Bruker CryoProbe User manual

BRUKER
CryoProbe System
Installation
Version 1

The information in this manual may be altered without notice.
BRUKER accepts no responsibility for actions taken as a result
of use of this manual. BRUKER accepts no liability for any mis-
takes contained in the manual, leading to coincidental damage,
whether during installation or operation of the instrument. Un-
authorised reproduction of manual contents, without written
permission from the publishers, or translation into another lan-
guage, either in full or in part, is forbidden.
This manual was written by
M. Schick, D. Marek,D. Oberli, S. Gloor
© March 28, 2001: Bruker AG
Fällanden, Switzerland
P/N: Z31555
DWG-Nr: 1266001

CryoProbe Installation BRUKER 3 (93)
Contents
Contents ............................................................... 3
1 Safety .................................................................... 7
1.1 Terms and symbols .............................................................. 7
1.2 Disclaimer ........................................................................... 8
1.3 Emergency .......................................................................... 8
1.4 Personnel safety .................................................................. 9
1.5 Safety of CryoProbe equipment ......................................... 11
1.6 First aid ............................................................................. 11
2 Introduction ........................................................ 13
2.1 How to use this manual ..................................................... 13
2.2 CryoProbe System overview .............................................. 13
2.3 Conventions ...................................................................... 14
3 Initial setup ......................................................... 17
3.1 Before delivery .................................................................. 17
3.2 Transport ........................................................................... 17
3.3 Check the site preparations ............................................... 18
3.4 Before you unpack ............................................................. 19
3.5 Unpacking ......................................................................... 19
3.6 Positioning the units .......................................................... 21
3.7 BCU05 cooling test (optional) ............................................ 22
3.8 Spectrometer modifications ............................................... 22
Access to the magnet bottom ........................................ 22
Cranked magnet pillar braces (optional) ........................ 23
Blue spinning stator ...................................................... 24
Replacing the shim system (optional) ............................ 24
Attach the Mounting Hardware ...................................... 25
3.9 Handling ............................................................................ 27
3.10 Mounting ........................................................................... 28
3.11 Sample spinning test ......................................................... 33
3.12 Joining the CryoCoupler .................................................... 34
3.13 Load firmware ................................................................... 38
3.14 Boot the CryoController ..................................................... 39
3.15 Hook up the He steel-cylinder ............................................ 41
3.16 Interconnect the He Compressor ....................................... 43
3.17 Warning labels ................................................................... 45
3.18 Connecting ........................................................................ 46
3.19 Power-on ........................................................................... 49
3.20 VT setup ........................................................................... 50
3.21 Initial He fill ....................................................................... 52
3.22 Cool-down ......................................................................... 52

4 (93) BRUKER CryoProbe Installation
Contents
3.23 Load additional XWIN-NMR software .................................... 54
3.24 Put HPPR CRP assembly into operation ............................ 54
3.25 How to proceed ................................................................. 55
4 Customizing the CryoProbe System ................... 57
4.1 Experimental parameters .................................................. 57
RF power levels ........................................................... 57
Safety attenuators ........................................................ 57
Standard parameter sets .............................................. 57
Lock power ................................................................... 57
Sample temperature control .......................................... 57
Sample tubes and spinners .......................................... 58
Receiver sensitivity ...................................................... 58
4.2 Acceptance tests ............................................................... 58
4.3 User training ..................................................................... 58
5 Troubleshooting .................................................. 59
5.1 Fuses and reset buttons .................................................... 59
5.2 General failure .................................................................. 60
No mains ...................................................................... 60
Spinning problems ........................................................ 60
Indicator on CryoProbe sticks out ................................. 61
CryoController failure ................................................... 61
Leak in He supply ......................................................... 62
5.3 Cool-down problems ......................................................... 62
COOL DOWN command is ignored ................................... 62
Insufficient vacuum ....................................................... 62
He Compressor does not run ........................................ 63
Periodic hiss is missing ................................................ 65
Cool-down doesn’t reach cold state .............................. 66
5.4 How to open the CryoCooling Unit ..................................... 67
5.5 Refill He ............................................................................ 67
6 Relocation of a CryoPlatform .............................. 69
6.1 Relocation ......................................................................... 69
6.2 CryoProbe System storage ................................................ 69
6.3 Disposal ............................................................................ 69
Pressure release .......................................................... 70
Toxic materials 70
7 Bruker contact ..................................................... 73
7.1 CryoProbe information ...................................................... 73
7.2 CryoProbe service ............................................................ 73
A Check lists ........................................................... 75

Contents
CryoProbe Installation BRUKER 5 (93)
1.1 Site preparation checks ..................................................... 75
1.2 Preparations for the installation visit .................................. 75
1.3 User training ...................................................................... 76
A Related documents ............................................. 79
B Conversion of metric units ................................. 81
C Glossary .............................................................. 83
Figures ................................................................ 89
Tables .................................................................. 91

6 (93) BRUKER CryoProbe Installation
Contents

CryoProbe Installation BRUKER 7 (93)
Safety 1
1000000
Read these safety instructions carefully and make them accessible to everybody
working with the CryoProbe System. A CryoProbe can be operated easily and
safely provided the correct procedures are obeyed and certain precautions ob-
served.
Terms and symbols 1.1
0
WARNING: Disregard of this may lead to personal injury.
CAUTION: Disregard of this may permanently damage the system.
IMPORTANT: Disregard of this can lead to malfunctions.
NOTE: Hint for good operating practice.
Figure 1.1. Hot surface!
The labelled item may be hot. Be careful when touching it!
Figure 1.2. High voltage!
The labelled item houses a dangerous voltage. Do not open it!
Figure 1.3. Dangerous device!
The labelled item presents a potential hazard. Read the manual if
you don’t know how to handle it!
Figure 1.4. Cold surface!
The labelled item may be cold. Be careful when touching it!

8 (93) BRUKER CryoProbe Installation
Safety
Disclaimer 1.2
0
BRUKER is not responsible or liable for any injury or damage that occurs as a con-
sequence of non-approved manipulations on the CryoProbe System.
Emergency 1.3
0
The main switch on the CryoCooling Unit front serves as an EMERGENCY OFF. It
powers down the systems for cryogenic cooling, vacuum, sensors, and helium
gas compression. All valves are reset to their default positions. The CryoPreamps
inside the CryoProbe, however, are not affected by an EMERGENCY OFF because
they are supplied from the HPPR. If the system is kept OFF, it will slowly warm up
due to thermal conduction.
NOTE: Because an EMERGENCY OFF shuts down also the supervisor electronics,
it should only be used as a last resort.
When powered on again, the CryoController will first analyze the system state and
determine a way to reach a stable situation before restarting the He Compressor
etc.
See the CryoProbe System User Manual for details.
Figure 1.5. Wear protective gloves!
Put on protective gloves before handling the labelled item.
Figure 1.6. Wear protective goggles!
Put on protective goggles before handling the labelled item.
Figure 1.7. Strong attraction by magnet!
The item is magnetic and presents a potential hazard in the vicinity of
a magnet. Keep it away from the magnet!
!

Personnel safety
CryoProbe Installation BRUKER 9 (93)
Personnel safety 1.4
0
All persons who work with or in the close vicinity of a CryoProbe System must be
informed about its safety issues and emergency procedures.
WARNING: Do not disconnect any tube or cable from a running CryoProbe Sys-
tem unless WARM and UNPLUG light up on the CryoCooling Unit front panel.
If in doubt: Put on goggles and protective gloves!
WARNING: Do not manipulate connectors, screws, valves or pressure relief
valves other than those that are explicitly described in the CryoProbe System
manuals for operator use.
Inherent safety
The CryoProbe System is designed for inherent safety. Pressure relief valves,
sensors, and error handling in hardware and software have been included to pro-
tect operator, equipment, and environment.
CE certification
CryoProbe, CryoCooling Unit and He Compressor are CE certified.
Technically qualified personnel only
Only persons with a basic technical understanding of electricity, pressurized gas
systems, and cryogenics should operate and maintain a CryoProbe System. User
interface, system messages, and manuals require a good understanding of the
English language.
No user-serviceable parts inside
There are no user-serviceable parts inside a CryoProbe, a CryoCooling Unit cabi-
net, a He Compressor, or any other component of a CryoProbe System. Do not
open these devices.
BRUKER warranty expires if the CryoProbe was opened by unauthorized per-
sonnel.
WARNING: Two persons are required to lift the heavy panels of the CryoCooling
Unit. Be careful with the panels, there might be sharp edges on their inside which
could cause injuries.
WARNING: If you have to work with an open CryoCooling Unit cabinet, put on
protective goggles and gloves.
Pressurized cold helium gas cycle
The CryoPlatform works with helium gas (He) that is pressurized up to about
25 bar and cooled to cryogenic temperatures around 20 K. All pressurized parts
are kept in strong enclosures which are designed to hold back gas jets or ejected
particles in case of a rupture. If unprotected skin is exposed to cold He, severe
cold burns are possible.
The helium gas volume inside the cryogenic cooling cycle is small and presents
virtually no danger of suffocation. However, the He steel-cylinder contains a sub-
stantial gas volume, note the warning below ("Pressurized helium gas supply"
on page 10).

10 (93) BRUKER CryoProbe Installation
Safety
NOTE: If a pressure or vacuum leak appears, the CryoProbe System will be auto-
matically stopped and warmed up to ambient temperature.
Pressurized helium gas supply
WARNING: Move, connect, and operate the He steel-cylinder carefully. Obey all
safety precautions pertinent to high pressure gas containers and magnetic ob-
jects.
WARNING: The He steel-cylinder and its entire transport path must always be
outside the 0.5 mT range of the magnet.
WARNING: Fix the He steel-cylinder reliably to a wall. All local safety regulations
for the installation of pressurized gas systems must be obeyed.
The helium pressure hose between the He steel-cylinder and the CryoCooling
Unit carries a steel wire that must be fixed to the units at its ends. If crossing of
walkways cannot be avoided, the He Hose must be covered or buried. Moreover,
the He Hose must be fixed to a wall or to the floor once every meter.
WARNING: If the He Hose is not fixed it can whip around in case of a rupture.
WARNING: If a large quantity of helium gas escapes from the He steel-cylinder
during a short period, there is a danger of suffocation, particularly in small rooms.
Care for good ventilation and fresh air supply after an accidental release of large
quantities of helium gas.
Overpressure release noise
Overpressure in the system is avoided by software control and mechanical safety
valves. In case of malfunction of software as well as human interference into valve
settings, the release valves can open with an extremely loud bang! The sound
protection cabinet will reduce the noise to a safe level, therefore do not operate
with an open cabinet.
WARNING: If a service action on an open CryoCooling Unit cabinet cannot be
avoided while the He Compressor runs or while the helium gas supply is manipu-
lated, the ears must be protected.
Electrical safety
The CryoCooling Unit’s degree of protection against electrical hazard complies
with IEC IP20, i.e. all electrical parts are protected against touching.
WARNING: All electrical connectors must be used as supplied by BRUKER. Do not
substitute them by other types.
No hazardous substances
There are virtually no substances in a CryoProbe System that could be hazardous
for an NMR user. See the CryoProbe Installation manual for materials that need
special consideration upon relocation or disposal.
Lifting the CryoProbe
WARNING: Two persons are needed to insert and remove the CryoProbe.
When kneeling down at the magnet bore, your body posture is not suited to lift the
heavy CryoProbe (~12 kg) on your own. For two persons it is very easy. Take
care not to injure your back!

Safety of CryoProbe equipment
CryoProbe Installation BRUKER 11 (93)
Magnetic stray field
When working within the 0.5 mT stray field of the magnet, all magnetic parts and
tools must be avoided or handled with great care.
Safety of CryoProbe equipment 1.5
0
CAUTION:
- Do not bend the CryoProbe.
Do not hold the CryoProbe at its upper tube, carry it only at its body.
- Do not open the CryoProbe.
There are no user-serviceable parts inside. A CryoProbe cannot be sealed
or reassembled without special equipment. Even undoing some screws can
destroy factory settings and will in general render the CryoProbe unusable.
- Never force a CryoCoupler into position.
- Do not obstruct the operation of the safety-valves on the top and front faces of
the CryoProbe body.
- Do not move a cryogenically cold device.
- Do not try to fix a leak on a cold part because cracking of frozen o-rings, valves
etc. may occur.
- Excessive RF power can destroy the CryoProbe or the HPPR CRP. Obey the
limitations given on the specific ‘LIMITATIONS - WARNINGS’ sheet. See also
User Manual.
First aid 1.6
0
If cold helium gas comes in contact with eyes or skin, immediately flood the affect-
ed area with cold or tepid water.

12 (93) BRUKER CryoProbe Installation
Safety

CryoProbe Installation BRUKER 13 (93)
Introduction 2
2000000
BRUKER CryoProbes™ offer a dramatic increase in signal-to-noise ratio (S/N) by
reducing the operating temperature of the NMR coil assembly and the preamplifi-
er. Their spectroscopic handling is very similar to a conventional probe. While the
sample temperature is stabilized at a user-defined value around room tempera-
ture, the NMR coil assembly - located a few millimeters from the sample - is
cooled with cryogenic helium gas. An automatic closed-cycle cooling system con-
trols all functions and guarantees excellent stability during short and long-term ex-
periments. As a result, the system is easy to handle. CryoProbes open new fields
for NMR applications e.g. where low sample concentration or long measurement
time are critical.
How to use this manual 2.1
0
This CryoProbe System Installation Manual guides you through the initial setup
and test of a CryoProbe System. Several procedures are the same as in daily
use, so they are described in the CryoProbe System User Manual. The two man-
uals are complementary and must both be available for an installation.
Use the appropriate "Check lists" on page 75 to keep track of your actions.
If you have a specific question, use
-“Contents”,
- “Index” or
-“Frequently asked questions”
to locate the answer.
Novice users of a CryoProbe System should read "Safety" on page 7.
Further information can be found in the manuals listed in "Related documents"
on page 79.
CryoProbe System overview 2.2
0
A CryoProbe System consists of several subunits: CryoProbe, CryoPlatform,
cryo-compatible HPPR CRP, He steel-cylinder, and optional water chiller (Figure
2.1.).
The term ‘CryoPlatform’ summarizes the parts required to operate a CryoProbe
such as the CryoCooling Unit, the He Compressor, the Mounting Hardware at the
magnet etc. It is compatible with all BRUKER CryoProbes and only one per spec-
trometer is needed.

14 (93) BRUKER CryoProbe Installation
Introduction
Conventions 2.3
0
SMALL CAPS ITALIC setting of a hardware switch or button
Courier small contents of a file
Courier small italic system response
Courier file or directory name
Courier bold Unix™ or Windows™ NT keyboard command
Figure 2.1. The CryoProbe™ System
AVANCE Console
Magnet
CryoProbeTM
He-Compressor
Water Cooled, European
Version: O00247
HPPR CRP
(Cryo-compatible HPPR Z003422
BRUKER
CryoPlatformTM
Default configuration: BH 0410
Room temperature He Gas
pressure lines & Cables
Length 6m: Z47199
Transferline
(Part of
CryoCooling
Unit)
BRUKER
Water
Chiller
(Optional)
Transferline
Support
Mounting Kit
for 500 MHz BRUKER
SB Magnet with Boss2
shim system: Z 46554
He Gas
cylinder
(to be
provided
by
customer)
Connenction to He-Gas
cylinder incl. Pressure
reduction valve:
Z46261
CryoCooling
Unit
With 2m Transferline:
Z45447
CryoProbe
Mounting
Hardware
Water
Chiller
Option
European
Version:
BH 0420

Conventions
CryoProbe Installation BRUKER 15 (93)
Courier italic bold BRUKER NMR Suite keyboard command
Times bold Unix or Windows NT object clicked with the mouse
Times italic bold BRUKER NMR Suite object clicked with the mouse
Times italic host name, User name etc.
< > place holder

16 (93) BRUKER CryoProbe Installation
Introduction

CryoProbe Installation BRUKER 17 (93)
Initial setup 3
3000000
Before delivery 3.1
0
Before an installation date with BRUKER is fixed, the customer needs to read the
following remarks and work through the "Site preparation checks" on page 75
for the NMR laboratory.
The checklist "Preparations for the installation visit" on page 75 is intended
for the BRUKER engineer.
General
All necessary preparations for the CryoProbe System must have been completed
before BRUKER engineers arrive at the customer site and perform the installation.
BRUKER personnel will connect all units of a the CryoProbe System as far as re-
quired for test and operation but they will not work on the laboratory infrastructure
(e.g. mount cable channels, fix tubes to the wall, drill holes or the like) to make the
installation ‘look nice’.
NOTE: The spectrometer cannot be used for NMR experiments (with e.g. a con-
ventional setup) during installation and test of the CryoProbe System.
Other laboratory equipment
Other devices in the laboratory may depend on the same supplies as the Cryo-
Probe System, e.g. pneumatic gas and electricity. It must be checked if these de-
vices can continue their operation while the CryoProbe System is hooked up to
the shared supplies.
Reference data
Get a set of reference spectra with a conventional probe to estimate spectrometer
performance and external disturbances. The spectra should be fairly new. Check
e.g. lineshape, sensitivity, water suppression, lock stability spikes and vibrations,
t1-noise etc.
NOTE: Sensitivity is the major issue for the CryoProbe and it is influenced by nu-
merous external factors. The CryoProbe cannot reach its specs if any other spec-
trometer component fails to do so!
Transport 3.2
0
The CryoProbe System is shipped in three steps: first a Site Preparation Set con-
taining the He Compressor and some tubes which must be installed by the cus-
tomer in the NMR lab to provide the infrastructure for the CryoProbe System. After
the site preparation work has been completed, CryoCooling Unit and HPPR CRP
are sent off and installed by a BRUKER engineer. Finally, the CryoProbe is deliv-

18 (93) BRUKER CryoProbe Installation
Initial setup
ered and installed in a third step. If circumstances permit, the second and third
step are done at together.
Crate dimensions
All dimensions in [mm], width ⌠length ⌠height.
1.a wooden crate 770 ⌠600 ⌠930, 150 kg water-cooled He Compressor,
or
1.b wooden crate 820 ⌠700 ⌠1130, 170 kg: air-cooled He Compressor,
2. wooden crate 1210 ⌠1380 ⌠1520, 620 kg: CryoCooling Unit,
3. cardboard box 350 ⌠440 ⌠510, 27 kg: HPPR CRP,
4. cardboard box 1200 ⌠800 ⌠500,
pallet 1200 ⌠800 ⌠140,
flightcase 1010 ⌠510 ⌠340, 30 kg:
i.e. in total 1200 ⌠800 ⌠640, 40 kg: CryoProbe,
+ some smaller items in cardboard boxes.
The crates are not returned to BRUKER but preferably kept at the customers site.
CAUTION: All components of a CryoProbe system are fragile! The CryoCooling
Unit must be shipped in upright position. There are shock watches and tilt indica-
tors on its shipping crate.
Transport pathways
Check transport pathways and transportation means before sale. Do size or
weight of the CryoProbe System exceed the capabilities of elevators, floors etc.?
Usually, the same transport pathway as used for the magnet delivery will be fine
(see Avance Site Planning 200-700, § 1.5). A pallet truck suffices as transport aid.
If the transport pathway in the destination building is too narrow for the CryoCool-
ing Unit shipping case, this unit might be unpacked and carried on a pallet truck to
its final site. Then, all passages must be only at least 100 cm wide. Note that the
pallet truck does not go straight under the CryoCooling Unit but only at about a
45° angle.
WARNING: Avoid magnetic transport aids when moving devices inside the mag-
net’s 0.5 mT stray field. Even heavy equipment like a pallet truck may be attracted
and cause fatal damage.
Environmental conditions for transport and storage
The allowed ranges of temperature, humidity, atmospheric pressure, dust, and
maximum accelerations are the same as for AVANCE spectrometers.
Check the site preparations 3.3
0
Have all necessary preparations been done in the lab? Are all supplies available?
Use the "Site preparation checks" on page 75.

Before you unpack
CryoProbe Installation BRUKER 19 (93)
Before you unpack 3.4
0
Ensure safety
Read the instructions for "Safety" on page 7 before starting the installation.
Check instrument cases for damage
Inspect the cases, shock watches, and tilt indicators.
In case of damage: Do not unpack! You need to do certain things now for legal
reasons. Call your BRUKER service office and ask for advice:
- Should you accept the goods or refuse them? (Note: Usually, BRUKER is the ‘cus-
tomer’ of this transport, but not BRUKER’s ‘NMR customer’ who owns the lab.)
- Do you need to write a statement?
- Is the visit of an insurance expert necessary?
- Should you unpack and install?
Record actual NMR spectrometer status
Mark the incoming gas pressure on the gauge at the rear of the spectrometer cab-
inet with a waterproof pen or write down the reading with a precision of 0.1 bar. If
there is a pressure gauge on the magnet suspension, mark or record that value,
too.
Is a NMR performance reference data set available (sensitivity, lineshape, water
suppression, etc.)? Are any spectral artifacts visible like spikes or noise?
IMPORTANT: Before installing the CryoProbe System, make sure there are no
performance problems with the conventional parts of the spectrometer. The Cryo-
Probe cannot reach its specifications if any other spectrometer component fails to
do so!
Unpacking 3.5
0
Use the shipping and packing lists to check if all parts arrived and if they are com-
plete. In case of obvious damage, proceed according to the recommendations
given in "Check instrument cases for damage" on page 19. Keep all packing
material and transport certificates until the CryoProbe System runs satisfactorily.
The CryoProbe flight case is ideal for storing the CryoProbe when not in use.
CryoProbe
Keep the CryoProbe in its flightcase until you can mount it into the magnet. Leave
the protective caps on sample cavity, CryoCoupler, and RF sockets until you
make the connections.
In the upper right corner of the CryoProbe front, there is a little hole with an indica-
tor screw inside. This screw must not stick out but be flush with the front plate. If
the screw sticks out, a problem with the vacuum insulation may have occurred -
contact BRUKER! Do not try to move the screw, neither in/out nor by rotation. When
cooling down the CryoProbe, this indicator will move in.

20 (93) BRUKER CryoProbe Installation
Initial setup
CAUTION: The CryoProbe is heavy (~12 kg) but fragile. Hold it only at its body,
not at the tube. Never bend the tube!
If only an additional CryoProbe is to be installed on a working CryoPlatform, con-
tinue with "Handling" on page 27.
CryoCooling Unit
Disassemble the crate and remove the transport fixtures. The CryoCooling Unit
weights ~400 kg. It is most convenient to lift it off the pallet with a fork-lift truck. It
can also be lifted with a hoist. There are four eyes (for hooks or ropes) on the in-
ner frame of the CryoCooling Unit. To access them, remove the top panel of the
CryoCooling Unit (see "How to open the CryoCooling Unit" on page 67).
IMPORTANT: Take special care of the He Transferline when unpacking and mov-
ing the CryoCooling Unit. Avoid tight bending! If the radius becomes smaller than
0.7 m, i.e. if a 180° turn has less than 1.4 m diameter, its internal structure can be
damaged.
On the back panel, there’s a plug without cable connected to REMOTE SWITCH.
Make sure this plug is in place. If the plug is missing, the mains of the whole Cryo-
Cooling Unit is inhibited.
He Compressor
Check the SUPPLY PRESSURE gauge on the He Compressor front. It should indi-
cate about 0.1 bar (i.e. 0.01 MPa 0.1 kgf/cm2). If the pressure gauge reads plain
0 bar, contact BRUKER: this is a major problem and a lengthy gas purifying cycle is
required.
Water-cooled He Compressor (P/N O00247) only: Set the selector switch accord-
ing to the available mains voltage and frequency. The switch is hidden behind the
right side panel. See section 2.5 in the He Compressor operation manual which is
delivered with the CryoPlatform.
NOTE: On the backside of the He Compressor, keep the protective cap on the
HELIUM GAS CHARGE. This connector is never used.
Figure 3.1. CryoProbe handling