sample volumes for each analyte. Lab study samples are requested to be collected on a Monday/Tuesday and received by ISOTEC on Tuesday/Wednesday. Samples should be packaged in a cooler (with ice) and shipped overnight (AM) delivery to the following address: In-Situ Oxidative Technologies, Inc. 51 Everett Drive, Suite #A-10 West Windsor, New Jersey 08550 Attn: Prasad Kakarla If you should need to be supplied with sample containers and/or a sample shuttle, please contact ISOTEC. Please enclose a standard chain-of-custody with the samples. In addition, please enclose contaminant information by including latest laboratory analytical data on the above samples collected. ISOTEC must be notified at least 48 hours prior to sample shipment to prepare for lab study. If you should have any questions concerning the sampling event, please do not hesitate to contact Prasad Kakarla at (609) 275-8500 (ext. 111).