CEM Phoenix User manual

Operation ManualOperation Manual
Operation Manual
Innovators in
Microwave Technology
600134
Rev. 12

I
Phoenix™ and
Phoenix AirWave™
Microwave Furnace
Copyright © 2001 by CEM Corporation
All Rights Reserved
This manual contains proprietary information
which shall not be disclosed or reproduced or transferred
to other documents without prior written permission
from CEM Corporation.
Phoenix is a trademark of CEM Corporation.
CEM is a registered trademark of CEM Corporation.
U.S. patents 5,066,834; 5,252,274;
5,318,754; 5,378,878; 5,441,681; and 5,468,135
Other U.S. and foreign patents pending
CEM Corporation
Matthews, North Carolina 28106
[phone] FAX: [phone] e-mail: [email protected]
MANUFACTURED IN THE
UNITED STATES OFAMERICA
600134
Rev. 12
4/2013

II
CAUTION
DO NOT install the Phoenix inside a fume hood.
To avoid the possibility of a thermal overload, the Phoenix should not be
physically located inside a fume hood. Vapors should be vented into a fume
hood by means of the exhaust hose only.
Installation of the Phoenix inside a fume hood will void any written or
implied warranty from the manufacturer.
WARNING
The muffle furnace included with this instrument contains ceramic fiber
material and high temperature cement coating.
• Possible carcinogen based on tests with laboratory animals.
• May be irritating to skin, eyes and respiratory tract.
• May be harmful if swallowed or inhaled.
• Cristobalite (crystalline silica) formed at high temperatures
(above 1600° F) can cause severe respiratory disease.
For further information, call [phone] and request Material Safety
Data Sheet part number 600531.

III
Operating Precautions
Do not tamper with the safety interlocks. The Phoenix™ is equipped with three door
safety interlock switches which prevent the instrument from producing microwave
power if the door is open. Tampering with the safety interlocks may allow microwave
production when the door is open, which is very dangerous.
Do not place any object between the front of the microwave cavity and the door or
allow soil or cleaner residue to accumulate on sealing surfaces.
Do not operate the instrument if it is damaged. It is particularly important that the
instrument door close properly and that there is no damage to the door (bent), hinges
or latches (broken or loosened), or door sealing surfaces.
The instrument utilizes high voltages and microwave radiation. It should be adjusted
or repaired only by qualified service personnel trained in repair and maintenance of
high voltage and microwave power systems.
The possibility of instrument-induced electromagnetic interference (EMI) is minimal
if precautions outlined in this manual are followed. However, it is recommended
that the user post a sign warning pacemaker wearers that a microwave device is in
operation. Also, the instrument should not be placed close to any electrical device
susceptible to EMI. If the instrument is suspected of inducing EMI, the door and the
front of the cavity should be carefully inspected for damage. A microwave leakage
measurement should be performed as outlined in the Maintenance and Service sec-
tion of this manual. Leakage above the legal limit of 5 mW/cm2should be reported
to the CEM Service Department.
WARNING
Improper installation or use of the instrument grounding wire and/or
plug can result in electrical shock.
The Phoenix instrument must be grounded. In the event of an electrical short circuit,
grounding reduces the risk of electric shock by providing an escape wire for the
electric current. This instrument is equipped with a cord having a grounding wire
with a grounding plug. The plug must be plugged into a dedicated outlet that is
properly installed and grounded.
If grounding instructions are not completely understood or if doubt exists that the
instrument is properly grounded, consult a qualified electrician or service technician.
If it is necessary to use an extension cord, use only a 3-wire extension cord with
a 3-blade grounding plug that has a 3 -slot electrical receptacle. The marked rating
of the extension cord shall be equal to or greater than the electrical rating of the
instrument.

IV
Warnings, Cautions and Notes
Warnings, cautions and notes are included throughout this manual and should be read
thoroughly and strictly followed.
WARNING - A warning is inserted for essential information used to emphasize
dangerous or hazardous conditions to the operation, cleaning and maintenance of the
instrument which may result in personal injury.
CAUTION - A caution is inserted for essential information used to emphasize
procedures which, if not strictly followed, may result in damage or destruction to the
instrument or improper instrument operation.
NOTE - A note is inserted for emphasis of procedures or conditions which may
otherwise be misin-terpreted or overlooked and to clarify possible confusing situa-
tions.
To the best of our knowledge, the information contained herein is accurate. However,
CEM Corporation cannot accept liability of any kind for the accuracy or complete-
ness of the information contained in this manual. The final determination of the
suitability and proper use of the instrument described herein, the accuracy of the
information and data obtained from such use, and whether such use infringes any
patents or the legal safeguards of others are the sole responsibility of the user.

V
Table of Contents
Introduction............................................................................................................ 1
Installation.............................................................................................................. 2
Installation Site .................................................................................................... 2
Unpacking............................................................................................................ 3
Inspection............................................................................................................... 6
Instrument Description........................................................................................... 7
Keyboard.............................................................................................................. 7
Door Protection....................................................................................................12
Furnace Door Holder Installation ........................................................................12
Instrument Startup................................................................................................12
External Balance Installation ...............................................................................16
External Balance Setup........................................................................................16
Printer Installation................................................................................................17
Personal Computer Setup.....................................................................................17
Setup Menu ............................................................................................................19
Auto Start/Stop.....................................................................................................20
External Balance ..................................................................................................21
System Options ....................................................................................................21
Timers ................................................................................................................21
Set Clock............................................................................................................22
Screen Saver Time .............................................................................................22
Tests ...................................................................................................................23
Information ........................................................................................................23
Controls..............................................................................................................24
Language............................................................................................................24
Password ............................................................................................................25
Program Options ................................................................................................ 25
Printer Setup.......................................................................................................26
Company Name .................................................................................................27
Delete Method....................................................................................................27
Quick Test - No External Balance..........................................................................29
Quick Test - External Balance ...............................................................................33
Standard ...............................................................................................................36
Syringe .................................................................................................................39
Edit/Create Method................................................................................................45
Create Method......................................................................................................45
Standard or Drying.............................................................................................46
Load Method..........................................................................................................49
Perform Method.....................................................................................................51
Standard or Drying Method - No External Balance.............................................51
Standard or Drying Method - External Balance ..................................................52
Standard .............................................................................................................54
Syringe ............................................................................................................... 58

VI
Table of Contents (Continued)
Ramping Method - No External Balance.............................................................63
Ramping Method - External Balance (Standard).................................................65
Ramping Method - External Balance (Syringe)...................................................65
Print Menu .............................................................................................................79
Maintenance, Troubleshooting and Service...........................................................81
Routine Maintenance ...........................................................................................81
Microwave Leakage Measurement......................................................................83
Microwave Power Measurement .........................................................................84
Calibration............................................................................................................87
Furnace Temperature Calibration.......................................................................87
Enter Previous Calibration Values .....................................................................89
Troubleshooting Guide.........................................................................................90
Error Messages.....................................................................................................92
Component Removal and/or Replacement ..........................................................94
Fuses ..................................................................................................................94
Instrument Cover ...............................................................................................94
Furnace Thermocouple ......................................................................................97
Spare Parts ...........................................................................................................98
Specifications .........................................................................................................99
Warranty................................................................................................................101
Customer Support ...............................................................................................102
Options..................................................................................................................103
Sulfated Ash..........................................................................................................105

1
Introduction
The Microwave Muffle Furnace, Model Phoenix, is a special purpose microwave
system designed for laboratory use in heating/ashing a wide range of materials. Its
primary purpose is the rapid oxidation of samples for the gravimetric determination
of ash content (loss on ignition).
Calculations for the Phoenix include
• % LOD (Loss on Drying) = Initial Weight-Final Weight (Dried Sample Weight)
x 100
• % Ash = Final Weight (Ash Weight)/Sample Weight x 100
• % ROI (Residue on Ignition) = Final Weight (Ash Weight)/Sample Weight)
x 100
• % LOI (Loss on Ignition) = Initial Weight - Final Weight (Ash Weight)/Sample
Weight) x 100
• % Total Residue = Final Weight (Dried)/Sample Weight x 100
• % Vol. Residue = Dried Weight – Ash Weight/Dried Weight x 100
• % Fixed Residue = Final Weight (Ashed)/Dried Weight x 100
The Phoenix system can be equipped with either a high temperature furnace or a
high capacity furnace. The high temperature furnace is for applications requiring
temperatures up to 1200 ºC. It can accommodate up to eight (8) CEM quartz fiber
crucibles. The high capacity furnace is for applications at or below 1000 ºC. It can
accommodate up to 15 CEM quartz fiber crucibles.
The Phoenix consists of
• a microwave power system.
• a stainless steel microwave cavity with exhaust fan,
• a programmable digital computer,
• a muffle furnace, either high temperature or high capacity
• an internal temperature control system,
• internal calibration software,
• two (2) RS-232 ports and one (1) parallel printer port,
• exhaust hose to vent fumes, and
• furnace door holder.
Available accessories for use with the Phoenix include
• ashing crucibles and accessories,
• balances,
• printers, and
• calibration source instrumentation

2
Installation
The Phoenix instrument should be installed on a laboratory work bench with access
to a fume hood or other means of fume disposal.
Installation Site
To install the Phoenix, choose a location that:
1. provides at least 8 in. (20 cm) space on each side and 6 in. (15 cm) space in the
rear for proper ventilation.
2. is free from vibration of large equipment.
3. provides a temperature range of 41°F(5°C) to 104°F (40°C).
4. provides adequate bench space for sample handling and printer placement.
5. permits the instrument to be connected to a dedicated, grounded outlet. The
Phoenix instrument should be operated on a stabilized, constant voltage AC
power supply, and the voltage must be within ±10% of the specified level.
(Refer to the “Specifications” in this manual.)
Note: Measure line voltage to ensure that it meets system specifications.
CAUTION
Line voltage fluctuations greater than 10% will affect instrument
performance.
6. provides access to a fume hood or other means of fume disposal.
CAUTION
Do not install the Phoenix instrument inside a fume hood. Placing
the instrument in a fume hood can cause a thermal overload. Vent
the Phoenix into a fume hood means of the exhaust hose.
7. (AirWave only) permits access to a compressed air supply (minimum 90 psi
@ 13 SCFM through a 1/4” to 5/16” ID air line with valve open and air flowing
through system) (maximum 150 psi air pressure). If the Phoenix AirWave is
more than 50 feet from the compressed air supply, the air line should be
increased to 5/8” ID. Compressed air supply should be increased if the exhaust
hose is more than 16 feet. Air flow is reduced by approximately 10% by each
additional 8-foot section of hose. The exhaust system is equipped with a male
quick disconnect coupler plug “M” style to be coupled with an “M” style female
coupler body (customer supplied).

3
8. (Phoenix Only) The exhaust system is designed to push fumes through the
exhaust hose (3” ID) at approximately 125 CFM (unducted). The exhaust system
will push fumes through the flexible exhaust hose at approximately 55 - 75 Kmh
(40 - 55 mph). The exhaust hose should be a maximum length of 16 feet
(maximum 8 feet vertical within 16 feet).
WARNING
To avoid insufficient exhaust, never permit the exhaust flow rate to
fall below 50 CFM.
Unpacking
1. Carefully open the shipping cartons, using caution to avoid puncturing or
tearing the foam packaging. Remove the foam and cardboard packing material.
NOTE
Retain all packing material for use if returning the instrument to the
manufacturer for service.
2. With at least two people for lifting, locate the handles on each side of the
lifting carton and lift the instrument from the shipping carton and place it on a
laboratory bench. Carefully remove the lifting carton and plastic wrap from
the instrument.
3. Open the instrument door and remove the packing from the four studs in the
bottom of the instrument cavity.

4
Cor poration
Quartz F iber
Ashing Cr
ucibles
Reorder part number:
303030
Reorderpart number: 303030
Corporation
Quartz Fibe r
Ashing Dis ks
Reorder part numbe r:
20157 0
Innovatorsin MicrowaveTechnology
Corporation
4. Verify that all accessories are included.
Phoenix Accessories:
• Muffle Furnace with heating insert
• Thermocouple
• Exhaust Hose
• Fuses, 15 AMP (2)
• Pedestal Access Tool
• Power Cord
• Operation Manual
• Ashing Disks (Package of 200)
• Ashing Crucibles (Package of 20)
• 7/16” Wrench
Figure 1. PhoenixAccessory Kit
Furnace
Assembly
(307030)
Furnace
Door Holder
(573170)
Ashing
Crucibles
(303040)
Exhaust
Hose
(920880)
Ashing
Disks
(201550)
Operation
Manual
(600134-Phoenix) Power Cord
Fuses
(15 AMP)
(118320)
Thermocouple
(Standard)
(271065) Wrench
(301520)
Pedestal
Access
Tool
(301710)

5
Corporation
Quartz Fiber
AshingCrucibles
R eorder pa rt number:
303030
Reorder part number: 3 03030
Corporation
QuartzF iber
Ashing Dis ks
Re
order partnumber:
201570
Innovatorsin Microwave Technology
Cor poration
Phoenix AirWave Accessories:
• Muffle Furnace with heating insert
• Thermocouple
• Exhaust Elbow
• Exhaust Hose
• Fuses, 15 AMP (2)
• Pedestal Access Tool
• Power Cord
• Operation Manual
• Ashing Disks (Package of 200)
• Ashing Crucibles (Package of 20)
• Airflow Amplifier Assembly
• 7/16” Wrench
Figure 2. PhoenixAirWave Accessory Kit
Furnace
Assembly
(307030)
Ashing
Disks
(201550)
Operation
Manual
(600134)
Thermocouple
(Standard)
(271065)
Pedestal
Access
Tool
(301710)
Furnace
Door Holder
(573170)
Ashing
Crucibles
(303040)
Exhaust
Hose
(233040)
Power Cord
Exhaust
Elbow
(233045)
Fuses
(15 AMP)
(118320)
Wrench
(301520)
Airflow Amplifier
Assembly
(500990)
Chimney
(009515)

6
Inspection
1. Inspect each part of the instrument for any cracks, dents, or warping.
2. Inspect the door for any damage and for proper alignment. When closed, the
door should seat firmly against the front of the microwave cavity. The push
button on the top of the instrument must release and engage the door latch
mechanism.
WARNING
If damage is noted, do not attempt instrument operation.
If the instrument has been damaged in shipping, contact the freight carrier to report
damage and to file a damage report. Contact the CEM Service Department or the
local subsidiary or distributor to report damage and to request service information.
CEM Corporation
Service Department
P.O. Box 200
3100 Smith Farm Road
Matthews, NC 28106-0200 USA
Within the United States:
[phone] or [phone]
Fax: [phone]
E-mail: [email protected]
Outside the United States:
Telephone: [phone]
Fax: [phone]
Web: http:\\www.cemx.com
CEM Microwave Technology Ltd.
2 Middle Slade
Buckingham Industrial Park
Buckingham MK18 1WA
United Kingdom
Telephone: [phone]
Fax: [phone]
CEM GmbH
Carl-Friedrich-Gauss-Str. 9
47475 Kamp-Lintfort
Germany
Telephone: [phone]
Fax: [phone]
CEM S.r.l.
Via Dell’Artigianato, 6/8
Italy
Telephone: [phone]
Fax: [phone]

7
Display Keyboard
Figure 3a. Phoenix (Front View with Door Open)
Serial
Port J2
External
Balance
Port J1
Parallel
Printer
Port
Pedestal
Access
Furnace Door
Holder
Mounting
Studs (4)
Instrument Description
• Display - shows menus, method parameters and instrument status on an 8 line x
40 character vacuum fluorescent display.
• Keyboard - allows the operator to enter setup parameters and company names
and control operational parameters such as time.
Figure 3b. PhoenixAirWave (Front View with Door Open)
Display Keyboard
Serial
Port J2
External
Balance
Port J1
Parallel
Printer
Port
Pedestal
Access
Furnace Door
Holder
Mounting
Studs (4)

8
Figure 4b. Phoenix (Front View with Door Open, Furnace Installed, Furnace
Door Holder Installed, and Furnace Door in Holder)
Furnace
Door Holder
Furnace
Door
Furnace
Figure 4a. PhoenixAirWave (Front View with Door Open, Furnace Installed)
Furnace

9
Keyboard
• Start/Stop – begins the method currently displayed on the screen or pauses and
restarts the operation during any stage of the method
• Time – begins the countdown of the programmed dwell time
• Home – returns to the main menu from any point in the software selections
• Select – enters selected parameter, method, etc. and in some instances advances
to the next screen
• Setup – permits entering or editing of system parameters
• Print – permits printing of method data, system information, method program
and/or setup parameters
• Arrows – scroll through selections
• Back – returns to the previous screen
• Next – advances to the next screen
• Balance – permits entering of start weight or automatic weighing from external
balance
•PC – permits data to be sent to a Personal Computer
Figure 5. Phoenix Keyboard

10
• BlowerAssembly – exhausts heat and smoke from instrument cavity during
sample ashing.
• Magnetron Cooling Fan – draws air through the magnetron.
• Fuses – prevent electrical power overload.
• Power Cord Receptacle – receives the female end of the power cord.
• Power Cord – conducts electrical power from the AC outlet to the instrument. It
is detachable.
• On/Off Switch – turns electrical power to the instrument on and off.
• Nameplate – lists instrument model and serial number.
• Voltage Selection Switch – permits unit to operate properly with line voltages
from 208 to 230V (60 Hz) or 220 to 240V (50 Hz).
• Solenoid Connector – connects solenoid to power panel. (AirWave only)
• Filter Dryer – removes water and contaminate. (AirWave only)
• Air Regulator – regulates pressure to the airflow amplifier. (AirWave only)
• Pressure Gauge – permits monitoring of regulated pressure in airflow amplifier.
(AirWave only)
• Airflow Amplifier – exhausts heat and smoke from instrument cavity during
sample ashing (AirWave only)
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iafihb
Nameplate
Power
Cord
On/Off
Switch
Power
Cord
Receptacle
Fuses Voltage
Selection
Switch
Blower
Assembly
Magnetron
Cooling
Fan
Figure 6. Phoenix (Rear View)

11
Figure 7. PhoenixAirWave (Rear View)
Power
Cord
On/Off
Switch
Power
Cord
Receptacle
Fuses Voltage
Selection
Switch
Magnetron
Cooling
Fan
Nameplate
Air
Hose
Exhaust
Hose
Exhaust
Elbow
Connector
Collar
Pressure
Gauge
Air
Regulator
Mounting
Bracket
Filter
Dryer
Solenoid
Airflow
Amplifier
Solenoid
Wire
Solenoid
Connector

12
Door Protection
An infrared safety sensor is installed in the top of the instrument to protect the
instrument door from damage in the event that the furnace door is missing. When the
sensor is activated, the instrument door is prevented from closing.
WARNING
Do not force the instrument door to close. Forcing the door will
result in damage to the interlock system, the door mechanism and/or
door alignment.
The Phoenix is also equipped with a mechanical door protection device incorporated
into the furnace door holder. When the instrument door is open and the furnace door
is positioned in the furnace door holder, a metal rod extends through the top of the
furnace door holder, preventing the instrument door from closing.
Furnace Door Holder Installation
1. Close the instrument door.
2. Using the four (4) mounting studs on the front base of the instrument, attach the
door holder to the lower front of the Phoenix (figures 3 and 4).
Instrument Startup
Note: Proceed to step 10 for instructions for startup of the Phoenix.
Phoenix AirWave only
1. Using the two screws provided, install the airflow amplifier assembly mounting
bracket (figure 7) on the back of the instrument cover.
2. Place the connector collar of the assembly on the exhaust outlet of the instru-
ment.
3. Install the airflow amplifier assembly (figure 7) on the collar and attach it with
the provided screws.
4. Connect the solenoid wiring to the solenoid connector.
5. Connect the exhaust elbow to the airflow amplifier exhaust outlet, and tighten
the screw to secure the elbow.

13
6. Connect the exhaust hose to the exhaust elbow, and tighten the hose clamp
securely. Place the open end of the exhaust hose in a fume disposal mechanism.
7. Using an “M” style 1/4” quick disconnect socket hose coupling, connect a
compressed air line to the plug coupling of the airflow amplifier assembly.
Maximum air pressure is 150 psi.
CAUTION
Air flow to the system should be on at all times during operation.
The airflow solenoid will automatically turn air on when the “Start”
key is pressed and microwaves are being produced. Air will be
turned off when the system is below 50 C.
NOTE
The pressure gauge is factory is set at 60 psi; however, pressure set-
ting can be affected by the compressed air source.
8. If necessary, unlock and adjust the pressure gauge (large black knob directly
above the gauge) clockwise to raise the pressure or counterclockwise to decrease
the pressure.
9. Lock the pressure gauge at 60 psi.
Note: Proceed to step 11 for continuing Phoenix AirWave startup.
Phoenix only
10. Connect the exhaust hose to the cavity exhaust outlet by pushing the plastic
elbow as far into the exhaust outlet as possible. Orient the plastic elbow so that
the exhaust hose extends toward the fume disposal mechanism. Place the open
end of the exhaust hose in a fume hood or other fume disposal mechanism.
Phoenix and Phoenix AirWave
11. Remove the door and top of the muffle furnace. Place the heating element into
the furnace bottom (figures 8 and 9).
12. Position the bottom portion of the muffle furnace with the heating element in the
center of the instrument cavity. Place the top of the furnace on the installed
furnace bottom. Ensure that the thermocouple ports in the furnace and the top of
the instrument cavity are aligned. For AirWave, insert the metal chimney into the
large opening in the top of the furnace. Align the chimney with the instrument
exhaust outlet.