Agilent Technologies 355 SCD Manuale utente

Agilent Technologies

Operation and Maintenance

Manual

Agilent 355 Sulfur and 255 Nitrogen

Chemiluminescence Detectors

Notices

No part of this manual may be reproduced

in any form or by any means (including

electronic storage and retrieval or transla-

tion into a foreign language) without prior

agreement and written consent from Agi-

lent Technologies, Inc. as governed by

United States and international copyright

laws.

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 docu-

ment is provided “as is,” and is sub-

ject to being changed, without notice,

in future editions. Further, to the max-

imum 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 par-

ticular purpose. Agilent shall not be

liable for errors or for incidental or

consequential damages in connection

with the furnishing, use, or perfor-

mance 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 sep-

arate 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 sub-

contract, Software is delivered and

licensed as “Commercial computer soft-

ware” 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. Gov-

ernment will receive no greater than

Restricted Rights as defined in FAR

52.227-19(c)(1-2) (June 1987). U.S. Govern-

ment 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 haz-

ard. It calls attention to an operat-

ing 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 per-

formed or adhered to, could result

in personal injury or death. Do not

proceed beyond a WARNING

notice until the indicated condi-

tions are fully understood and met.

Acknowledgements

Torx® is a registered trademark of Textron

Inc.; Teflon® is a registered trademark of

E.I. du Pont de Nemours and Company.

Kimwipe® is a registered trademark of the

Kimberly-Clark Corporation.

Operation and Maintenance Manual 3

Warnings

English

WARNING

This symbol on the instrument indicates that the user should refer to the man-

ual for operating instructions.

WARNING

Any operation requiring access to the inside of the equipment, could result in

injury. To avoid potentially dangerous shock, disconnect from power supply

before opening the equipment.

WARNING

For continued protection against fire hazard replace fuse with same type and

rating.

WARNING

This symbol indicates that to comply with European Union Directive

2002/96/EC for waste electrical and electronic equipment (WEEE), the Ana-

lyzer should be disposed of separately from standard waste.

WARNING

This is a safety Class I product. It must be wired to a mains supply with a protective

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.

WARNING

If this instrument is used in a manner not specified by Agilent, the protection provided by

the instrument may be impaired.

WARNING

High voltage is present in the instrument when the power cord is connected, even if the

main power switch is in the standby mode. To avoid potentially dangerous shock, discon-

nect the power cord before removing the side panels.

4 Operation and Maintenance Manual

WARNING

Ozone is a hazardous gas and a strong oxidant. Exposure to ozone should be minimized

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.

WARNING

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

WARNING

Hydrogen is an extremely flammable gas. Use appropriate care when handling. Inspect

all connections with a suitable leak detector.

WARNING

Oxygen rich environments can promote combustion and even result in spontaneous com-

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.

WARNING

Exceeding the gas inlet pressure of 25 psig (1.72 bar) may damage the hydrogen and oxi-

dant sensors or burst their connective tubing.

Operation and Maintenance Manual 5

Español

WARNING

Cualquier operación que requiera acceso al interior del equipo, puede causar

una lesión. Para evitar peligros potenciales, desconectarlo de la alimentación

a red antes de abrir el equipo.

WARNING

Para protección contínua contra el peligro de fuego, sustituir el fusible por

uno del mismo tipo y características.

WARNING

Este símbolo en el instrumento indica que el usuario debería referirse al man-

ual para instrucciones de funcionamiento.

WARNING

Esto es un producto con clase I de seguridad. Debe conectarse a una red que disponga de

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.

WARNING

Si este instrumento se usa de una forma no especificada por Agilent, puede desactivarse

la protección suministrada por el instrumento.

6 Operation and Maintenance Manual

Français

WARNING

Chaque opération à l'intérieur de l'appareil, peut causer du préjudice. Afin

d'éviter un shock qui pourrait être dangereux, disconnectez l'appareil du

réseau avant de l'ouvrir.

WARNING

Afin de protéger l'appareil continuellement contre l'incendie, échangez le fus-

ible par un fusible du même type et valeur.

WARNING

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

WARNING

Ceci est un produit de Classe de sécurité I. L'instrument doit être branché sur

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.

WARNING

Si l'instrument n'est pas utilisé suivant les instructions de Agilent, les dispositions de

sécurité de l'appareil ne sont plus valables.

Operation and Maintenance Manual 7

Deutsch

WARNING

Vor dem Öffnen des Gerätes Netzstecker ziehen!

WARNING

Für kontinuierlichen Schutz gegen Brandgefahr dürfen bei Sicherungswech-

sel nur Sicherungen der gleichen Stärke verwendet werden!

WARNING

Dieses Symbol auf dem Gerät weist darauf hin, dass der Anwender zuerst das

entsprechende Kapitel in der Bedienungsanleitung lesen sollte.

WARNING

Dies ist ein Gerät der Sicherheitsklasse I und darf nur mit einem Netzkabel mit

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.

WARNING

Wenn das Gerät nicht wie durch die Firma Agilent, vorgeschrieben und im Handbuch

beschrieben betrieben wird, können die im Gerät eingebauten Schutzvorrichtungen

beeinträchtigt werden.

8 Operation and Maintenance Manual

Italiano

WARNING

Qualsiasi intervento debba essere effettuato sullo strumento può essere

potenzialmente pericoloso a causa della corrente elettrica. Il cavo di alimen-

tazione deve essere staccato dallo strumento prima della sua apertura.

WARNING

Per la protezione da rischi da incendio in seguito a corto circuito, sostituire I

fusibili di protezione con quelli dello stesso tipo e caratteristiche.

WARNING

Il simbolo sullo strumento avverte l'utilizzatore di consultare il Manuale di

Istruzioni alla sezione specifica.

WARNING

Questo strumento è conforme alle specifiche per I prodotti in Classe I - Il cavo di

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.

WARNING

Se questo strumento viene utilizzato in maniera non conforme alle specifiche di Agilent,

le protezioni di cui esso è dotato potrebbero essere alterate.

Operation and Maintenance Manual 9

Dutch

WARNING

Iedere handeling binnenin het toestel kan beschadiging veroorzaken. Om ied-

ere mogelijk gevaarlijke shock te vermijden moet de aansluiting met het net

verbroken worden, vóór het openen van het toestel.

WARNING

Voor een continue bescherming tegen brandgevaar, vervang de zekering door

een zekering van hetzelfde type en waarde.

WARNING

Het symbool geeft aan dat de gebruiker de instructies in de handleiding moet

raadplegen.

WARNING

Dit is een produkt van veiligheidsklasse I. Het toestel moet aangesloten worden op het

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.

WARNING

Indien het toestel niet gebruikt wordt volgens de richtlijnen van Agilent, gelden de

veiligheidsvoorzieningen niet meer.

10 Operation and Maintenance Manual

The following symbols are used on the equipment:

Caution - Refer to manual for

operating instructions

Caution - Risk of electrical

shock.

Caution - Hot surface.

Atención - Ver documentación

pertinente.

Atención - Riesgo de sacudidas

eléctricas.

Atención - Superficie caliente.

Attention - Consultez les

ocuments d'accomagnement.

Attention - Risque de choc

électrique.

Attention - Surface brûlante.

Vorsicht - Siehe beiliegende

Unterlagen.

Vorsicht - Risiko eines

Elektroschocks.

Vorsicht - Heisse Oberfläche.

Pericolo - Vedi

documentazione allegata.

Pericolo - Pericolo di scosse

elettriche.

Pericolo - Superficie rovente.

Voorzichtig - Raadpleeg di

bijehorende documentatie.

Voorzichtig - Hoge spanning,

levensgevaar.

Voorzichtig - Heet oppervlak.

Operation and Maintenance Manual 11

Contents

1 Introduction

2 System 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

12 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 Oil- Sealed 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 O

2

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

Operation and Maintenance Manual 13

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

5Operation

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 75

Table 1. Typical Operating Conditions 75

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

14 Operation and Maintenance Manual

6Maintenance

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

Operation and Maintenance Manual 15

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

16 Operation and Maintenance Manual

17

Agilent 355 Sulfur and 255 Nitrogen Chemiluminescence Detectors

Operation and Maintenance Manual

Agilent Technologies

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.

18 Operation and Maintenance Manual

19

Agilent 355 Sulfur and 255 Nitrogen Chemiluminescence Detectors

Operation and Maintenance Manual

Agilent Technologies

2

System Description

Specifications 20

Theory of Operation 23

Description of Major Components 25

20 Operation and Maintenance Manual

Specifications

Technical Information — 355 SCD

Technical Information — 255 NCD

Sensitivity

*

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

Typical < 0.5 pg S/second (signal to noise 3.3:1)

Typical Selectivity g S/g C > 2 x 10

7

Linearity >10

4

Precision and Stability

†

† 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.

<2% RSD 2 hours

<5% RSD 72 hours

Ozone flow through the Post Ozone Restrictor 20-30 mL/min at 3-6 psig

Typical reaction cell pressure 4 - 8 Torr RV5 Oil Sealed Pump

6 - 12 Torr Dry Piston Pump

Typical Burner Pressure 250-400 Torr operating

Typical Burner Temperature 800 °C

Typical Air Flow Rate 65 SCCM recommended

3-10 SCCM recommended with FID adapter

Typical Hydrogen Flow Rate 40 SCCM recommended

Signal Output Ranges 0-1V, 0-10V

Typical time to reach 800 °C from room

temperature

10 min typical(120 VAC, 60 Hz)

Typical safety shroud outside temperature <65 °C at 800 °C Burner temperature typical

Recorder output 0-1 V or 0-10 V

Sensitivity <3 pg N/second (signal to noise 3:1) in both N

and nitrosamine modes

Selectivity g N/g C > 2 to 10

7

in N mode (selectivity in

nitrosamine mode is matrix-dependent)

Linearity >10

4

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