Related Manuals for Agilent Technologies 8355 Sulfur
Summary of Contents for Agilent Technologies 8355 Sulfur
- Page 1 Agilent 8355 Sulfur and 8255 Nitrogen Chemiluminescence Detectors User Manual Agilent Technologies...
- Page 2 A CAUTION notice denotes a hazard. without prior agreement and written permitted by applicable law, Agilent It calls attention to an operating consent from Agilent Technologies, Inc. as disclaims all warranties, either express procedure, practice, or the like that, if governed by United States and...
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Page 3: Table Of Contents
Contents Getting Started Manuals, Information, Tools and Where to Find Them Safety Information Online help Education Opportunities Overview of the 8355 SCD and 8255 NCD Overview of Installation and First Startup System Description Specifications 8355 SCD 8255 NCD MDL calculations Theory of Operation Description of Major Components Burner assembly... - Page 4 Typical Operating Conditions Adjusting the Operating Conditions Start-up Resource Conservation Shutdown Configure Auto Flow Zero on the GC Automatic Configuration of the Detector Maintenance Maintenance Log and Early Maintenance Feedback (EMF) Maintenance Schedule Tracking Detector Sensitivity Consumables and Replacement Parts Exploded Parts View of the SCD Exploded Parts View of the NCD Detector Maintenance Method...
- Page 5 Leaks Ozone leaks Hydrogen leaks Oxidizer leaks Checking for hydrogen and oxidizer leaks Power Problems No power Ozone Generation Problems Coking Hydrogen Poisoning Contaminated Gases Performance Verification About Chromatographic Checkout Prepare for Chromatographic Checkout Prepare sample vials Check SCD Performance Check NCD Performance 8355 SCD and 8255 NCD User Manual...
- Page 6 8355 SCD and 8255 NCD User Manual...
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Page 7: Getting Started
Manuals, Information, Tools and Where to Find Them Overview of the 8355 SCD and 8255 NCD Overview of Installation and First Startup This chapter introduces the Agilent 8355 Sulfur Chemiluminescence Detector (SCD) and the Agilent 8255 Nitrogen Chemiluminescence Detector (NCD), and provides details about where to find helpful information and tools, such as GC manuals, flow calculators, and so forth. -
Page 8: Manuals, Information, Tools And Where To Find Them
Getting Started Manuals, Information, Tools and Where to Find Them This manual describes how to operate the 8355 SCD and the 8255 NCD as installed on an Agilent 7890B Gas Chromatograph (GC). This manual also provides operating recommendations, maintenance procedures, and troubleshooting. For installation instructions, see “Overview of Installation and First Startup”... -
Page 9: Education Opportunities
Getting Started Education Opportunities Agilent has designed customer courses to help you learn how to use your GC to maximize your productivity while learning about all of the great features of your new system: For course details and education opportunities, visit http://www.agilent.com/chem/education, or call your local Agilent sales representative. -
Page 10: Overview Of The 8355 Scd And 8255 Ncd
Getting Started Overview of the 8355 SCD and 8255 NCD Figure 1 through Figure 5 show the controls, parts, and components of the 8355 SCD and 8255 NCD used or accessed during installation, operation, and maintenance. Status LED Status LED Power switch Power switch 8355 SCD... - Page 11 Getting Started Hydrogen gas input Burner heater connector Oxidizer gas input Heater/sensor Ozone generator connector gas input Through-hole for sample transfer line Thermocouple connector Communications cable Vacuum connection Vacuum pump Power connection power connection Figure 2 Detector back view 8355 SCD and 8255 NCD User Manual...
- Page 12 Getting Started Upper hydrogen output Hydrogen gas input (SCD only) Oxidizer gas output Oxidizer gas input Lower hydrogen output Ozone generator gas input Figure 3 Detector gas connections plug Pump oil pan Figure 4 RV5 Vacuum pump 8355 SCD and 8255 NCD User Manual...
- Page 13 Getting Started Maximum oil level mark Sight gage Oil level Minimum oil level mark Figure 5 RV5 Vacuum pump oil sight gage 8355 SCD and 8255 NCD User Manual...
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Page 14: Overview Of Installation And First Startup
Getting Started Overview of Installation and First Startup Below is an overview of the installation process. Installation and service of the detector should only be performed by Agilent-trained service personnel. If not already installed, install the GC and Agilent data system. - Page 15 Agilent 8355 SCD and 8255 NCD User Manual System Description Specifications Theory of Operation Description of Major Components This chapter provides typical performance specifications, and describes the theory of operation for the 8355 SCD and 8255 NCD. Agilent Technologies...
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Page 16: System Description
System Description Specifications This section lists the published specifications for a new detector, installed on a new Agilent 7890B GC, when used in a typical laboratory environment. The specifications apply to the Agilent checkout sample. 8355 SCD Specification Minimum Detection Limit (MDL), <... -
Page 17: Mdl Calculations
System Description MDL calculations The MDL specifications are defined using the Agilent checkout standard for SCD or NCD. Sensitivity is typically reported as: peak area Sensitivity = amount Calculate a minimum detection limit (MDL) from the following formula: 2 x noise MDL = sensitivity where the noise is the ASTM noise reported by the Agilent data... -
Page 18: Theory Of Operation
System Description Theory of Operation The SCD and NCD chemiluminescence detectors detect target molecules by chemically transforming them in several steps to an excited species that emits light. The light from this emission is converted to an electrical signal by a photomultiplier tube (PMT). - Page 19 System Description the spectrum. The light emitted is directly proportionally to the amount of nitrogen in the sample: NO + O NO + O + h (~600 to 3,000 nm) The light (h ) emitted by the chemical reaction is optically filtered and detected by a PMT.
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Page 20: Description Of Major Components
System Description Description of Major Components Burner assembly The burner assembly mounts on top of the GC in a detector location, and contains the column connection. For the SCD, the burner provides two heated zones, one at the base and one farther up the assembly. In the burner base region, the column effluent mixes with the lower hydrogen flow and air or oxygen at high temperature. - Page 21 System Description Figure 6 shows the flow paths for the SCD burner assembly. Upper hydrogen Ceramic tube, upper Burner Ceramic tube, lower Oxidizer Base heater Lower hydrogen Column Figure 6 SCD flows For the NCD, the burner provides two heated zones, one at the base and one farther up the assembly.
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Page 22: Ozone Generator
System Description Figure 7 shows the flow paths for the NCD burner assembly. To detector Quartz tube Burner Oxidizer Base heater Hydrogen Column Figure 7 NCD Flows Ozone generator The ozone generator provides ozone that reacts with any SO or NO in the reaction cell to generate SO * and NO * respectively. -
Page 23: Reaction Cell And Photomultiplier Tube (Pmt)
System Description The GC regulates the ozone gas supply pressure to maintain a fixed flow from the ozone generator. Reaction cell and photomultiplier tube (PMT) The ozone generator discharges ozone into the reaction cell. This ozone reacts with any SO or NO to generate SO * and NO respectively. -
Page 24: Fid Adapter (Optional)
System Description FID adapter (optional) The SCD burner normally mounts onto the GC oven directly as a stand-alone detector. However, some applications also require simultaneous detection of hydrocarbon components using a single column without splitting. For this reason, Agilent offers an optional FID adapter to mount the burner assembly onto an FID for the simultaneous collection of FID and SCD chromatograms. -
Page 25: Operation
NCD. This chapter assumes familiarity with using the data system, if used, and the GC front panel keyboard and display. For more information, please see the data system online help and the instrument documentation available on the Agilent GC and GC/MS User Manuals and Tools DVDs. Agilent Technologies... -
Page 26: Introduction
Operation Introduction Integrated version When installed on an Agilent 7890B or 7890A+ GC, program and operate the SCD and NCD as you would any other detector on the GC. For Agilent data system users, use the integrated GC driver to access the operating parameters. For standalone GC users, access these parameters from the GC front panel and keyboard. -
Page 27: Setting Parameters
Operation Setting Parameters This section lists the parameter ranges for the SCD and NCD. The available setpoints provide a wide range suitable for a large variety of applications as well as for method development. See “Adjusting the Operating Conditions” on page 33 for important details about the relationships between the setpoints. -
Page 28: Software Control
Operation Software control When using an Agilent data system, open an online session and edit the instrument acquisition parameters to change method settings. Select the detector from the method editor, typically Detectors > Front Detector (or Back Detector or Aux Detector, as appropriate for your setup). - Page 29 Operation Figure 9 Example NCD parameters in a data system For tandem configurations, for example a front FID-SCD, the FID will be the front detector, and the XCD will be an Aux detector. To access configuration parameters using data system control, select Configuration >...
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Page 30: Gc Keyboard Control
Operation GC keyboard control To access the method parameters for an SCD or NCD, press the [Front Det], [Back Det], or [MS/Aux Det] (tandem FID-XCD configuration only) key. (7890A and some 7890B GCs may have key [Aux Det #] instead of [MS/Aux Det]. See Table To turn on the PMT voltage, press [Config], then press the key for the detector ([Front Det], [Back Det], or [Aux Det #]). -
Page 31: Detector Stability And Response
Operation Detector Stability and Response The time required for system stabilization varies depending on the application, system cleanliness, the presence of active sites, and other factors. • When starting an existing system, typically wait at least 10 minutes before using the system to collect data. •... -
Page 32: Typical Operating Conditions
Operation Typical Operating Conditions Table 3 lists the recommended starting conditions for SCD and NCD methods. These conditions should provide acceptable results for a wide variety of applications. However, optimize these conditions as needed to improve the performance of the specific application. -
Page 33: Adjusting The Operating Conditions
Operation Adjusting the Operating Conditions Table 1 on page 27 lists the range of values for each parameter, as limited by the GC firmware.Table 1 on page 27 lists the range of values for each parameter, as limited by the detector firmware. -
Page 34: Start-Up
Operation Start-up How to start the detector depends on whether or not you have created a method for the detector. If a valid method exists: After you have used the SCD/NCD (at least one valid method exists), start the detector by loading the method. - Page 35 Operation temperature reaches 200 °C. Once the detector temperatures reach these minimum limits, the GC turns on the hydrogen flow. If needed, also turn on the PMT voltage. See “Automatic Configuration of the Detector” on page 39. 8355 SCD and 8255 NCD User Manual...
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Page 36: Resource Conservation
Operation Resource Conservation To conserve resources during periods of inactivity, for example, overnight or over a weekend, use the 7890B GC’s resource conservation features to load a sleep method. (See the GC Operation Manual for details on using sleep and wake methods.) A sleep method for an SCD or NCD should do the following: •... -
Page 37: Shutdown
Operation Shutdown When turning off the detector for a long period of time, or to perform maintenance on the GC or detector, shut down the detector as follows: Access the method parameters. At the GC front panel, press [Front Det] or [Back Det], or •... - Page 38 Operation To activate: On the GC keypad, press [Options]. Scroll to Calibration and press [Enter]. Scroll to select the appropriate detector (front, back, aux 2, or aux 1) and press [Enter]. Scroll to Autoflow zero (H2 Lower) and press [On/Yes]. (To turn off autozero, instead press [Off/No].
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Page 39: Automatic Configuration Of The Detector
Operation Automatic Configuration of the Detector The detector does not require configuration. The SCD detector automatically is set to use: • Air or Oxygen for the oxidizer gas • Oxygen for the O3 generator gas For the NCD, the detector is set to use oxygen for both the oxidizer and O3 generator gases. - Page 40 Operation The PMT voltage can be turned on or off only at the GC front panel. To enable or disable the PMT voltage: At the GC keyboard, press the keys to access the detector, for example, press [Config][Front Det] for an XCD mounted in the front position, or press [Config][Back Det] for an XCD mounted in the back position.
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Page 41: Maintenance
Replace the Vacuum Pump Oil Replace the Ozone Trap Change the Oil Mist Filter Clean the Detector Exterior Calibrate the Flow and Pressure Sensors This chapter describes the routine maintenance procedures needed for normal use of the SCD and NCD. Agilent Technologies... -
Page 42: Maintenance Log And Early Maintenance Feedback (Emf)
Maintenance Maintenance Log and Early Maintenance Feedback (EMF) When using the detector with an Agilent 7890B GC, use the Early Maintenance Feedback (EMF) feature to track routine maintenance. The EMF feature is available at the GC front panel and in any Agilent data system, and can help you replace the filters and oil before contamination becomes a problem. -
Page 43: Maintenance Schedule
Maintenance Maintenance Schedule To maintain optimum performance of the Agilent 8355 SCD and 8255 NCD, routinely replace the ozone trap, oil coalescing filter, and vacuum pump oil. Refer to Table 4 for the expected life span of each item. Table 4 Recommended Edwards RV5 vacuum pump maintenance schedule Component... -
Page 44: Tracking Detector Sensitivity
Maintenance Tracking Detector Sensitivity In addition to using the EMF features of the GC and detector, also track detector sensitivity. Sensitivity reflects the performance characteristics of a given system, and decreased sensitivity may indicate the need for routine detector maintenance. The MDL specifications are defined using the Agilent checkout standard for SCD or NCD. -
Page 45: Consumables And Replacement Parts
Maintenance Consumables and Replacement Parts See the Agilent catalog for consumables and supplies for a more complete listing, or visit the Agilent Web site for the latest information (http://www.chem.agilent.com/store). Table 5 Consumables and parts for the SCD and NCD Description/quantity Part number Detector parts Ceramic tube, inner, small (SCD) (pack of 3)... - Page 46 Maintenance Table 6 Filters for the SCD and NCD Description/quantity Part number Gas Clean filter, sulfur (filters sulfur and moisture) CP17989 Gas Clean Filter SCD Kit, for sulfur CP17990 chemiluminescence detectors Table 7 Nuts, ferrules, and hardware for capillary columns Column id (mm) Description Typical use...
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Page 47: Exploded Parts View Of The Scd
Maintenance Exploded Parts View of the SCD (For tandem FID-SCD, see the FID details) Figure 12 SCD Exploded parts view 8355 SCD and 8255 NCD User Manual... -
Page 48: Exploded Parts View Of The Ncd
Maintenance Exploded Parts View of the NCD Coupling 1/4-inch graphite ferrule, straight Quartz tube Shroud assembly Burner heater Burner lower nut 1/4-inch graphite ferrule, straight Jet assembly and coupling Detector base Insulation, top Insulation, bottom Insulation cup Ferrule Column nut Column installation tool Figure 13 NCD exploded parts view... -
Page 49: Detector Maintenance Method
Maintenance Detector Maintenance Method It is good practice to create a maintenance method for the GC that prepares the GC and detector for maintenance. Load this method before performing maintenance. A maintenance method for the SCD or NCD should do the following: Turn off the heater and burner to allow them to cool. -
Page 50: Attach A Column To The Detector
Maintenance Attach a Column to the Detector This procedure describes how to attach a column directly to an XCD. In a N O T E tandem FID-XCD installation, install the column into the FID as described in the FID instructions. See the GC documentation. Gather the following materials (see “Consumables and parts for the SCD and NCD”... - Page 51 Maintenance Prepare the detector for maintenance. Load the GC maintenance method and wait for the GC to become ready. (See “Detector Maintenance Method” page 49.) Wait until the inlets, oven, detectors, valve box, burner assembly, and detector base cool to a safe handling temperature (<...
- Page 52 Maintenance Tighten the column nut into the column measuring tool until the column nut grips the column. Tighten the nut an additional 1/8- to 1/4-turn with a pair of wrenches. Snug the septum against the base of the column nut. Use a column cutting wafer at 45°...
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Page 53: Replace The Inner Ceramic Tube (Scd)
Maintenance Replace the Inner Ceramic Tube (SCD) To replace the inner ceramic tube: The oven, inlets, and detectors can be hot enough to cause burns. WA RNING Cool these areas to a safe handling temperature before beginning. Wear clean, lint-free gloves to prevent contamination of parts with C A U T I O N dirt and skin oils. - Page 54 Maintenance Hydrogen gas is flammable. Turn off all detector (and column) WA RNING hydrogen gas flows before performing maintenance on the detector. Disconnect the transfer line and quickly cover the open end with the 1/8-inch cap. Use a 3/8-inch wrench on the transfer line and a 7/16-inch wrench on the upper fitting to hold the burner assembly steady.
- Page 55 Maintenance Reinstall the transfer line onto the outlet fitting. Tighten until snug (finger-tight). Do not overtighten. Restore the detector gas flows. Check for leaks at the upper hydrogen fitting. Correct a leak as needed. Restore the remaining detector operating conditions. Reset the EMF counter.
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Page 56: Replace The Quartz Tube (Ncd)
Maintenance Replace the Quartz Tube (NCD) To replace the NCD quartz tube: The oven, inlets, and detectors can be hot enough to cause burns. WA RNING Cool these areas to a safe handling temperature before beginning. Wear clean, lint-free gloves to prevent contamination of parts with C A U T I O N dirt and skin oils. - Page 57 Maintenance Hydrogen gas is flammable. Turn off all detector (and column) WA RNING hydrogen gas flows before performing maintenance on the detector. Remove the protective shroud. Remove the two T20 Torx screws, twist the shroud counter-clockwise to remove it from the mounting posts, then lift.
- Page 58 Maintenance Gently pull the quartz tube up through the burner assembly to remove. The graphite ferrule should remain in the rotating nut in the burner base. Use a dental tool or similar to remove the old graphite ferrule from the rotating nut in the burner base. Use two wrenches to disassemble the reducer, then remove the old ferrule.
- Page 59 Maintenance Reinstall the protective shroud. Restore the detector operating conditions. Reset the EMF counter. 8355 SCD and 8255 NCD User Manual...
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Page 60: Check The Vacuum Pump Oil
Maintenance Check the Vacuum Pump Oil Never add or replace the foreline pump oil while the pump is on. C A U T I O N Check the level and color of the pump oil weekly. Check the oil level in the window of the foreline pump. The oil level should be between the marks for Max and Min. -
Page 61: Add Vacuum Pump Oil
Maintenance Add Vacuum Pump Oil Add pump oil when the pump oil level is low. Materials needed • Funnel (9301-6461) • 5-mm Allen wrench (8710-1838) • Gloves, chemical resistant, clean, lint free (9300-1751) • Oil, synthetic, Mobile 1 (G6600-85001) • Safety glasses (goggles) Never add pump oil while the pump is on. - Page 62 Maintenance Remove the fill cap on the vacuum pump. Power cord receptacle Fill cap Add new pump oil until the oil level is near, but not over the maximum mark beside the oil level window. See Figure 16 page 60. Reinstall the fill cap.
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Page 63: Replace The Vacuum Pump Oil
Maintenance Replace the Vacuum Pump Oil Replace the pump oil every three months or sooner if the oil appears dark or cloudy. Materials needed • Container for catching used pump oil • Funnel (9301-6461), 5-mm Allen wrench (8710-1838) • Gloves, chemical resistant, clean, lint free (9300-1751) •... - Page 64 Maintenance Place a container under the drain plug of the vacuum pump. Fill cap Drain plug Remove the fill cap, then open the drain plug. Drain the oil completely by raising the motor end of the pump. Reinstall the drain plug. Add new pump oil until the oil level is near, but not over the maximum mark beside the oil level window.
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Page 65: Replace The Ozone Trap
Maintenance Replace the Ozone Trap To replace the ozone trap: Load a method to cool the detector, turn off the heaters, and turn off the hydrogen flow. • Turn off the heaters and allow the burner to cool. • Leave the oxidizer flow on. •... -
Page 66: Change The Oil Mist Filter
Maintenance Change the Oil Mist Filter The oil mist filter on the RV5 pump has two components: the charcoal odor filter and the oil coalescing filter element. To replace the filters, disassemble the oil mist filter assembly with the 4 mm long-handled hex wrench (provided). The smaller charcoal odor filter sits on top of the larger oil coalescing filter element. -
Page 67: Clean The Detector Exterior
Maintenance Clean the Detector Exterior Burn hazard. The burner assembly can be hot enough to cause WA RNING burns. Before touching, cool to a safe handling temperature (< 40 °C). Shock hazard. Before cleaning the detector, turn it off and unplug WA RNING its power cord. -
Page 68: Calibrate The Flow And Pressure Sensors
Maintenance Calibrate the Flow and Pressure Sensors The 8355 SCD and 8255 NCD use electronic pressure control modules. Typically, set the 7890B GC to use automatic flow zeroing. See “Configure Auto Flow Zero on the GC” on page 37. Calibration is generally not required. However, if needed the flow and pressure sensors can be manually zeroed. -
Page 69: Updating Firmware
Maintenance Updating Firmware The GC firmware controls the detector. Any updates for the detector will be applied through the GC firmware. See the GC Firmware Update Tool on the Agilent GC and GC/MS User Manuals & Tools DVDs, or download the tool from the Agilent web site GC support pages. - Page 70 Maintenance 8355 SCD and 8255 NCD User Manual...
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Page 71: Troubleshooting
Solving Detector Problems Troubleshooting Table Status Indicator LED Detector Messages Leaks Power Problems Ozone Generation Problems Coking Hydrogen Poisoning Contaminated Gases This chapter describes how to troubleshoot and resolve typical issues encountered while using an Agilent SCD or NCD. Agilent Technologies... -
Page 72: Solving Detector Problems
Troubleshooting Solving Detector Problems A basic understanding of the detector helps to diagnose and solve detector problems. Review the basic detector theory found “Theory of Operation” on page 18. Also, please note that this section is intended to troubleshoot problems in a detector that has previously been performing acceptably. -
Page 73: Troubleshooting Table
Troubleshooting Troubleshooting Table Table 8 Troubleshooting Detector Issues Problem Possible cause Diagnosis Corrective action Detector problems No response No ozone Little or no difference in “No ozone”. output signal between ozone On and Off. No ozone High voltage transformer No difference in output Contact Agilent for service. - Page 74 Troubleshooting Table 8 Troubleshooting Detector Issues Problem Possible cause Diagnosis Corrective action Excessive response Incorrect range setting for Edit the range to better scale analog out (standalone the data. detector only) Leak in the oxidizer lines. Check for leaks in the detector and repair any leaks.
- Page 75 Troubleshooting Table 8 Troubleshooting Detector Issues Problem Possible cause Diagnosis Corrective action Leak in burner. Check for leaks in the detector and repair any leaks. See “Leaks” page 78. Burner pressure lower than Cracked or misaligned inner Check that the inner ceramic “Replace the Inner expected and poor response ceramic tube.
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Page 76: Status Indicator Led
Troubleshooting Status Indicator LED Use the detector status LED to quickly determine the status and readiness of the detector. The LED changes color depending on the current state of the detector. • Green: Indicates that power is available for the heaters, chiller (NCD), vacuum pump, and ozone generator. -
Page 77: Detector Messages
Troubleshooting Detector Messages Check the GC status display for detector messages. The GC will display and status and error messages that occur during operation, as well as log detector maintenance and error messages in the GC log files. See the GC operating manuals for details. -
Page 78: Leaks
Troubleshooting Leaks Ozone leaks Ozone is a hazardous gas and a strong oxidant. Exposure to ozone WA RNING should be minimized by using the instrument in a well-ventilated area and by venting the exhaust of the vacuum pump to a fume hood. -
Page 79: Checking For Hydrogen And Oxidizer Leaks
Troubleshooting page 79. If you suspect a leak inside the detector mainframe, contact Agilent for service. Do not open the detector mainframe. Checking for hydrogen and oxidizer leaks To check for a leak in the hydrogen or oxidizer flow paths, do the following: Check all external fittings for leaks. -
Page 80: Power Problems
Troubleshooting Power Problems When troubleshooting power problems on an SCD or NCD, remember that the power supplied to the detector electronics and flow modules comes from the GC and is controlled by the GC power switch. The power supplied to the SCD/NCD heaters, NCD chiller, vacuum pump, and ozone generator comes from the detector mainframe and is controlled by the detector power switch. -
Page 81: Ozone Generation Problems
Troubleshooting Ozone Generation Problems Before troubleshooting the ozone generator, first verify that the other components of the system operate normally. For example, check for leaks in the detector external connections, check for leaks in the inlet and inlet column fitting, check that the vacuum pump operates normally, check that the inlet and ALS are operating normally, and so on. -
Page 82: Coking
Troubleshooting Coking Contamination from some sample matrices can reduce sensitivity. For example, crude oils containing volatile metal complexes may contaminate the ceramic tubes. In addition, incomplete combustion of certain hydrocarbon-containing compounds leaves behind coke deposits on the ceramic tubes. Coke deposits may be removed from the burner by reducing the hydrogen flow rate. -
Page 83: Hydrogen Poisoning
Troubleshooting Hydrogen Poisoning Hydrogen poisoning of the SCD ceramic tubes can occur when the relative oxidizer flow is very much lower than the hydrogen flow. Whether this state occurs due to inappropriate method setpoints or due to a problem with the oxidizer flow, this condition results in extremely reduced or no response. -
Page 84: Contaminated Gases
Troubleshooting Contaminated Gases Agilent recommends the use of clean gases that meet the requirements in the Site Preparation Guide. In addition, Agilent highly recommends the use of high quality traps to eliminate as much possible contamination as possible. The use of clean gases is essential for optimal performance. -
Page 85: Performance Verification
Agilent 8355 S SCD and 8255 S NCD User Manual Performance Verification About Chromatographic Checkout Prepare for Chromatographic Checkout Check SCD Performance Check NCD Performance This chapter describes how to verify that the detector is operating normally. Agilent Technologies... -
Page 86: About Chromatographic Checkout
Performance Verification About Chromatographic Checkout The tests described in this section provide basic confirmation that the GC and detector can perform comparably to factory condition. However, as detectors and the other parts of the GC age, detector performance can change. The results presented here represent typical outputs for typical operating conditions and are not specifications. -
Page 87: Prepare For Chromatographic Checkout
Performance Verification Prepare for Chromatographic Checkout Because of the differences in chromatographic performance associated with different consumables, Agilent strongly recommends using the parts listed here for all checkout tests. Agilent also recommends installing new consumable parts whenever the quality of the installed ones is not known. For example, installing a new liner and septum ensures that they will not contribute any contamination to the results. -
Page 88: Prepare Sample Vials
Performance Verification Table 10 Recommended parts for checkout by inlet type (continued) Recommended part for checkout Part number Liner, Ultra Inert, splitless, single taper, glass wool 5190-2293 Cool On-column inlet Septum 5183-4758 Septum nut 19245-80521 Syringe, 5-µL on-column 5182-0836 0.32-mm needle for 5-µL syringe 5182-0831 7693A ALS: Needle support insert, COC G4513-40529... -
Page 89: Check Scd Performance
Performance Verification Check SCD Performance Gather the following: • Evaluation column, DB-1 30 m × 0.32 mm × 1.0 μm (part number 123-1033) • SCD performance evaluation (checkout) sample (5190-7003): 0.7 ± 0.002 mg/L diethyl disulfide and 1.0 ± 0.003 mg/L tert-butyldisulfide in isooctane. •... - Page 90 Performance Verification burner cleanliness. Noise will also greatly decrease over time. For a well-stabilized system, noise measured by Agilent OpenLAB CDS should be approximately 5 display units or less. Checkout can continue before the baseline becomes completely stable. Set the analog range to 9, if using an AIB. If using an Agilent 35900E A to D set to 10, or set to 12 if testing for linearity.
- Page 91 Performance Verification Table 11 SCD Checkout conditions (continued) Septum purge 15 mL/min Detector Base temperature 280°C Burner temperature 800 °C Upper H flow 38 mL/min Lower H flow 8 mL/min Oxidizer flow 50 mL/min, Air O3 Generator flow O3 Generator power Vacuum pump FID-SCD Tandem settings FID temp...
- Page 92 Performance Verification Table 11 SCD Checkout conditions (continued) Solvent A post washes Solvent A wash volume 8 µL (maximum) Solvent B pre washes Solvent B post washes Solvent B wash volume 8 µL (maximum) Injection mode (7693A) Normal Airgap Volume (7693A) Viscosity delay Solvent Wash Draw Speed (7693A) Solvent Wash Dispense Speed...
- Page 93 Performance Verification The following chromatogram shows typical results for a new detector with new consumable parts installed. Note that the response for a tandem FID-SCD installation will be approximately 1/10 of the response shown in this example due to the reduced amount of sample that reaches the SCD. SCD1 A, Front Signal (C:\CHEM32\2\DATA\XCD-DATA-FEB2015\SCD\EXAMPLE.D) 2500 2000...
- Page 94 Performance Verification Compound Amount injected Sulfur S amount Typical ASTM Typical Typical MDL (mg/L) content injected noise Sensitivity (pg S/µL) (pg/µL) (Area/pg*s) Diethyl disulfide 0.700 52.50 % 367.500 2.453 9.504 0.469 tert-Butyldisulfide 1.000 36.00 % 360.000 2.453 10.993 0.446...
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Page 95: Check Ncd Performance
Performance Verification Check NCD Performance Gather the following: • Evaluation column, HP-5 30 m × 0.32 mm × 0.25 μm (part number 19091J-413) • NCD performance evaluation (checkout) sample (5190-7002): 3-methylindole 10.0 ± 0.1 mg/L, 9-methylcarbazole 14.1 ± 0.1 mg/L, and nitrobenzene 9.51 ±... - Page 96 Performance Verification However, a new burner (or a burner with a new quartz tube) can have a very high baseline after first ignition. In this case, the baseline should gradually decrease, depending on burner cleanliness. Noise will also greatly decrease over time. For a well-stabilized system, noise measured by Agilent OpenLAB CDS should be approximately 4 display units or less.
- Page 97 Performance Verification Table 12 NCD Checkout conditions (continued) Cool on-column inlet Temperature Oven Track Septum purge 15 mL/min Detector Base temperature 280°C Burner temperature 900 °C Chiller temperature flow 3 mL/min Oxidizer flow 8 mL/min, Oxygen O3 Generator flow O3 Generator power Vacuum pump Oven Initial temp...
- Page 98 Performance Verification Table 12 NCD Checkout conditions (continued) Airgap Volume (7693A) Viscosity delay Solvent Wash Draw Speed (7693A) Solvent Wash Dispense Speed 1500 (7693A) Sample Wash Draw Speed (7693A) Sample Wash Dispense Speed 1500 (7693A) Inject Dispense Speed (7693A) 3000 Plunger speed (7683) Fast, for all inlets except COC.
- Page 99 Performance Verification The following chromatogram shows typical results for a new detector with new consumable parts installed. NCD1 A, Front Signal (C:\CHEM32\2\DATA\XCD-DATA-FEB2015\NCD\EXAMPLE.D) 4000 3000 2000 1000 For a new installation, calculate the MDL of nitrogen for the detector. Calculate MDL as: 2 x noise MDL = sensitivity...
- Page 100 Sensitivity (pg N/µL) (mg/L) (pg/µL) (Area/pg*s) Nitrobenzene 9.510 11.37 % 1081.29 1.080 2.813 0.7679 3-Methylindole 10.000 10.67 % 1067.00 1.080 2.668 0.810 9-Methylcarbazole 14.100 7.72 % 1088.52 1.080 2.795 0.773 Agilent Technologies, Inc. Printed in USA March 2017...