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GC Method Compliance and Large
Valve Oven Application
Solution Focused
Kelly Beard
June 20, 2016
Compliant Methods
Compliant Methods
June 27, 20163
• What are our options?– Analyzers and Analyzer Kits
• High Volume
• Well Known Analysis
• Many Options
– Application Notes
• Lower Volume
• Usually Requires a Consultant
• Possible Future Analyzer, Given Acceptable Sales Quantiles
– Channel Partner Solutions
• Requires Third Party Software or
• Requires Third Party Hardware
Analyzers and Application KitsUpdated HPI Solution Guide
Searchable, 139 pages – PN: 5991-1561EN
Links to Analyzer Chapter
January 2013
Analyzer Overview
4
Analyzers and Application Kits
January 2013
Analyzer Overview
5
Analyzers and Application Kits
January 2013
Analyzer Overview
6
Analyzers and Application Kits
January 2013
Analyzer Overview
7
Analyzers and Application Kits
January 2013
Analyzer Overview
8
Application Notes
January 2013
Analyzer Overview
9
• Example: D5769 – Determination of Benzene,
Toluene, Total Aromatics in Finished Gasolines by
Gas Chromatography/Mass Spectrometry
– Fred Feyerherm developed application, via ASTM method
• Very successful
• Custom Calculations
• Consultant is Requited for Application
– Very popular lately
• Sales Quantities have Increased
• Analyzer Kit In Developed as a Result
Channel Partner
January 2013
Analyzer Overview
10
• ASTM D6730 – Standard Test Method for
Determination of Individual Components in Spark
Ignition Engine Fuels by 100-meter Capillary (with
PreColumn) High Resolution Gas Chromatography
– Detailed Hydrocarbon Analysis
• Difficult Analysis with 100’s of Compounds
• Requires Custom Software
• Software is Difficult to Support via Agilent Field Resources
• Many Software and Third Party Providers
Channel Partner
January 2013
Analyzer Overview
11
• ASTM D5599 – Standard Test Method for
Determination of Oxygenates in Gasoline by Gas
Chromatography and Oxygen Selective Flame
Ionization Detection
– O-FID Analysis
• Requires a Custom Platinum Catalyst
• Requires Custom Reporting
• Hardware can not be Supplied by Agilent
• Wasson-ECE is our Partner of Choice for this Analysis with Many
Years of Experience on the Application.
Channel Partner
January 2013
Analyzer Overview
12
• ASTM D8003 – Standard Test Method for
Determination of Light Hydrocarbons and Cut Point
Interals in Live Crude Oils and Condensates by Gas
Chromatography
– New Live Crude Oil Analysis
• Requires HPLIS Third Party Injection Source
– Intended for the introduction of pressurized liquid samples containing
very polar, high boiling or high carbon number analytes
• Requires Custom Reporting
• Hardware can not be Supplied or Supported by Agilent
Channel Partner
January 2013
Analyzer Overview
13
• Reformulyzer - Hydrocarbon Group Type Analysis
– PAC Provided Solution
• Test Methods: ASTM D5443, ASTM D6839, IP 566, EN ISO 22854,
SH/T 0741, GB/T 28768-2012, GOST R EN ISO 22854
– Intended for the introduction of pressurized liquid samples containing
– Extensive Hardware Addition
Questions
January 2013
Analyzer Overview
14
Introducing the 7890B Large Valve Oven Isothermal Zone for Valves and Columns
• Temperature control:
- Independent control of LVO and GC
oven zones
• Temperature Limit:
- Max 330˚C (valve and column dependent)
• Valve configurations:
- Accommodates 4/6/10/14 port valves
including Hastelloy valves
• Column Compatibility:
- Large Mandrel: Accommodates 15 feet of
1/8 inch OD metal column
- Small Mandrel: Accommodates 7 Ft of 1/8”
OD metal column
June 27, 201615
LVO Analyzer Training
6-port Valve
Variable Restrictor
Column Mandrel
12-port Valves
Valve or Mandrel Position
Introducing the 7890B Large Valve OvenIsothermal Zone for Valves and Columns
6 Internal Positions:
Valves or Columns
- Up to six (6) heated
valve positions
- Four (4) needle
valve positions
- Uses 1 heated zone
June 27, 201616
LVO Analyzer Training
Large Valve Oven Features/Benefits
Feature
6 position isothermal valve oven for actuated valves,
microgasifiers, needle valves, and columns (including 1/8 in
packed columns) with access to valves connections without
removing actuators
Benefit
Open configuration that allows for easy maintenance;
maximizing up-time. Also allows for multiple configurations
for method development as well as set SP1 and configured
Feature
Use only one 7890B heated zone
Benefit
Current multi-valve configurations may quickly consume 6
heated zones, LVO uses 5 leaving 1 for future applications
Feature
Dual thermal zones allow for thermal isolation between
column oven and LVO
Benefit
Ability to configure analyses that require multiple thermal
zones. Can run isothermal temperatures in the LVO while
temperature ramping the GC oven
7890B with Large Valve Oven
June 27, 201617
LVO Analyzer Training
Fast Refinery Gas Analysis with Micropacked ColumnsSimultaneous O2 and H2S determination
7890 GC System, LVO, Column, Sample
Option 112 S/SL Inlet
Option 210 FID with EPC
Option 220 TCD with EPC
Option 221 Left Mount TCD
Option 002 or 003 Fast Oven
Option 311 and 312 Cryo
G3445B
Option #532
June 27, 201618
LVO Analyzer Training
Performance FeaturesLVO RGA Analyzers
Fast RGA Analyzer
• Total run time is 8 minutes
- LVO at 70 °C
• Hydrocarbons to C5 (C6+ backflush)
• Permanent Gases
• O2 and H2S
Compounds Limit
Hydrocarbons 0.01 Mol%
Hydrogen Sulfide 500 ppm
Carbonyl Sulfide 300 ppm
Hydrogen 0.01 Mol%
O2, N2, CO, CO2 0.01 Mol%
June 27, 2016
19
Fast RGA with Micropacked ColumnsGC/FID/TCD/TCD
Micropack System Flow DiagramMicropack LVO Plumbing
June 27, 201620
LVO Analyzer Training
Fast RGA with Micropacked Columns – Helium CarrierSelected Method Parameters
Split/Splitless inlet: 120 ºC, 100:1 split
FID (front): 250 ºC
TCD (rear): 260 ºC
He carrier
Ref. 30 mL/min
Makeup 2 mL/min
TCD (side): 250 ºC
N2 carrier
Ref. 45 mL/min
Makeup 2 ml/min, neg. polarity
Main Oven Program: 60 ºC ( 1 min) to 80 ºC @ 20 ºC/min
to 190 ºC @ 30 ºC/min
Large Valve Oven: Isothermal, 65 ºC and 70 ºC
June 27, 201621
LVO Analyzer Training
Fast RGA with Micropacked ColumnsAnalytical Performance – Hydrocarbon Channel (FID), LVO at 70 °C
June 27, 201622
LVO Analyzer Training
Fast RGA with Micropacked ColumnsAnalytical Performance – Permanent Gas Channel (TCD), LVO at 70 °C
1 2 3 4 5 6
June 27, 201623
LVO Analyzer Training
Fast RGA with Micropacked ColumnsAnalytical Performance – Oxygen Stability
Stability of Oxygen – Isothermal Oven at 70 °C
70 °C 75 °C
Stability of Oxygen – Isothermal Oven at 75 °C
June 27, 201624
LVO Analyzer Training
Fast RGA with Micropacked Columns – Helium CarrierApplication Note
June 27, 201625
LVO Analyzer Training
Fast Refinery Gas Analysis System
Based on the Agilent 7890B GC System
and G3507A Large Valve Oven Using
Micropacked Columns
Fast RGA LVO AnalyzerValue Overview Analyzer, G3445B #532
Large Valve Oven
• External Thermal Zone
• Isothermal Operation
• Up to 6 valves or columns
• Expands capability of 7890
Micropacked Columns
• Built for speed
• Rapid 8 minute cycle time
Isothermal Zone
• Protect temperature sensitive columns
• Simultaneous analysis of hydrogen disulfide (H2S) and oxygen (O2)
• Stable response for oxygen (O2)
Three Channel Analytical Method• Simultaneous analysis of hydrogen hydrocarbons and permanent gases
Simultaneous analysis of O2 and H2S <8 Minutes
February 2014
GC/FID/MS Blood Alcohol Analyzer
26
LVO Based Fast RGA with Hydrogen CarrierAnalytical Performance (G3445B, #533 – Available on July 1, 2014 CPL)
FID Channel
C6+
June 27, 201627
LVO Analyzer Training
Fast Refinery Gas Analysis with Micropacked ColumnsSimultaneous O2 and H2S determination using Hydrogen Carrier Gas
7890 GC System, LVO, Column, Sample
Option 112 S/SL Inlet
Option 210 FID with EPC
Option 220 TCD with EPC
Option 221 Left Mount TCD
Option 002 or 003 Fast Oven
Option 311 and 312 Cryo
G3445B
Option #533
June 27, 201628
LVO Analyzer Training
Overview - GC Platforms & Positioning
Gas Chromatograph
Agilent RestrictedPage 29
7820 GC
Entry Level
Price/Performance
6850 GC
Small footprint
7890 GC
Highest flexibility
Industry leader
Technologies
LTM /7890 GC
Fast heating/
cooling
490 Micro GC
Fast Gas Analysis
Compact Size
Thank You.
HPI Solution overview
Agilent Restricted
Neophyte training Shanghai,Sep, 2007Page 30