SPI Supplies SPI-DRY Operation Manual

Critical point dryer

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

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Summary of Contents for SPI Supplies SPI-DRY

  • Page 1 SPI-DRY Critical Point Dryer Operation Manual SPI Supplies Part #13200JE-AB Rev. 2.2 April 2021...
  • Page 2 Toll-free from USA/Canada 1-(610)-436-5400 FAX: 1-(610)-436-5755 E-mail: spi3spi@2spi.com 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 ...
  • Page 3 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.
  • Page 4: Section 1 - Contents

    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.
  • Page 5: Table Of Contents

    Section 4 - Description .................... 14 Equipment ..................14 4.1.1 Accessories ................14 Overview ..................15 Technical Specification ..............15 4.3.1 SPI-DRY Critical Point Dryer Specifications ......15 Physical Description ............... 16 4.4.1 Chamber body ................. 16 4.4.2 Control Valves ................ 16 4.4.3 System Gauges ...............
  • Page 6 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 Troubleshooting ................32 Preventive Maintenance ..............32 Section 8 - Spare Parts & Accessories ..............33 SPI Supplies SPI-DRY Critical Point Dryer...
  • Page 7: Illustrations

    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 SPI-DRY Critical Point Dryer...
  • Page 8: Section 2 - Health And Safety

    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.
  • Page 9: Hazard Labels Used On Equipment

    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 SPI-DRY Critical Point Dryer...
  • Page 10: Instrument Functionality Signs

    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. SPI Supplies SPI-DRY Critical Point Dryer...
  • Page 11: Risk Analysis

    Hazardous Gases SPI Supplies has no control over the gases used within the system. It is therefore viewed as the customers responsibility to assess the hazards involved and take appropriate precautions when using explosive, toxic or corrosive gases or gases which may result in hazardous products as a result of a chemical reaction.
  • Page 12: Good Working Practices

    Always make sure you understand a procedure well before attempting it for the first time. Critical Point Dryer Specific Safety Hazards The following Safety Hazards are specific to the SPI Supplies 13200JE-AB Critical Point Dryers. The equipment uses Liquid Carbon Dioxide (CO ) or alternatively Freon (CCIF ).
  • Page 13: Section 3 - Introduction

    Return of Goods If goods are to be returned to SPI Supplies for repair or servicing the customer should contact SPI Supplies or their local distributor before shipment. A "Return Authorisation Number" should be obtained in advance of any shipment. This number is to be clearly marked on the outside of the shipment. To...
  • Page 14: Section 4 - Description

    Description Equipment Each SPI-DRY Critical Point Dryer when supplied as a complete package includes the basic instrument, specimen holder, high pressure CO transfer hose, accessory kit, and an operation manual. Items can be ordered as a full package or separately against the following numbers:...
  • Page 15: Overview

    Overview The SPI Supplies SPI-DRY Critical Point Dryer (CPD) is designed to handle the dehydration of biological (as well as other materials) samples prior to examination the high vacuum environment of the scanning electron microscope (SEM). Although a variety of liquid gases may be used for the critical point drying process, the procedures...
  • Page 16: Physical Description

    Physical Description The SPI Supplies SPI-DRY Critical Point Dryers are comprised of cylindrical, water heated/cooled pressure chambers, horizontally mounted, with attached gauges and valves. Three manually operated valves, positioned around the chamber, are provided to control the flow of inlet and exhaust gases, as well as the venting of the system. The pressure system incorporates a bursting disc, rated at 1850 psi, located in the gas line between the chamber and the pressure gauge, see figure 7.1.
  • Page 17: Safety Valve

    The capsules measure 12mm in diameter by 11mm high and are available in three different pore sizes, the smallest at 30 µm. The inside diameter is 8mm, because of the roughly 2mm thickness of the wall. SPI Supplies SPI-DRY Critical Point Dryer...
  • Page 18: Section 5 - Installation

    If any damage is found, notify the carrier and SPI Supplies (or local agent) immediately. If it is necessary to return the shipment, use the packaging as supplied and follow the instructions in this manual for return of goods paragraph 3.1.
  • Page 19: Connection Of Services

    As carbon dioxide is heavier than air, the concentration of exhaust gas will be greater at ground level and the oxygen concentration correspondingly reduced. During the flushing, the CO exhaust is very cold, and can cause frost burns. SPI Supplies SPI-DRY Critical Point Dryer...
  • Page 20: Section 6 - Operation

    Trial Run Before processing samples for the first time, it is suggested to run the CPD without any samples in order to gain familiarity with the process and the controls. SPI Supplies SPI-DRY Critical Point Dryer...
  • Page 21 The VENT valve should be adjusted to give a vent time of 4-5 minutes. After a critical point run, cool the chamber to 20 C before attempting another run. Repeat the above procedure several times, until comfortable with the workings of the critical point dryer. SPI Supplies SPI-DRY Critical Point Dryer...
  • Page 22: Tissue Preparation

    Washing Fixation Dehydration Substitution with CO miscible liquid Substitution with CO Heating to super-critical temperature Pressure release NOTE: If dehydration is done with acetone, step (d) is omitted because acetone is miscible with CO SPI Supplies SPI-DRY Critical Point Dryer...
  • Page 23: Washing

    Specimens must be washed free of mucus, blood, serum or any other contaminant likely to be fixed on the surface. The washing medium must be physiological, i.e. must not cause any changes in shape or form of the tissue. SPI Supplies SPI-DRY Critical Point Dryer...
  • Page 24: Fixation

    Repeat with 70%, 80%, 90%, 95% and 100% each for 15 minutes. NOTE: The more care taken with this, the better the result. Rapid dehydration causes shrinkage of tissues. Larger pieces of tissue require proportionately longer periods of time. SPI Supplies SPI-DRY Critical Point Dryer...
  • Page 25: Substitution

    (over a period of 4-5 minutes). Once the chamber has de-pressurized, slowly open the VENT valve fully, to ensure the chamber reaches atmospheric pressure before attempting to remove the rear door. SPI Supplies SPI-DRY Critical Point Dryer...
  • Page 26 Mount the samples on the desired mount, and prepare them for examination in the SEM (or other instrument). NOTE: If the system is to be used again right away, the chamber must first be cooled to 20 C or below before another run is started. SPI Supplies SPI-DRY Critical Point Dryer...
  • Page 27: Section 7 - Maintenance

    Regularly clean the inside and outside surfaces of the pressure vessel including the O-ring and associated seating surfaces with isopropyl alcohol. Regularly inspect all connection points for wear and/or leaks. Figure 7.1: Cross-section view of the SPI-DRY Critical Point Dryer SPI Supplies SPI-DRY Critical Point Dryer...
  • Page 28: Chamber Components

    (a) To remove the INLET or VENT valve, loosen the valve locking nut by one turn. (b) Remove the valve by rotating in a counter clockwise direction. (c) Remove the insert and O-ring for inspection and cleaning. SPI Supplies SPI-DRY Critical Point Dryer...
  • Page 29: Gauge Maintenance

    To prevent blockages, regularly strip and clean the transfer boat drain valve as follow: (a) Remove the screw in the end of the transfer boat. (b) Extract the valve slider and spring. (c) Clean out the drain hole using a 1/32” diameter drill. SPI Supplies SPI-DRY Critical Point Dryer...
  • Page 30: Troubleshooting

    Any known problems associated with this type of instrument have been listed below with the possible cause and suggestions to what to do. If problems continue to occur, contact the Customer Service Department at SPI Supplies or your local agent. OBSERVATION...
  • Page 31: Preventive Maintenance

    Inspect all connections (gas and water) for signs of wear, any leakage from pipes and that they are securely retained in position. Inspect door sealing surface for any damage and the “O” ring is clean Cleaning Table 7.2 – Preventive Maintenance SPI Supplies SPI-DRY Critical Point Dryer...
  • Page 32: Section 8 - Spare Parts & Accessories

    13215E-AB 13204-AB High Pressure Transfer Hose 13207-AF Gasket for High Pressure Transfer Hose Table 8.1 - Spare Parts for the SPI-DRY Critical Point Dryer PART NUMBER DESCRIPTION Holder for 3mm grids – Regular 13201-AB Holder for 2.3mm grids – Regular 13203-AB Holder for 3mm grids –...

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