Agilent Technologies G6600-90006 manual Theory of Operation, Sulfur Chemiluminescence Detector

Page 23

Theory of Operation

Sulfur Chemiluminescence Detector

The Agilent model 355 Sulfur Chemiluminescence Detector (SCD) is a sulfur-selective detector for gas chromatography. Operation of the SCD is based on the chemiluminescence (light-producing reaction) from the reaction of ozone with sulfur monoxide (SO) produced from combustion of the analyte:

Sulfur compound (analyte) SO + H2O + other products

SO + O3 SO2 + O2 + hη (<300–400 nm)

A vacuum pump pulls the combustion products into a reaction cell at low pressure, where excess ozone is added. Light produced from the subsequent reaction is optically filtered and detected with a blue-sensitive photomultiplier tube and the signal is amplified for display or output to a data system. Figure 1 is a pneumatic flow diagram that illustrates how the components of the system are integrated.

The Detector has an enclosed, dedicated (Dual Plasma) Burner designed to enhance production of the SO intermediate. This Dual Plasma Burner mounts in the detector port of the GC. A Dual Plasma Controller provides temperature control and gas-flow regulation to operate the Dual Plasma Burner.

The Agilent model 355 SCD provides high sensitivity (<0.5 pg S/sec), with linear and equimolar response over four orders of magnitude (per Sulfur atom) while maintaining high selectivity over common solvents. The Agilent SCD is compatible with most commercially available gas chromatographs.

Nitrogen Chemiluminescence Detector

Operation of the Agilent model 255 Nitrogen Chemiluminescence Detector is based on the chemiluminescence or light-producing reaction of ozone with nitric oxide formed from combustion. Reacting nitric oxide with ozone results in the formation of electronically excited nitrogen dioxide. The excited nitrogen dioxide emits light, a chemiluminescence reaction, in the red and infrared region of the spectrum. The light emitted is directly proportionally to the amount of nitrogen in the sample,

NO + O3 NO2 NO2 + hη (>800 nm)

The light (hη) emitted by the chemical reaction is optically filtered and detected by a photomultiplier tube. The signal from the photomultiplier tube is amplified for display or output to a data system. Organic compounds containing nitrogen react to form nitric oxide, carbon dioxide, and water.

H2/O2

 

 

---------------

NO + CO2

+ H2O

R-N + O2

Δ

 

Operation and Maintenance Manual

23

Image 23
Contents Operation and Maintenance Manual Manual Part Number WarrantySafety Notices AcknowledgementsWA R N I N G EnglishIs not in use Español Français Deutsch Italiano Veiligheidsvoorzieningen niet meer DutchFollowing symbols are used on the equipment Contents Overview InstallationOperation Front Panel Controls and Initial StartupPump Maintenance MaintenanceIndex TroubleshootingOperation and Maintenance Manual Introduction Operation and Maintenance Manual System Description Technical Information 255 NCD SpecificationsTechnical Information 355 SCD Power requirements Physical SpecificationsVoltage Nitrogen Chemiluminescence Detector Theory of OperationSulfur Chemiluminescence Detector Dual Plasma Burner with the 355 SCD Dual Plasma ControllerDual Plasma Burner Description of Major ComponentsCross-Section of the Dual Plasma Burner for the 355 SCD Cross-Section of the Dual Plasma Burner for the 255 NCD Chemiluminescence Reaction Cell and Photomultiplier Tube Ozone Generator355 SCD Left Side 355 SCD Right Side 255 NCD Left Side View Vacuum Pump Pressure TransducerNCD Reaction Cell Chemical TrapOil Coalescing Filter FID Adapter OptionalNCD Photomultiplier Tube and Cooler Schematic for 355 SCD Schematic for 255 NCD, in Nitrogen Mode Schematic for 255 NCD, in Nitrosamine Mode Operation and Maintenance Manual Installation Overview Selecting a Location Power RequirementsCombustion Gas Requirements Environmental ConsiderationsTwo-stage pressure regulators Venting Gases Unpack and Inspect the Instrument Required Installation ToolsInstalling the Edwards RV5 Pump Oil-Sealed Vacuum Pump Set Up the Vacuum PumpWA R N I N G Ard RV5 Oil-Sealed Vacuum Pump and Associated Traps Front Side RV5 Oil- Sealed Vacuum Pump and Associated Traps Top Setting the Gas Ballast Position RV5 Installing the Welch Dry Piston Vacuum Pump Operation Notes Welch Pump Welch Dry Piston Pump Operation and Maintenance Manual SCD 230 V Unit Rear Panel Diagram Connect the Power CordInstall the Dry Compressed Air or O2 Supply Install the Signal Output Cables Additional information Install the Dual Plasma BurnerDual Plasma Controller Rear Panel Install the Dual Plasma ControllerPacked Columns and Columns with an Outside Diameter 0.8 mm Install Column ConnectionsCapillary Columns Install the Transfer Line Front Panel Controls and Initial Startup Detector Front Panel Controls Power ControlsDisplay Output Controls Signal ControlsDual Plasma Controller Front Panel Dual Plasma Controller ControlsVacuum Test Initial StartupRecorder Test Initial Checkout Detector Interface SetupIgnition Operation Start-Up Procedure Coking Detector OperationDetector Stability and Response Column BleedFluctuating Pressures Contaminated GasesTypical Operating Conditions Typical Operating ConditionsExpected Detection Limits for Chromatographic Conditions Detection LimitsComplete Shutdown Instrument Shut-DownDaily Shutdown Special Operating Modes Using the 255 NCD in Nitrosamine ModeOperation and Maintenance Manual Operation and Maintenance Manual Maintenance Operating Life of Components for Edwards RV5 Vacuum Pump Pump MaintenanceCleaning the Detector Changing the Oil Mist Filter RV5 Equipment Reaction Cell CleaningReaction Cell, PMT Housing and PMT Socket WA R N I N G Flow Sensor Calibration MDL Detector SensitivitySCD Proper Ferrule Orientation to the Large Ceramic Tube Orientation of the Double Taper Ferrule Tightening the Heater Swivel Nut Operation and Maintenance Manual NCD Proper Ferrule Orientation to the Large Quartz Tube Burner Assembly Detail Tube Replacement for the SCD Positioning the Upper Tube in the Union Fitting 100 Operation and Maintenance Manual Operation and Maintenance Manual 101 Tube Replacement for the NCD Operation and Maintenance Manual 103 NCD Tube Replacement Detail Troubleshooting Solving Detector Problems Dual Plasma Controller Fuses Power ProblemsDetector Fuse Vacuum Pump FuseFuse Positions on the Power Supply Board High Voltage Transformer Ozone Generation ProblemsPlugged Restrictor Lines Response Problems Temperature Reading Problems Troubleshooting Detector Issues Diagnosing General ProblemsDetector gases Troubleshooting Pump Issues Troubleshooting Burner Issues Index Agilent Technologies, Inc