OP OPTOGRAF RAF TM : Process RAMAN for Gas Phase Analysis A New - - PowerPoint PPT Presentation

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OP OPTOGRAF RAFTM:

Process RAMAN for Gas Phase Analysis – A New Univariate “Pipe Centric” Process Analyzer

Peter van Vuuren OptografTM Product Manager Kaiser Analytics Ann Arbor, MI

Edmonton ISA Dinner Meeting – February 2013

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• Optograf Data – Optograms
• Optograf Application Processes
• Optograf Hardware
• Process Interfaces – OptoDRS and OptoAST

Topics

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Optograf Airhead Fiber Optic Probe – Sample Interface OptoDRS/AST – Process Interface

What Kind of Data does the Optograf Produce, How is it Analyzed?

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Seconds

5 15 35 45 55 65 75 25 55

Gas Chromatography: Bread and Butter Technique for Petrochemical Analyses

Benefits of Chromatography:

• Speciation
• Peak Area Analysis
• Simple Calibration
• Technician Friendly - Chromatogram

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*

Not a Chromatogram, but a RAMAN Gas Phase Spectrum

• r Optical “Chromatogram" or “Optogram”

RAMAN Spectrum of Syngas Stream

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*

“Optical” Chromatogram (Optogram) of Syngas

• In Service at a Major

Coal Gasification Facility in SA

• At ~ 100 psig
• Peak area analysis
• 2 – 5 min cycle/update

times

• Probes in existing GC

fast loops

• Calibrate/Validate

with GC standard

• Excellent correlation

with Lab Analysis

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Benefits of Optography

Transition to Optography is easy:

• Technicians already know how to handle the data
• Know how to calibrate
• Know how to validation
• Know how to analyze

Only need to know hardware maintenance

• Simpler to learn to maintain

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Industrial Applications of RAMAN

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– –

this

SYNGAS

Gasifier

Coal Coke Biomass Waste Black Liqour Flexi- coking Natural Gas

Ammonia/ Fertilizers Electricity/ SNG/ FuelCell

IGCC

Synthetic Fuels

Gasoline/Diesel

Methanol Oxo-Alcohols DME Steel

DRI Process

Tailgas Conversion Gas Treatment

Rectisol Amine Treatment

Reformer H2

Refinery

Raw Syngas

UCG*

*UCG = Underground Coal Gasification

SYNGAS Production/Utilization

Bitumen

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* * * *

Raw Gasifier Syngas – Depending on Feed, akin to Sour and Acid Gas

• This sample contains all the

components (and more) of Sour and acid Gas streams except Ar/H2O

• The peaks for the relevant

components will be at the same frequency; only the peak heights (and peak areas) will be different

N2

Not measured (redundant)

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Syngas - Chemical Plant

*H2 H2 CO CH4 CO2 N2

* * * *

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AGR SRU/TGT

Refinery Processes – RAMAN Opportunities

Refinery Gas Hydrotreaters – Recycle Gas H2 Production Other

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H2 CO2 CH4 CO CH4 H2 88 vol% CH4 10 vol% CO 1 vol% CO2 1 vol% Pressure: 100 psig Temp: 25 degC

H2 Recycle Gas

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Typical Steam Cracker Process Application of Optograf & TDLAS

Optograf Applications typical in the Hot Ends:

• 1. Feed

Ethane Ethane /Propane

• 2. Feed Butane
• 3. TLA Measurement

Severity/Selectivity

• 4. Cold Box Effluent

H2/Fuel gas

• 5. Demethanizer OVHD
• 6. De-ethanizer OVHD

1 6 5 4 3 2 8 7 TDLAS Applications typical in the Cold Ends:

• 7. CO2 after Caustic Wash/Dryer
• 8. Acetylene Converter Midbed
• 9. Ethylene Quality

NH3 Acetylene Moisture CO2 9

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H2 Product - Chemical Plant

*H2

* * * *

H2 CH4 Impurities: Propylene, Ethylene, CO2, O2

C3H6 O2 H2 CH4 CO2 C2H4 CO2 C2H4

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Benzene Product + Toluene Overlay (Red) Aromatics Recovery

Benzene Toluene

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Gas Treatment Plant Overview - Potential Optograf TM Applications

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Amine Treatment Plant – Gas Industry (H2S CO2) CO2 Sequestration

         

H2S CO2 CH4 H2S CO2 (TDL) H2S CO2 (liq) H2S CO2 (liq) H2S CO2 CH4 Similar to Flexsorb, Selexol, Benfield Processes

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Sour Gas @ 85 psig and 240 sec exposure (update) time

CH4 CO2 N2 H2S CH4 C2H6 C3H8 Sour Gas Blend Composition: CH4 75 vol% H2S 10 vol% CO2 10 vol% C2H6 2 vol% C3H8 1 vol% N2 2 vol%

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Acid Gas @ 85 psig and 240 sec exposure (update) time

CO2 H2S CH4 Blend Composition: CH4 1 vol% H2S 60 vol% CO2 39 vol%

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• What is an OptografTM
• What is Unique
• What is its Main Benefits
• How does it Work

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What is an OptografTM

• It is a PROCESS RAMAN Spectrometer (Sir Chandrasekhara Venkata Rāman)

Shine laser light on a sample – collect scattered light in which is the information about the composition of the stream

• Breakthrough technology is gas phase analysis
• Initial focus on gas phase analysis - OptografTM is unique product
• It produces a spectrum that in many cases looks like a chromatogram and is

analyzed like a chromatogram OptografTM = “Optical” Chromatograph = “Chromatography” with light Optogram = “Optical” Chromatogram

• Typically Applies to Component Concentrations of >0.1%
• It uses fiber-optic probes to interface with the process
• It has no moving parts (except a non-critical fan):

No columns, no valves, no stream switching, no consumables (carrier gas, instrument air etc.)

• Like TDLAS, main benefit of the OptografTM = Low Cost to Own

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What is an OptografTM?

Optograf Base Unit

(18”Wx10”Dx32”H)

• Fan Enclosure
• Fan for Heat Discharge
• MTBF Fan: 20000 hrs
• Safety Interlocks for

Lasers

• Cyclops Type Z Indicator
• CSA/ATEX Div II/ Zone II

Certifications

• Embedded Computer
• Data Acquisition, Data

Analysis, Display/Diagnostics

• Communications with

DCS (Modbus/IPC)

• Remote Access (future)
• Spectrograph
• High performance CCD Camera
• 4 Lasers (operate at 532 nm – green)
• Internal Temp Control via Solid State A/C

and Control of External heat Dissipation

• Temp Spec: -20oC to 50oC
• Wall Mounted
• In many locations, A/C Shelter is Optional
• Touchscreen
• Access to analysis

data, spectra, sensors, history etc.

• Green, Yellow and Red

Status Labeling

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• Improved sensitivity for gas phase analysis (reflector design)
• Overall noise of all optical and electrical components reduced

Breakthrough Advance: The “Airhead” – A Gas Phase RAMAN Probe

316 STAINLESS BODY, TEFLON AND SAPPHIRE IMMERSED MATERIALS. BALANCE IS 316 AND 303 STAINLESS STEEL PRESSURE RATING 1000 PSI TIP TEMPERATURE IS 150 DEG C, CABLE ENTRY TEMPERATURE IS 80 DEG C

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Optograf Base Unit

(18”Wx10”Dx32”H)

What is an OptografTM?

Fiber-optic probes = Process Interface = Pipe-centric Enabler

• Rule of thumb: up to 100 meters
• Can be installed in cable trays (conduit not required)
• Obviate the need for heat traced sample

transport lines to the analyzer or shelter

4 Probes (4 Lasers): Operating in parallel Multiplexing not required

Wetted Materials:

316 SS Teflon Sapphire

Pressure:

1000 psi

Temperature:

150oC (@ tip) 80oC (cable entry)

Size:

Fit 1” Swagelok X-Tee

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Inside Shelter (no exposure to sample) Outside Shelter P ,T Xmitter AirheadTM

Most Recent Gen II Installation with its 4- Channel/4-Probe Smart Sampling System

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Simplified Schematic of the OptografTM Gas Phase Analyzer System

CCD Detector 1650x200 pixels Green Laser (532 nm)

Sample Flow Sapphire Window Focusing Optics

Excitation Fiber

Transmission Grating

Fast Loop at Shelter RTD Pressure Gas Probe

Collection Fiber

Reflector Slit Notch

Embedded Computer/ Touchscreen

Chan1 Chan2 Chan3 Chan4

Chan1 Chan2 Chan3 Chan4

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TDC3000 (DCS)

OptografTM

Field Installation – Outside Shelter Wall/At Pipe

Analyzer Shelter/GP Area Technician Office

Modbus Protocol

Modbus Master/ Interface

IS Barriers (Inside Enclosure)

4 –20 mA RS485: Com2 Fiber-optic Cable Remote Workstation

Plant network

@ Pipe or Fast Loop at Shelter RTD Pressure Gas Probe

Stream 1

@ Pipe or Fast Loop at Shelter RTD Pressure Gas Probe @ Pipe or Fast Loop at Shelter RTD Pressure Gas Probe

Instrument/Control Room Stream 4 Stream 3 Stream 2

@ Pipe or Fast Loop at Shelter RTD Pressure Gas Probe

OptografTM System/Communications Configuration

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 Simpler maintenance requirements

• No valves no columns
• No Carrier Gases or Logistics management
• No stream switching
• Mounting in an air-conditioned shelter optional

< -20oC or > 45oC

• In Canada, requires a heated enclosure
• In KSA, requires either passively cooled or A/C shelter

 Safe design – no sample to the analyzer or shelter  No Toxic Gas exposure at Analyzer or Shelter Maintenance Benefits

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Performance Data

• Linearity
• Repeatability

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Hydrogen Sulfide (2611 nm) Methane (2917 nm) Hydrogen (588 nm) Nitrogen (2328 nm)

Linearity Reference Gas

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Pressure Effects on Spectra

500000 1000000 1500000 2650 2640 2630 2620 2610 2600 2590 2580 2570 2560

1012 psig 750 psig 501 psig 249 psig 125 psig 51 psig H2S @ 2611 cm-1

Linearity Plots

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y = 14535x + 142418 R2 = 1 0.000E+00 2.000E+06 4.000E+06 6.000E+06 8.000E+06 1.000E+07 1.200E+07 1.400E+07 1.600E+07 200 400 600 800 1000 1200 Pressure (psig) Area

Linearity Summary

y = 3048.6x + 40130 R2 = 1 0.000E+00 5.000E+05 1.000E+06 1.500E+06 2.000E+06 2.500E+06 3.000E+06 3.500E+06 200 400 600 800 1000 1200 Pressure (psig) Area

y = 44333x + 269753 R2 = 1

0.000E+00 5.000E+06 1.000E+07 1.500E+07 2.000E+07 2.500E+07 3.000E+07 3.500E+07 4.000E+07 4.500E+07 5.000E+07 200 400 600 800 1000 1200 Pressure (psig) Area

y = 572.14x + 11031 R2 = 0.9999

0.000E+00 1.000E+05 2.000E+05 3.000E+05 4.000E+05 5.000E+05 6.000E+05 7.000E+05 200 400 600 800 1000 1200 Pressure (psig) Area

H2S CH4 H2 N2

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Syngas Synthetic FAT Repeatability Blend

H2 H2 CH4 CO2 CO

* * * *

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CO2 CO H2 CH4 mean Vol% 3.52 24.57 61.89 8.52 stdev 0.03 0.08 0.11 0.02 sigma % 0.71 0.33 0.18 0.26 2 sigma % 1.43 0.67 0.37 0.53

Syngas Application: Repeatability Data

• Syngas Synthetic Blend
• 43 Hours
• Ambient Temp Change:

12DegC to 22DegC

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Touch Screen User Interface Examples

• Summary Screen
• Optogram Screens
• History Screens (Not shown)

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Main Screen

Progress bar Sampling Status Indicator System Status Button Latest Analysis

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Stream Detail – Analysis Tab

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Installed Base

An #

• No. of

Streams Model Location End-User #Streams.Application Status Date

1 4 Gen 1 Secunda Sasol 1 -4: Syngas to FT Reactors Installed Jun-08 2 4 Gen 1 Secunda Sasol 1 -4: Syngas to FT Reactors Installed Jun-08 3 4 Gen 1 Secunda Sasol 1 -4: Syngas to FT Reactors Installed Jun-08 4 4 Gen 1 Secunda Sasol 1 -4: Syngas to FT Reactors Installed Jun-08 5 4 Gen 1 Secunda Sasol 1-4: FT Reactor OVHD Installed Jun-08 6 4 Gen 1 Secunda Sasol 4 - FT Reactor OVHD Installed Jun-08 7 4 Gen II Secunda Sasol 4 - FT Reactor OVHD Installed 8 4 Gen II Secunda Sasol 1-4: Reformer Syngas Installed 9 3 Gen II Secunda Sasol 1: Demethanizer OVHD Train 1 Installed Jul-10 2: H2 Purity Installed Jul-10 3: ColdSep Feed Gas Installed Jul-10 10 3 Gen II Sasol See #9 for 1-3: Train 2 Installed Jul-10 11 1 Gen II Australia Anonymous 1: Raw Syngas UCG Installed Jun-11 12 3 Gen II Houston Shell 1-3: Confidential FAT Completed Dec-11 13 4 Gen II Secunda Sasol/Fluor 1-4: Reformer Syngas/H2 Rich Gas FAT Completed Mar-12 14 4 Gen II Sasol/Fluor 1-4: Reformer Syngas/CH4 Rich Gas FATCompleted 12-Mar 15 3 Gen II Sasol/Fluor 1-3: Light HC Gases FAT Completed Mar-12 16 2 Gen II Sasol/Fluor 1-2: Light HC Gases FAT Completed 12-Mar 17 1 Gen II Burghausen OMV 1: Cracked Gas Analysis Ready for FAT May-12 18 7 Gen II Canada Agrium (NH3) 1: Primary Reformer Exit Order shipped - ready for FAT Jun 2012 2: Secondary Reformer Exit Order shipped - ready for FAT 3: HTS Converter Exit Order shipped - ready for FAT 4: LTS Converter Exit Order shipped - ready for FAT 19 Gen II Canada Agrium (NH3) 5: CO2 Absorber Exit Order shipped - ready for FAT Jun 2012 6: Methanator Exit Order shipped - ready for FAT 7: NH3 Recycle/PSA Inlet Order shipped - ready for FAT 20 1 Gen II Edwardsport, IN GE (IGCC) 1: CO2 Recycle Gas (Syngas) Fat Completed - shipped May 2012 21 1 Gen II France GPN Ammonia 1: Feedgas to Primary Reformer+OptoAST Analyzer Started Up May-12 22 1 Gen II Coffeyville, KS CVREnergy (NH3) 1: Shift Converter Feed+OptoDRS Order in Preparation May-12 23 1 Gen II Chile MulpunEnergy (UCG) 1: Well-head Syngas+OptoDRS Order in Preparation May-12

67 Streams

New Technology but Proven TRL = 9

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Technology Development & Deployment Scale

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THANK YOU

In Summary:

Optograf is an Optical Chromatograph:

• Speciation by Frequency
• Univariate Data Analysis (Peak Area)
• Calibrated/Validated like a Chromatograph
• Unique Spectroscopic System – H2, N2, no H2O

Reduced Maintenance Requirements

• No Columns, Valves, Carrier Gas, Stream Switching
• Technician does not need to understand chromatography
• Lower Skill Level required
• Typically Lower Capital Cost (if no shelter, Sample transport system etc.)
• Lower Overall Cost to Own

Wide Range of Applications

• Syngas Production/Utilization
• Steam Crackers (Hot Ends)
• Refining
• Gas Processing
• (Aromatics Recovery)