Is Method 1664A Silica Gel Treated N-Hexane Extractable Material (SGT-HEM: Non- Polar Materials) a Measure of Total Petroleum Hydrocarbons?
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1 Is Method 1664A Silica Gel Treated N-Hexane Extractable Material (SGT-HEM: Non- Polar Materials) a Measure of Total Petroleum Hydrocarbons? Dr. Michael W. Miller, NJ DEP Office of Quality Assurance; Michael S. Wright, TRC Omi Environmental Corp. Dr. Alexander M. Allen, ConocoPhillips Bayway Refinery; Boguslaw Dudek, ConocoPhillips Bayway Refinery Contact: M.W. Miller, NJDEP-OQA, P.O.B. 424, Trenton, NJ 08625, miller1@dep.state.nj.us
2 TPH Defined Total Petroleum Hydrocarbons (TPH) is defined by U.S. EPA Method Method 418.1, Aqueous Matrix TPH extracted with Freon 113 Silica Gel Clean-up Extract analyzed by IR Spectroscopy Method can not be used for gasoline
3 Freon 113 Restrictions Montreal Protocol on Substances that Deplete the Ozone Layer, required by Clean Air Act Amendments of 1990 Effective January 1, 2002, laboratories are no longer allowed to purchase Freon 113 that was produced or imported after December 31, 2001 for laboratory analysis
4 Freon 113 Restrictions Recycled Freon will be allowed until 2005 Method requires a quality of Freon 113 that may not be readily available in recycled form
5 Freon 113 Replacement Development of GC methods SW846 Method 8015B GRO, GC/FID Petroleum with carbon numbers C8-C40 NJ OQA-QAM-025 FL TPH SW846 Method 8015B DRO, GC/FID C12-C28
6 Solvent Replacement The USEPA evaluated replacement solvents for Freon 113 and determined that n-hexane had similar extraction properties. Method O&G Development of a method with a gravimetric determinative procedure, USEPA Method 1664A n-hexane Extractable Materials (HEM)
7 USEPA Method 1664A n-hexane Extractable Materials (HEM) Liquid-Liquid and alternatively a solid phase extraction procedure (HEM-SPE) Treating the n-hexane extract with silica gel, 1664A Silica Gel Treated n-hexane Extracted Material (SGT-HEM) Extract is called Non-Polar Material (NPM) Non-Polar Material does not equal Total Petroleum Hydrocarbons.
8 New Jersey Permits Over 400 Discharge Permits specify method Surface Water Ground Water Industrial Discharge ConocoPhillips Bayway Refinery (Bayway) in Linden, NJ is one of these permitees
9 1664A SGT-HEM-SPE vs Side-by-side study procedure based on the Analytical Method Guidance for EPA Method 1664A Implementation and Use (40 CFR part 136), (USEPA, 2000)
10 Experimental Reagents: ACS Reagent Grade Standards: 1664A, stearic acid, hexadecane 418.1, hexadecane, iso-octane, chlorobenzene Hydrocarbons: octane, decane, dodecane, tetradecane Diesel Fuel, Winter Blend #2 Equipment: Horizon SPE-DEX 3000XL Automated Solid Phase Extractor System Horizon SPEED VAPTM II 9000 Solvent Evaporation System Nicolet Impact 410 FTIR
11 Initial Precision and Recovery (IPR) 1664A HEM and 1664A SGT-HEM-SPE HEM IPR must be established before SGT-HEM- SPE can be used for Regulatory samples.
12 Table 1. IPR HEM EPA value %R 87.5% % Pass RSD 15% 11% Pass MDL 1.1mg/L 1.4mg/L Pass SGT-HEM-SPE %R 94% % Pass RSD 9.5% 28% Pass MDL 0.91mg/L 1.4mg/L Pass
13 1664A SGT-HEM-SPE vs Sample sets over 7 weeks Each sample set contained 3 split samples per method Waste water samples obtained before treatment QC of each method followed Three analytical batches Method Bank, Lab. Control Sample (LCS), Matrix Spike
14 1664A SGT-HEM-SPE vs Experimental Method Separatory Funnel Liq. - Liq. Extraction Nicolet Impact 410 FTIR spectrophotometer Method 1664A SGT-HEM-SPE Horizon SPE-DEX 3000XL Automated Solid Phase Extractor System Horizon SPEED VAPTM II 9000 Solvent Evaporation System Evaporation Temperature 28 C
15 Table A SGT-HEM-SPE vs 418.1Comparison 1664A SGT-HEM PHC Data Set 'i' Data Set 'j' Date Raw Data (ppm) 11/15/ /18/ /19/ /05/ /06/ /09/ /12/ /16/02*
16 Table 2a. 1664A SGT-HEM-SPE vs 418.1Comparison Date 1664A SGT-HEM Data Set 'i' PHC Data Set 'j' Log Transformation 11/15/ /18/ /19/ /05/ /06/ /09/ /12/
17 Table 2b. 1664A SGT-HEM-SPE vs Comparison 1664A SGT-HEM Data Set 'i' PHC Data Set 'j' Triplicate Means Date Mean STD. DEV. Mean STD. DEV. Mean TM"i", TM"j" 11/15/ /18/ /19/ /05/ /06/ /09/ /12/
18 Table 2c. 1664A SGT-HEM-SPE vs 418.1Comparison Method Specific Mean for Data Set 'i' Method Specific Mean for Data Set 'j' Mean-Square Error Root Mean Square Deviation RMSD (max) Method by Sample Interaction F calc Ratio F(value)
19 Effect of Evaporation Temp. on Hydrocarbon Recovery Hydrocarbon standards: n-octane (C8), n- decane (C10), n-dodecane (C12), n-tetradecane (C14) and Winter Blend #2 (diesel) Seven (7) aliquots of each set of standards (total 35 samples) evaporation at 28 C, and at 45 C (specified Horizon SPEED-VAP ) 1664A SGT-HEM-SPE Distillation of Winter Blend #2: Water bath 85 C to achieve a vapor temperature of 70 C
20 Table 3. Effect of Temperature on Recovery of Low Mol. Wt. TPH C8 C10 C12 C14 Diesel Mean 28 o C SD 28 o C Mean 45 o C SD 45 o C 0.93% 21.3% 77.0% 89.3% 85.8% % 6.88% 59.1% 90.9% 83.8% t value Sig. Diff. 2 sample No Yes Yes No No
21 Recovery of Diesel Using Method1664A SGT-HEM-SPE Conditions: Diesel: Winter Blend #2 Distillation: Water Bath 85 C, Vapor Temp. 70 C Dry Extract in Oven 1 hr. at 70oC Results: Seven (7) Samples Study Mean 30.4% Std. Dev RSD 9.4%
22 Conclusions: Discharge Side by Side Comparison A direct correlation was not established between the results from method and method 1664A SGT-HEM-SPE Each method produce higher or lower results based on sample conditions Biological oxidation and extended aeration, are used to treat the Bayway wastewater prior to discharge Discharge expected to contain only higher weight organic compounds, EPA1664A SGT-HEM-SPE should be considered suitable for quantification At an evaporation temperature of 28 C, the mean recovery of the modeled discharge material (diesel fuel standard) was 85.8%
23 Conclusions: Temp. Dependence 1664A SGT-HEM-SPE PHC compounds with carbon numbers as low as C12 can be recovered using an evaporation temp. 28 C At 45 C method 1664A SGT-HEM-SPE is not suitable for PHC compounds with carbon numbers less than C A SGT-HEM-SPE distillation procedure for recovering NPM from n-hexane extract cannot be use for materials with Mol. Wts. similar to diesel or #2/3 fuel oil
24 Conclusions Method and Method 1664A SGT-HEM-SPE are empirical methods designed to measure a mixture of compounds Molecular Weight distribution of discharge should be known The recovery of NPM in Method 1664A SGT-HEM-SPE is Temperature dependent Since every discharge has different composition a comparison study should be performed between Method and Method 1664A SGT-HEM-SPE
25 Method Recommendations Petroleum Type Gasoline Kerosene <C14 Diesel/ Fuel Oil #2 Fuel Oil #4/#6 Analytical Method SW B GRO GC/FID C8-C40 SW B DRO 1664A SGT-HEM 28 C 1664A SGT-HEM 28 /45 C GC/FID C8-C40
26 Acknowledgments The NJDEP has not subjected this manuscript to internal review. Therefore, the research results presented herein do not, necessarily, reflect Departmental policy. Mention of trade names of commercial products does not constitute endorsement or recommendation for use. The authors wish to thank Ms. Barbara J. Andrukiewicz, ConocoPhillips Bayway Refinery Laboratory Manager, for conducting the project at the facilities laboratory. The authors also wish to thank Ms. Denise Scangamor of the TRC Omni Environmental Corporation staff for formatting the paper and Dr. Bernie Wilk, and Marty Hackman of NJDEP- OQA for their technical and editorial suggestions.
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