Method Detection Limits for EPA Method 8015 Diesel Range ...

1 Method Detection Limits for EPA Method 8015. Diesel Range Organics Using fully automated extraction and Concentration equipment Michael Ebitson and David Gallagher, Horizon Technology, Inc., Salem, NH. Introduction One of the most frequently desired quantities in environmental chemistry is the amount of Diesel Range organics (DROs) contained within a sample. The analysis of DROs is performed in almost every major environmental laboratory under the EPA Method 8015. This Method is commonly used to determine the contamination of alkanes from C10 to C28 caused by leaky underground storage containers. In addition to testing under Method 8015, many state-run environmental agencies have used Method 8015 as the foundation for their own, more in depth, methods; for example, the Massachusetts VPH and EPH.

2 Methods and the Florida TRPH Method . The simplicity of EPA Method 8015 lends itself easily to The Horizon Technology SPE-DEX 4790 automated extraction automation. As such, the Method Detection Limit (MDL) System, Envision Platform Controller, and DryVap automated extraction of the target Range for the study was done using Drying and Concentrating System. the Horizon Technology SPE-DEX 4790 automated extraction unit with Envision controller. The drying and 2. Spike the Diesel standard into one liter such that the concentration of the final extract was performed using the final concentration is mg/L and the Oil standard DryVap Concentrator System with DryDisk technology.

3 Into another such that it is mg/L. Final analysis was done using a gas chromatograph (GC) 3. Add the 1-Chlorooctadecane surrogate into each. with flame ionization detector (FID). 4. Extract the samples using the SPE-DEX 4790 and the Method shown below in Table 2. The SPE-DEX 4790 is an automated solid phase extractor 5. Dry and concentrate the extracts using the DryVap . specifically designed to extract a wide Range of target settings shown in Table 3 to a final volume of 5 mL. analytes from both influent and effluent sample matrices. 6. Perform the final analysis using GC-FID. The Envision controller is a web based controller system 7.

4 To complete the MDL study, extract seven replicates which provides a simple yet elegant Method of interacting of each type using steps one through six over three, with up to eight extractor units. The DryVap non-consecutive, days. Concentrator System used in conjunction with DryDisk . allows for an automated way to both dry and concentrate a Table 1: Purge Method sample extract. Step Solvent Dry Time Prewet 1 Methanol 15 s The benefits of the Horizon Technology fully automated extraction and concentration systems are many and include Prewet 2 MeCl 15 s such things as decreased solvent usage, no sodium sulfate Prewet 3 MeCl 15 s cost, less human interaction, precise and accurate results, Rinse 1 Acetone 5s and faster turn-around-times.

5 Rinse 2 Acetone 5s Rinse 3 MeCl 10 s Instrumentation Table 2: extraction Method Horizon Technology Step Solvent Soak Time Dry Time - SPE-DEX 4790 automated extraction System Prewet 1 MeCl 2:00 min 0:30 min - Envision Controller Prewet 2 MeCl 2:00 min 0:30 min - Atlantic DVB Disk Prewet 3 Methanol 2:00 min 0:05 min - DryVap Concentrator System Prewet 4 Reagent Water 1:00 min 0:05 min - DryDisk Solvent Drying System Prewet 5 Reagent Water 1:30 min 0:02 min Agilent 6890N GC-FID. Process Sample Supelco SPB-1 15 m x mm x um Air Dry 0:30 min Diesel and 5w-30 Motor Oil Standard Rinse 1 Acetone 3:00 min 0:30 min 1-Chlorooctadecane Surrogate Spike Rinse 2 MeCl 3:00 min 0:30 min Rinse 3 MeCl 2:00 min 0:30 min Method Summary Rinse 4 MeCl 2:00 min 0:30 min Rinse 5 MeCl 2:00 min 2:00 min 1.

6 Obtain two liters of DI water and acidify to pH<2. Horizon Technology, Inc., 45 Northwestern Dr. Salem, NH, 03079 USA Pg. 1 of 3. Tel: (603) 893-3663 Fax: (603) 893-4994 AN056-100211. Method Detection Limits for EPA Method 8015 Total Petroleum Hydrocarbons Using fully automated extraction equipment Table 3: DryVap Settings Table 5: 5w-30 Motor Oil MDL Results Dry Volume 20 mL Replicate Recovery (mg/L). Heater 1 1 2 Heater Timer Off 3 Autorinse Off 4 5 Results 6 7 The MDL study shown in Tables 4 and 5 below were Average: produced over three non-consecutive days and includes Std. Dev.: seven replicates of each spike. They show that the Diesel MDL: standard is easier to replicate than the oil standard, as indicated by their standard deviations.

7 This is likely caused by the buildup of oil residue within the injection port and Conclusions column of the GC. Also, Figures 1 and 2 below show typical chromatograms from a GC-FID for Diesel and oil From the MDL data shown we can see that, using the respectively. These chromatograms were for 5 ppm spikes complete Horizon Technology solution for extraction , and showed average surrogate recoveries of drying, and concentration, a laboratory will see highly reproducible results. Table 4: Diesel MDL Results Replicate Recovery (mg/L) automated SPE will not only allow you continual 1 compliance with the EPA, but will reduce labor and solvent 2 costs, allow faster turnaround times, and improve on both 3 laboratory precision and accuracy.

8 4 5 Acknowledgements 6 7 Horizon would like to thank Randall Heu and Hawaiian Average: Electric Company for their assistance in performing this Std. Dev.: study. MDL: Figure 1: GC-FID Chromatogram of a 5 ppm Diesel Spike ( Diesel recovery, 86% surrogate recovery). Horizon Technology, Inc., 45 Northwestern Dr. Salem, NH, 03079 USA Pg. 2 of 3. Tel: (603) 893-3663 Fax: (603) 893-4994 AN056-100211. Method Detection Limits for EPA Method 8015 Total Petroleum Hydrocarbons Using fully automated extraction equipment Figure 1: GC-FID Chromatogram of a 5 ppm 5w-30 Motor Oil Spike ( Diesel recovery, 85% surrogate recovery). Horizon Technology, Inc.

9 , 45 Northwestern Dr. Salem, NH, 03079 USA Pg. 3 of 3. Tel: (603) 893-3663 Fax: (603) 893-4994 AN056-100211.