CEM Star Owner's manual

Corporation

Operation Manual

i

Operation Manual

STAR Plus System 2™

and

STAR Plus System 6™

This manual contains proprietary information which shall not be reproduced

or transferred to other documents or disclosed to others

without prior written permission of CEM Corporation.

CEM is a registered trademark of CEM Corporation.

US Patent No. 5,796,080

titled “Microwave Apparatus for Controlling Power Levels

in Individual Multiple Cells”

CEM Corporation

Matthews, North Carolina 28106

(704) 821-7015 FAX: 704-821-7894

e-mail: inf[email protected]

MANUFACTURED IN THE

UNITED STATES OF AMERICA

600127

Rev. 0

9/2001

ii

Operating Precautions

The STAR System 2/6 must be grounded. In the event of an electrical short circuit, grounding reduces the risk of electric shock by

providing an escape wire for electric current. This instrument is equipped with a cord having a grounding wire with a grounding

plug. The plug must be plugged into an outlet that is properly installed and grounded. Consult a qualiﬁ ed electrician or service

technician if the grounding instructions are not completely understood or if doubt exists as to whether the instrument is properly

grounded. If it is necessary to use an extension cord, use only a 3-wire extension cord that has a 3-blade grounding plug and

a 3-slot receptacle that will accept the plug from the instrument. The marked rating of the extension cord must be equal to or

greater than the electrical rating of the instrument.

The possibility of instrument-induced electromagnetic interference (EMI) is minimal if the instrument is operated as outlined

in this manual. The instrument should not be placed close to any electrical device susceptible to EMI. It is suggested by the

manufacturer that the user post a sign warning pacemaker wearers that a microwave device is in operation. If the instrument is

suspected of inducing EMI, a microwave leakage measurement should be performed as outlined in this manual. Leakage measured

above the legal limit of 5 mW/cm 2 should be reported to the CEM Service Department.

This instrument utilizes high voltages and microwave radiation. Instrument service and repair should be performed only by those

trained in repair and maintenance of high voltage and microwave power systems.

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 empha-size 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 misinterpreted or overlooked and

to clarify possible confusing situations.

This instrument complies with United States Code of Federal Regulations (CFR) Title 21, Part 1030 for microwave leakage.

A veriﬁ cation report is on ﬁ le.

This instrument complies with United States Code of Federal Regulations (CFR) Title 47, Federal Communications Commission

(FCC) Part 18 – Industrial, Scientiﬁ c and Medical (ISM) Equipment – emissions requirements. A veriﬁ cation report is on ﬁ le.

The name “Teﬂ on” is used throughout this manual. Teﬂ on is a registered trademark of the E.I. DuPont Company.

iii

Table of Contents

Introduction ....................................................................................................................................................................................... 1

Installation ......................................................................................................................................................................................... 3

Tools Required .................................................................................................................................................................................. 3

Accessories Required......................................................................................................................................................................... 3

Installation.......................................................................................................................................................................................... 3

Unpacking System Components........................................................................................................................................................ 4

Instrument Inspection......................................................................................................................................................................... 6

Instrument Description....................................................................................................................................................................... 7

Instrument.................................................................................................................................................................................... 9

Keyboard ................................................................................................................................................................................... 11

Component Installation.................................................................................................................................................................... 12

General Safety.................................................................................................................................................................................. 16

Compounds Unsuitable for Open Cavity Microwave Digestion ..................................................................................................... 17

System Cautions .............................................................................................................................................................................. 18

Instrument Setup .............................................................................................................................................................................. 19

Reagent Volume......................................................................................................................................................................... 19

Auto Print .................................................................................................................................................................................. 19

Clear Method ............................................................................................................................................................................. 20

Printer Setup .............................................................................................................................................................................. 20

Change Reagent Name .............................................................................................................................................................. 21

Set Clock ................................................................................................................................................................................... 22

Calibrate Temperature ............................................................................................................................................................... 22

Set Overtime.............................................................................................................................................................................. 24

Maximum System Temperature................................................................................................................................................. 24

Software Version........................................................................................................................................................................ 24

Program/Edit Method....................................................................................................................................................................... 25

Reagent Volume......................................................................................................................................................................... 25

Select Vessel .............................................................................................................................................................................. 25

Change Method Name............................................................................................................................................................... 25

Update Initial Reagent............................................................................................................................................................... 25

Reagent Volume......................................................................................................................................................................... 26

Stage .......................................................................................................................................................................................... 27

Evaporation Stage...................................................................................................................................................................... 27

Ramp Time ................................................................................................................................................................................ 28

Temperature Target .................................................................................................................................................................... 28

Time at Temperature.................................................................................................................................................................. 28

Update Reagent ......................................................................................................................................................................... 28

Reagent Volume......................................................................................................................................................................... 29

Prime Method................................................................................................................................................................................... 30

Instrument Operation ....................................................................................................................................................................... 31

Pause Method ............................................................................................................................................................................ 31

Stop Method .............................................................................................................................................................................. 31

Insufﬁ cient Reagent................................................................................................................................................................... 32

Manual Reagent Addition (Must Use for HF) ........................................................................................................................... 32

In-Process Reagent Addition ..................................................................................................................................................... 34

Method Completed .................................................................................................................................................................... 34

Print ........................................................................................................................................................................................... 35

Routine Maintenance, Troubleshooting and Service ....................................................................................................................... 37

Routine Maintenance................................................................................................................................................................. 38

Routine Maintenance Schedule ................................................................................................................................................. 38

Reagent Pump Flush.................................................................................................................................................................. 39

Scrubber Solution Replacement ................................................................................................................................................ 39

Microwave Leakage Measurement............................................................................................................................................ 40

Calibrate Temperature ............................................................................................................................................................... 40

Veriﬁ cation of Temperature Calibration .................................................................................................................................... 41

Troubleshooting Chart ............................................................................................................................................................... 44

iv

Table of Contents (Continued)

Error Messages .......................................................................................................................................................................... 47

Service ....................................................................................................................................................................................... 49

Spill Removal....................................................................................................................................................................... 50

Vessel Liner Replacement.................................................................................................................................................... 52

Reagent Delivery Conﬁ rmation ........................................................................................................................................... 53

Diaphragm Replacement - Single Head Vacuum Pump ...................................................................................................... 54

Diaphragm & Valve Replacement - Dual Head Vacuum Pump........................................................................................... 56

Pump Replacement .............................................................................................................................................................. 59

Speciﬁ cations ................................................................................................................................................................................... 63

Emissions and Safety Approvals ............................................................................................................................................... 64

Warranty .................................................................................................................................................................................... 65

1

Introduction

STAR Plus System 2 and STAR Plus System 6 are designed for laboratory use in digesting, dissolving, hydrolyzing, leaching,

or evaporating a wide range of materials. Their primary purpose is the rapid preparation of samples for analysis by atomic

absorption (AA) and inductively coupled plasma (ICP) emission spectroscopy and gas or liquid chromatography. The STAR

systems are a breakthrough in microwave technology. The technology permits multiple cavities to operate independently with

individual methods and temperature feedback control. Thus, the STAR System 6 can digest up to six samples simultaneously or

with staggered start times. The unique design incorporates a single magnetron, which generates microwave energy for the entire

system. Microwaves are directed through a waveguide with up to six cavities positioned along its length. A microwave slot is

positioned between the waveguide and each cavity. When the slot is open, microwaves enter the cavity; when the slot is closed,

microwaves cannot enter the cavity. Simultaneous temperature feedback is obtained from all cavities; therefore, microwave energy

is supplied to each cavity based on the needs of the sample. The innovative STAR technology systems are either two or six

individual microwave cavities. A sample placed inside a microwave-transparent vessel with a polar liquid or ionic solution

(usually an acid) is subjected to rapid heating, causing the sample to rapidly digest or dissolve. Each cavity is independent,

permitting simultaneous performance of up to six different methods. With the temperature automatically controlled, the STAR

systems ensure consistent and reproducible results for each digestion in each cavity. Large sample sizes can be digested, achieving

lower detection limits and simplifying preparation for trace metals analyses. Other difﬁ cult or problem samples, including highly

reactive materials, can also be readily digested. An automated reagent addition, with up to four reagents, is available as an option.

The reagent addition module eliminates operator handling of the reagents and constant monitoring of the system operation.

WARNING

Do not use the automated reagent addition for pumping hydroﬂ uoric acid (HF). HF must be added manually or

with the CEM HF Pumping Station.

Each system is equipped with a vapor containment module to treat the vapors produced during the digestion process.

2

3

Installation

For use with all reagents other than hydroﬂ uoric acid, the STAR System 2/6 should be installed on a laboratory work bench

with access to a fume hood or other means of fume disposal. For use with hydroﬂ uoric acid, the STAR System must be installed

in a fume hood.

Tools Required

• Flat Blade Screwdriver

• #2 Phillips Screwdriver

• Pliers

• Lab Coat

• Gloves

• Eye Protection

Accessories Required

• Waste Container (bottle)

• Reagents (i.e. HNO3 , H2 SO4 , H2 O2 , and HCl)

• Containers for Reagents (up to 4)

Installation

To install the STAR System 2/6 , follow the procedures outlined below. Choose a location for instrument installation that:

1. provides at least 8 in. (20 cm) open space on each side and 6 in. (15 cm) open space in the rear of the instrument for

ventilation.

2. is free from vibration of large equipment and/or excessive walk-through trafﬁ c.

3. provides adequate bench space for sample handling and optional accessories (printer), if applicable.

4. permits the instrument to be connected to a dedicated, grounded outlet. The STAR System 2/6 should be operated on a

stabilized, constant voltage AC power supply, and the voltage must be within ±10% of the speciﬁ ed level. (See “Speciﬁ ca

tions” 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.

5. provides a temperature range of 60 °F (15 °C) to 104 °F (40 °C) and a humidity range of 10-85 percent relative humidity.

6. provides access to a fume hood or other means of fume disposal.

CAUTION

Do not place the STAR System inside a fume hood unless hydroﬂ uoric acid is used. Vent the instrument fumes

into a fume hood by means of the out-put tubing attached to the vacuum pump. Contact CEM Corporation for

information on the proper external air intake.

4

Unpacking System Components

1. Unpack the system components – main instrument, vapor containment system (including vacuum pump, reagent

addition module and accessories.

2. Remove all protective materials. Retain all packing and protective materials.

3. Verify that all accessories listed below and illustrated in ﬁ gure 1 are included.

System 2 System 6

Vessel (Pyrex glass) 2 6

Condenser 2 6

Shield 2 6

Vessel Rack 1 1

Power Cord 1 1

Fuse 2 2

Communication Cable 1 1

Operation Manual 1 1

Boiling Tube (Not Illustrated) 30 30

Fume Exhaust Tubing (1 /4” Teﬂ on®) 2 6

(Not Illustrated)

Reagent Waste Tubing (1 /4” Teﬂ on®) 2 6

(Not Illustrated)

Vapor Module Plug

STAR System Accessory Kit

In

novators in Microwave

Technolo

gy

Corporation

5

STAR System 6 Main Instrument

STAR System 6 Vapor Collection Module

STAR System 6 Reagent Addition Module STAR System Scrubber

6

Instrument Inspection

1. Inspect the instrument for cracks, dents or warping.

WARNING

If damage is noted, do not attempt instrument startup.

2. 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 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 28105-0200 USA

Within the continental United States

(800) 726-5551

Outside the United States

Telephone: (704) 821-7015

Fax: (704) 821-7894

Telex: 802118

CEM Ltd. CEM GmbH CEM S.r.l.

Unit 2 Middle Slade Carl-Friedrich-Gauss-Str. 9 Via Dell’Artigianato, 6/8

Buckingham Ind. Park 47475 Kamp-Lintfort 24055 Cologno al Serio (Bg)

Buckingham MK18 1WA Germany Italy

United Kingdom Tel: (49) 2842-96440 Tel: (39) 35-896224

Tel: (44) 1-280-822873 Fax: (49) 2842-964411 Fax: (39) 35-891661

Fax: (44) 1-280-822342

7

Instrument Description

Vapor Collection

Module

Vapor Collection

Module

Main

Instrument

Main

Instrument

Reagent Addition

Arm

Reagent Addition

Arm

Display &

Keyboard

Display &

Keyboard

Lighted

Window

for Cavity

Lighted

Window

for Cavity

Condenser

Vessel

STAR System 2 (Front View)

STAR System 6 (Front View)

8

STAR System 6 (Rear View)

STAR System 6 (Side Views)

On/Off

Switch

Computer

Port

Vapor Collection

Port

Printer

Port

Voltage

Selection

Switch

Power

Cord

Receptacle

9

Instrument

Vessel – holds the sample during a digestion

Cavity – positions the vessel and provides the microwave energy to perform the digestion

Condenser – condenses vapors and directs reagents to ﬂ ow down the sides of the vessel

Vessel Liner – directs spillage into the spill tray

Shield – prevents contact with reagents should an event occur during a digestion

Reagent Addition Arm – routes vapors from vessel and directs reagent(s) to vessel

Vapor Containment System– removes vapors and routes them to the fume hood during the digestion process (includes vapor

collection module and vapor scrubber)

Vapor Collection Module – directs fumes from the vessel to the vapor scrubber

Vapor Scrubber – contains solutions to neutralize vapors during the digestion process

Reagent Addition Module (optional) – automatically adds reagents to the cavity in programmed quantities

Reagent Pump – Adds one reagent to one cell

Vacuum Pump – pulls vapors from vessel through the vapor collection module and directs them into the fume hood

Vessel-in-Position Sensor – prevents operation if the vessel is not installed

Temperature Sensor – monitors the temperature during the diges-tion and provides feedback control

10

STAR System Reagent Addition Module (Front View)

STAR System Reagent Addition Module (Rear View)

to Star

System

11

Keyboard

Select – permits selection of the applicable cavity for setup, editing and/or operation and permits emergency reagent addition

when a cavity is paused during a method

Start/Pause – begins the method currently displayed on the selected cavity screen or pauses the operation during any stage

of the method

Stop – stops operation of method and returns to the cavity main screen

Edit – permits editing of parameters for the method displayed on the selected cavity

Home – returns the selected cavity to the main screen

Print – permits printing of method data, method program and/or setup parameters

Setup – permits editing of system parameters

Change – incrementally increases or decreases current parameter displayed on selected cavity (upper case letters, lower case

letters, numbers and symbols) or scrolls through selections such as methods, reagents, etc.

Next – advances to the next method parameter during editing or setup menus

Back – returns to the previous screen during editing or setup menus

STAR System Keyboard

12

4. Facing the main instrument, place the reagent addition module on the left side and the scrubber module on the right side

of the main instrument.

5. Lift the arm from the receptacle in cell #1; pull it forward and position it over its cell.

6. Carefully pry each side of the cover of cell #1 to release it from the positioning pins on each side of the arm.

7. Lift the front of the cover and slide the cover away from the area.

8. Locate the tubing bundle mounted on the top of the reagent module for cavity #1.

Note: The number of tubes in the bundle is dependent upon the number of reagents being utilized.

9. Slide a ﬁ tting on the end of the ﬁ rst length of tubing with approximately 2” of tubing extending beyond the ﬁ tting.

10. Slide a ferrule on the tubing with the tapered end of the ferrule facing the installed ﬁ tting. Insert the ferrule into the

ﬁ tting until it is snug.

11. Insert one length of tubing in the bundle into one of the four ports in the reagent head of arm #1, ensuring that the tubing

extends beyond the head into the chamber of the arm, but not beyond the tip which ﬁ ts into the vessel.

Installation of Vapor Collection Module on Main Instrument

Component Installation

1. Position the main instrument on the selected installation site (bench area if not using HF or inside a fume hood if adding

HF manually.

2. Ensure that the vessel support ring is properly installed and seated. Using an index ﬁ nger, position the liner in each cavity so

that the opening in the bottom of the liner is positioned above the opening in the RF stub (ﬁ gure 6, page 8). Note: If liners

are not installed, refer to “Vessel Liner Replacement,” page 75, for procedures for installing vessel liners.

3. Position the vapor collection/reagent addition module on top of the main instrument. Secure the vapor collection

module with the two bolts.

13

12. Tighten the ﬁ tting ﬁ nger tight.

13. Install each length of tubing in the bundle for cavity #1 as outlined in steps 10 through 13.

14. Install a plug into each opening of the reagent head that does not contain tubing for a reagent.

Installation of Vapor Collection Module on Main Instrument

15. Once all tubing and/or plugs are installed, position the cover over the arm. Place the 1/8” tubing into the smaller slot in the

back of the cover and the 1/4” tubing in the larger slot. Position the back of the cover over the locator pin on the back of

the arm, ensuring that the tubing is not crimped. Then push the front of the cover into place, ensuring that the locator pins

engage the holes in each side of the cover.

16. Lift the arm assembly and push it toward the back of the instrument and position the tip of the arm into the receptacle.

17. Repeat steps 10 through 17 for each cavity of the instrument.

18. Fill the reagent containers as required.

WARNING

Proper precautions must be taken to avoid contact with reagents or reagent vapors. Protective gear should be worn

as outlined in the user’s safety program for hazardous materials and the reagent manufacturer’s material safety

data sheet. Refer to these guidelines for proper handling of the reagent.

19. Place one of the plastic stopers provided in the accessory kit into each reagent container. Position the reagent tubing in the

appropriate reagent containers. Ensure that the tubing is placed into the correct

reagent container so that the proper reagent will be added to the sample as required.

WARNING

Do not use the reagent addition module for pumping HF.

WARNING

The tubing must be secured in the reagent container.

14

20. Connect the tubing extending from the scrubber module to the manifold installed on the vapor collection module.

21. Place a suitable waste container behind the main instrument. Place the tubing labeled “waste” into the container. Ensure that

the tubing extends sufﬁ ciently into the container to prevent it from pulling free, but not far enough to extend into the waste.

The waste level should always be below the tubing.

22. Install the safety shields. Place a vessel in each cell.

23. If using a printer, connect the printer cable into the printer port on the back of the main instrument.

Perform printer setup as outlined in the printer literature.

24. Plug the main instrument into a dedicated electrical outlet.

25. Ensure that the voltage selection switch is in the proper position to parallel electrical line voltage.

26. To position the vapor collection arm on the vessel, lift the arm and pull forward to position the reagent head over the vessel.

15

STAR System 6 Installed on Work Bench

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CEM Star Owner's manual

CEM Star Owner's manual

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