SPI Supplies SPI-DRY User manual

Rev. 2.2 April 2021
SPI-DRYTM
Critical Point
Dryer
Operation Manual
SPI Supplies Part #13200JE-AB

SPI Supplies 2 SPI-DRY Critical Point Dryer
Structure Probe, Inc. / SPI Supplies
Street address for UPS, FedEx, DHL, other couriers, trucks
206 Garfield Ave.
West Chester, PA 19380 ·
Mailing address P.O. Box 656 West Chester,
PA 19381-0656 USA
Phone: [phone]-SPI
Toll-free from USA/Canada 1-(610)-436-5400
FAX: [phone]
E-mail: [e-mail]
For further information regarding any of the other products designed and manufactured by SPI Supplies,
contact your local representative or directly to SPI Supplies at the address above.
Carbon and Sputter Coaters
Plasma Reactor for ashing and etching
High Vacuum Bench Top Evaporators
Critical Point Dryers
Electron Microscopy Consumables

SPI Supplies 3 SPI-DRY Critical Point Dryer
Warranty
The SPI Supplies unit you have purchased is guaranteed to be free of defects in workmanship on the
day of shipment. This warranty covers parts and labor for a period of one year, excluding shipping
charges or consumables. Breakage of glassware is specifically excluded from this warranty.
Proper use of your unit, according to the operation manual, should result in trouble-free operation. Any
improper use of the SPI Supplies unit through modifications or unreasonable operating procedures will
void this warranty.
Disclaimer
SPI Supplies instruments are designed for simplicity of installation and operation. This manual provides
full and complete information in both these areas. SPI Supplies therefore assumes no liability or
responsibility of any kind for damage or injury resulting from incorrect installation or operation of the
machine.

SPI Supplies 4 SPI-DRY Critical Point Dryer
1 Contents
1.1 Manual Layout
This Operation Manual is divided up into the following major section, each section dealing with specific
topics, as follows:
Section 1 - Contents
Section 2 - Health and Safety
General section which applies to all SPI Supplies products detailing the very important issues of
Health and Safety applicable when using sample preparation equipment.
Section 3 - Introduction
Introduces this manual.
Section 4 - General Description
Identifies each of the equipment items and provides an overview of their functions and how they
work.
Section 5 - Installation
Instructions on how this instrument should be installed and the connections which should be made
between the equipment items.
Section 6 - Operation
Instructions on how to start-up and run the instrument.
Section 7 - Maintenance
Instructions on routine maintenance checks ensure that the system is functioning correctly.
Information on how to identify faults in the system, and how to rectify these faults.
Section 8 –Troubleshooting
Spare parts and consumables

SPI Supplies 5 SPI-DRY Critical Point Dryer
1.2 Section Contents
Section 1 - Contents ................................................................................................4
1.1 Manual Layout ...............................................................................4
1.2 Section Contents ............................................................................5
1.3 Illustrations .....................................................................................7
1.4 Tables ............................................................................................7
Section 2 - Health and Safety ..................................................................................8
2.1 Safety Policy ..................................................................................8
2.2 Conformity ......................................................................................8
2.3 Servicing ........................................................................................8
2.3.1 Disclaimer ...............................................................................8
2.3.2 Operators and Service Engineers ..........................................8
2.4 Hazard Signals and Signs ..............................................................9
2.4.1 Hazard Signal Words .............................................................9
2.4.2 Hazard Labels used on Equipment ........................................9
2.4.3 Hazard Warning Labels used in Equipment Manuals ............9
2.4.4 Instrument Functionality Signs ...............................................10
2.4.5 Serious Damage to Instruments .............................................10
2.4.6 Hazard to Operator ................................................................10
2.5 Risk Analysis ..................................................................................11
2.5.1 Personal Operational Risks ....................................................11
2.5.2 Hazardous Materials ..............................................................11
2.6 Good Working Practices ................................................................12
2.7 Critical Point Dryer Specific Safety Hazards ..................................12
Section 3 - Introduction............................................................................................13
3.1 Return of Goods .............................................................................13
3.2 Returns Procedure .........................................................................13
Section 4 - Description ............................................................................................14
4.1 Equipment ......................................................................................14
4.1.1 Accessories ............................................................................14
4.2 Overview ........................................................................................15
4.3 Technical Specification ..................................................................15
4.3.1 SPI-DRY Critical Point Dryer Specifications ..........................15
4.4 Physical Description .......................................................................16
4.4.1 Chamber body.........................................................................16
4.4.2 Control Valves ........................................................................16
4.4.3 System Gauges.......................................................................17
4.4.4 Safety Valve ...........................................................................17
4.4.5 Specimen Holder ....................................................................17
4.4.6 Microporous Specimen Capsules ..........................................17

SPI Supplies 6 SPI-DRY Critical Point Dryer
Section 5 - Installation .............................................................................................18
5.1 Unpacking Checklist ......................................................................18
5.1.1 Site Selection .........................................................................18
5.2 Connection of Services ..................................................................19
5.2.2 Water ......................................................................................19
5.2.3 Carbon Dioxide (CO2) ............................................................19
5.2.4 Carbon Dioxide (CO2) Exhaust ..............................................19
Section 6 - Operation ...............................................................................................21
6.1 Critical Point Drying Method ..........................................................21
6.1.1 Drying Fluids ..........................................................................21
6.2 Trial Run .........................................................................................232
6.3 Tissue Preparation .........................................................................23
6.3.1 Washing .................................................................................24
6.3.2 Fixation ...................................................................................25
6.3.3 Dehydration ............................................................................25
6.3.4 Substitution .............................................................................26
6.4 Complete Trial Operation Run .......................................................26
Section 7 - Maintenance ..........................................................................................28
7.1 Chamber Components....................................................................29
7.1.1 Viewing Window Maintenance ...............................................29
7.1.2 End Plate Maintenance ..........................................................29
7.1.3 Drain Valve Maintenance .......................................................29
7.1.4 Gas Control Valve Maintenance ............................................29
7.1.5 Inlet/Vent Valve Maintenance ................................................30
7.1.6 Gauge Maintenance ...............................................................30
7.1.7 Transfer Boat Maintenance ....................................................31
7.1.8 Bursting Disc Assembly .........................................................31
7.2 Troubleshooting .............................................................................32
7.3 Preventive Maintenance ................................................................32
Section 8 - Spare Parts & Accessories...................................................................33

SPI Supplies 7 SPI-DRY Critical Point Dryer
1.3 Illustrations
Figure 2.1 - Hazard Warning Symbols .......................................................................9
Figure 2.2 - International Warning Symbols ...............................................................9
Figure 2.3 - Typical Signs as shown in this Manual....................................................10
Figure 2.4 - Typical Signs as shown in this Manual ...................................................10
Figure 2.5 - Typical Warnings, as shown in this Manual ............................................10
Figure 6.1 - Phase Diagram .......................................................................................21
Figure 6.2 - Process Flow Chart ................................................................................24
Figure 7.1 - Cross section of SPI DRY Critical Point Dryer ........................................28
Figure 7.2 - Gauge Mountings ...................................................................................30
Figure 7.3 - Safety Valve Assembly............................................................................31
1.4 Tables
Table 2.1 - Personal Operational Risks .....................................................................11
Table 7.1 - Troubleshooting .......................................................................................32
Table 7.2 - Preventive Maintanence ..........................................................................32
Table 8.1 - Spare Parts ..............................................................................................33
Table 8.2 - Accessories ..............................................................................................33

SPI Supplies 8 SPI-DRY Critical Point Dryer
2 HEALTH AND SAFETY
Safety is very important when using any instrumentation and all users of our equipment should read
this section.
This section of the Manual applies to all specimen preparation equipment supplied by SPI Supplies,
not just the particular instrument for which the manual refers.
Included in this section are details on warning notations and good working practices.
2.1 Safety Policy
This section contains important information relating to all health and safety aspects of the equipment.
As such it should be read, and understood, by all personnel using the instrument whether as an
operator or in a service capacity.
SPI Supplies is committed to providing a safe working environment for its employees and those that
use its equipment.
SPI Supplies regularly reviews its operations to make environmental, health and safety improvements
in line with applicable legislation.
The equipment has been designed as a free-standing bench mounted instrument. SPI Supplies cannot
be held responsible for any damage, injury or consequential loss arising from the use of its equipment
for any other purposes, or any unauthorized modifications made to the equipment.
All service work carried out on the equipment should only be undertaken by suitably qualified
personnel. SPI Supplies is not liable for any damage, injury or consequential loss resulting from
servicing by unqualified personnel. SPI Supplies will also not be liable for damage, injury or
consequential loss resulting from incorrect operation of the instrument or modification of the instrument.
2.2 Conformity
This instrument is supplied in a form that complies with the protection requirements of the EC
Electromagnetic Compatibility Directive 89/336/EEC and the essential health and safety requirements
of the low voltage directive 72/23/EEC both as amended by 92/31/EEC. Any modifications to the
equipment, including electronics or cable layout may affect the compliance with these directives.
2.3 Servicing
2.3.1 Disclaimer
All service work on the equipment should be carried out by qualified personnel. SPI Supplies cannot
be liable for damage, injury or consequential loss resulting from servicing from unqualified personnel.
SPI Supplies will also not be liable for damage, injury or consequential loss resulting from incorrect
operation of the instrument or modification of the instrument.
2.3.2 Operators and Service Engineers
A normal operator of the equipment will not be trained in or qualified for service work on the equipment
and may cause a hazard to himself/herself or others if such work is attempted. Operators should
therefore restrict themselves to the normal operation of the equipment and not remove covers from the
electronic equipment or dismantling of the instruments.
Service Engineers who are suitably trained to assess and isolate electrical, mechanical and vacuum
hazards should be the only personnel who access the equipment.
2.4 Hazard Signals and Signs
2.4.1 Hazard Signal Words
The standard three hazard signal words are defined as follows:
DANGER - imminently hazardous situation or unsafe practice that, if not avoided, will result
in death or severe injury.
WARNING - potentially hazardous situation or unsafe practice that, if not avoided, could
result in death or severe injury.

SPI Supplies 9 SPI-DRY Critical Point Dryer
CAUTION - potentially hazardous situation or unsafe practice that, if not avoided, may result
in minor or moderate injury or damage to equipment.
2.4.2 Hazard Labels used on Equipment
Several hazard symbols may be found on the equipment, they are shown below with their meaning:
Caution, risk of electric shock
Caution (refer to accompanying documents)
Easily touched higher temperature parts
Warning, risk of electric shock
Figure 2.1 - Hazard Warning Symbols
2.4.3 Hazard Warning Labels used in Equipment Manuals
The international warning signs used in equipment manuals as shown in Figure 2.2.
Figure 2.2 - International Warning Symbols
Where appropriate these are used when a specific identifiable risk is involved in either using or
maintaining the instrument. These take the form of warning triangles or signs with a graphical
description of the hazard.

SPI Supplies 10 SPI-DRY Critical Point Dryer
2.4.4 Instrument Functionality Signs
CAUTION
Extreme care should be taken during transfer to prevent surface drying of the specimen.
Should air drying occur, the specimen will be irreversibly damaged.
Figure 2.3 - Typical Warning sign as shown in this Manual
This typical sign applies to cautions where there is a risk to the functionality of equipment due to
incorrect operation. These cautions or warnings will be contained in a box and be accompanied by a
circular warning symbol as shown in Figure 2.3.
2.4.5 Serious Damage to Instruments
WARNING
Do NOT depress button “P” as this will change the program.
Figure 2.4 - Typical Warning sign as shown in this Manual
This typical caution sign is used where serious damage will be caused by incorrect operation of
instrumentation. They will follow the same form as functionality warnings but with a triangular warning
symbol as shown in Figure 2.4.
2.4.6 Hazard to Operator
WARNING
HAZARD TO HEALTH!
Risk of asphyxiation in poorly ventilated rooms.
As carbon dioxide is heavier than air, the concentration of exhaust gas will be
greater at ground level and the oxygen concentration correspondingly reduced.
Figure 2.5 - Typical Warning as shown in this Manual
These warnings will generally occur in relevant installation and maintaining sections where there exists
a potential hazard to the engineer working on the instrument. They will take the form of the triangular
warning symbol accompanied by an international warning sign and bold type lettering beginning with
“WARNING-HAZARD TO HEALTH!” as shown in Figure 2.5.