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Hit “esc” to quit hit any key to continue Effects of Aging on Surface Inertness and Analyte Recoveries in SUMMA Passivated and Fused Silica Lined Canisters.

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Presentation on theme: "Hit “esc” to quit hit any key to continue Effects of Aging on Surface Inertness and Analyte Recoveries in SUMMA Passivated and Fused Silica Lined Canisters."— Presentation transcript:

1 hit “esc” to quit hit any key to continue Effects of Aging on Surface Inertness and Analyte Recoveries in SUMMA Passivated and Fused Silica Lined Canisters

2 hit “esc” to quit hit any key to continue Objectives Test Canisters from 4 Manufacturers for the Relative Aging Effects of Repeated Sampling on TO14 Standard Recoveries Repeat Test After Exposure to 1% Ozone for 8 hours Test Aged Canisters using a Spectra Gas TO15 Mixture

3 hit “esc” to quit hit any key to continue Canisters in Study 4 Manufactures - 2 SUMMA, 2 Fused Silica Lined 2 Cans from Each Manufacturer SUMMA cans labeled S1 - S4 Fused Silica Lined Canisters Labeled FS1-FS4

4 hit “esc” to quit hit any key to continue Silonite Coated 6L Canisters

5 hit “esc” to quit hit any key to continue Silonite TM Coating of Canisters Improves Recovery of Reactive Compounds Increases Range of Compounds Amenable to Canister Sampling and Analysis Compounds Containing: –Sulfur –Nitrogen –Oxygen

6 hit “esc” to quit hit any key to continue Analysis of Cylinder - 9 December ppm 2.65 ppm 2.54 ppm Analysis of Mini Canister # December ppm 2.44 ppm Analysis of Mini Canister # December ppm 2.56 ppm Let time pass.... Analysis of Mini Canister # January ppm 2.53 ppm Analysis of Mini Canister # January ppm 2.47 ppm 40 Day Formaldehyde Stability in Silonite Coated MiniCan Data Courtesy of Dr. Daniel Riemer, NCAR

7 hit “esc” to quit hit any key to continue New Silonite CanisterUsed SUMMA Canister 10 PPB TO14 Std 5 PSIG Holding Time - 1 Day 1-Day TO14 Stability 10PPB

8 hit “esc” to quit hit any key to continue Clean up Test Blank Test After 100 PPB TO14 Exposure New Silonite CanisterUsed SUMMA Canister

9 hit “esc” to quit hit any key to continue Canister Study Test all Canisters at the Beginning of Study –Fill Canister with 10 PPB TO14 Mix –Equilibrate 1 Day and Analyze Clean All 8 Canisters Together (3 cycles at 100 C) Fill Canisters with Ambient Air using Glass Filtered Grab Sampler Wait 1 Day, then Repeat Cleaning Perform Operation 30 Times

10 hit “esc” to quit hit any key to continue 8 Canister Cleaning System

11 hit “esc” to quit hit any key to continue Glass Filtered Grab Sampling

12 hit “esc” to quit hit any key to continue Standard Introduction and Analysis

13 hit “esc” to quit hit any key to continue Automates the GC analysis of gas phase samples Complete heating of sample flow path. Easily accessed for trap and tubing replacement Multiple trapping stages allow matrix to be eliminated before GC injection Stage Preconcentrator 7100 Preconcentrator

14 hit “esc” to quit hit any key to continue Internal Standard Calibration Standard Sample Glass BeadsTenax Cryogen in N2, O2 H20, CO2 Focuser To GC Helium PUMPMFC Helium Carrier 7100 Preconcentration and Matrix Management 3-Stage Preconcentration Sample Headspace

15 hit “esc” to quit hit any key to continue Fast Injection and Proper Water Management Minimizes Tailing of Polar Compounds Column: HP1, 60m, 0.32mm ID, 1um film. Flow rate: 1.5 ccm Carrier: He

16 hit “esc” to quit hit any key to continue New SILONITE Coated Canister Before Study Concentration - 10 PPB Pressure - 10 PSIG Volume CC Water Management - Microscale Purge and Trap Instrumentation 7100/5973 Column - DB1 Starting Temperature - 35 deg. C Scan , 6 min, then amu

17 hit “esc” to quit hit any key to continue S1S3 10 PPB/10 PSIG TO14, 1 Day Stability - SUMMAs

18 hit “esc” to quit hit any key to continue FS 1FS 3 10 PPB/10 PSIG TO14, 1 Day Stability - FSL Cans

19 hit “esc” to quit hit any key to continue S1S3 10 PPB/-4 PSIG TO14, 1 Day Stability - SUMMAs

20 hit “esc” to quit hit any key to continue 10 PPB/-4 PSIG TO14, 1 Day Stability - FSL Cans FS 1 FS 3

21 hit “esc” to quit hit any key to continue FS 1 10 PPB/-4 PSIG TO15, 1 Day Stability - SUMMAs FS 3

22 hit “esc” to quit hit any key to continue 10 PPB/-4 PSIG TO14, 1 Day Stability - FSL Cans FS 1FS 3

23 hit “esc” to quit hit any key to continue Possible Reasons for Poor Recoveries in Canisters Coating or Surface Treatment was not Initially Inert Welds have Active Surfaces Contaminants have been Introduced –Particulates –Semi-Volatiles –Reaction Products –Dirt

24 hit “esc” to quit hit any key to continue Pressurized Field Sampling Causes Condensation of Water in transfer lines and Canisters Water can Promote Polymerization Reactions White Deposits Found in Bottom of Canisters which were Repeatedly Sampled to Positive Pressure in the Field Not Required for Today’s Samplers / Analyzers

25 hit “esc” to quit hit any key to continue Removing Heavy Contaminants from Canisters Evacuate Canisters Use Vacuum to Draw in 200 cc of DI Water Heat to 60 deg. C for 8 Hours (or Overnight) Pressurize Cans to 20 psig Shake Canister Well, Invert, Blow out Water Perform Normal Cycle Cleaning

26 hit “esc” to quit hit any key to continue Conclusion Both SUMMA and Fused Silica Lined Canisters Showed no Detectable Loss of Inertness after 30 Samplings of Ambient Air Although Individual Recoveries of TO15 Standard Varied, Both Canister Types Provided Good Recoveries of Spectra Gas TO15 Compounds Ozone Exposure did not Change Recoveries Canister Cleanliness is Extremely Important. Canisters Should be Checked Regularly for Analyte Recovery If Recoveries are Found to be Low, Enhanced Cleanup Techniques are Available to Remove Adsorbing / Absorbing Contaminants


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