Agilent Technologies Cryogenic Manuel utilisateur

Agilent Technologies

Cryogenic Systems

Operation

User Guide

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

Agilent Technologies, Inc. as governed by

United States and international copyright

laws.

Manual Part Number

91-002699-00A

Edition

First edition, August 2011

Printed in USA

Agilent Technologies, Inc.

5301 Stevens Creek Boulevard

Santa Clara, CA 95051 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.

Government 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

hazard. It calls attention to an oper-

ating 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.

Cryogenic Systems Operation 3

Contents

1 Introduction

Safety 8

Warning notices 8

Caution notices 11

Radio-frequency emission regulations 12

Agilent Cold Probes 13

Closed-Cycle Cryogenic System 14

CryoBay (cryogenics bay) 14

He compressor 15

Document of Certification 16

2 Cryogenic Operation

Preparing for Cryogenic Operation 18

Connect the CCC transfer arm (stinger) to the probe 18

Connect the vacuum system to the probe vacuum chamber 22

Final System Checks, Cautions and Warnings 23

Configuring VnmrJ for Cryogenic Operation 25

Starting Cryogenic Operation 26

Start the cryogenic process as follows: 26

Stopping Cryobay Operations 28

Cryobay monitor functions 28

Warming both the CCC and the probe 28

Disconnecting the Agilent Cold Probe from the CryoBay 30

Vent the cryogenic transfer line 30

Disconnecting the Agilent Cold Probe from the CryoBay 31

Removing the Agilent Cold Probe from the Magnet 33

Removing the Agilent Cold Probe from magnet when <285 K 35

Agilent Cold Probe/Cryogenic System Care When Not in Use 37

Agilent Cold Probe will remain attached to the CryoBay 37

Agilent Cold Probe disconnected from the CryoBay 39

3 Maintenance and Service

Preventative Maintenance and Service Intervals 42

Changing the Helium Gas Supply (Compressed Gas Cylinder) 43

Filling the Helium Compressor 44

4Cryogenic Systems Operation

Turbo Pump Operation 46

Compressor Maintenance 46

Closed-Cycle Chiller (CCC) Maintenance 47

Changing Cooling-Water Filters (Water-Cooled Compressor) 47

Cooling-water requirements 47

Changing cooling-water filters 47

4 Principles of Operation

Cryogenic System Components 50

Principles of Operation 51

External CryoBay Controls and Connections 54

Internal CryoBay Assemblies 55

Operation Cycle, Status Messages, and States 55

Idle 55

Start 57

Stop 58

Detach 58

Vacuum purge 59

Pump probe 59

5 CryoBay Monitor

Opening the CryoBay Monitor (Main Window) 64

VnmrJ 64

Vertical panel - view menu 66

Stand-alone CryoBay control computer 67

CryoBay Controls Window 68

CryoBay Controls - Loading Files 70

CryoBay Controls – Advanced 73

CryoBay Data Log 74

VnmrJ 74

Stand-alone CryoBay control computer 74

Data log sequence of readings displayed 74

CryoBay Controls–Help Menu 75

About CryoBay 76

Service counter 76

About panel 76

Cryogenic Systems Operation 5

6 Error Messages

Fault Codes 78

CryoBay Actions Under Fault Conditions 80

General Operation Faults 81

Start window - cannot start. System not warm 81

Detach probe window - detach probe failed 81

Fault Code Causes, Actions and Corrections 82

7 Unexpected Events

Advanced Notice of Utility Shutdown 92

Single-Phase Power Failure 93

Three-Phase Power Failure (Compressor) 94

Cooling-Water Failure (Water-Cooled Compressor) 94

Compressed Air for Pneumatics Failure 95

Vacuum 95

Purging 95

Cooling or operating 95

Temperature Controller Gas Failure 95

Alternative gas source is available 95

Alternative gas source is not available 95

Host Computer Failure 96

Recovering from an Unexpected Event 97

CCC has not reached room temperature (285 K) 97

CCC has reached room temperature 98

Safety Shutdown 99

Sources of power 99

Safety shutdown of the system 99

Powering system back on after safety shutdown 101

8 Appendix

CryoBay Sample Eject Air and Sample Catcher 104

Turning on or off the CryoBay sample eject air 105

Adjusting the CryoBay sample eject air 107

Inserting a sample using a sample catcher 109

Ejecting and removing a sample using a sample catcher 109

Swagelok and Aeroquip Fittings 110

Swagelok connector installation 110

Retightening swagelok connectors 111

6Cryogenic Systems Operation

Aereoquip connectors 112

Connecting to helium compressor and CCC 113

Disconnecting from helium compressor 113

Cryogenic Systems Operation

User Guide

Agilent Technologies

Introduction

A Cryogenic system consists of an Agilent Cold Probe and

closed- cycle cryogenic system.

The cryogenic system circulates cold He gas to maintain key

probe components at an operating temperature of

approximately 25 kelvin.

Safety 8

Agilent Cold Probes 13

Closed-Cycle Cryogenic System 14

8Cryogenic Systems Operation

1Introduction

Safety

Warning notices

Observe the following precautions during installation,

operation, maintenance, and repair of the instrument.

Failure to comply with these warnings, or with specific

warnings elsewhere in Agilent manuals, violates safety

standards of design, manufacture, and intended use of the

instrument. Agilent assumes no liability for customer failure

to comply with these precautions.

The superconducting magnet system generates strong

magnetic fields that can affect operation of some cardiac

pacemakers or harm implanted or attached devices such as

prosthetic parts and metal blood vessel clips and clamps.

Pacemaker wearers should consult the user manual provided

by the pacemaker manufacturer or contact the pacemaker

manufacturer to determine the effect on a specific

pacemaker. Pacemaker wearers should also always notify

their physician and discuss the health risks of being in

proximity to magnetic fields. Wearers of metal prosthetics

and implants should contact their physician to determine if

a danger exists.

Refer to the manuals supplied with the magnet for the size

of a typical 5- gauss stray field. This gauss level should be

checked after the magnet is installed.

The strong magnetic field surrounding the magnet attracts

objects containing steel, iron, or other ferromagnetic

materials, which includes most ordinary tools, electronic

equipment, compressed gas cylinders, steel chairs, and steel

carts. Unless restrained, such objects can suddenly fly

towards the magnet, causing possible personal injury and

extensive damage to the probe, dewar, and superconducting

WARNING

Persons with implanted or attached medical devices such as

pacemakers and prosthetic parts must remain outside the 5-gauss

perimeter from the centerline of the magnet.

WARNING

Keep metal objects outside the 10-gauss perimeter from the

centerline of the magnet.

Introduction 1

Cryogenic Systems Operation 9

solenoid. The greater the mass of the object, the more the

magnet attracts the object.

Only nonferromagnetic materials such as plastics, aluminum,

wood, and nonmagnetic stainless steel, should be used in the

area around the magnet. If an object is stuck to the magnet

surface and cannot easily be removed by hand, contact

Agilent service for assistance.

Refer to the manuals supplied with the magnet for the size

of a typical 10- gauss stray field. This gauss level should be

checked after the magnet is installed.

Dangerous high voltages that can kill or injure exist inside

the instrument. Before working inside a cabinet, turn off the

main system power or unplug the unit.

Any unauthorized modification could injure personnel or

damage equipment and potentially terminate the warranty

agreements or service contract. Written authorization

approved by an Agilent product manager is required to

implement any changes to the hardware of a NMR

spectrometer. Maintain safety features by referring system

service to an Agilent service office.

Operation with flammable gases or fumes present creates the

risk of injury or death from toxic fumes, explosion, or fire.

If the magnet dewar should quench (sudden appearance of

WARNING

Only qualified maintenance personnel shall remove equipment

covers or make internal adjustments.

WARNING

Do not substitute parts or modify the instrument.

WARNING

Do not operate in the presence of flammable gases or fumes.

WARNING

Leave area immediately in the event of a magnet quench.

10 Cryogenic Systems Operation

1Introduction

gasses from the top of the dewar), leave the area

immediately. Sudden release of helium or nitrogen gases can

rapidly displace oxygen in an enclosed space creating a

possibility of asphyxiation. Do not return until the oxygen

level returns to normal.

In contact with the body, helium and nitrogen can cause an

injury similar to a burn. Never place your head over the

helium and nitrogen exit tubes on top of the magnet. If

helium or nitrogen contacts the body, seek immediate

medical attention, especially if the skin is blistered or the

eyes are affected.

Unless the probe is removed from the magnet, never look

down the upper barrel. You could be injured by the sample

tube as it ejects pneumatically from the probe.

A sample tube subjected to a change in temperature can

build up excessive pressure, which can break the sample

tube glass and cause injury by flying glass and toxic

materials. To avoid this hazard, establish the freezing and

boiling point of a sample before doing a variable temperature

experiment.

The magnet dewar has a high center of gravity and could tip

over in an earthquake or after being struck by a large object,

injuring personnel and causing sudden, dangerous release of

nitrogen and helium gasses from the dewar. Therefore, the

WARNING

Avoid helium or nitrogen contact with any part of the body.

WARNING

Do not look down the upper barrel.

WARNING

Do not exceed the boiling or freezing point of a sample during

variable temperature experiments.

WARNING

Support the magnet and prevent it from tipping over.

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