ADVANCES IN MICRO GAS CHROMATOGRAPHY

Transcription

1 ADVANCES IN MICRO GAS CHROMATOGRAPHY

2 Fast Analysis of Hydrogen Sulfide in a Natural Gas Matrix using a Temperature Programmable Micro GC Fusion Gulf Coast Conference 2015 Debbie Alcorn INFICON, Inc. 2 Technology Place East Syracuse, NY 13057, USA INFICON Advances in Micro Gas Chromatography 2

3 Outline Natural Gas and Hydrogen Sulfide Analysis Micro GC History Micro GC Fusion Features Micro GC Configuration Diablo EZReporter for Physical Property Calculation Isothermal versus Temperature Programming Repeatability and Data Conclusion INFICON Advances in Micro Gas Chromatography 3

4 INFICON Global Presence 900 employees; offices in 17 countries INFICON Advances in Micro Gas Chromatography 11/18/15 4

5 Natural Gas Analysis Natural gas composition analysis is critical for : Producers and gatherers Gas distribution companies Gas utility companies Gas engine and appliance manufacturers Independent testing laboratories Due to variations in natural gas composition, it is important to measure physical properties, especially for custody transfer situations Hydrogen sulfide (H 2 S) occurs naturally in natural gas Software automatically calculates physical properties such as: Heating Value (BTU/cu. ft) The amount of heat released during the combustion of a specified amount of a substance Relative Density/Specific Gravity The ratio of the density of a substance to the density of water INFICON Advances in Micro Gas Chromatography 11/18/15 5

6 Hydrogen Sulfide Analysis H 2 S facts: Toxic and corrosive 10 ppm is the OSHA permissible exposure limit (PEL) ppm can deaden a person s sense of smell 800 ppm is the lethal concentration for 5 minutes of exposure Foul odor Can occur in high percentage in natural gas H 2 S is removed from gas streams to prevent damage to equipment and personal injury It is desirable to have a transportable instrument to analyze both high and low level H 2 S in a natural gas matrix

7 Micro GC History 3000 Micro GC (µgc) has over ten years of proven excellent analytical performance Micro GC Fusion expands the capability of the 3000 Micro GC INFICON Advances in Micro Gas Chromatography 11/18/15 7

8 3000 Micro GC Microelectromechanical systems (MEMS) based GC Isothermally heated capillary columns Micro Thermal conductivity detector (µtcd) Analysis can be conducted directly on-site or in a lab 3000 Micro GC in the field 3000 Micro GC in the lab INFICON Advances in Micro Gas Chromatography 11/18/15 8

9 The Next Generation Micro GC Fusion Micro GC Fusion builds on proven 3000 Micro GC technology Utilizes the same MEMS injectors and TCD Traditional Micro GC technology is limited due to: Isothermal column temperature, leading to long run times and potential carryover issues Ambient temperature effects Software and operating system compatibility Micro GC Fusion addresses these issues using new technology INFICON Advances in Micro Gas Chromatography 11/18/15 9

10 Micro GC Fusion Features Micro GC Fusion new features include: Temperature programmable columns for fast temperature ramping Additional heated zones to minimize ambient temperature effects Web-based interface to eliminate software compatibility issues Front panel display Solid-state hard drive for data storage Optional integrated sample conditioner INFICON Advances in Micro Gas Chromatography 11/18/15 10

11 Benefits of Temperature Programming Temperature ramping based on resistive column heating allows for: Faster runs Rapid column cleaning Sharper peaks Expanded application range (ex. extended natural gas analysis) Ramping profile is independently optimized for each module Cooldown time is optimized to achieve short cycle times

12 Integrated Sample Conditioner An optional integrated sample conditioner can be configured The sample conditioner allows for: Reduction of sample pressures of up to 1000 psi down to approximately 5-10 psi Filtering of particulates Heated sample at 100 C A quick connect replaces the standard 1/16 in. inlet

13 Calibration Gas Standards Extended Natural Gas Component Calibration Gas Concentration Nitrogen 1.550% Carbon Dioxide 1.201% Methane % Ethane 3.001% Propane 1.996% Isobutane 1.003% n-butane 0.998% Isopentane 0.299% n-pentane 0.300% C6s 0.598% C7s 0.332% C8 Plus 0.068% Component H 2 S Air Component H 2 S Methane Calibration Gas Concentration 100 ppm Balance Calibration Gas Concentration 25 ppm Balance

14 Natural Gas Analysis - Rt-Q-Bond Column: 12m RT-Q-Bond Injector: Variable Ramp: 45 C 250 C (2.5 C/s) INFICON Advances in Micro Gas Chromatography 11/18/15 14

15 Isothermal vs. Temperature Programming Isothermal runs result in broad, late eluting peaks Isothermally, analyzing up to C8 Plus components could take over 20 to 30 minutes Temperature programming elutes C8 Plus compounds within 5 minutes A 100 ppm H 2 S in air standard was diluted with extended natural gas to demonstrate the benefit of temperature programming

16 Isopentane n-pentane Propane Isobutane n-butane Ethane Isothermal Column: 20m Rxi-1ms Injector: Large Variable Column Temperature: 45 C Hexanes ~30 ppm H 2 S Heptanes Octanes Plus 18 minutes

17 Isopentane CO2 n-pentane Isobutane n-butane Propane Ethane Ethane Propane Temperature Programming Column: 20m Rxi-1ms Injector: Large Variable Ramp: 45 C(85s) 200 C (100s), 1.5 C/s ~30 ppm H 2 S Hexanes Heptanes Octanes Plus 270 seconds

18 Diablo EZReporter for Physical Property Calculation Allows customized viewing of results Calculates physical properties such as: Component and gross heating values (BTU/cu. ft) Relative density (specific gravity) Wobbe Index And more Creates reports in PDF, CSV, or TXT format INFICON Advances in Micro Gas Chromatography 11/18/15 18

19 Micro GC Fusion Repeatability - NGA Percent relative standard deviation (%RSD) is used to measure instrument performance 10 runs were conducted using the extended natural gas standard Property Gross Heating Value Ideal (BTU/cu. ft) Gross Heating Value Real (BTU/cu. ft) %RSD Component (Rt-Q-Bond) Calibration Gas Concentration Retention Time %RSD Concentration/Area %RSD Nitrogen 1.550% Carbon Dioxide 1.201% Methane % Ethane 3.001% Propane 1.996% Isobutane 1.003% n-butane 0.998% Isopentane 0.299% n-pentane 0.300% C6s 0.598% Group range C7s 0.332% Group range C8 Plus 0.068% Group range 2.76

20 Compliance with GPA 2261 Component (Rt-Q-Bond) Repeatability Calibration Gas Concentration Acceptable Range 10 Run Average Normalized Concentration Pass/Fail Nitrogen 2% 1.550% Pass Carbon Dioxide 3% 1.201% Pass Methane 0.2% % Pass Ethane 1% 3.001% Pass Propane 1% 1.996% Pass Isobutane 2% 1.003% Pass n-butane 2% 0.998% Pass Isopentane 3% 0.299% Pass n-pentane 3% 0.300% Pass Hexanes Plus 10% 0.998% Pass INFICON Advances in Micro Gas Chromatography 11/18/15 20

21 Micro GC Fusion Repeatability H 2 S Percent relative standard deviation (%RSD) is used to measure instrument performance 10 runs were conducted using 25 ppm H 2 S in methane Component Calibration Gas Concentration Retention Time %RSD Concentration /Area %RSD H2S 25 ppm

22 Propane Ethane Ethane Propane Low PPM H 2 S Analysis 25 ppm H 2 S in methane was diluted to ~ 2.7 ppm H 2 S using a gas tight syringe with the extended natural gas standard Column: 20m Rxi-1ms Injector: Large Variable Ramp: 45 C(85s) 220 C (100s), 2 C/s ~2.7 ppm H 2 S

23 Conclusion Micro GC Fusion is an ideal instrument for natural gas and H 2 S analysis Micro GC Fusion shows excellent separation of low level H 2 S on the Rxi-1ms column Using new temperature programming, a full analysis up to C8 Plus can be conducted in under 5 minutes INFICON Advances in Micro Gas Chromatography 11/18/15 23

24 For more information, visit: Or Booth #440 24

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