CEM Phoenix Owner's manual

Operation ManualOperation Manual

Operation Manual

Innovators in

Microwave Technology

600134

Rev. 12

I

Phoenix™ and

Phoenix AirWave™

Microwave Furnace

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

(704) 821-7015 FAX: (704) 821-7894 e-mail: [email protected]

MANUFACTURED IN THE

UNITED STATES OF AMERICA

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 mufﬂ e furnace included with this instrument contains ceramic ﬁ ber

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 (800) 726-3331 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 qualiﬁ ed 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/cm2 should 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 qualiﬁ ed 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 ﬁ nal 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

Speciﬁ cations .........................................................................................................99

Warranty ................................................................................................................101

Customer Support ...............................................................................................102

Options .................................................................................................................. 103

Sulfated Ash ..........................................................................................................105

1

Introduction

The Microwave Mufﬂ e 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 ﬁ ber

crucibles. The high capacity furnace is for applications at or below 1000 ºC. It can

accommodate up to 15 CEM quartz ﬁ ber crucibles.

The Phoenix consists of

• a microwave power system.

• a stainless steel microwave cavity with exhaust fan,

• a programmable digital computer,

• a mufﬂ e 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 speciﬁ ed level.

(Refer to the “Speciﬁ cations” in this manual.)

Note: Measure line voltage to ensure that it meets system speciﬁ cations.

CAUTION

Line voltage ﬂ uctuations 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 ﬂ owing

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 ﬂ ow 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 ﬂ exible 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 insufﬁ cient exhaust, never permit the exhaust ﬂ ow 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

Reorder part number: 30303 0

Corporation

Quartz F iber

Ashing Disks

Reorder par t number:

20157 0

Innovators in M icrowave Technology

Corporation

4. Verify that all accessories are included.

Phoenix Accessories:

• Mufﬂ e 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. Phoenix Accessory 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

Ashing Crucibles

R eorder part number:

303030

Reorder part number: 303030

Corporation

Quartz F iber

Ashing Dis ks

Re

order part number:

201570

Innovators in Microwave Technology

Cor poration

Phoenix AirWave Accessories:

• Mufﬂ e 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)

• Airﬂ ow Ampliﬁ er Assembly

• 7/16” Wrench

Figure 2. Phoenix AirWave 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)

Airﬂ ow Ampliﬁ er

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 ﬁ rmly 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 ﬁ le 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:

(800) 726-5551 or (704) 821-7015

Fax: (704) 821-4369

E-mail: [email protected]

Outside the United States:

Telephone: (704) 821-7015

Fax: (704) 821-4369

Web: http:\\www.cemx.com

CEM Microwave Technology Ltd.

2 Middle Slade

Buckingham Industrial Park

Buckingham MK18 1WA

United Kingdom

Telephone: (44) 1-280-822873

Fax: (44) 1-280-822342

CEM GmbH

Carl-Friedrich-Gauss-Str. 9

47475 Kamp-Lintfort

Germany

Telephone: (49) 2842-96440

Fax: (49) 2842-964411

CEM S.r.l.

Via Dell’Artigianato, 6/8

Italy

Telephone: (39) 35-896224

Fax: (39) 35-891661

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 ﬂ uorescent display.

• Keyboard - allows the operator to enter setup parameters and company names

and control operational parameters such as time.

Figure 3b. Phoenix AirWave (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. Phoenix AirWave (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

• Blower Assembly – 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 airﬂ ow ampliﬁ er. (AirWave only)

• Pressure Gauge – permits monitoring of regulated pressure in airﬂ ow ampliﬁ er.

(AirWave only)

• Airﬂ ow Ampliﬁ er – exhausts heat and smoke from instrument cavity during

sample ashing (AirWave only)

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ninuh jaef8opaj 90pfadf. Hifcopa ka[op

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. Phoenix AirWave (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

Airﬂ ow

Ampliﬁ er

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 (ﬁ gures 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 airﬂ ow ampliﬁ er assembly mounting

bracket (ﬁ gure 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 airﬂ ow ampliﬁ er assembly (ﬁ gure 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 airﬂ ow ampliﬁ er 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 airﬂ ow ampliﬁ er assembly.

Maximum air pressure is 150 psi.

CAUTION

Air ﬂ ow to the system should be on at all times during operation.

The airﬂ ow 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 mufﬂ e furnace. Place the heating element into

the furnace bottom (ﬁ gures 8 and 9).

12. Position the bottom portion of the mufﬂ e 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.

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CEM Phoenix Owner's manual

CEM Phoenix Owner's manual

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