Copyright 2009 PerkinElmer LAS and CARO Analytical Services, Inc.
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1 Optimizing Sampling and Analytical Parameters for Soil Vapour Samples using Automated Thermal Desorption / Gas Chromatography / Mass Spectrometry (ATD/GC/MS) Stephen Varisco, Technical Manager, CARO Analytical Services Lee Marotta, GC/MS Product Specialist, PerkinElmer LAS Miles Snow, GC/MS Product Specialist, PerkinElmer LAS Copyright 2009 PerkinElmer LAS and CARO Analytical Services, Inc.
2 Outline Objective: Soil Vapour Tube Background CARO Analytical Services Soil Vapour Regulations Thermal Desorption Technology Advantages Operation Tube Design and Adsorbent Optimization Limitations of current tubes for soil vapour samples Objectives of new tube New Tube Performance Characteristics
3 Background information on CARO Analytical Services British Columbia based Full Service Environmental Testing Capabilities Technical Leadership in Soil Vapour Co-authored BC SV Reference Methods ISO Accreditation for SV ( Client Collaboration Knowledgeable & Accessible Staff Equipment Rentals, Client Training SR&D Projects VOC Artifacts in Tubing ( Custom TD Tube Development VOC Sorption on Tubing in progress
4 Regulatory Background 23 US States regulate Soil Vapour Intrusion British Columbia Contaminated Sites Regulations, Schedule 11 Effective January 1, regulated parameters: >90% via TD Stringent regulations Trichloroethene (TCE) 1.0 ug/m 3 (dry cleaning site) Benzene 1.5 ug/m 3 (gasoline site) Why is soil vapour important? Protection of Human Health Test water and soil first? Or Test vapour first?
5 Advantages and Operation of Thermal Desorption Technology
6 Advantages of Thermal Desorption Technology Air Toxics Charcoal Tubes 1. Established methodology 2. Convenient transport 3. Easy to clean immediate reuse fast turnaround 4. Cost effective 5. Large sample volumes 6. Suitable for non-polar and polar compounds 7. Inherent Water Management 8. Enables Recollection to preserve sample
7 State 1: Sample Tube Desorption IS and/or surrogate spike Optional inlet split Desorb flow Temperature Flow Time xxxxxx Peltier-cooled trap no need for liquid cryogen Inert gas
8 Stage 2: Transfer of Sample to Instrument Optional outlet split or Recollect on same tube or new tube Column Flow = 2.5mL/min Recollect Flow = 10mL/min %Recollected = 80% GC Detector heated trap Carrier gas in Analytical column
9 Optimizing Sample Integrity with Thermal Desorption Automatic Internal Standard addition Recollection onto the same tube or new tube Automated Leak Checking Impedance Testing Excellent Water Management
10 Total Ion Chromatogram of a 74 TO-15 and TO-17 Component Mix Linearity AT_032609_ Mass Range: 35 to 300 AMU Conc: 20ng on Column Broad Boiling Point Range: Chloromethane to Naphthalene Mar :37: Scan EI+ TIC 3.23e % Time
11 Tube Design and Adsorbent Optimization
12 Thermal Desorption Tube Multiple Adsorbents accommodate wide boiling point range sample Weaker Adsorbent Strong Adsorbent Strongest Adsorbent Sample Stream Carrier for Desorption DESORB ADSORB
13 Goal Optimize a Tube for Soil Vapour Intrusion Sampling Soil vapour differs from other air sampling applications: Higher moisture Greater analyte range Wider concentration range Limitations of current industry-standard sorbent tubes: Lack of a weak adsorbent prevents release beyond nc12 Ensure Safe sampling volumes for the low boilers
14 Characteristics of New Thermal Desorption Tube Broadest Analytical Range dichlorodifluoromethane to phenanthrene nc3 nc22+ Protects the Strong Adsorbents Prevents irreversible adsorption Clean after one desorption cycle Good Safe Sampling Volumes Optimal Water Management
15 Soil Vapour Intrusion Tubes Performance Characteristics
16 Precision, Linearity (average for Class) and Reporting Limits Instrumentation: PerkinElmer TurboMatrix 650 Thermal Desorber PerkinElmer Clarus 600 GC/MS Compound Class # Comp Precision (%RSD) Dynamic Range Reporting Limit Outliers n=8 0.2 to 200 ng 10 liter sample (FS) on RL Gasses 6 6.9% ug/m3 non-aromatic Halogens % ug/m3 CHCl 3 =0.05ppb Aromatics % ug/m3 Halogenated Aromatics 9 1.4% ug/m3 Others % ug/m3
17 Recovery Results EXCELLENT 79 components investigated 400ng VOC mix + 250ng PAH Range: difluorodichloromethane to phenanthrene Recovery procedure Analyzed spiked tube Analyzed blank tube Re-analyzed spiked tube which should be clean Non-detectable carryover Slight carryover of 4 heaviest PAHs Significantly below method criterion PAH Compounds % Carryover (very low) 1-Methyl Napthalene 0.3 Anthracene 0.2 Fluorene 0.6 Phenanthrene 1.2 AT_040809_07 % 0 AT_040809_11 % 0 Spiked Tube Re-inject of spiked tube Apr :13:55 Scan EI e Scan EI e8 Time
18 Tube Robustness Diesel Carryover <1% new 650_040809_ ,000ng Diesel spiked tube Apr :57:46 Scan EI+ TIC 6.96e8 % new 650_040809_ Reanalysis of this tube to determine Carryover Scan EI+ TIC 6.96e8 % Time
19 What is Breakthrough? Goal: Regulated compounds do not break through EPA TO-17: The volume sampled when the amount of analyte collected in a back-up sorbent tube reaches a certain percentage (typically 5%) of the total amount collected by both sorbent tubes Calculation: BT / (BT+spiked)*100% BT = concentration of back tube Spiked = concentration of front tube Safe Sampling Volume (SSV): 2/3 of Breakthrough Volume Assessing breakthrough in the real-world: Sampling in series Sampling in parallel (distributed volume pairs)
20 Manifold used for determining breakthrough & moisture retention Injector Nitrogen carrier gas Spiked Clean water bubbler Sample Tube spiked 300ng of 79 components Total = 23,700ng on tube Passed humidified N 2 through tube flow rate = 100mL/min Time = 100min Mimic 10L sampling All studies performed in triplicate
21 Slight Breakthrough of only two Components out of 79 VOCs VOC gasses: 10L of sample 70% humidity Component % BT Dichlorodifluoromethane 1.0 Chloromethane 5.4 Vinyl Chloride nd Bromomethane nd Chloroethane nd Trichlorofluoromethane nd
22 Water Management
23 Methods of Water Removal 1. Nafion Drier / Desiccants Polar Compounds Removed - Cannot be used 2. Hydrophobic adsorbents 3. Minimize sampling volumes while maintaining regulated detection limits 4. Dry Purging Typically not required for indoor air
24 Why Remove Moisture? Mass Spectrometer (detector) problems Signal quenching Increased maintenance Poor chromatography Can cause false negatives AT_050609_BT_ With Dry Purge 3.54 Water 07-May :49:07 Scan EI+ Sum 1.85e7 AT_050209_BT_ No Dry Purge May :04:33 Scan EI+ Sum TIC 1.59e9 1.85e % 6.43 % Time 01 Time
25 Real World Sample Petroleum Contamination (Tank Pull Site) Abundance Component Result (ug/m3) 1,2,4-trimethylbenzene ,3,5-trimethylbenzene 16.2 Benzene 1.6 Dichlorodifluoromethane 9.1 Ethylbenzene 12.3 Naphthalene 20.9 Tetrachloroethene 9.9 Toluene Trichlorofluoromethane Xylenes (total) 80.0 nc6-nc TIC: a-39.D Time--> nc6 nc10 nc13
26 Summary Thermal Desorption Technology Tubes well-suited for vapour intrusion investigations Instrumentation Advancements Analytical Integrity Team developed new Thermal Desorption Tube that Achieves 1. Broadest Analytical Range 2. Protection of the Strong Adsorbents 3. Good Safe Sampling Volumes 4. Optimal Water Management Presentation available for download at or
27 Acknowledgements Project Team: CARO Analytical Services: Stephen Varisco, Technical Manager Luba Tsurikova, Senior Analyst Patrick Novak, Business Manager Brent Mussato, President PerkinElmer: Lee Marotta, Senior Product Specialist Miles Snow, Senior Product Specialist Copyright 2009 PerkinElmer LAS and CARO Analytical Services, Inc.
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