Agilent Technologies G6600-90006 User Manual

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Agilent 355 Sulfur and 255 Nitrogen

Chemiluminescence Detectors

Operation and Maintenance

Manual

Agilent Technologies

Notices

No part of this manual may be reproduced in any form or by any means (including electronic storage and retrieval or translation into a foreign language) without prior agreement and written consent from Agilent Technologies, Inc. as governed by United States and international copyright laws.

Acknowledgements

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Manual Part Number

G6600-90006

Edition

First edition, June 2007

Replaces G6600-90002

Printed in USA

Agilent Technologies, Inc.

2850 Centerville Road

Wilmington, DE 19808-1610 USA

Warranty

The material contained in this document is provided “as is,” and is subject to being changed, without notice, in future editions. Further, to the maximum extent permitted by applicable law, Agilent disclaims all warranties, either express or implied, with regard to this manual and any information contained herein, including but not limited to the implied warranties of merchantability and fitness for a particular purpose. Agilent shall not be liable for errors or for incidental or consequential damages in connection with the furnishing, use, or performance of this document or of any information contained herein. Should Agilent and the user have a separate written agreement with warranty terms covering the material in this document that conflict with these terms, the warranty terms in the separate agreement shall control.

Technology Licenses

The hardware and/or software described in this document are furnished under a license and may be used or copied only in accordance with the terms of such license.

Restricted Rights Legend

If software is for use in the performance of a U.S. Government prime contract or subcontract, Software is delivered and licensed as “Commercial computer software” as defined in DFAR 252.227-7014 (June 1995), or as a “commercial item” as

defined in FAR 2.101(a) or as “Restricted computer software” as defined in FAR 52.227-19 (June 1987) or any equivalent agency regulation or contract clause. Use, duplication or disclosure of Software is subject to Agilent Technologies’ standard commercial license terms, and non-DOD Departments and Agencies of the U.S. Government will receive no greater than Restricted Rights as defined in FAR 52.227-19(c)(1-2) (June 1987). U.S. Government users will receive no greater than Limited Rights as defined in FAR 52.227-14 (June 1987) or DFAR 252.227-7015 (b)(2) (November 1995), as applicable in any technical data.

Safety Notices

CAUTION

A CAUTION notice denotes a hazard. It calls attention to an operating procedure, practice, or the like that, if not correctly performed or adhered to, could result in damage to the product or loss of important data. Do not proceed beyond a CAUTION notice until the indicated conditions are fully understood and met.

WARNING

A WARNING notice denotes a hazard. It calls attention to an operating procedure, practice, or the like that, if not correctly performed or adhered to, could result in personal injury or death. Do not proceed beyond a WARNING notice until the indicated conditions are fully understood and met.

Warnings

English

	WA RN ING	This symbol on the instrument indicates that the user should refer to the man-
	WA RN ING	ual for operating instructions.
		ual for operating instructions.

	WA RN ING	Any operation requiring access to the inside of the equipment, could result in
	WA RN ING	injury. To avoid potentially dangerous shock, disconnect from power supply

		before opening the equipment.

	WA RN ING	For continued protection against fire hazard replace fuse with same type and
	WA RN ING	rating.
		rating.

	WA RN ING	This symbol indicates that to comply with European Union Directive
	WA RN ING	2002/96/EC for waste electrical and electronic equipment (WEEE), the Ana-

		lyzer should be disposed of separately from standard waste.

	WA RN ING	This is a safety Class I product. It must be wired to a mains supply with a protective
	WA RN ING	earthing ground incorporated into the power cord. Any interruption of the protective

		conductor, inside or outside the equipment, is likely to make the instrument dangerous.
		Intentional interruption is prohibited.

	WA RN ING	If this instrument is used in a manner not specified by Agilent, the protection provided by
	WA RN ING	the instrument may be impaired.
		the instrument may be impaired.

	WA RN ING	High voltage is present in the instrument when the power cord is connected, even if the
	WA RN ING	main power switch is in the standby mode. To avoid potentially dangerous shock, discon-

		nect the power cord before removing the side panels.

Operation and Maintenance Manual

	WA RN ING	Ozone is a hazardous gas and a strong oxidant. Exposure to ozone should be minimized
	WA RN ING	by using the instrument in a well-ventilated area and by venting the exhaust of the vac-

		uum pump to a fume hood. The ozone generator should be turned off when the instrument
		is not in use.

WA RN ING	Burner temperature Is extremely hot. Do not touch. Allow to cool before servicing.
WA RN ING

	WA RN ING	Hydrogen is an extremely flammable gas. Use appropriate care when handling. Inspect
	WA RN ING	all connections with a suitable leak detector.
		all connections with a suitable leak detector.

	WA RN ING	Oxygen rich environments can promote combustion and even result in spontaneous com-
	WA RN ING	bustion under conditions of high pressure and exposure to contamination. Use only oxy-

		gen rated components and ensure that components are oxygen clean prior to use with
		pure oxygen.

	WA RN ING	Exceeding the gas inlet pressure of 25 psig (1.72 bar) may damage the hydrogen and oxi-
	WA RN ING	dant sensors or burst their connective tubing.
		dant sensors or burst their connective tubing.

4	Operation and Maintenance Manual

Español

	WA RN ING	Cualquier operación que requiera acceso al interior del equipo, puede causar
	WA RN ING	una lesión. Para evitar peligros potenciales, desconectarlo de la alimentación

		a red antes de abrir el equipo.

	WA RN ING	Para protección contínua contra el peligro de fuego, sustituir el fusible por
	WA RN ING	uno del mismo tipo y características.
		uno del mismo tipo y características.

	WA RN ING	Este símbolo en el instrumento indica que el usuario debería referirse al man-
	WA RN ING	ual para instrucciones de funcionamiento.
		ual para instrucciones de funcionamiento.

	WA RN ING	Esto es un producto con clase I de seguridad. Debe conectarse a una red que disponga de
	WA RN ING	tierra protectora en el cable de red. Cualquier interrupción del conductor protector,

		dentro o fuera del equipo, puede ser peligroso. Se prohibe la interrupción intencionada.

	WA RN ING	Si este instrumento se usa de una forma no especificada por Agilent, puede desactivarse
	WA RN ING	la protección suministrada por el instrumento.
		la protección suministrada por el instrumento.

Operation and Maintenance Manual

Français

	WA RN ING	Chaque opération à l'intérieur de l'appareil, peut causer du préjudice. Afin
	WA RN ING	d'éviter un shock qui pourrait être dangereux, disconnectez l'appareil du

		réseau avant de l'ouvrir.

	WA RN ING	Afin de protéger l'appareil continuellement contre l'incendie, échangez le fus-
	WA RN ING	ible par un fusible du même type et valeur.
		ible par un fusible du même type et valeur.

WA RN ING	Le symbol indique que l'utilisateur doit consulter le manuel d'instructions.
WA RN ING

	WA RN ING	Ceci est un produit de Classe de sécurité I. L'instrument doit être branché sur
	WA RN ING	l'alimentation secteur par un fil de secteur prévu d'une prise de masse. Chaque

		interruption du conducteur protégeant, à l'intérieur ou á l'extérieur de l'appareil peut
		rendre l'instrument dangereux. Interruption intentionnelle est interdite.

	WA RN ING	Si l'instrument n'est pas utilisé suivant les instructions de Agilent, les dispositions de
	WA RN ING	sécurité de l'appareil ne sont plus valables.
		sécurité de l'appareil ne sont plus valables.

6	Operation and Maintenance Manual

Deutsch

WA RN ING	Vor dem Öffnen des Gerätes Netzstecker ziehen!
WA RN ING

	WA RN ING	Für kontinuierlichen Schutz gegen Brandgefahr dürfen bei Sicherungswech-
	WA RN ING	sel nur Sicherungen der gleichen Stärke verwendet werden!
		sel nur Sicherungen der gleichen Stärke verwendet werden!

	WA RN ING	Dieses Symbol auf dem Gerät weist darauf hin, dass der Anwender zuerst das
	WA RN ING	entsprechende Kapitel in der Bedienungsanleitung lesen sollte.

	WA RN ING	Dies ist ein Gerät der Sicherheitsklasse I und darf nur mit einem Netzkabel mit
	WA RN ING	Schutzleiter betrieben werden. Jede Unterbrechung des Schutzleiters au erhalb oder

		innerhalb des Gerätes kann das Gerät elektrisch gefährlich machen. Absichtliches
		Unterbrechen des Schutzleiters ist ausdrücklich verboten.

	WA RN ING	Wenn das Gerät nicht wie durch die Firma Agilent, vorgeschrieben und im Handbuch
	WA RN ING	beschrieben betrieben wird, können die im Gerät eingebauten Schutzvorrichtungen

		beeinträchtigt werden.

Operation and Maintenance Manual

Italiano

	WA RN ING	Qualsiasi intervento debba essere effettuato sullo strumento può essere
	WA RN ING	potenzialmente pericoloso a causa della corrente elettrica. Il cavo di alimen-

		tazione deve essere staccato dallo strumento prima della sua apertura.

	WA RN ING	Per la protezione da rischi da incendio in seguito a corto circuito, sostituire I
	WA RN ING	fusibili di protezione con quelli dello stesso tipo e caratteristiche.

	WA RN ING	Il simbolo sullo strumento avverte l'utilizzatore di consultare il Manuale di
	WA RN ING	Istruzioni alla sezione specifica.
		Istruzioni alla sezione specifica.

	WA RN ING	Questo strumento è conforme alle specifiche per I prodotti in Classe I - Il cavo di
	WA RN ING	alimentazione dalla rete deve essere munito di "terra". Qualsiasi interruzione del cavo di

		terra all'interno ed all'esterno dello strumento potrebbe risultare pericolòsa. Sono
		proibite interruzioni intenzionali.

	WA RN ING	Se questo strumento viene utilizzato in maniera non conforme alle specifiche di Agilent,
	WA RN ING	le protezioni di cui esso è dotato potrebbero essere alterate.

8	Operation and Maintenance Manual

Dutch

	WA RN ING	Iedere handeling binnenin het toestel kan beschadiging veroorzaken. Om ied-
	WA RN ING	ere mogelijk gevaarlijke shock te vermijden moet de aansluiting met het net

		verbroken worden, vóór het openen van het toestel.

	WA RN ING	Voor een continue bescherming tegen brandgevaar, vervang de zekering door
	WA RN ING	een zekering van hetzelfde type en waarde.
		een zekering van hetzelfde type en waarde.

	WA RN ING	Het symbool geeft aan dat de gebruiker de instructies in de handleiding moet
	WA RN ING	raadplegen.
		raadplegen.

	WA RN ING	Dit is een produkt van veiligheidsklasse I. Het toestel moet aangesloten worden op het
	WA RN ING	net via een geaard netsnoer. Bij onderbreking van de beschermende geleider, aan de

		binnenzijde of aan de buitenzijde van het toestel, kan gebruik het toestel gevaarlijk
		maken. Opzettelijke onderbreking is verboden.

	WA RN ING	Indien het toestel niet gebruikt wordt volgens de richtlijnen van Agilent, gelden de
	WA RN ING	veiligheidsvoorzieningen niet meer.
		veiligheidsvoorzieningen niet meer.

Operation and Maintenance Manual

The following symbols are used on the equipment:

Caution - Refer to manual for	Caution - Risk of electrical	Caution - Hot surface.
operating instructions	shock.
Atención - Ver documentación	Atención - Riesgo de sacudidas	Atención - Superficie caliente.
pertinente.	eléctricas.
Attention - Consultez les	Attention - Risque de choc	Attention - Surface brûlante.
ocuments d'accomagnement.	électrique.
Vorsicht - Siehe beiliegende	Vorsicht - Risiko eines	Vorsicht - Heisse Oberfläche.
Unterlagen.	Elektroschocks.
Pericolo - Vedi	Pericolo - Pericolo di scosse	Pericolo - Superficie rovente.
documentazione allegata.	elettriche.
Voorzichtig - Raadpleeg di	Voorzichtig - Hoge spanning,	Voorzichtig - Heet oppervlak.
bijehorende documentatie.	levensgevaar.

10	Operation and Maintenance Manual

1Introduction

2System Description

Specifications 20
Technical Information — 355 SCD					20
Technical Information — 255 NCD					20
Physical Specifications		21
Theory of Operation	23
Sulfur Chemiluminescence Detector					23
Nitrogen Chemiluminescence Detector						23
Dual Plasma Controller		24
Description of Major Components				25
Dual Plasma Burner		25
Figure 1. Cross-Section of the Dual Plasma Burner for the 355 SCD							26
Figure 2. Cross-Section of the Dual Plasma Burner for the 255 NCD							27
Dual Plasma Controller		27
Ozone Generator	28
Chemiluminescence Reaction Cell and Photomultiplier Tube 28
Figure 3. 355 SCD Left Side			29
Figure 4. 355 SCD Right Side			30
Figure 5. 255 NCD Left Side View					31
Figure 6. 255 NCD Right Side View					32
Pressure Transducer		32
Vacuum Pump	32
Chemical Trap	33
Oil Coalescing Filter		33
FID Adapter (Optional)		33
NCD Reaction Cell 33
NCD Photomultiplier Tube and Cooler						34
Figure 7. Schematic for 355 SCD				35

Figure 8.	Schematic for 255	NCD, in Nitrogen Mode 36
Figure 9.	Schematic for 255	NCD, in Nitrosamine Mode 37

Operation and Maintenance Manual

3 Installation

Overview 40
Step 1: Selecting a Location		41
Power Requirements	41
Figure 10. Drawing of the Detector with Dual Plasma Burner and Controller							42
Environmental Considerations			42
Combustion Gas Requirements			42
Step 2: Unpack and Inspect the Instrument					45
Required Installation Tools		45
Step 3: Set Up the Vacuum Pump			46
Installing the Edwards RV5 Pump Oil-Sealed Vacuum Pump 46
Figure 11. RV5 Oil-Sealed Vacuum Pump and Associated Traps (Front Side)							49
Figure 12. RV5 Oil-Sealed Vacuum Pump and Associated Traps (Back Side)							49
Figure 13. RV5 OilSealed Vacuum Pump and Associated Traps (Top) 50
Figure 14. RV-5 Oil-S ealed Vacuum Pump Exhaust Line 51
Installing the Welch Dry Piston Vacuum Pump						52
Figure 15. The Welch Dry Piston Pump					54
Figure 16. Oil Drain Kit with Ballast Control						54
Step 4: Connect the Power Cord			56
Figure 17. SCD Rear Panel Diagram				56
Step 5: Install the Dry Compressed Air or O2 Supply 57
Step 6: Install the Signal Output Cables				58
Standard Cable Connection		58
HP 3390 Series Integrator Cable Connection						58
HP 3396 Integrator Cable Connection					58
HP 5890 GC Analog Input Board			58
Agilent 6890 GC Analog Input Board					58
Step 7: Install the Dual Plasma Burner				59
Figure 18. Dimensions of GC Liner Cut-Outs						59
Step 8: Install the Dual Plasma Controller					60
Figure 19. Dual Plasma Controller Rear Panel						60
Step 9: Install Column Connections			61
Capillary Columns	61
Figure 20. Measuring Column Insertion					61

12	Operation and Maintenance Manual

Packed Columns and Columns with an Outside Diameter > 0.8 mm 61

Step 10: Install the Transfer Line 62

4 Front Panel Controls and Initial Startup

Detector Front Panel Controls		64
Figure 21. Front Panel Controls			64
Power Controls	64
Display Output Controls		65
Signal Controls	65
Dual Plasma Controller Controls			66
Figure 22. Dual Plasma Controller Front Panel 66
Initial Startup	67
Detector Interface Setup 69
Initial Checkout	69

Monitoring Oxidizer and Hydrogen Flow with the Dual Plasma Controller 70

5 Operation

Start-Up Procedure	72
Detector Operation	73
Detector Stability and Response 73
Column Bleed	73
Coking 73
Hydrogen Poisoning		73
Contaminated Gases		74
Fluctuating Pressures		74

Typical Operating Conditions

Table 1. Typical Operating Conditions

Detection Limits	76
Table 2. Expected Detection Limits for Chromatographic Conditions 76
Instrument Shut-Down		77
Daily Shutdown	77
Complete Shutdown		77
Special Operating Modes		78

Using the 255 NCD in Nitrosamine Mode 78

Using the SCD in High Sensitivity Mode for Nonhydrocarbon Gaseous Samples 78

Operation and Maintenance Manual

6 Maintenance

Pump Maintenance	82
Table 3. Operating Life of Components for Edwards RV5 Vacuum Pump 82
Cleaning the Detector	83
Changing the Oil Mist Filter (RV5)			84
Reaction Cell Cleaning	85
Figure 23. Reaction Cell, PMT Housing and PMT Socket						86
Figure 24. Reaction Cell		86
Flow Sensor Calibration		88
Detector Sensitivity	89
Assembling the Dual Plasma Burner for Component Replacement with the SCD								90
Figure 25. Ferrule Placement on Lower Burner Tube					90
Figure 26. Proper Ferrule Orientation to the Large Ceramic Tube							91
Figure 27. Large Ceramic Tube Properly Inserted into the Quartz Heater Assembly									91
Figure 28. Orientation of the Double Taper Ferrule					92
Figure 29. Positioning the Upper Tube in the Union Fitting						92
Figure 30. Tightening the Heater Swivel Nut				93
Figure 31. Proper Alignment of the Burner				93
Assembling the Dual Plasma Burner for Component Replacement with the NCD								95
Figure 32. Ferrule Placement on Lower Burner Tube					95
Figure 33. Proper Ferrule Orientation to the Large Quartz Tube							96
Figure 34. The Quartz Tube Properly Inserted into the Quartz Heater Assembly								96
Figure 35. Burner Assembly Detail 97
Figure 36. Burner Assembly Alignment 97
Tube Replacement for the SCD			98
Figure 37. Orientation of the Double Taper Ferrule					98
Figure 38. Positioning the Upper Tube in the Union Fitting						99
Figure 39. Proper Ferrule Orientation to the Large Ceramic Tube							99
Figure 40. Large Ceramic Tube Properly Inserted into the Quartz Heater Assembly									100
Figure 41. Tightening the Heater Swivel Nut				100
Figure 42. Proper Alignment of the Burner				101
Tube Replacement for the NCD			102
Figure 43. Proper Ferrule Orientation to the Large Quartz Tube							102
Figure 44. Large Quartz Tube Properly Inserted into the Quartz Heater Assembly									103
Figure 45. NCD Tube Replacement Detail				104
Figure 46. NCD Tube Replacement Detail				104

14	Operation and Maintenance Manual

7 Troubleshooting

Solving Detector Problems 106

Power Problems	107
Detector Fuse	107

Vacuum Pump Fuse 107

Dual Plasma Controller Fuses 107

Table 4. Fuses for 100 V, 120 V and 230 V Versions of 355 SCD and 255 NCD 108 Figure 47. Fuse Positions on the Power Supply Board 108

Ozone Generation Problems		109
Ozone Generator	109
High Voltage Transformer		109
Plugged Restrictor Lines		110
Response Problems	111
Temperature Reading Problems 112
Diagnosing General Problems		113
Table 5. Troubleshooting Detector Issues			113
Table 6. Troubleshooting Pump Issues			115
Table 7. Troubleshooting Burner Issues			116

Index

Operation and Maintenance Manual

16	Operation and Maintenance Manual

Agilent 355 Sulfur and 255 Nitrogen Chemiluminescence Detectors

Operation and Maintenance Manual

1 Introduction

This manual will guide you in the installation, operation, and troubleshooting of the Agilent 355 Sulfur Chemiluminescence Detector (SCD) and the Agilent 255 Nitrogen Chemiluminescence Detector (NCD). This manual is intended for use with the Agilent 355 SCD or 255 NCD with the Dual Plasma Burner and Controller.

This operation and service manual has some important conventions, such as the use of boxed warnings. This information is deliberately set out from the text for emphasis and should be followed to assure operator safety and proper instrumental operation.

If you are installing the 355 SCD or 255 NCD yourself, follow the installation procedures described in the following sections. If your instrument is already installed, turn to the Operation section to begin.

Agilent Technologies

18	Operation and Maintenance Manual

Agilent 355 Sulfur and 255 Nitrogen Chemiluminescence Detectors Operation and Maintenance Manual

System Description

Specifications 20

Theory of Operation 23

Description of Major Components 25

Agilent Technologies

Specifications

Technical Information — 355 SCD

Sensitivity*

Typical Selectivity

Linearity

Precision and Stability†

Ozone flow through the Post Ozone Restrictor Typical reaction cell pressure

Typical Burner Pressure

Typical Burner Temperature

Typical Air Flow Rate

Typical Hydrogen Flow Rate

Signal Output Ranges

Typical time to reach 800 °C from room temperature

Typical safety shroud outside temperature Recorder output

Typical < 0.5 pg S/second (signal to noise 3.3:1) g S/g C > 2 x 107

>104

<2% RSD 2 hours <5% RSD 72 hours

20-30 mL/min at 3-6 psig

4 - 8 Torr RV5 Oil Sealed Pump

6 - 12 Torr Dry Piston Pump

250-400 Torr operating

800 °C

65 SCCM recommended

3-10 SCCM recommended with FID adapter

40 SCCM recommended

0-1V, 0-10V

10 min typical(120 VAC, 60 Hz)

<65 °C at 800 °C Burner temperature typical 0-1 V or 0-10 V

* Burner temperature 800 °C, 80 SCCM air, and 60 SCCM hyrdrogen, test compound dimethyl sulfide in toluene.

†Based on thiopene in benzene at 1 ppm mass sulfur, 1 µL injection split 1:10, 30 m, 0.32 mm ID, 1 µm thick CP wax (n=10 for 2.5 hours; n=42 for 72 hours).

Subject to change without notice.

Technical Information — 255 NCD

Sensitivity	<3 pg N/second (signal to noise 3:1) in both N
	and nitrosamine modes
Selectivity	g N/g C > 2 to 107 in N mode (selectivity in
	nitrosamine mode is matrix-dependent)
Linearity	>104

20	Operation and Maintenance Manual

Repeatability*	<1.5% RSD 8 hours (~ the same in N and
	nitrosamine)
	<2% RSD 18 hours (~3% RSD in nitrosamine
	mode over 21 hours)
Gas flow through Ozone Generator	20-30 mL/min at 3-6 psig (inlet pressure)
Typical reaction cell pressure	4 - 8 Torr RV5 Oil Sealed Pump
	6 - 12 Torr Dry Piston Pump
Typical Burner Pressure	130 - 150 torr operating
Typical Burner Temperature	900 °C
Typical Hydrogen Flow Rate	6-10 SCCM
Typical Oxygen Flow Rate	8 - 15 SCCM
Signal Output Ranges	0-1V, 0-10V, 0 - 10V

*Burner temperature 950 °C, 11 SCCM oxygen, and 6 SCCM hydrogen; 25 ppm N as nitrobenzene in toluene; 0.2 µL injection on column (HP 19095-121Z), n=7 for 3 hours; n=13 for 18 hours and n=10

n-dipropylnitrosamine in toluene at 4 µg/mL, 0.2 µL injection on column (HP 19095-121Z).

Physical Specifications

Power requirements

355 SCD Detector	115 VAC, 50/60 Hz, 1400 W
	100 VAC, 50/60 Hz, 1400 W
	220-240 VAC, 50/60 Hz, 650W
255 NCD Detector	115 VAC, 50/60 Hz, 1400 W
	100 VAC, 50/60 Hz, 1400 W
	220-240 VAC, 50/60 Hz, 650W
Dual Plasma Controller	100-120 VAC, 50/60 Hz, 200 W
	220-240 VAC, 50/60 Hz, 200 W

Dimensions and weight

Detector	Height: 16.0 in (40.6 cm)
	Width: 9.2 in (23.4 cm)
	Depth: 21.8 in (55.3 cm)
	355	SCD Weight: 34.0 lbs (15.0 kg)
	255	NCD Weight: 37.5 lbs (17.0 kg)

Operation and Maintenance Manual

Dual Plasma Controller	Height: 5.0 in (12.7 cm)
	Width: 9.5 in (24.1 cm)
	Depth: 12.5 in (31.8 cm)
	Weight: 9.9 lbs (4.5 kg)
Dual Plasma Burner	Height: 12.3 in (31.2 cm)
	Diameter: 4.0 in (10.2 cm)
	Weight: 1.9 lbs (0.9 kg)
Oil Sealed Vacuum Pump (RV5)	Height: 10.3 in (26.1 cm)
	Width: 6.0 in (15.2 cm)
	Depth: 16.9 in (43.0 cm)
	Weight: 47.3 lbs (21.5 kg)
or
Oil Free Dry Piston Pump	Height: 12.0 in (30 cm)
	Width: 9.0 in (22.9 cm)
	Depth: 14.0 in (35.6 cm)
	Weight: 29.9 lbs (13.6 kg)
Installation Category	II
Pollution Degree	2
Ambient Temperature	50 - 104 °F (10-40 °C)
Relative Humidity	Up to 95%, noncondensing
Normal Operating Environment	Intended for indoor use only
Maximum Altitude	2,000 m (6,562 ft)
Mains Supply Voltage	Fluctuation not to exceed 10% of nominal
	voltage

22	Operation and Maintenance Manual

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

Operation and Maintenance Manual

Dual Plasma Controller

The Dual Plasma Controller provides all operational parameters of the Dual Plasma Burner except for the Detector base temperature. The Detector base temperature is controlled by circuitry in the GC. Parameters monitored or regulated by the Controller include Burner temperature, Burner temperature set-point, hydrogen and oxidant flow rates, and Burner pressure. The temperature set-point, actual pressure, oxidant and hydrogen flow rates are displayed by rotation of a 4-position switch. Power, valve operation, temperature within set-point range and fault conditions are indicated with LED illumination on the front display panel.

The Dual Plasma Controller incorporates several safety features. The safety circuitry detects faults such as power loss, vacuum loss, thermocouple failure, heater element failure, broken ceramic tube, or high temperature. When a fault is detected, the Fault LED illuminates and hydrogen and oxidant flow is stopped by normally-closed solenoid valves.

Dual Plasma Burner with the 355 SCD

The Dual Plasma Burner is based on the same chemistry and basic principles of earlier SCD Burner designs. A key difference, however, is the addition of a second “flame” or “plasma,” the lower is oxygen-rich and the upper is hydrogen-rich. The Burner consists of a tower assembly that contains an outer sheath for burn protection, a heating element, thermocouple, and combustion tubes. Conversion of sulfur containing compounds to SO occurs within the ceramic reaction chamber housed in the Burner assembly. Agilent also provides a Flame Ionization Detector (FID) option for the simultaneous collection of hydrocarbon and sulfur chromatograms for some GCs.

Dual Plasma Burner with the 255 NCD

Compounds eluted from the GC column are combusted in the Dual Plasma Burner first by an oxygen rich flame (plasma) followed by catalytic combustion on a Noble metal screen. For hydrocarbons, this two stage combustion technique results in complete conversion of the matrix to products, such as carbon dioxide and water, which do not chemiluminesce with ozone. Nitrogen atoms in a compound are converted into nitric oxide and potentially other nitrogen oxide species. In the second stage, the catalyst is used to convert other nitrogen oxide species to nitric oxide, resulting in a high efficiency of conversion.

24	Operation and Maintenance Manual

Description of Major Components

Dual Plasma Burner

The Dual Plasma Burner consists of a tower assembly that contains an outer sheath for burn protection, a heating element, thermocouple, and combustion tubes. In the SCD, conversion of sulfur containing compounds to SO occurs within the ceramic reaction chamber housed in the Burner assembly and potentially interfering hydrocarbons are oxidized to CO2 and H2O, with air as the oxidant. In the NCD, oxygen is used as the oxidant.

A fitting is located on top of the Burner. The vacuum line from the Detector box is connected directly to the top of this fitting and H2 is input to the longer side of this fitting. The air inlet is connected to the base of the Burner.

The Burner is mounted onto the GC by a model-specific mounting kit (see www.Agilent.com/chem or contact Agilent for the most current information). The GC column is inserted into the Burner using a 1/32" knurled nut and fused silica adapter ferrule.

A cross-section illustration of the Dual Plasma Burner for the 355 SCD is shown in Figure 1 and for the 255 NCD is shown in Figure 2.

Operation and Maintenance Manual

Figure 1 Cross-Section of the Dual Plasma Burner for the 355 SCD

26	Operation and Maintenance Manual

Figure 2 Cross-Section of the Dual Plasma Burner for the 255 NCD

Dual Plasma Controller

The Dual Plasma Controller powers the Dual Plasma Burner and supplies its gases. Hydrogen and oxidant should be provided at 25 psig (1.72 bar) and the Controller is plugged into an appropriate AC electrical outlet.

	WA RN ING	Exceeding the gas inlet pressure of 25 psig (1.72 bar) may damage the hydrogen and oxi-
	WA RN ING	dant sensors or burst their connective tubing.
		dant sensors or burst their connective tubing.

The parameters monitored or regulated by the Controller include Burner

Operation and Maintenance Manual

temperature, hydrogen and oxidant flow rates, and Burner pressure. The temperature, actual pressure, oxidant and hydrogen flow rates are selected for display by rotation of a 4-position control knob. Power, valve operation, temperature within set-point range and fault conditions are indicated with LED illumination on the front display panel.

Ozone Generator

The SCD and NCD produce ozone by corona discharge using a clean, pressurized air or oxygen source. Use of oxygen should increase ozone production and, hence, Detector response. High voltage to the ozone generator is applied only when the reaction cell pressure is less than 100 torr in the SCD and less than 200 torr in the NCD. Gas flow through the ozone generator is controlled by a pressure regulator and flow restrictors.

	WA RN ING	Ozone is a hazardous gas and a strong oxidant. Exposure to ozone should be minimized by
	WA RN ING	using the instrument in a well ventilated area, changing the chemical trap regularly, and

		venting the exhaust of the vacuum pump. The ozone generator should be turned off when
		the instrument is not in use to reduce maintenance requirements.

Chemiluminescence Reaction Cell and Photomultiplier Tube

Sulfur monoxide (formed in the Burner) and ozone (produced in the ozone generator located in the Detector) are mixed in the reaction cell. The cell is designed such that the reaction between SO and O3 occurs directly in front of the photomultiplier tube (PMT). A UV band pass filter (300 - 400 nm) located between the reaction cell and the PMT selectively transmits the light emitted by the SO/O3 reaction. Efficient combustion in the ceramic tubes coupled with the UV band pass filter eliminates interference from non-sulfur containing analytes (e.g. nitric oxide, olefins, etc.) which also undergo chemiluminescent reactions with ozone. A background signal is typically present as a result of ozone-wall interactions and low level sulfur contamination of Detector gases. This background signal can be used as a troubleshooting aid (see Section 10).

28	Operation and Maintenance Manual

		10	9
			9
3	4	5	6

6	2
	2
7	1
8



1.	Ozone Generator	6.	Vacuum Line
		6.	Vacuum Line
2.	High Voltage Transformer	7.	Particulate Filter
3.	Photomultiplier Tube Socket	8.	Pre-Ozone Restrictor
3.	Photomultiplier Tube Socket
4.	Photomultiplier Housing	9.	Post-Ozone Restrictor
4.	Photomultiplier Housing	10. Pressure Transducer
5.	Reaction Cell	10. Pressure Transducer
5.	Reaction Cell

Figure 3 355 SCD Left Side

Operation and Maintenance Manual

Agilent Technologies G6600-90006 User Manual

11	IN OFST	OUT OFST
	RV1	RV2
	I	AMP 1
	TP8	TP10
	TP8	TP12

TP2	TP13
	OUT

						TP5	TP4TP6 TP7
				TP2				13
TP4						12			TP3
TP4				TP3
				TP3					ALCO
TP5				TP12
TP1			TP13	TP8	HV/100		TO
GND			TP13		TP11		TO
							FRONT	TP1
			TP14	TP9			PANEL	TP9
			TP14	TP9				TP9	USA
TP6	TP7	TP16	TP15	TP10					USA
				TP10				TP11
								TP11

16					SIEVERS RESEARCH
16	ELECTRONICS		HV
	ELECTRONICS		RV1
			LOAD	PUMP	NEUT
			P4	PUMP	P5
	OZONE			OUT	WHT
	OZONE
		15	LOAD		NEUT
			P6	OZONE	P7
				GEN	WHT
					WHT
	PUMP		LINE		NEUT
			P2	AC	P3
					WHT


11.	Amplifier Cable	15.	Fuses
12.	HV Cable	16.	Pressure Regulator
13.	PMT Amplifier	17.	Transfer line
14.	EMI Filter	18.	Front panel display

Figure 4 355 SCD Right Side

30	Operation and Maintenance Manual

+ 88 hidden pages

Agilent Technologies G6600-90006 User Manual

Contents

1 Introduction

System Description

Specifications

Physical Specifications

Theory of Operation

Sulfur Chemiluminescence Detector

Nitrogen Chemiluminescence Detector

Dual Plasma Controller

Description of Major Components

Dual Plasma Burner

Dual Plasma Controller

Ozone Generator

Chemiluminescence Reaction Cell and Photomultiplier Tube