PerkinElmer TITAN MPS User manual

TITAN MPS
Customer Users Guide
ATOMIC SPECTROSCOPY

Titan MPS
Users Guide

Release Information
Any comments about the documentation for this product should be addressed to:
User Assistance
PerkinElmer
710 Bridgeport Avenue
Shelton, CT 06484-4794
U.S.A.
Or emailed to: in[email protected]
Notices
The information contained in this document is subject to change without notice.
Except as specifically set forth in its terms and conditions of sale, PerkinElmer makes no warranty of any kind with
regard to this document, including, but not limited to, the implied warranties of merchantability and fitness for a partic-
ular purpose.
PerkinElmer shall not be liable for errors contained herein for incidental consequential damages in connection with fur-
nishing, performance or use of this material.
Copyright Information
This document contains proprietary information that is protected by copyright.
All rights are reserved. No part of this publication may be reproduced in any form whatsoever or translated into any
language without the prior, written permission of PerkinElmer, Inc.
Copyright © 2013 PerkinElmer, Inc.
Trademarks
Registered names, trademarks, etc. used in this document, even when not specifically marked as such, are protected by
law.
PerkinElmer is a registered trademark of PerkinElmer, Inc.
Titan MPS, WinLab32 for AA, and AAnalyst, are trademarks of affiliates of PerkinElmer, Inc.
Windows is a trademark and Microsoft is a registered trademark of Microsoft Corporation.
Part Number Release Publication Date
E9931099 AJune 2013

Table of Contents
Introduction ....................................................................................... xiii
Safety and Regulatory Information................................................... xiii
Safety Practices
Overview ...............................................................................................1
Qualified Users .....................................................................................2
Proper Use .............................................................................................2
General Safety Information ..................................................................4
Safety and Emissions ............................................................................7
Precautions ............................................................................................9
Environmental Conditions ..................................................................11
Electrical Safety ..................................................................................12
Fuses ...................................................................................................13
EMC Compliance ...............................................................................14
United States (FCC) ............................................................................14
Warning Labels on the Instrument ......................................................15
WEEE Instructions for PerkinElmer Products ...................................20
Warranty/Limitation of Warranty 22
Preparing Your Laboratory
Introduction .........................................................................................23
Environmental Requirements .............................................................23
Exhaust Line Venting Requirements ..................................................24
Lab Space Requirements ....................................................................24
Microwave Radiation 2..........................................................................6
System Description
Titan Microwave Prep System ...........................................................27
Pressure Vessels and Turntables .........................................................34
Specifications ......................................................................................37
Installation
Unpacking ...........................................................................................39
Power Cord Options ............................................................................41
Installation ..........................................................................................46
Operation
Method Preparation .............................................................................53
System Login ......................................................................................57
Performing a Digestion .......................................................................59
Pressure Calibration ............................................................................69
Method Creation and Editing Favorites ..............................................73
Creating a Method ..............................................................................77
Selecting and Renaming Datafiles ......................................................79
The Real Time Data Display ..............................................................82

Data Review File Management and Export ........................................84
Reviewing Digestions on the Titan MPS ............................................85
Flow Charts .........................................................................................91
Start Digestion ....................................................................................93
Sample Details ....................................................................................94
Digestion Results ................................................................................95
Change / Rename Datafile ..................................................................96
Create Method .....................................................................................97
Edit Method ........................................................................................98
Data Management ...............................................................................99
File Management / Data Export ........................................................100
Maintenance
Cleaning ............................................................................................101
Turntable System ..............................................................................106
Fuse Replacement .............................................................................107
Repairs/Customer Service .................................................................107
Maintenance Tips ..............................................................................108
Output Power Measurement .............................................................108
Troubleshooting
Overview ...........................................................................................113
Microwave Oven ...............................................................................114
Control Unit ......................................................................................116
Pressure Digestion Vessel .................................................................117
Appendix
References .........................................................................................119
Conversion Table ..............................................................................121
Index of Controller Screens ..............................................................121

xiii
Introduction
Introduction
Please read this users guide carefully before operating the Titan MPS microwave
sample preparation system. Failure to follow these instructions could result in
damage to the instrument as well as personal injury.
Safety warnings are printed in boldfacethroughoutthisguide and are illustrated the
in section Safety Warnings and Icons on page xiii. Follow these safety warnings!
Safety and Regulatory Information
Safety Warnings and Icons
The signal words described below are used in connection with warnings
throughout this manual. For your own safety and to avoid property damage, you
must strictly heed these warnings!
The safety signals are printed in boldface or are otherwise marked throughout this
Safety Information in the Manual
Safety information is contained in Chapter 1 of this manual. Beforesetting upand
operating this instrument, carefully read the safety precautions described in
this chapter and observe them at all times.
In this manual, the following graphic symbols and special text formats are used to
indicate important safety information.
Any of the following safety conventions can be used throughout this guide:
Caution Theprotectionprovidedby this instrumentmay be compromisedif the
instrument is used in a manner not specified by PerkinElmer.

xiv
A warning indicates an operation that could cause personal injury if
precautions are not followed.
This symbol alerts you to the risk of electric shock that could result in personal
injury to yourself or other persons.
Details about these circumstances are in a box like this one.
This symbol alerts you to the risk of hot surfaces that could cause personal
injury to yourself or other persons.
Details about these circumstances are in a box like this one.
This symbol alerts you to the risk of strong magnetic fields that could cause
injury to persons wearing a heart pacemaker or having metallic implants.
Details about these circumstances are in a box like this one.
Caution A caution indicates an operation that could cause instrument damage
if precautions are not followed.
!
Warning
Warning

xv
Safety and Regulatory Information
How this Guide is Organized
Thoroughly read the Safety chapter before using the instrument. Consult the
appropriate reference materials listed at the end of the Safety chapter.
Read Chapter... To find out about...
Introduction This chapter contains a brief
introduction on the instrument, the
conventions and warnings used in the
manual.
1 Safety Practices Important safety information is
provided in this chapter.
2 Preparing Your Laboratory The preparation of your laboratory
needed for the Titan MPS.
3 System Description This chapter contains information on
the components of the instrument, how
it works and instrument specifications.
4 Installation Information on moving and reinstalling
your instrument is provided.
5 Operation Information on hardware and software
operation.
6 Maintenance Maintenance and cleaning procedures
for the various components of your
instrument are provided.
7 Troubleshooting Performance checks, troubleshooting
information and software,
8 Appendix References, conversion tables and
method screens.

xvi
Using the Index
Use the index to look up information on the different hardware components. For
example, if you need to find information on cleaning the glass ring, look up "glass
ring" in the index. Also, use the index to look up information on the following
topics:
• installation
• maintenance
• troubleshooting
A Word on Troubleshooting
We recommend that you consult the troubleshooting information included in this
manual before you call a PerkinElmer service engineer. The Troubleshooting
chapter contains suggestions to help you determine what the problem may be, offer
a solution and prevent extended downtime or the need for a service call.
Conventions Used in this Manual
Normal text is used to provide information and instructions.
Bold text refers to text that is displayed on the screen.
UPPERCASE text, for example ENTER or ALT, refers to keys on the PC
keyboard. '+' is used to show that you have to press two keys at the same time, for
example, ALT+F.
All eight digit numbers are PerkinElmer part numbers unless stated otherwise.

Safety Practices 1
Overview
This chapter describes the general safety practices and precautions that must be
observed when operating the Titan MPSTM.
This advice is intended to supplement, not supersede, the normal safety codes in
the user's country. It is also a supplement to the PerkinElmer standard Safety and
Health Policy. The information provided does not cover every safety procedure
that should be practiced. Ultimately, maintenance of a safe laboratory environment
is the responsibility of the analyst and the analyst's organization.
Please consult all documentation supplied before you start working with the
instrument. Carefully read the safety information in this chapter and in the other
manuals supplied. When setting up the instrument or performing analyses or
maintenance procedures, strictly follow the instructions provided.
Note This instrument requires no specified inspection or preventive
maintenance to ensure the continuous functioning of its safety features.
Warning
Prohibited for persons with heart pacemakers!
The microwave device must not be operated by persons with heart
pacemakers.

2Safety Practices
Qualified Users
Only qualified users should operate this instrument. Qualified users with respect to
this manual are relevantly schooled and trained specialists with a basic knowledge
of chemistry. They should be trained in the safe handling of chemicals.
Proper Use
The instrument emits microwave radiation!
Never operate the microwave oven if the drop lid or the related lock
mechanism have been damaged. Contact Perkin Elmer Inc. to obtain the
required service (Refer to the Repairs/Customer Service on page 107 for
contacts).
Note PerkinElmer products should only be used in a laboratory setting.
Explosion hazard!
The instrument is not designed for extraction and digestion procedures
employing organic solvents.
!
Warning
!
Warning

3
Proper Use
The Titan MPS (Microwave Preparation System) has been specially developed for
sample preparation for AAS and ICP spectroscopy procedures. The Titan MPS has
been designed to perform chemical digestion procedures under extreme pressure
and temperature conditions in chemical laboratories. Digestion is understood to
meanthe decomposition of a solidmaterialby means ofa suitable digestion reagent
at increased temperature in a vessel that is permeable with regard to microwaves.
The digestion solutions are directly heated through the absorption of the
microwave radiation by the polar digestion reagent, which generally also contains
ionic components.
Digestion reagents used can include nitric acid (70%), hydrochloric acid (37%),
hydrofluoric acid (49%), phosphoric acid (85%), and sulfuric acid (96%), as well
as mixtures of these acids. The maximum initial weight for organic compounds
depends on the digestion vessel being used and the sample's carbon content and
must always be carefully chosen. The use of organic solvents is strictly prohibited
since the Titan MPS is not designed to prevent the spontaneous combustion of any
solvent vapors that may escape into the oven chamber.
Heating in the pressure vessel can frequently result in digestion temperatures in
excess of 200 °C (392°F). The Titan MPS has been specially developed for sample
preparation for AAS and ICP spectroscopy procedures. Temperature spikes >280
°C (>536°F) can occasionally occur during the course of exothermic reactions and
can result in irreversible damage to the Teflon vessels. Since such scorching can
only be avoided by proper sample and reagent selection by the operator and not by
Observe all operating instructions!
Since sample composition is generallynot precisely defined, a certain
residual risk exists when performing pressure digestion processes.
Careful working practices and conscious compliance with safety
regulations can only minimize this risk, not totally eliminate it. Due to
different degrees of mixing, even identical samples can exhibit totally
different behaviors during the course of the digestion! Please strictly
comply with the operating instructions, particularly when handling the
pressure vessels, i.e. when removing and opening the vessels. Incorrect
handling of the hot, pressurized vessels can result in injuries from
escaping acid vapors!
!
Warning

4Safety Practices
a reliance on the Titan MPS's microwave power regulation, damage of this kind is
excluded from the warranty!
Qualified handling, proper transport, storage, set-up, and use, as well as
conscientious maintenance are all prerequisites for the trouble-free and safe
operation of the Titan MPS microwave digestion system.
The system may only be used within the context of data and applications specified
in this documentation and other associated manuals.
The digestion system may only be used:
• According to the provided manuals
• In 100% working condition
• Without unauthorized alterations or modifications
• By qualified and trained users
General Safety Information
Performing microwave digestion procedures involves taking into account various
safety precautions which go beyond those for general laboratory practices. The
following general safety information should therefore be read carefully prior to
using the system, and should be observed at all times.
The following information must be followed when working with the associated
digestion vessels!
We can assume no liability for damages resulting from improper handling or a
failure to comply with this information.
Always wear eye protection!
Always wear safety glasses/goggles and protective gloves during work
which may involve contact with chemicals, particularly when working
with acids and the pressure vessels!
!
Warning

5
General Safety Information
Explosion hazard!
Use extreme caution when working with perchloric acid. When
possible, avoid the use of perchloric acid. Organic solvents (alcohols,
hydrocarbons, etc.) must not be used as reagents in the pressure
vessels or the microwave.
Highly reactive substances which spontaneously react at higher
temperatures or in the presence of oxidizing agents or which may be
nitrated and are potentially explosive may not be digested in the
microwave.Examplesofsuchsubstancesinclude:explosives(TNT,etc.),
perchlorates, ether, pyrophoric substances, etc.
Pressure vessels!
Use only digestion vessels and spare parts authorized by Perkin Elmer for
use with the Titan MPS.(Refer to the Repairs/Customer Service on page
107 section for contact addresses).
Always wear safety glasses/goggles and protective gloves when working
with the pressure vessels!
Note any changes in the appearance of the pressure vessel which could
indicate possible material fatigue, e.g., deformation of the vessel,
difficultyscrewingon lids, etc. even when the vessel is cold and notunder
pressure. All such vessels should be immediately returned to Perkin
Elmer Inc. for inspection.
!
Warning
!
Warning

6Safety Practices
Pressure vessels!
Neverattempt to useforce toopen thevessels.Never use tools toopen
the vessels! The pressure vessels are equipped with a rupture disc which
produces a spontaneous pressure release upwards through the screw-on
tube connections in case of excessive vessel pressure. In some cases, such
a spontaneous pressure release may occur after the vessel has been
removed from the microwave oven.
Hot gases and vapors may be released from the digestion vessel when
it is opened! Always make sure the vent opening on pressure vessels
faces away from both yourself and other individuals!
Only open the digestion vessel under a fume hood or other exhaust
system.
Particular care is required when working with hydrofluoric acid (HF).
Due to the extreme damage it inflicts. Observeall relevant datasheets and
safety instructions!
Note Replace the vessels after around 5000 digestions to maintain reliable
operating conditions and to prevent negative influences on your analysis
results (e.g. memory effects etc.). Perkin Elmer includes its digestion
vessels in the one year warranty coverage. Nevertheless all of the vessels
are subject to a certain aging process, which also depends on the type and
frequency of the application. Typically the service life is 5,000 digestion
processes or at least 3 years.
!
Warning

7
Safety and Emissions
Safety and Emissions
In the following situations, the instrument must be disconnected from the power
outlet and be locked out to prevent accidental use:
• If the instrument evidences visible signs of damage;
• If the instrument parts or components are found to be loose;
• If the instrument fails to operate;
• If the instrument is to be stored for extended periods of time under
unfavorable conditions (e.g., outdoors, in very moist or humid
environments).
The instrument operates with 230 volts and generates
microwave radiation!
The Titan MPS must always be carefully connected to a grounded
conductor. Provided the wall outlet used is equipped with a ground
connection, the supplied power cord will ensure proper connection. If it
is necessary to use an extension cord to connect the system to the power
supply, only a three-wire cord with a ground connection may be
employed.
The instrument should not be set up near any devices which are sensitive
to electromagnetic radiation. Should there be any suspicion or indication
of increased levels of microwave radiation, please immediately inform
the Service Department at Perkin Elmer Inc. (Refer to the Repairs/
Customer Service on page 107 section for the contact address).
Repair and servicing of the equipment may only be performed by
trained personnel.
Prohibited for persons with heart pacemakers!
The microwave device must not be operated by persons with heart
pacemakers.
!
Warning
!
Warning

8Safety Practices
Drop Lid
The system is equipped with a solid, PFA-coated, stainless steel housing with a
drop safety lid for maximum user safety. The door-locking mechanism can only be
opened by means of the software control. In addition, four interlock switches are
installed which shut the microwave off if the lid is opened by force during
microwave operation.
Rupture Discs
Allvesselsare equipped with a rupture disc which produces a spontaneouspressure
release upwards through the screw-on tube connections in case of excessive vessel
pressure. In some cases, such a spontaneous pressure release may occur after the
vessel has been removed from the microwave oven.
Gas Exhaust
High Voltage!
The housing cover may only be removed by authorized trained personnel!
The instrument must be disconnected from the power outlet before being
serviced.
Rupture discs as overpressure protection!
Use only original Perkin Elmer rupture discs and pressure seals. These
can be obtained from Perkin Elmer Inc. (Refer to the Repairs/Customer
Service on page 107 section for contact addresses). Never usemore than
one rupture disc per vessel!
Hot acid vapors may be released.
The supplied vent tubes must therefore always be properly connected and
attached to an exhaust system. Make sure the PFA tubing is securely
attached so that it cannot pop off its connection fitting during a rupture
disc pressure release.
!
Warning
!
Warning

9
Precautions
All pressure vessels are equipped with a sealed connection to a gas collection
system which, in turn, must be connected to an exhaust system via PFA tubing. The
PFA tubing is connected to the screw-on connection located in the center of the top
of the microwave. Any hot acid vapors released when the rupture disc activates are
safely removed through this PFA vent tubing.
Temperature Control
The system is equipped with Direct Temperature Control (DTC) of all sample
temperatures as described in the section, Temperature Monitoring on page 33. An
emergency shut-off occurs in case of a rupture disc break.
Pressure Control
The system is also equipped with a pressure monitoring system for a reference
vessel located at position one as described in the Repairs/Customer Service on
page 107.
Over Temperature Protection
For safety reasons, the microwave automatically switches itself off in case the
magnetron, the microwave oven, or the high voltage transformer overheats.
Precautions
Be sure to read and understand the precautions listed below. It is also
recommended to post a copy of the precautions near or on the instrument
shelf.
Caution The protection provided by this instrument may be impaired if the
instrument is used in a manner not specified by PerkinElmer.
!
Warning

10 Safety Practices
The following precautions must be observed when using this instrument:
• Be sure that the voltage in the laboratory meets the voltage requirements
of this instrument.
• Before the instrument is installed, the area around, under and behind the
instrument's planned location is to be cleared of any dirt and dust to
prevent their entry into the instrument's interior which could cause a
negative effect on performance.
•Donotposition the instrument so that it is difficult to disconnect thepower
switch and power plug located on the right side of the instrument.
• Keep the work area scrupulously clean to avoid contaminating your
samples and to maintain a safe working environment. Clean up spilled
chemicals immediately and dispose of them properly.
•Donot allow smoking in the work area. Smoking is a source of significant
contamination and also a potential route for ingesting harmful chemicals.
The laboratory manager is responsible for warning users of this
instrument concerning biohazardous materials that are processed in this
instrument and about waste that results from the operation of this
instrument.
Warning: Explosive Atmosphere
This instrument is notdesigned for operation in an explosive atmosphere.
Note Important Note for North American-Users:
Voltage of the power supply has to be in the range of 230V ± 15V AC.
Even with a maximum load of approximately 2700 W the supply-voltage
should not drop below 215 V AC. Low voltage can result in low
microwave power delivery, excessive magnetron or inverter heating and
erratic temperature and pressure measurements.
!
Warning
!
Warning