CHALLENGES WITH PETROLEUM SPILL CHARACTERIZATION Ralph Ruffolo Ontario Ministry of the Environment and Climate Change Laboratory Services Branch 125

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1 CHALLENGES WITH PETROLEUM SPILL CHARACTERIZATION Ralph Ruffolo Ontario Ministry of the Environment and Climate Change Laboratory Services Branch 125 Resources Road, Toronto, Ontario, CANADA M9P 3V6

2 Ministry of the Environment and Climate Change Laboratory Services Branch Created in 1972 with a current staff complement of just over 2000 staff Laboratory Services Branch has 140 staff (Full service laboratory 160,000 square feet) The Branch provides analytical laboratory services for the needs of the Ministry of the Environment and Climate Change to ensure: a province-wide full service analytical laboratory that delivers readily available and high quality analytical testing Organic, Inorganic, General Chemistry, Microscopy, Microbiology and Toxicology testing Provide support of compliance, abatement, enforcement, litigation, audit of drinking water quality, environmental monitoring programs and standard setting initiatives Emergency analytical response on a 24/7 basis as needed Patriciate on international analytical committees Provide expert consultation and reference centre services for environmental analysis 2

3 Topics Covered Background on petroleum hydrocarbon analysis Canadian perspective Conventional analytical approach Environmental Case Studies Look at some advanced methodologies Additional forensic indicators/techniques Challenges to consider 3

4 Typical Chemical Components in Petroleum It is not practical to measure each chemical component separately Varying methods of sample preparation/analysis will yield vastly different results 4

5 Data Reported Why Standardize Petroleum Methods? Prior to 2004 in ONTARIO No uniform analytical methodology No defined reporting No standardized calibration Thus: Between laboratory results were incomparable Considered a new approach METHOD STANDARIZATION PHC Data from Interlab Study Design Value Recovery 35% to 350% Interlab Median Reference Method for the Canada-Wide Standard Petroleum Hydrocarbons in Soils Tier 1 Canadian Council Ministers of the Environment 5

6 Canadian Council of the Ministers of the Environment (CCME) PHC Method Highlights Contains prescriptive and prescribed benchmark elements Standardizes preparation, calibration, analysis and reporting Standardized reporting of petroleum hydrocarbons F1 (nc 6 to nc 10 ) volatile fraction Purge and Trap (benchmark) GC/FID F2 (nc 10 to nc 16 ) F3 (nc 16 to nc 34 ) extracted followed analysis by GC/FID F4 (nc 34 to nc 50 ) Soxhlet (benchmark) F4G (silica gel treated) Gravimetric Requires a single silica gel treatment with a prescribed amount Intent of the silica gel is to remove natural biogenic content in samples 6

7 Petroleum Product Profiles by GC/FID nc 10 to nc 50 Range Norm. 800 FID1A, ( \11045K D) Gasoline Norm FID1A, ( \11007K D) Diesel fuel gasoline min min FID1A, ( \10327K D) *FID1 A, ( \10022J D \10022J D) Norm W30 Oil pa Bunker C min min FID1A, ( \11045K D) Norm Transmission fluid Norm FID1A, ( \10321K D) Crude min min Useful in distinguishing petroleum products 7

8 Case 1: Product Found in an Open Pit Remediation activity were being conducted from a fuel oil UST removal (under Officers Order) Neighbouring property detected some strong odour which lead to finding pure product in an open pit. Two samples were analyzed one from January and a second from September 8

9 Samples Collected from Open Pit in January and September FID1A, ( \17265K D) pa GC/FID September sample Degraded Fuel Oil nc 13 nc 22 0 pa FID1A, ( \17020K D) nc 16 min nc 10 nc 20 January sample Fuel Oil min 9

10 Samples Collected from Open Pit January sample September sample 10

11 Biomarker Analysis Biomarkers are more resilient and less prone to weathering Biomarkers signatures are related back to the original crude oil Fingerprinting analysis by Mass Spectrometry Typical n-alkanes distribution (n-c 10 to n-c 40 ) Branched alkanes (pristane and phytane) Bicyclic sesquiterpanes (C 14 to C 16 ) at m/z 123 Biomarker terpanes/hopanes at m/z 191 Biomarker steranes at m/z 217 and 218 sesquiterpane terpanes 11

12 (m/z 123) 10 common (m/z 191) 25 common 12

13 Instrumentation GC/FID Gives response if compound burn/combust Gives equal response independent of molecular weight Inexpensive (excellent candidate for petroleum) GC/MSD Yields structural information based on the fragmentation pattern of ionized molecules (biomarkers) However, can get significant mass discrimination MSD can operates in Full Scan or Selected Ion Monitoring (SIM) 13

14 Alkanes and Isoprenoids m/z - 85 nc 17 nc 18 pristane phytane January sample September sample 14

15 Sesquiterpane Biomarkers m/z ` 8 nc 13 to nc 18 range January sample September sample These appears to be two different sources and are not related 15

16 CASE 2: Mysterious Ooze Leaking from Two Potential Sources into a Tributary Two potential inputs 1. Municipal service manhole 2. Storm water input from adjacent apartment complex 16

17 Sampling of Outfall and 2 Potential Sources pa FID1A, ( \17020K 020.D) Manhole Fuel oil pa min FID1A, ( \17020K 021.D) GC/FID monitoring well Lubricating oil min *FID1A, ( \17020K 014.D \17205K 02.D) pa nc 10 nc 16 nc 22 Outfall Combination? nc min 17

18 Sesquiterpane SIM Experiments m/z nc 13 to nc 18 range Outfall 2 4 Manhole 9 1 MSD not sensitive enough even in SIM mode 18

19 An Additional Sample was Collected Serval Months Later pa FID1A, ( \17130K D) May - manhole sample pa pa min FID1A, ( \17020K D) January manhole sample min FID1A, ( \17020K D) January - monitoring well sample min 19

20 Are Manhole Product Samples From May and January the Same? m/z nc 13 to nc 18 range 2 4 May - manhole sample January manhole sample

21 8 Biomarker Ratios : good agreement indicating these samples are same source 21

22 Case 3: Barge Sinks in Harbour Late Winter : EMERGENCY RESONSE (10 days) partially submerged barge reported about 1,200 litres (320gal) of diesel fuel and 100 litres (27gal) of hydraulic fluid. WTP shut down. About 10,000 peoples drinking water affected. Boil water advisory in place for about 10 days. 22

23 23 Samples obtained during barge recovery along with a surface water sample from Bay

24 nc 10 Product 1: brown sludge from boomed area nc 16 nc 20 Diesel fuel Product 2: collected from surface of water in boomed area Hydraulic fluid nc 18 nc 40 Sample collected from surface of water in Bay near water intake Is this a mixture of both products? 24

25 Sesquiterpane Biomarker : Full Scan m/z Product 1 (diesel) Bay sample Product 2 (hydraulic) MSD not sensitive enough in Full Scan 25

26 Sesquiterpane SIM experiments m/z nc 13 to nc 18 range 2 4 Product 1 (diesel) Bay sample Product 2 (hydraulic) Better but still not great

27 Sterane/Hopane Biomarker SIM experiment m/z nc 21 to nc 34 range 4 11 Bay sample Product 2 (hydraulic) Product 1 (diesel) 9 1/8 2/8 7/8 9/8 5/6 9/8 10/8 11/8 13/8 15/8 correlation coefficient Bay sample Product Product

28 Closing Comments GC/FID data can be extremely useful in identification of product type Standardized petroleum methods facilitate data comparison between laboratories Biomarker data can often provide an additional line of evidence for source tracking THANK YOU 28

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