Usg Zetium en

ZETIUM
USER GUIDE
ZETIUM
USER GUIDE
EDITION NOTICE: 4023 000 43228, September 2021

This is the original publication of Edition 8 of this document, to be used with the
Zetium instrument.
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DISCLAIMER
Although diligent care has been used to ensure that the information in this material is
accurate, nothing herein can be construed to imply any representation or warranty as
to the accuracy, correctness or completeness of this information and we shall not be
liable for errors contained herein or for damages in connection with the use of this
material. Malvern Panalytical reserves the right to change the content in this material
at any time without notice.
COPYRIGHT NOTICE
© 2021 Malvern Panalytical. This publication or any portion thereof may not be copied
or transmitted without our express written permission.
Malvern Panalytical Ltd. Malvern Panalytical B.V.

Grovewood Road, Malvern, Lelyweg 1, 7602 EA Almelo,
Worcestershire, WR14 1XZ, The Netherlands
United Kingdom
Tel. +44 1684 892456 Tel. +31 546 534 444

Fax. +44 1684 892789 Fax. +31 546 534 598
info@malvernpanalytical.com
www.malvernpanalytical.com
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TABLE OF CONTENTS
Chapter 1. Introduction. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7
1.1 General. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7
1.2 Intended use. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7
1.3 Recommended skill levels. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7
1.4 Glossary of terms and abbreviations. . . . . . . . . . . . . . . . . . . . . . 8
Chapter 2. Safety. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 11
2.1 Introduction to safety aspects. . . . . . . . . . . . . . . . . . . . . . . . . . 11
2.1.1 Authorized personnel. . . . . . . . . . . . . . . . . . . . . . . . . . . . 11
2.1.2 Safety guarantee. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 11
2.1.3 Alerts and labels. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 12
2.2 Safety standards. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 12
2.3 Malvern Panalytical's approach. . . . . . . . . . . . . . . . . . . . . . . . . 13
2.4 User responsibilities. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 14
2.4.1 What to do in case of an emergency. . . . . . . . . . . . . . . . 15
2.5 General hazards. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 15
2.5.1 Ionizing radiation. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 15
2.5.2 Toxic material. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 16
2.5.3 Flammable material. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 19
2.5.4 Hot surface. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 20
2.5.5 Earth leakage current. . . . . . . . . . . . . . . . . . . . . . . . . . . . . 20
2.6 Safety measures. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 20
2.6.1 HT keyswitch. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 20
2.6.2 INSTANT POWER OFF button. . . . . . . . . . . . . . . . . . . . . . 20
2.6.3 X-RAYS lamps. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 20
2.6.4 Double independent safety loops. . . . . . . . . . . . . . . . . . 21
2.6.5 Xsafe. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 21
2.6.6 Motion safety. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 21
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2.7 Safe use of the instrument. . . . . . . . . . . . . . . . . . . . . . . . . . . . . 21

2.7.1 Location of alerts and hazards Zetium (1 kW). . . . . . . . 23
2.7.2 Location of alerts and hazards Zetium (2.4 to 4 kW). . 28
Chapter 3. System description. . . . . . . . . . . . . . . . . . . . . . . . . . 33

3.1 Introduction. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 33
3.2 Location of components. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 34
3.2.1 Zetium (1 kW) components. . . . . . . . . . . . . . . . . . . . . . . . 34
3.2.2 Zetium (2.4 kW to 4 kW) components. . . . . . . . . . . . . . . 38
3.3 Control panel. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 42
3.3.1 ON button and POWER ON indicator. . . . . . . . . . . . . . . 42
3.3.2 OFF button and POWER OFF indicator. . . . . . . . . . . . . . 42
3.3.3 ON/OFF button and LIGHT ON indicator. . . . . . . . . . . . 43
3.3.4 HT keyswitch and HT ENABLED indicator. . . . . . . . . . . . 43
3.3.5 INSTANT POWER OFF button. . . . . . . . . . . . . . . . . . . . . . 43
3.4 Optical path. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 44
3.4.1 X-ray tube. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 44
3.4.2 Tube filters. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 45
3.4.3 Sample position. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 45
3.4.4 Collimator mask. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 46
3.4.5 Primary collimator. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 46
3.4.6 Analyzing crystals. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 47
3.4.7 Detectors. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 48
3.4.8 Goniometer. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 49
3.4.9 HiPer channels (2.4 kW to 4 kW only). . . . . . . . . . . . . . . 49
3.4.10 ED core. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 50
3.4.11 Small spot mapping (4 kW only). . . . . . . . . . . . . . . . . . . 50
3.4.12 HiPer small spot mapping (2.4 kW to 4 kW only). . . . 50
3.4.13 Measuring medium. . . . . . . . . . . . . . . . . . . . . . . . . . . . . 51
3.5 Dust removal device. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 51
3.6 HiCap sample changer. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 51
3.7 Smart Manager. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 52
Chapter 4. Operate the instrument. . . . . . . . . . . . . . . . . . . . . . 53

4.1 Introduction. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 53
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TABLE OF CONTENTS
4.2 Switch on the instrument. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 53

4.3 Monitor the status of the system. . . . . . . . . . . . . . . . . . . . . . . . 54
4.4 Switch off the instrument. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 54
Chapter 5. Measure samples. . . . . . . . . . . . . . . . . . . . . . . . . . . . 55

5.1 Measurement overview. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 55
5.2 Sample loading. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 55
5.2.1 Sample changer layout. . . . . . . . . . . . . . . . . . . . . . . . . . . 57
5.2.2 Put trays on the sample changer. . . . . . . . . . . . . . . . . . . 57
5.2.3 Put sample cups on the sample changer. . . . . . . . . . . . 58
5.2.4 Load the cups manually. . . . . . . . . . . . . . . . . . . . . . . . . . 59
5.2.5 Direct loading tool. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 60
Chapter 6. User maintenance. . . . . . . . . . . . . . . . . . . . . . . . . . . 63

6.1 Introduction. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 63
6.2 Use TCM5400. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 64
6.2.1 Install TCM5400. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 64
6.2.2 Connect to the instrument with TCM5400. . . . . . . . . . . 64
6.3 Test of the safety integrity. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 65
6.4 Clean the instrument. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 66
6.5 Remove the panels. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 66
6.6 Fill the cooling system. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 67
6.7 Examine the oil level of the vacuum pump. . . . . . . . . . . . . . . 70
6.8 Examine the alumina pellets. . . . . . . . . . . . . . . . . . . . . . . . . . . . 73
6.9 Maintain the gas systems. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 75
6.9.1 Replace the cylinder of the detector flow gas. . . . . . . . 76
6.9.2 Leakage test of the gas system. . . . . . . . . . . . . . . . . . . . 79
6.9.3 PHD test of the flow detector. . . . . . . . . . . . . . . . . . . . . . 79
6.10 Replace the primary water filter. . . . . . . . . . . . . . . . . . . . . . . 81
6.11 Clean the dust removal device. . . . . . . . . . . . . . . . . . . . . . . . . 82
6.12 Consumable materials. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 83
Chapter 7. Troubleshooting. . . . . . . . . . . . . . . . . . . . . . . . . . . . . 85
7.1 Introduction. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 85
7.2 Instrument is off-line. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 85
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TABLE OF CONTENTS
7.2.1 Reset Xsafe. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 85

7.3 HT generator does not switch on. . . . . . . . . . . . . . . . . . . . . . . 86
7.4 No remote support connection. . . . . . . . . . . . . . . . . . . . . . . . . 87
7.5 Sample changer alignment is incorrect. . . . . . . . . . . . . . . . . . 87
7.5.1 Calibrate the sample changer. . . . . . . . . . . . . . . . . . . . . 87
Chapter 8. Disposal instructions. . . . . . . . . . . . . . . . . . . . . . . . 89

8.1 WEEE Directive. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 89
8.2 Hazardous substances. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 89
8.2.1 Beryllium. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 89
8.2.2 Lead. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 90
8.2.3 X-ray tube. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 90
8.2.4 Detector. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 90
8.2.5 Crystals. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 93
8.2.6 Tube filter. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 94
8.2.7 Vacuum pump. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 95
8.2.8 Foreline trap. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 96
Index. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 99
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CHAPTER 1 INTRODUCTION
1.1 General
This User Guide gives a description of the hardware and instructions that are related to
safety, operation, user maintenance and disposal of these systems:
• 9430 054 00101 Zetium (1 kW configuration)

• 9430 054 00241 Zetium (2.4 kW configuration)
• 9430 054 00701 Cement edition of Zetium
Before you use this User Guide, make sure that the instrument is installed correctly,
the software is set up and the applications are created.
For more information, refer to the SuperQ Help that is supplied with the software.
1.2 Intended use

The Zetium instrument together with the SuperQ application software is designed to
do routine X‑ray measurements and analyses over a long period of time.
It is expected that the system will mostly be used by laboratory or factory personnel.
The system must not be used for purposes other than intended.
If the equipment is used in a manner not specified by the manufacturer, the protection
provided by the equipment may be impaired.
1.3 Recommended skill levels

The system may be operated by personnel with various skill levels. A person may only
operate the system after adequate training is received for the required skill level.
The skill levels are:
Operator
• Does not need in-depth knowledge of X-ray theory or applications.

• Must have knowledge of the visible hardware, such as how to switch the
instrument on/off and how to use the sample changer for loading and unloading
samples.
7
• Must be able to follow instructions on how to measure samples using applications

and how to execute pre-defined tests.
Application engineer
• Must have a thorough knowledge of the analysis process.

• Must have enough knowledge of the hardware to know the limits of what can or
cannot be done when using the system.
• Must know how to set up and maintain applications.
• Must know how to develop applications for specific application areas.
System engineer
• Must have enough knowledge to set up and maintain the system, both hardware
and software.
• Responsible for maintaining the password mechanism, global variables (names of
filters and targets, global compound database, monitors, etc.).
• Must have an understanding of the function of the main aspects of the analysis
procedure including but not limited to applications, monitors and sample lists.
• Must have enough knowledge of the hardware to start safe actions (not
overruling security).
• Must know the actions to take when the system indicates a malfunction.
1.4 Glossary of terms and abbreviations

Term or abbreviation Description
Bg. Background.
CE Conformité Européenne. The CE mark shows that the product
conforms to the applicable European Directive(s). Compliance
with the applicable European Directives is stated in the
Declaration of Conformity.
CSE Counting Statistical Error (kcps).
CSErel, CSE% Relative Counting Statistical Error (% relative).
EMO Emergency Off (button).
ESD Electrostatic discharge.
HT High tension.
Installation category These levels are assigned to 4 different installation categories
(over voltage categories) in IEC 61010. Our systems are all
categorized level II, Local level, appliances.
LLD Lower Limit of Detection (ppm).
PHD Pulse Height Distribution (%).
8
Term or abbreviation Description
PTB Physikalisch-Technische Bundesanstalt. An independent test

house (notified body) executing type tests at supply center
locations. German government must be informed by these test
reports and they issue a so-called Zulassung (permission
number). This permission number is written into the
Declaration of Conformity and can be seen on the instrument
type plate. In most cases the classification of
Malvern Panalytical equipment is Vollschutz .
Qualified Service Engineer Person who is trained, educated and authorized by the
Malvern Panalytical organization to execute service work to a
specified level and product area.
R Rate or count rate (kcps).
Radiation level Dose rate in Sievert/hour. The dose rate of 1 Sievert/hour (Sv/h)
is equal at the dose rate of 100 Röntgen/hour (R/h). In practice
this will result in this similarity:
1 microSievert/hour = 0.1 milliRöntgen/hour.
RMS Root Mean Square value.
Safety class Classification of electrical equipment with regard to protection
against electric shock. These are described in detail in
IEC 61010.
°2θ Degrees 2theta.
9
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CHAPTER 2 SAFETY
2.1 Introduction to safety aspects

Read this chapter before you start to use your instrument.
This chapter helps you to maintain and operate the analytical X‑ray instrument in
accordance with very high safety standards. It gives you information on how to keep
the instrument in a safe condition and how to prevent accidents. It is important that
you read this information to know the safety aspects of the Malvern Panalytical
instrument.
A Malvern Panalytical instrument is fully safe when it is correctly installed and when the
instructions in this User Guide are obeyed during operation.
If the safety information in this chapter does not comply with the related local (national
or regional) rules, always obey the local rules.
2.1.1 Authorized personnel

NOTE: Authorized Personnel = Person who is trained, educated and authorized by the
Malvern Panalytical organization to execute service work to a specified level and
product area.
Procedures given in this User Guide can be done by the user. The installation,
maintenance and repair procedures of the instrument that are not in this User Guide
must only be done by Authorized Personnel .
All repairs, adjustments and alignments to any part of the instrument must obey all
applicable local regulations.
2.1.2 Safety guarantee

The Malvern Panalytical safety guarantee is included when a Malvern Panalytical
instrument is supplied. It remains covered throughout its life when the instrument is
maintained and repaired by Malvern Panalytical service engineers.
WARNING ‑ General Hazard

It is not permitted to make changes or additions to the system if they are not
approved.
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CHAPTER 2 SAFETY
2.1.3 Alerts and labels

Special alerts that relate to the safety of personnel and/or equipment can be found in
this manual. Where it is necessary, alert labels with the applicable symbol are attached
to the instrument.
Obey all instructions in the alerts in the manual and on the labels attached to the
different parts of the instrument.
Alerts in this manual are shown as follows:
DANGER ‑ Electrical Hazard

Shows an immediately dangerous condition which, if not prevented, can result
in death or very serious injury.
(The symbol relates to the specified hazard)
WARNING ‑ Ionizing Radiation

Shows a dangerous condition where there is risk of bad injury.
CAUTION ‑ General Hazard

Shows a condition that can cause damage to equipment or property, or where
there is a risk of small injury.
NOTE: Gives the user more information about the procedure or system.
2.2 Safety standards

Malvern Panalytical supplies a Declaration of Conformity with all instruments. The
Declaration of Conformity is a legal statement by Malvern Panalytical that shows that
the responsibilities related to the supplied instrument have been completed. The
customer must keep this document with the instrument for its full life cycle.
Another important declaration for users of analytical X‑ray instruments is the X‑ray
Safety Declaration, which is also supplied with all instruments.
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CHAPTER 2 SAFETY
The instrument complies with the requirements of the Machine Directive 2006/42/EC
and EMC Directive 2004/108/EC and the applicable X‑ray safety regulations.
Refer to the applicable standards, normative documents and directives in the

Declaration of Conformity and the X‑ray Safety Declaration of the instrument.
This product is certified by MET Laboratories to meet these standards:
• CSA C22.2 No. 61010-1 - 2012

• CSA C22.2 No. 61010-2-091 - 2014
• UL 61010-1 - 2012
• UL 61010-2-091 - 2014
2.3 Malvern Panalytical's approach

Malvern Panalytical makes and supplies analytical X‑ray instruments that obey the
applicable international product regulations. As a result, Malvern Panalytical complies
with these approaches:
• Specification of the worldwide lowest radiation level: less than 1 µSv/h at 10 cm

distance from the outer surface of the instrument.
• Risk calculations and assessments related to the use of the instrument that show
that the absorbed dose stays easily within the ICRP (International Commission on
Radiological Protection) level for public. This level is 1 mSv/year.
• Overall risk assessment related to the safety of the instrument.
• Instrument design, production and documentation is certified by notified bodies
PTB and/or CSA and/or MET. Refer to the Declaration of Conformity and the X‑ray
Safety Declaration for more information.
• Malvern Panalytical's environmental policy is deployed across the organization.
These steps are taken:
a. Design rules are applied to decrease energy consumption, packaging and
weight.
b. Environmental information is supplied with the instrument for the service
engineers and users.
• Emission of sound, made by the instrument during normal operation, complies
with the requirements of the Machine Directive.
• Moving parts are safe to operate. Precautions have been taking during the
development of the instrument, and there are alert labels on the instrument and
in the manuals.
Organizational requirements such as ISO 9001, ISO 14001, radiation safety board
inspections and audits make sure that these approaches are obeyed.
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CHAPTER 2 SAFETY
2.4 User responsibilities

To keep the instrument at the classified safety level, the user has these responsibilities:
1. The user must make sure that the instrument is correctly installed. The user s site
facilities must comply with the specifications in the pre-installation and installation
information, and comply with the applicable safety requirements. The user is also
responsible for these installation requirements:
a. A correct ground (earth) must be available.
b. The floor or table must be sufficient for the weight distribution of the
instrument.
2. Installation and maintenance must be done by Authorized Personnel.
3. Safety devices must NEVER be bypassed.
4. The user must make sure that persons that use the system are fully instructed in
the safety procedures.
5. The user must make sure that when the system is operated, the applicable local
safety regulations are obeyed.
6. All X‑ray analysis systems must be monitored regularly (based on a local risk
assessment) with a suitable X‑ray radiation monitor.
7. If the instrument is left unattended in a dangerous condition, do as follows:
a. Remove the HT (high-tension) key.
b. Disconnect the instrument from the mains power supply.
c. Attach a DO NOT OPERATE warning notice to all power buttons and mains
power switches or connections.
8. When X‑rays are generated, the fail-safe X‑rays warning lamps must be on. This
lamp must be clearly in view to all persons in the area.
9. In some countries, an X‑rays warning lamp and the international ionizing radiation
sign must be installed on the outer side of the room.
10. After installation or a maintenance/repair procedure is done, the user and the
service engineer must make sure that the safety interlocks operate correctly.
11. A Malvern Panalytical service engineer or application specialist can do a remote
support session on the instrument to troubleshoot, to examine the system after
repair or for application support. Before the remote support session is started,
the user must take precautions to make sure that the instrument can be operated
safely without local intervention.
12. Although the instrument is made and tested to be safe, maintenance is very
important. Information about user maintenance is given in this manual. Other
maintenance must be done by Authorized Personnel.
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CHAPTER 2 SAFETY
2.4.1 What to do in case of an emergency

If an emergency or a possible exposure to radiation from an analytical X‑ray instrument
occurs, do as follows:
1. Switch off the instrument and make sure that it cannot be switched on again.
2. Take the necessary medical/remedial first aid steps.
3. Do not take steps to correct the fault that caused the accident and/or exposure.
NOTE: If there is an X‑ray exposure incident, calculation of the absorbed dose is

more difficult if the fault is corrected.
4. Put a sign on the instrument to make sure that the instrument will not be used or
changed.
5. You must tell these persons about the emergency:
• The user
• The (Radiation) Safety officer
• The local Malvern Panalytical representative
6. If it is an X‑ray exposure accident and the exposure is more than the level set in
local regulations, refer the exposed person for medical examination.
2.5 General hazards
2.5.1 Ionizing radiation

Protection against ionizing radiation is a safety aspect that is included in the applicable
standards. The basic principle is to decrease the radiation near the instrument to a
level that is as low as reasonably achievable (ALARA principle).
When the instrument is correctly operated within the specifications, the radiation level
at a distance of 10 cm from the outer surface of the instrument is less than 1 µSv/h.
WARNING ‑ Ionizing Radiation

X-rays are dangerous. The instrument generates X-rays which can be
dangerous to health if precautions are not taken.
It is important for the health and safety of the user that the instructions given
in the instrument manuals are obeyed.
Obey local safety regulations.
15
CHAPTER 2 SAFETY
2.5.2 Toxic material

The instrument can contain materials that can be hazardous to health. A hazardous
substances label is attached to the rear of the instrument. Refer to Figure 2.1.
Some analyzing crystals can contain poisonous materials.
Unknown samples can contain poisonous material. Take precautions when you touch
unknown samples.
For more information, refer to the Safety Data Sheets.
16
CHAPTER 2 SAFETY
Figure 2.1 Hazardous substances label
2.5.2.1 Beryllium
Some items in the instrument contain beryllium (Be).
17
CHAPTER 2 SAFETY
WARNING ‑ Toxic Material

Beryllium and compounds of beryllium (for example beryllium oxide) are
poisonous.
Do not touch, swallow or breathe in beryllium.
Do not get beryllium on your bare skin. Always wear gloves when you touch
items that contain beryllium.
If there are dust or fumes of beryllium, use a dust mask and protective
clothing.
Disposal of beryllium must obey all applicable local regulations.
Refer to the safety information in this document and the related Safety Data
Sheet for more details.
Safety Data Sheet: (https://uqr.to/epa4)
2.5.2.2 Lead
Lead (Pb) is used as a protection material against X‑rays.

Lead and compounds of lead (for example lead oxide) are poisonous.
Do not touch, swallow or breathe in lead.
Do not get lead on your bare skin. Always wear gloves when you touch items
that contain lead.
If there are dust or fumes of lead, use a dust mask and protective clothing.
Disposal of lead must obey all applicable local regulations.
Refer to the safety information in this document and the related Safety Data
Sheet for more details.
Safety Data Sheet: (https://uqr.to/i8t3)
18
CHAPTER 2 SAFETY
2.5.2.3 Crystals
Some analyzing crystals can contain toxic materials. Access to the crystals is only for
Authorized Personnel.

The crystals can contain toxic elements. These crystals are toxic if swallowed,
and contact with acids can make a very toxic gas.
Always handle crystals with extreme care and in well-ventilated areas, and
wear powder-proof gloves, protective cloths and eye protection. Avoid skin
contact and, after handling the crystals, wash your hands thoroughly.
Disposal of toxic material must comply with all applicable national regulations.
Refer to the related Safety Data Sheet for more details.
Safety Data Sheet:
TlAP crystal: (https://uqr.to/epxm)
InSb crystal: (https://uqr.to/epad)
LiF crystal: (https://uqr.to/epae)
2.5.3 Flammable material
WARNING - Flammable Material

The end-user is at all times responsible for treating (the substances or
materials used for fabricating) its samples with all due care and diligence.
Malvern Panalytical cannot be held liable for any damage resulting from the
use of flammable, combustible or other hazardous substances or materials in
(the preparation of) any samples.
19
CHAPTER 2 SAFETY
2.5.4 Hot surface

Parts of the instrument can become hot during operation. These parts are identified by
an alert label.
Samples can become hot during a measurement. Take precautions when you touch
samples or sample cups after a measurement.
2.5.5 Earth leakage current

The leakage current of instruments that are permanently connected to the mains
power supply can, in some conditions, be more than 10 mA. A second earth (ground)
connection to the instrument can be necessary because of local regulations.
2.6 Safety measures

These sections give information about safety measures that are used in the
instrument.
2.6.1 HT keyswitch
All instruments have an HT keyswitch. The removable HT key helps the local radiation
safety officer to control who uses the system.
To prevent unauthorized use of the system, remove the HT key. A normal mains power
is available for other functions.
2.6.2 INSTANT POWER OFF button

Press the INSTANT POWER OFF button in an emergency (unsafe) situation. It switches
off the mains voltage to the instrument immediately.
2.6.3 X-RAYS lamps

The X‑RAYS lamps are on when the instrument generates X‑rays. The X‑RAYS lamps are
part of the safety circuit. If one of the lamps is defective, the HT generator cannot be
switched on and X‑rays cannot be generated.
Only when the instrument senses that all conditions are safe, can the X‑RAYS lamps
come on and X‑rays be generated.
20
CHAPTER 2 SAFETY
2.6.4 Double independent safety loops

Double independent safety loops are necessary for fail-safe operation of the
instrument. For X‑ray safety, it is important to do a test of these loops regularly. Record
the results of the test.
2.6.5 Xsafe
Xsafe is a safety protection system that gives the user protection against X‑rays. This
system contains an electronic board that permanently monitors switches in the
instrument to make sure that it is safe for X‑rays to be generated.
The X‑ray tube in an instrument is energized by a high tension power supply. The safety
circuits automatically make sure that the high tension and X‑rays are immediately
switched off if there is a dangerous situation.
If the high tension is switched off, the water valve in the cooling system automatically
closes after 5 seconds. After these 5 seconds, the high tension can be switched on
again.
To make sure that Xsafe operates correctly, do a test of the operation of the safety
switches at least once a year.
NOTE: The Zetium has no visual indication of the Xsafe status.
2.6.6 Motion safety

The motion safety system gives the user protection against movements of the sample
changer.
The motion safety system makes sure that no movements are possible while the
sample changer cover is open.
2.7 Safe use of the instrument

During normal operation of the instrument with all panels in position, there are no
safety risks for the operator.
The next sections show possible safety risks from the instrument during sample
handling or with 1 or more panels removed, which is possible during user
maintenance.
21
CHAPTER 2 SAFETY

The instrument does not have brakes.
During normal operation of the instrument, the cup feet must be screwed
down to touch the floor to prevent movement of the instrument.
22
CHAPTER 2 SAFETY
2.7.1 Location of alerts and hazards Zetium (1 kW)
2
5
1. Pinch hazard: moving 4. Switch off instrument

robot arm before moving
2. Hot surface: sample cup 5. X-ray beams when
energized
3. Hot surface: vacuum
pump
Figure 2.2 Zetium (1 kW) - front
23
CHAPTER 2 SAFETY
1 1
1. Ionizing radiation: 2. Hot surface: vacuum

X‑RAYS lamp pump
Figure 2.3 Zetium (1 kW) - left
24
CHAPTER 2 SAFETY
1 1
1. Ionizing radiation:
X‑RAYS lamp
Figure 2.4 Zetium (1 kW) - right
25
CHAPTER 2 SAFETY
1. Hot surface: electronics 3. Disconnect from mains

rack supply before opening
2. Toxic material: system
contains hazardous
substances
Figure 2.5 Zetium (1 kW) - rear
26
CHAPTER 2 SAFETY
1 1
2
1. Ionizing radiation: 2. Disconnect from mains

X‑RAYS lamp supply before opening
Figure 2.6 Zetium (1 kW) - rear with panel
27
CHAPTER 2 SAFETY
2.7.2 Location of alerts and hazards Zetium (2.4 to 4 kW)
5
2
1. Pinch hazard: moving 4. Switch off instrument

robot arm before moving
2. X-ray beams when 5. Hot surface: sample cup
energized
3. Hot surface: vacuum
pump
Figure 2.7 Zetium (2.4 kW to 4 kW) - front
28
CHAPTER 2 SAFETY
1 1
X‑RAYS lamp
Figure 2.8 Zetium (2.4 kW to 4 kW) - left
29
CHAPTER 2 SAFETY
1 1
X‑RAYS lamp
Figure 2.9 Zetium (2.4 kW to 4 kW) - right
30
CHAPTER 2 SAFETY
1. Hot surface: electronics 3. Disconnect from mains

rack supply before opening
2. Toxic material: system
contains hazardous
substances
Figure 2.10 Zetium (2.4 kW to 4 kW) - rear
31
CHAPTER 2 SAFETY
1 1
1. Ionizing radiation: 2. Disconnect from mains

X‑RAYS lamp supply before opening
Figure 2.11 Zetium (2.4 kW to 4 kW) - rear with panel
32
CHAPTER 3 SYSTEM DESCRIPTION
3.1 Introduction
The Zetium is a multi-function analysis platform with a single goniometer-based
measuring channel, that includes the full measuring range. You can control the system
with an analytical software package installed on an external PC.
These industry configurations of the Zetium instruments are available:
• Metals edition of Zetium

• Minerals edition of Zetium
• Cement edition of Zetium
• Polymers edition of Zetium
• Petro edition of Zetium
• Ultimate edition of Zetium
The instrument can be configured for 1 kW, 2.4 kW, 3 kW or 4 kW power. The industry
configurations are available in 2.4 kW, 3 kW and 4 kW power.
These options are available:
• Fixed HiPer channels, for simultaneous measurements with the goniometer. Refer
to Section 3.4.9.
• ED core, for simultaneous ED and WD analysis. Refer to Section 3.4.10.
• Small spot mapping, to measure a spot of 0.5 mm at all positions on the sample.
Refer to Section 3.4.11.
• HiPer small spot mapping, to measure a spot of 0.5 mm at all positions on the
sample with increased sensitivity. This option cannot do ED bulk measurements.
Refer to Section 3.4.12.
Table 3.1 Options
1 kW 2.4 kW 3 kW 4 kW
Fixed channels n/a ✔ ✔ ✔

ED core n/a ✔ ✔ ✔
Small spot mapping n/a n/a n/a ✔
HiPer small spot mapping n/a ✔ ✔ ✔
33
3.2 Location of components
3.2.1 Zetium (1 kW) components
1 1
6
5
1. Handles for opening cover 4. Dust removal device (optional)

2. Sample changer gripper 5. Vacuum pump
3. Control panel 6. Foreline trap
Figure 3.1 Zetium (1 kW) - front
34
1. Water cooling fans 3. Water treatment unit

2. HT generator
Figure 3.2 Zetium (1 kW) - left
35
1. Dust filter and cabinet cooling

fan
Figure 3.3 Zetium (1 kW) - right
36
1. Electronics rack 3. Input/output gas and vacuum connections

2. PC connections
Figure 3.4 Zetium (1 kW) - rear
37
3.2.2 Zetium (2.4 kW to 4 kW) components
2 2
3
1. Sample changer gripper 4. Dust removal device (optional)

2. Handles for opening cover 5. Vacuum pump
3. Control panel
Figure 3.5 Zetium (2.4 kW to 4 kW) - front
38
1. Water treatment unit
Figure 3.6 Zetium (2.4 kW to 4 kW) - left
39
1. Foreline trap
Figure 3.7 Zetium (2.4 kW to 4 kW) - right
40
3 4
1. Electronics rack 3. Input/output water connections

2. PC connections 4. Input/output gas and vacuum connections
Figure 3.8 Zetium (2.4 kW to 4 kW) - rear
41
3.3 Control panel

3 4 5 6 7 8
2
1 9
13 12 11 10
1. HT keyswitch 8. LIGHT ON indicator
2. HT ENABLED indicator 9. INSTANT POWER OFF button
3. POWER OFF indicator 10. ON/OFF button
4. POWER ON indicator 11. X-rays warning
5. X-RAYS ON indicator 12. ON button
6. kV indicator 13. OFF button
7. mA indicator
Figure 3.9 Control panel
3.3.1 ON button and POWER ON indicator

When you press the ON button, the instrument switches to the ON condition. In this
condition, all instrument systems except the HT supply and the closed loop cooling of
the anode are in operation.
When the instrument is in the ON condition, the indicators are as follows:
• The POWER ON indicator is on.

• The POWER OFF indicator is off.
3.3.2 OFF button and POWER OFF indicator

When you press the OFF button, the instrument switches to the OFF condition. In this
condition, the HT supply is off but the peripherals and the internal lights are in
operation.
When the instrument is in the OFF condition, the indicators are as follows:
• The POWER OFF indicator is on.

• The POWER ON indicator is off.
42
3.3.3 ON/OFF button and LIGHT ON indicator

The ON/OFF button switches the interior lights on or off. When the interior lights are
on, the LIGHT ON indicator is on.
3.3.4 HT keyswitch and HT ENABLED indicator

When you turn the HT keyswitch clockwise, the HT generator goes on. If the safety
loops are closed, the HT generator is automatically set to 30 kV, 30 mA.
When the HT generator is in the ON condition, the indicators are as follows:
• The HT ENABLED indicator is on.

• The X-RAYS ON indicator is on.
• The kV and mA indicators on the control panel show the settings.
• The X-RAYS lamps on the sides of the instrument are on.
• If installed, the external X-RAYS ON lamp is on.
When you turn the HT keyswitch counter-clockwise, the HT generator goes off.
If the HT key is removed from the instrument and an unsafe condition is sensed, you
cannot switch the high tension on again. You must use the HT keyswitch to reset the
Xsafe system. Refer to Section 7.2.1. If a safe condition is sensed, the HT generator
goes on.
NOTE: The HT key can be removed and kept in a safe place.
3.3.5 INSTANT POWER OFF button

When you press the INSTANT POWER OFF button (IPO), the mains power supply in the
instrument is immediately switched off. If there is an emergency or unsafe condition,
press this button.
43
3.4 Optical path

3
7 2
8
4
1
5
9
10
1. X-ray tube 6. Crystal changer
2. Tube filters (optional) 7. Flow detector
3. Sample 8. Sealed detector (optional)
4. Collimator masks 9. Scintillation detector
5. Collimators 10. Fixed HiPer channel/ED core (optional)
Figure 3.10 Optical path
3.4.1 X-ray tube

The X-ray tube is an end window type and made of ceramic. There is a minimum
distance between the nose of the tube and the sample surface. The anode is at a
maximum of 60 kV above ground potential and is cooled with deionized water. In
Zetium in 1 kW configurations, the filament is also cooled with water.
Table 3.2 Available X-ray tubes
1 kW 2.4 kW 3 kW 4 kW
X-ray tube SST R SST R-mAX SST R-mAX SST R-mAX

Maximum kV 60 kV 60 kV 60 kV 60 kV
Maximum mA 50 mA 160 mA 160 mA 160 mA
NOTE: The SST R-mAX50 X-ray tube is included in the Ultimate edition of Zetium. This
X-ray tube has a thin window that increases sensitivity for light elements with a
44
maximum of 15 %. The SST R-mAX50 is available as an option for all other

Zetium configurations or as a retrofit.
The best kV and mA settings for each element are automatically set by the analytical
software.
Usually, a rhodium (Rh) anode is used in the X-ray tube, but other anodes can be
supplied for specified applications.
The window of the X-ray tube with Rh anode is made of beryllium and is 75 μm thick. It
transmits Rh L characteristic lines, which are important for the excitation of elements
with a low atomic number.
3.4.2 Tube filters

A maximum of 4 tube filters can be installed in the instrument. These filters are
available:
• Beam filter of 100 μm brass, to make the background and detection limits better
in the range 20-30 keV.
• Beam filter of 150 μm beryllium (WPA device), for protection of the X‑ray tube,
usually when liquids are measured.
• Beam filter of 200 μm aluminium, to make the background and detection limits
better in the range 6-10 keV.
• Beam filter of 300 μm aluminium, usually used in combination with Cr anode X-ray
tubes but it can also be used to remove Rh L-lines.
• Beam filter of 300 or 400 μm brass, to decrease Rh K-lines.
• Beam filter of 750 μm aluminium, to make the background and detection limits
better in the range 13-17 keV.
• Beam stop to protect the tube from dust and to prevent detector deterioration
when the instrument is in idle mode.
3.4.3 Sample position

The sample cup with sample is put inside the loading position to measure the sample.
The plunger moves the sample cup into the turret. The turret turns to put the sample
over the X-ray tube.
These turrets are available:
• 1 sample position for single loading.

• 2 sample positions for continuous loading.
• Turret for small spot mapping.
45
Sample cups are available for a number of sample sizes and types.
3.4.4 Collimator mask

The collimator mask is installed between the primary collimators and the sample. The
collimator mask makes sure that the collimators only see fluorescent radiation from
the sample and not from the sample cup. Thus, the selected mask size must be the
same as the diameter of the sample cup opening.
These collimator masks are available:
• Fixed masks for sample sizes of 27 mm, 30 mm, 35 mm and 37 mm. Only 1 mask
can be installed in the instrument.
• 3-position switchable mask for sample sizes of 27 mm, 30 mm and 37 mm.
• 6-position switchable mask for sample sizes of 6 mm, 10 mm, 20 mm, 27 mm, 30
mm and 37 mm.
Table 3.3 Available collimator masks
1 kW 2.4 kW 3 kW 4 kW
Fixed masks ✔ ✔ ✔ ✔
3-position switchable mask ✔ ✔ ✔ ✔
6-position switchable mask n/a ✔ ✔ ✔
When the instrument has a switchable collimator mask, you must select the aperture
size in the measurement program.
If other fixed or switchable collimator masks are necessary, contact your local
Malvern Panalytical representative.
3.4.5 Primary collimator

A maximum of 3 primary collimators can be installed in the instrument. These
collimators have of a large number of flat thin blades at a specified distance from each
other.
These collimators are available:
• 100 μm collimator for very high resolution.

• 150 μm collimator for high resolution.
• 300 μm collimator for medium resolution.
• 550 μm collimator for medium to coarse resolution.
• 700 μm collimator for coarse resolution.
• 4000 μm collimator for very coarse resolution (usually for Be, B, C, N).
46
3.4.6 Analyzing crystals

A maximum of 8 analyzing crystals can be installed in the crystal changer. The crystal
changer can rotate to put the selected crystal in the optical path.
These analyzing crystals are available:
• Ge(111) crystal, 2d = 0.653 nm, used for P, S and Cl analysis. It has a higher
dispersion than PE(002) and removes second order interferences.
• Ge(111) curved crystal, 2d = 0.653 nm, used for P, S and Cl analysis. It has a higher
dispersion than PE(002) and removes second order interferences. The crystal is
curved to produce higher intensities and sharper peaks with shorter tails.
• InSb(111) crystal, 2d = 0.7477 nm, used for Si analysis. The resolution is better
than a PE flat crystal and it gives approximately 2.5 times more intensity.
• InSb(111) curved crystal, 2d = 0.7477 nm, used for Si analysis where high
sensitivity is necessary. The crystal is curved and compared to the InSb flat crystal,
it gives higher intensities and sharper peaks with shorter tails.
• LiF200 crystal, 2d = 0.4027 nm, used for elements in the range K-U.
• LiF220 crystal, 2d = 0.2848 nm, used for elements in the range V-U. Its reflectivity
is approximately 40 % of the LiF200 crystal, but it has more dispersion than the
LiF200.
• LiF420 crystal, 2d = 0.1801 nm, used where very high resolution is necessary for
elements in the range Ni-U. Its reflectivity is approximately 10 % of LiF200 crystal
and 25 % of LiF220 crystal.
• PE(002) crystal, 2d = 0.8742 nm, used for elements in the range Al-Cl.
• PE(002) curved crystal, 2d = 0.8742 nm (for Zetium in 2.4 kW to 4 kW
configurations only), used for elements in the range Al-Cl. The crystal is curved to
give higher intensities and sharper peaks with shorter tails.
• PX1 crystal, 2d = 5.1 nm approximately, used for elements in the range O-Mg. It
has higher reflectivity than a TlAP crystal, is non-toxic and does not deteriorate
with time.
• PX4a crystal, 2d = 12 nm (for Zetium in 2.4 kW to 4 kW configurations only), to
make carbon analysis better.
• PX5 crystal, 2d = 11 nm (for Zetium in 2.4 kW to 4 kW configurations only), to
make nitrogen analysis better.
make beryllium analysis better.
make boron analysis better.
• PX8 crystal, 2d = 2.9800 nm, includes elements in the range O-Mg. It has higher
resolution than the PX1 crystal, but the PX1 has better reflectivity. The PX8 crystal
47
was made to replace the TlAP crystal and has higher reflectivity than the TlAP
crystal. It is non-toxic and does not decrease in performance like the TlAP crystal.
• PX10 crystal, 2d = 0.4027 nm, gives better performance for elements in the range
K-U. The PX10 is a higher performance alternative to the LiF200 crystal.
• TlAP100 crystal, 2d = 2.5750 nm, includes elements in the range O-Mg. It has
higher resolution than the alternative PX1 crystal, but the PX1 has better
reflectivity. Because the material of the crystal is toxic, the crystal surface has a
carbon layer.
3.4.7 Detectors
The size of the pulses that the detectors make are in proportion to the energy of the
incident radiation.
Table 3.4 Available detectors
1 kW 2.4 kW 3 kW 4 kW
Flow detector ✔ ✔ ✔ ✔
Sealed Xe gas detector (installed ✔ (optional) ✔ (optional) ✔ (optional) ✔ (optional)
as duplex)
Scintillation detector ✔ (optional) ✔ ✔ ✔
HiPer scint detector n/a ✔ (optional) ✔ (optional) ✔ (optional)
Secondary collimators are installed in the front of the scintillation and flow detectors.
3.4.7.1 Flow detector
The flow detector has a thin entrance window that is made of aluminized
polypropylene or gold. These windows are available:
• 6 μm for elements down to atomic number 13 Al.

• 2 μm for elements down to atomic number 11 Na.
• 1 μm for elements down to atomic number 4 Be.
• 1 μm PP for atomic number 5 B and atomic number 4 Be.
• 0.6 μm for elements down to atomic number 5 B.
Longer wavelengths are usually measured with a flow detector. Longer wavelengths
are for example the K-lines of Be to Ni and the L-lines of Hf to Ba.
Optionally, a sealed Xe gas detector can be attached to the rear of the argon flow
detector. These detectors operate as 1 duplex detector and give higher sensitivities for
the K-lines of V to Zn and L-lines of Ce to Ta. Radiation that is not absorbed and
measured by the argon flow detector, goes through an exit window and is measured in
the sealed Xe gas detector.
48
3.4.7.2 Scintillation detector
The scintillation detector converts X-rays into light, which is measured with a photo
multiplier. It decreases wavelengths such as the K-lines of Ni to Ba and the L-lines of Hf
to U.
3.4.7.3 HiPer Scint detector
The HiPer Scint detector is a high performance scintillation detector. It is included in

the Ultimate edition of Zetium. It is available as an option for all other Zetium in 2.4 kW
to 4 kW configurations.
These are the advantages compared to a standard scintillation detector:
• Larger linear range with a maximum of 3.5 Mcps.

• Improved LLDs for elements in the range from Ru to Cd.
• Extension of K-line analysis to Ce.
3.4.7.4 Counting electronics
The counting electronics process the pulses from the detectors. This includes pulse
amplification, pulse handling and counting facilities.
3.4.8 Goniometer
To measure at the Bragg angle, the crystal must be at an angle θ from the sample to
the X-ray beam, and the detector must be at an angle θ from the sample to the crystal.
To set the crystal and detector at the correct angle θ, the crystal is installed on the first
axis of the goniometer and the detectors are installed on the second axis of the
goniometer. The crystal axis turns at half the angular rotation of the detector axis. One
of the detectors (the scintillation detector or the flow detector (optionally as a duplex
detector)) will be at the correct Bragg angle.
The position of these axes must be very accurate. This is controlled by a Direct Optical
Positioning System (DOPS). DOPS uses an optical disk with a diode array reader that
frequently does checks to see if an axis is at the end position.
3.4.9 HiPer channels (2.4 kW to 4 kW only)

HiPer (high performance) channels are fixed channels. They have a focusing optical
system in which a curved crystal is used together with an entrance slit and an exit slit. A
focusing optical system is used to measure the characteristic radiation of 1 element in
the range B-Mg. An important element can be measured for a longer time, while other
elements are measured on the goniometer.
Each channel has an applicable detector installed.
49
A maximum of 2 HiPer channels can be installed, at angles of 29° and 44° of the
sample surface.
3.4.10 ED core
The ED core is used to analyze elements in the range Na-Am. The ED core can measure
simultaneously with the goniometer.
The ED core is installed at an angle of 29° of the sample surface. An SDD (Silicon Drift
Detector) is used for detection.
3.4.11 Small spot mapping (4 kW only)

With small spot mapping, you can measure spots of 0.5 mm at all positions on a
sample.
Small spot mapping uses the ED core to measure samples. This configuration has a
camera that is used to select the spot on the sample.
With small spot mapping, combined WD + ED bulk measurements are possible.
Figure 3.11 Small spot mapping
3.4.12 HiPer small spot mapping (2.4 kW to 4 kW only)

With HiPer small spot mapping, you can measure spots of 0.5 mm spots at all positions
on a sample. Compared to the regular small spot mapping, the special X‑ray optics
collect more photons and improve the sensitivity.
With HiPer small spot mapping, only WD bulk measurements are possible.
50
3.4.13 Measuring medium

The instrument can be used in vacuum or, if installed, in helium or nitrogen.
In vacuum, you can measure the full range of elements. In helium, you can measure
elements in the range of Na-U. In nitrogen, you can measure elements in the range of
Ti-U.
The helium and nitrogen gas systems can be used for liquids, loose powders or
granules. These samples cannot be measured in vacuum.
Do not measure liquids with an autoignition temperature of < 50 °C.
When the medium is set to vacuum, the system does a check to make sure that a
sample cup for solid samples is in the loading position.
3.5 Dust removal device

An optional dust removal device can be installed if the instrument is used in a dusty
environment. The dust removal device does not let dust into the measurement
chamber.
3.6 HiCap sample changer

The HiCap (high capacity) sample changer is optional for Zetium in 2.4 kW to 4 kW
configurations. With the sample changer bed for the HiCap sample changer, a large
number of single diameter samples can be put in the sample changer.
These versions of the sample changer beds for the HiCap sample changer are
available:
• For 32 mm samples, with 209 sample positions.

• For 40 mm samples, with 140 sample positions.
The HiCap sample changer layout also contains these items:
• Direct loading tool. Refer to Section 5.2.5.

• 8-position sample tray for sample cups and samples. This tray is designed for the
sample changer bed for the HiCap sample changer. It is different from the regular
8-position sample tray.
Only 1 8-position sample tray can be put on the sample changer bed for the
HiCap sample changer. For 32 mm samples, the sample positions are decreased
by 21. For 40 mm samples, the sample positions are decreased by 12.
51
3.7 Smart Manager

Smart Manager is an optional Internet of Things (IoT) tool for Zetium, available on an
annual subscription basis. Smart Manager needs IoT client software to be installed on
the instrument PC.
52
CHAPTER 4 OPERATE THE INSTRUMENT
4.1 Introduction
The system must be installed by a Malvern Panalytical service engineer and agree with
the specifications in the Zetium Pre-installation Manual.
If it is necessary to move the instrument, refer to the Zetium Pre-installation Manual for
the requirements about storage, transport and installation.
If you are not sure, always contact your local Malvern Panalytical representative.

Before you operate the instrument, obey these instructions:
The adjustable feet under the instrument must be lowered and touch the floor
to lock the instrument in position.
To prevent accidents, the floor around the instrument must be dry and there
must be no dirt or grease.
4.2 Switch on the instrument

1. Switch on the compressed air.
2. Make sure that the pressure of the compressed air is between 0.4 and 0.5 MPa.
3. Open the drain of the vacuum pump.
4. For Zetium in 2.4 kW to 4 kW configurations, open the drain of the cooling water.
5. Open the cooling water tap.
6. Open the main valve of the detector flow gas cylinder. The gas cylinder pressure
gauge must show a pressure of approximately 20 MPa. Refer to Figure 6.13.
7. Slowly open the reduction valve of the detector flow gas cylinder until the output
pressure gauge shows a pressure of 0.08 MPa.
8. If a helium gas cylinder or nitrogen gas cylinder is installed, do as follows:
a. Open the main valve of the gas cylinder. The gas cylinder pressure gauge must
show a pressure of approximately 20 MPa.
b. Slowly open the reduction valve of the gas cylinder until the output pressure
gauge shows a pressure of 0.08 MPa.
9. Connect the instrument to the mains power supply.
53
CHAPTER 4 OPERATE THE INSTRUMENT
10. Press the ON button to switch on the instrument.

11. Start the PC.
12. Start SuperQ.
13. Turn the HT keyswitch clockwise to switch on the HT generator.
14. Examine the instrument for water leaks:
a. For Zetium in 2.4 kW to 4 kW configurations, examine the external water
connections.
b. Remove the right panel.
c. Examine the water connections to the X-ray tube.
d. Install the right panel.
e. Wait until the temperature is stable. We recommend a warm-up time of 8
hours.
15. If the X-ray tube was switched off for more than 100 hours, do a fast conditioning
procedure.
For more information about the X-ray tube conditioning procedure, refer to the
related Tube Instruction Manual and SuperQ Help.
4.3 Monitor the status of the system

Use the Spectrometer status screen to monitor specific properties of the system.
You can monitor these properties:
• Flow of the cooling water

• Temperature of the cooling water
• Conductivity of the internal cooling water
• Gas flow of the detector
• Gas pressure of the detector
• Cabinet temperature
The values of these properties are dynamic.
4.4 Switch off the instrument

1. Press the OFF button to switch off the instrument. The instrument does a soft
power down.
2. Turn the HT keyswitch counter-clockwise to switch off the HT generator.
3. If it is necessary for the instrument to be switched off for a long period of time,
you can also switch off the mains power supply to the instrument.
54
CHAPTER 5 MEASURE SAMPLES
5.1 Measurement overview

These steps are necessary to do a measurement:
1. Put the sample into a sample cup.

2. Put the sample cup in the loading position or on a sample tray.
3. Start SuperQ.
4. Create an application.
5. Open the Sample Changer window.
6. Set up the measurement.
7. Click Measure to start the measurement. The sample automatically loads into the
measurement chamber and the measurement is done as given in the analytical
software.
The Results on-line window opens during a measurement. It shows the status of
the measurement and the temporary results.
5.2 Sample loading

You can load samples manually or automatically into the instrument.

If you measure unknown or toxic samples, refer to the Safety Data Sheet about
handling instructions.
WARNING - Flammable Material

The user is always responsible to use its samples, and its materials to prepare
these samples, very carefully and correctly.
Malvern Panalytical is not legally responsible for damage that is caused by

flammable samples, or by other hazardous materials in the samples or that
are used when the samples are prepared.
55

To prevent contamination of the measurement chamber and optical path, obey
these instructions:
Only use sample cups that are made for the related sample tray.
Only use sample cups that are approved for use in Malvern Panalytical
instruments.
For liquid cups, make sure that the cup lid is safely in position.
Do not keep temperature sensitive samples in the instrument for a long period.
If a pressed powder sample breaks or a liquid sample leaks in the

measurement chamber or the optical path, immediately switch off the
instrument. Do not clean the contaminated parts. A Malvern Panalytical service
engineer must clean the measurement chamber and the optical path.

Be careful when you load magnetic samples. Magnetic samples can have a
negative effect on the performance of the X-ray tube. Contact your local
Malvern Panalytical representative for more information.
56
5.2.1 Sample changer layout
E H
D G
C 5 6
4 F
A
3 2 1
A to S Sample tray positions

1. Unloading position 4. Loading position
2. Unloading position 5. Measuring position
3. Priority measurement position 6. Direct loading tool position
(optional)
Figure 5.1 Sample changer layout
If the instrument has one of the options, the sample changer layout is different. These
sample changer layouts are available:
• Sample changer bed for the HiCap sample changer, to increase the number of
samples to be measured. Refer to Section 3.6.
• Sample changer bed for small spot mapping, with a camera position.
5.2.2 Put trays on the sample changer

1. Open the sample changer cover.
2. Put the trays on the sample changer in the identified positions.
NOTE: The trays are kept in position by the spigots at each corner.
57
WARNING ‑ Pinch Hazard

Do not put your hand inside the loading position.
Figure 5.2 Put trays on the sample changer
5.2.3 Put sample cups on the sample changer

2. Put sample cups of the correct size on the trays, or put 1 sample cup in the
priority measuring position.

58
Figure 5.3 Put cups in position
5.2.4 Load the cups manually

You can put a cup with a sample directly in the loading position.

2. Open the loading cap with SuperQ.
3. Place the cup with the sample in the loading position.

WARNING ‑ Hot Surface

After a measurement, let the sample cup cool down before you touch it. The
sample cup can become hot during a measurement.
59
Figure 5.4 Put a sample cup in the loading position
5.2.5 Direct loading tool

The optional direct loading tool is used to load samples without cups, such as glass
disks or pressed powders. The direct loading tool puts the sample in a cup that is
located in the loading position.
The direct loading tool decreases time between measurements.

60
Figure 5.5 Direct loading tool
61
62
CHAPTER 6 USER MAINTENANCE
6.1 Introduction
Follow the safety precautions of this User Guide when you do any of these procedures.
Refer to Chapter 2.

If the system is in an unsafe condition and you go to a different room, do as
follows:
Disconnect the system from the mains power supply.
Put a warning notice on the instrument.
Remove the HT key.
To do these procedures, it can be necessary to move the instrument from its normal
operating position.
When you move the instrument back to its operating position, make sure that there is
a minimum distance of 250 mm between the wall and the sides and rear of the Zetium
in 2.4 kW to 4 kW configurations. For Zetium in 1 kW configurations, a minimum
distance of 750 mm is necessary between the wall and the sides and rear of the
instrument.
Table 6.1 Maintenance schedule
Maintenance procedure Maintenance interval Reference
Test of the safety integrity 1 year Refer to Section 6.3.

Clean the instrument When necessary Refer to Section 6.4.
Fill the cooling water system 1 year Refer to Section 6.6.
Examine the oil level of the vacuum 1 year Refer to Section 6.7.
pump
Examine the alumina pellets 6 months Refer to Section 6.8.
Replace the gas cylinder When necessary Refer to Section 6.9.1.
Replace the primary water filter 1 year Refer to Section 6.10.
Clean the dust removal device 6 months Refer to Section 6.11.
63
6.2 Use TCM5400

The TCM program is necessary for some user maintenance procedures.
6.2.1 Install TCM5400

1. In the Windows Explorer, go to C:\PANalytical\SuperQ\TCM.
2. Start 5400tcm.exe to install TCM5400.
3. In the Unzip to folder field, select the location where the TCM files must be
extracted.
4. Click Unzip.
5. Click OK.
6.2.2 Connect to the instrument with TCM5400

1. Connect a UTP cable between the PC and port X603 at the rear of the instrument.
Figure 6.1 Ports
2. Start TCM5400.exe.
3. In the Comm. Medium field, select TCP/IP Onsite.
4. Press F2 to connect to the instrument.
64
6.3 Test of the safety integrity

This test is necessary to make sure that the HT keyswitch, Xsafe and safety loops work
correctly and to move the related switches.
1. Start SuperQ.
2. Click System to start the system setup.
3. If there are samples in the turret or in the measurement chamber, unload the
samples as follows:
a. Go to System > Unload sample.
b. Remove the sample from the loading position.
c. If there is another sample in the turret, do steps a and b again.
4. Go to System > Set medium > Outside to set the medium to air. The message
Setting the medium to Outside is meant for maintenance purposes only!
This will also switch off the tube. Do you still want to set the medium to
Outside? shows.
5. Click Yes. The kV and mA settings continuously decrease.
6. When the X-ray tube is off, make sure that these lamps and indicator are off:
• X-RAYS lamps
• X-RAYS ON indicator on the control panel
• If installed, external X-RAYS ON lamp
8. Make sure that the HT ENABLED indicator on the control panel is off.
9. Turn the HT keyswitch clockwise. The HT generator must not switch on.
10. Go to System > Set medium > Vacuum to set the medium to vacuum.
13. Make sure that these lamps and indicators go on:
• HT ENABLED indicator on the control panel.
• X-RAYS lamps
• X-RAYS ON indicator on the control panel
• If installed, external X-RAYS ON lamp
65
6.4 Clean the instrument

Do not open the turrent lid. It is not permitted and it is not necessary for user
maintenance.
1. Clean the outer side of the instrument with a moist cloth.

2. Clean the sample loading opening, the sample cup and the sample cup inserts
with a clean dry brush or with a vacuum cleaner.

If a pressed powder sample breaks or a liquid sample leaks in the
measurement chamber or the optical path, immediately switch off the
instrument. Do not clean the contaminated parts. A Malvern Panalytical service
engineer must clean the measurement chamber and the optical path.
6.5 Remove the panels
WARNING ‑ Electrical Hazard

Be careful when you remove the panels. When the instrument is connected to
the mains power supply, parts can be live.
The panels are attached with Torx screws at the top of each panel. Refer to Figure 6.2.
These screws are located in identical positions for all panels.
1. Loosen the Torx screws.

2. Turn the panel away from the top of the instrument.
3. Lift the panel up to remove it.
The sample changer plate must only be removed by Authorized Personnel.
66
Figure 6.2 Front panel screws
6.6 Fill the cooling system

The cooling system is a closed-loop system that uses deionized water to cool the
anode of the X-ray tube. The system has these main parts:
• Water pump
• Water treatment unit
• Radiator (for Zetium in 1 kW configurations)
• Heat exchanger (for Zetium in 2.4 kW to 4 kW configurations)
67
10
8 2
7
4
1. Water filler cap 6. Water reservoir

2. Rotary flow meter 7. Filter container
3. Level switch 8. Deionizing material
4. Conductivity probe 9. Deionizing material container
5. Water IN/OUT 10. Plastic rings
Figure 6.3 Water treatment unit
1. Press the OFF button to switch off the instrument.

2. Disconnect the instrument from the mains power supply.
3. Remove the left panel.
4. Loosen, but do not remove, the retaining bolt that holds the water treatment unit
in position.
68
Figure 6.4 Retaining bolt of the water treatment unit
5. Turn the water treatment unit out of the instrument.

6. Remove the water filler cap.
Figure 6.5 Water filler cap
7. Put a small funnel into the filler opening.

8. Fill the water reservoir with deionized water.
69
Figure 6.6 Fill the water reservoir
9. Put the water filler cap back in position.

10. Put the water treatment unit back in position.
11. Tighten the retaining bolt.
12. Install the left panel.
6.7 Examine the oil level of the vacuum pump

If the oil is dirty or contains white foam, replace the old oil.
70
1. Level indicator 3. Drain plug

2. Filler cap
Figure 6.7 Vacuum oil pump

3. Remove the front panel.

The vacuum pump and the tray can be hot. Let it cool down before you touch it.
4. Loosen, but do not remove, the retaining bolt from the vacuum pump plate.
71
Figure 6.8 Location of the retaining bolt
5. Turn the plate out of the instrument to a position where you can see the oil level
window.
Figure 6.9 Oil level window in view
6. Make sure that the oil level is between the low and high marks.
7. If the vacuum oil is dirty or contains white foam, drain the vacuum oil as follows:
a. Put a container under the drain.
b. Remove the drain plug.
c. Collect the vacuum oil.
d. Discard the vacuum oil. Refer to local regulations.
8. If the oil level is beneath the low mark or if you have drained the oil, fill the
vacuum pump with oil as follows:
a. Remove the filler cap.
72
b. Put a funnel in the filler opening.

c. Fill the vacuum pump with oil until the oil is at the high mark of the oil level
window.
Figure 6.10 Funnel in the filler opening
9. Put the filler cap back in position.

10. Put the vacuum pump plate back in position.
11. Tighten the retaining bolt.
12. Install the front panel.
6.8 Examine the alumina pellets

1. Set the medium to air.
3. For Zetium in 1 kW configurations, remove the front panel.
4. For Zetium in 2.4 kW to 4 kW configurations, remove the right panel.
5. Remove the black plastic ring of the foreline trap.
73
Figure 6.11 Black plastic ring
6. Remove the spring.

7. Remove the basket with alumina pellets.
Figure 6.12 Remove the basket with alumina pellets
74
8. Loosen the wing nut.

9. Remove the lid of the basket.
10. Examine the alumina pellets. The alumina pellets must be white. If the alumina
pellets are brown, do as follows:
a. Remove the alumina pellets from the basket.
b. Put new alumina pellets in an ovenproof bowl.
c. Heat the new alumina pellets in an oven at 100 °C for approximately 1 hour.
NOTE: When you heat the alumina pellets in the oven before you put them in
the instrument, it makes the vacuum better. If an oven is not available,
continue with step e.

Wear protection or use a tool when you remove the alumina pellets from the
oven. The alumina pellets and the bowl will be hot.
d. Take the alumina pellets out of the oven.

e. Put the new alumina pellets in the basket.
11. Assemble the basket.
12. Put the basket in the foreline trap.
13. For Zetium in 1 kW configurations, install the front panel.
14. For Zetium in 2.4 kW to 4 kW configurations, install the right panel.
16. Start TCM5400.exe.
17. Connect to the instrument.
18. Go to Printed circuit > spEctrometer cards and APC's to open the Analog
sensor inputs form.
19. Press F9 to go to the general menu.
20. Press F2 to change the medium.
21. Press F2 again to set the medium to vacuum and examine the VACANA value.
The value must decrease continuously.
6.9 Maintain the gas systems

As standard, the Zetium instrument has a detector flow gas system. It can also have an
optional helium/nitrogen flushing gas system for the measurement chamber.
With this gas system, you can measure loose powders or liquid samples.
75
6.9.1 Replace the cylinder of the detector flow gas

NOTE: Do this procedure when the gas cylinder is empty.

The gas cylinder must be attached to the wall or in a suitable holder. A full
cylinder can have a pressure of up to 18 MPa and can explode if the cylinder
falls.

If gas lines from the cylinder to the instrument are on the floor, put protection
over the gas lines to prevent damage.
When the pressure in the detector flow gas cylinder is too low, the gas pressure sensor
does not work. This breaks the safety loop and prevents instrument operation.
You can use the same procedure to replace a helium or nitrogen gas cylinder, but
there are some differences:
• The pressure regulator is different.

• The connection nut of the pressure regulator has a right thread.
• The system flushes automatically.
NOTE: If you put the gas cylinder inside a room, make sure that the gas cylinder is at
room temperature before you connect it to the instrument.
76
2 1
2
3
6 7 8
1. Main valve of the gas cylinder 5. Output pressure outlet
2. Gas cylinder pressure gauge 6. Reduction valve
3. Flush valve 7. Overpressure relief valve
4. Output pressure gauge 8. Connection nut
Figure 6.13 Pressure regulator
1. Start the analytical software.

3. Turn the reduction valve (6) counter-clockwise to close it.
4. Turn the main valve of the gas cylinder (1) clockwise to close it.
5. Turn the connection nut (8) a small turn clockwise to remove the remaining
pressure, then loosen it completely.
6. Remove the pressure regulator from the gas cylinder.
7. Put the protective nut on the output connection of the gas cylinder.
8. Put the domed cover on the gas cylinder.
9. Remove the domed cover of the new gas cylinder.
10. Remove the protective nut from the output connection of the new gas cylinder.
11. Make sure that the outlet of the new gas cylinder points in a safe direction.
12. Quickly open and close the main valve of the new gas cylinder a small turn. This
blows out dust particles in the gas cylinder connection.
13. Connect the pressure regulator to the new gas cylinder as follows:
a. Put a new washer inside the connection nut.
77
Figure 6.14 Washer
b. Connect the pressure regulator to the gas cylinder and turn the connection
nut counter-clockwise.
c. Use 2 wrenches to tighten the connection nut and to make sure that the
pressure regulator does not turn.
Figure 6.15 Tighten the connection nut
14. If the flush valve (3) is installed, turn it clockwise to close it.
15. Open the main valve of the detector flow gas cylinder. The gas cylinder pressure
gauge must show a pressure of approximately 20 MPa.
16. If the flush valve is installed, flush the pressure regulator as follows:
a. Open the flush valve.
78
b. Keep the flush valve open for 2 seconds to flush the pressure regulator.
c. Close the flush valve.
17. Do a leakage test of the gas system. Refer to Section 6.9.2.
If there is no leak, continue with the next step.
18. Slowly open the reduction valve of the detector flow gas cylinder until the output
pressure gauge (4) shows a pressure of 0.08 MPa.
19. Set the medium to vacuum.
20. Do a test of the PHD on all flow detectors. Refer to Section 6.9.3.
6.9.2 Leakage test of the gas system

Do a leakage test of the gas system each time a gas cylinder is connected to the
instrument.
1. Close the main valve of the gas cylinder.

2. Close the reduction valve.
3. Slowly open the main valve of the gas cylinder.
4. Write down the pressure value.
5. Close the main valve of the gas cylinder.
6. Keep the main valve of the gas cylinder closed for approximately 30 minutes.
7. After approximately 30 minutes, compare the pressure value with the pressure
value of step 4.
If the pressure value is the same, there is no leak.
If the pressure has decreased, there is a leak in the connection between the gas
cylinder and the pressure regulator. Repair the leak.
6.9.3 PHD test of the flow detector

Because detector gases have different qualities, the PHD on flow detectors can change
position. After you change the gas cylinder of the detector flow gas, you must do a PHD
test on all flow detectors. If necessary, you must adjust the detector HV.
NOTE: This procedure is very generic. If you are not sure how to do this procedure,
contact your local service organization for support.
1. Identify the flow detectors:

a. Start SuperQ.
b. Click System to start the system setup.
c. Go to System > Configuration > Spectrometer configuration.
d. Go to tab Fixed channel(s).
79
e. Write down the channel numbers with a flow detector.

2. Start TCM5400.exe. Refer to Section 6.2.2.
3. Do a PHD test for each channel with a flow detector as follows:
a. Put a sample in the instrument.
b. Go to Detector check.
Figure 6.16 Check Detector form
4. Press F9 to go the the general menu.

5. Press F1 to load the sample.
6. In the P. Sh. Corr. field, select No.
7. In the Type/No. field, enter the number of a channel with a flow detector.
8. Press F1 to do a measurement. The Current [kcps] value must be
approximately 20.000 kcps.
If the value is not approximately 20.000 kcps, do as follows:
a. Adjust the kV, mA settings.
b. Do the PHD measurement again.
9. Make sure that the peak position stays on position 50 ± 1.
If the peak position is not on position 50 ± 1, adjust the detector HV until the peak
is at the correct position:
• To shift the peak position to the right, increase the value of Detector HV.
• To shift the peak position to the left, decrease the value of Detector HV.
80
10. If you want to measure the next channel with a different sample, unload the
sample.
11. Do steps 3 to 10 again for all channels.
12. When you have changed the detector HV setting, measure the available
instrument monitors with SuperQ.
6.10 Replace the primary water filter

This procedure is only for Zetium in 2.4 kW to 4 kW configurations.
The water filter of the cooling system is in the blue holder that is attached to the wall
near the instrument. When the water flow rate becomes too low, the water filter must
probably be replaced. If the water quality is not good, the filter must be replaced more
frequently.
If the water flow rate becomes too low, the safety loops break. This switches off the HT
generator and shows an error message on the screen.

4. Close the mains water supply at the wall tap.
5. Put a container under the water filter assembly to collect the water.
6. Press the red bleed button on top of the blue holder to remove the remaining
water pressure.
7. Turn the blue holder counter-clockwise to remove it from its bracket.
8. Lift the water filter out of the holder.
9. If loose contamination causes a blockage of the filter, put the holder in a strong
jet of water to clean it.
10. Put the cleaned filter or a new filter into the holder.
11. Install the blue holder in the bracket.
12. Open the mains water supply.
13. Press the red bleed button on top of the blue holder until the water starts to flow
from it.
14. Make sure that there are no leaks.
81
6.11 Clean the dust removal device

3. Remove the front panel.
4. Remove the nut of the dust removal device.
Figure 6.17 Remove the nut of the dust removal device
5. Remove the clamp.

6. Remove the dust container.
7. Clean the dust container.
8. Install the dust container.
82
6.12 Consumable materials

Table 6.2 Consumable materials for maintenance
Quantity Description Ordering code
4L Ultragrade 19 vacuum oil 5322 390 10135

1L Ultragrade 19 vacuum oil 5322 390 10098
1 O-ring between X-ray tube and optical path 5322 530 54662
1 Paper filter for water circuit (for Zetium in 2.4 kW to 4 kW 5322 480 54034
configurations only)
1 Alumina pellets 5322 390 84003
83
84
CHAPTER 7 TROUBLESHOOTING
7.1 Introduction
This chapter gives the most common problems with the system and their solutions.
If a problem is not in this chapter, or if the solution did not remove it, collect all relevant
information about the problem and contact your local Malvern Panalytical service
organization. Also refer to the Spectrometer status screen in SuperQ for more
information about the status of the system.
If possible, a Malvern Panalytical service engineer uses remote support to find a

solution for the problem. During a remote support session, your aid can be necessary.
If a remote support session did not remove the problem, a service visit can be
necessary.
7.2 Instrument is off-line

When the instrument is off-line, you cannot make a connection between the
instrument and the PC.
Table 7.1 Possible causes for instrument is off-line
Cause Solution Reference
The instrument is not switched Switch on the instrument. Refer to Section 4.2.
on (POWER OFF indicator is
on).
The UTP cable is not in port Put the UTP cable in port Refer to Figure 6.1.
X601. X601.
Incorrect port setting in Enter the correct port Refer to SuperQ Help
SuperQ. settings.
A fuse has blown. Contact your local
Malvern Panalytical
representative.
Xsafe is activated. Reset Xsafe. Refer to Section 7.2.1.
7.2.1 Reset Xsafe

NOTE: The Zetium has no visual indication of the Xsafe status.
When you think that the Xsafe system is activated, do as follows:
85

3. Switch on the instrument. Refer to Section 4.2.
7.3 HT generator does not switch on

If the HT generator does not switch on, there is usually a problem in the HT safety
circuit.
Table 7.2 Possible causes for HT generator does not switch on
Cause Solution Reference
HT keyswitch is in the OFF position (HT Turn the HT keyswitch Refer to Section 3.3.4.
ENABLED indicator is off). clockwise.
A fuse has blown. Contact your local
Malvern Panalytical
representative.
The water flow stopped during a 1. Make sure that the Refer to Section 6.10.
measurement, or the water flow is less chiller unit is Refer to the Tube
than 3 L/min (for Zetium in 2.4 kW to switched on and is Instruction Manual
4 kW configurations only) filled with water.
2. Make sure that the
water hoses are not
compressed and do
not have kinks.
3. Clean or replace the
water filters.
Medium is in air. Set the medium to Refer to SuperQ Help
vacuum.
The cylinder of the detector flow gas is Replace the cylinder of the Refer to Section 6.9.1.
empty. detector flow gas.
1 or more of the X-RAYS lamps is
defective:
• X-RAYS ON indicator on the Contact your local
control panel. Malvern Panalytical
service organization.
• 2 or more of the X-RAYS lamps on Contact your local
the corners of the instrument. Malvern Panalytical
service organization.
• External X-RAYS ON lamp. Contact your local
Radiation Safety Officer.
Xsafe is activated. Reset Xsafe. Refer to Section 7.2.1.
86
7.4 No remote support connection

Remote support via internet is done with TCP/IP through port X602 at the rear of the
instrument. If there is no remote support connection, contact your local
Malvern Panalytical service organization.
7.5 Sample changer alignment is incorrect

If the gripper arms of the sample changer do not pick up the sample cups correctly, or
if the sample cups are put in the wrong positions, the sample changer alignment can
be incorrect. You must calibrate the sample changer. Refer to Section 7.5.1.
7.5.1 Calibrate the sample changer

Do this procedure with 1 or more cup trays. Do NOT use other trays than cup trays.
1. In Windows Explorer, go to C:\PANalytical\SuperQ\Changer.

2. Start PW4400ChangerMaintenanceTool.exe.
3. Click Connect and Open Maintenance.
4. Select the override safety check box.
6. Put a sample cup in the gripper.
7. For the Cement edition of Zetium, do as follows:
a. Put trays on position A, B and D. If only 1 tray is available, put the tray on
position A and move the tray manually during the procedure.
b. In the Plate field, select Tray A-E.
8. For other instruments, do as follows:
a. Put trays on position A, E and F. If only 1 tray is available, put the tray on
position A and move the tray manually during the procedure.
b. In the Plate field, select Tray A-H.
9. Click Calibrate.
10. Calibrate the position. Use these buttons until the sample cup is in the correct
position:
• Use the left arrow set to move the gripper arm.
• Use the right arrow set to lift or lower the gripper arm.
• Use the Open and Close buttons to make sure that the gripper takes and
releases the sample cup correctly.
• Use the mm field to set the distance of the movements.
11. Click Next.
87
12. Do steps 10 and 11 again for the second tray.

13. Do step 10 again for the third tray.
14. Click Finish.
15. In the Plate field, select Load position.
16. Click Calibrate.
17. Do step 10 again.
18. Click Finish.
19. Remove the sample cup from the gripper.
20. If 1 or 2 steel ring inverters are installed, do as follows:
a. Put a steel ring in the gripper.
b. In the Plate field, select the correct inverter.
c. Click Calibrate.
d. Do step 10 again.
e. Click Finish.
f. If 2 steel ring inverters are installed, do steps b to e again.
g. Remove the steel ring from the gripper.
21. If the direct loading tool is installed, do as follows:
a. Put the direct loading tool in the gripper.
b. In the Plate field, select Direct loading tool.
c. Click Calibrate.
e. Click Finish.
f. Remove the direct loading tool from the gripper.
22. If small spot mapping is installed, do as follows:
a. Put a sample cup for small spot mapping in the camera position.
b. In the Plate field, select Camera position.
c. Click Calibrate.
e. Click Finish.
f. Remove the sample cup for small spot mapping from the camera position.
88
CHAPTER 8 DISPOSAL INSTRUCTIONS
8.1 WEEE Directive

The instrument complies with the WEEE Directive (Waste of Electrical and Electronic
Equipment), identified by this alert symbol on the instrument:
Figure 8.1 WEEE directive alert symbol
The function of the European WEEE Directive is to decrease the quantity of waste from
electrical and electronic equipment, and to decrease the hazardous substances of this
waste to protect human health and the environment.
8.2 Hazardous substances

When you dispose of hazardous materials, obey all applicable and local regulations to
prevent damage to the environment. You can also send the hazardous materials back
to Malvern Panalytical for disposal. Use a recorded shipping method.
On the instrument, the hazardous materials are identified with a label. Refer to Figure
2.1.
If you are not sure about the correct disposal procedure, contact your local
Malvern Panalytical representative.
8.2.1 Beryllium
Some items in the instrument contain beryllium (Be).

Beryllium is poisonous. Do not touch or breathe in beryllium.
For more information, refer to the toxic material section in the Safety chapter.
89
Refer to the Safety Data Sheet for the disposal procedure: (https://uqr.to/
epa4).
8.2.2 Lead
Lead (Pb) is used as a protection material against X‑rays.

Lead is poisonous. Do not touch or breathe in lead.
For more information, refer to the toxic material section in the Safety chapter.
Refer to the Safety Data Sheet for the disposal procedure: (https://uqr.to/
i8t3).
8.2.3 X-ray tube

The windows of the SST R, SST R-mAX and SST R-mAX50 X-ray tubes contain beryllium
(Be). The X-ray tubes contain lead (Pb).
For disposal instructions, refer to the Tube Instruction Manual supplied with the X-ray
tube.
8.2.4 Detector
The flow detector, sealed Xe gas detector (installed as duplex), scintillation detector,
HiPer Scint detector and SDD contain beryllium (Be).
NOTE: If the flow detector is used as part of a duplex detector, it does not contain
beryllium.
90
Figure 8.2 Flow detector in measurement chamber - beryllium coating
Figure 8.3 Flow detector on a measurement channel - beryllium coating
91
Figure 8.4 Sealed Xe gas detector as part of a duplex detector - beryllium plate inside
Figure 8.5 Scintillation/HiPer Scint detector - beryllium window
92
Figure 8.6 Silicon drift detector in the ED core - beryllium window
8.2.5 Crystals
The crystal changer and measurement channels can contain toxic materials. Access to
the crystals is only for Authorized Personnel.
Refer to the Safety Data Sheet for the disposal procedure:
TlAP crystal: (https://uqr.to/epxm)
InSb crystal: (https://uqr.to/epad)
LiF crystal: (https://uqr.to/epae).
93
Figure 8.7 Crystal of a crystal changer
Figure 8.8 Crystal of a measurement channel
8.2.6 Tube filter

The WPA device contains beryllium (Be).
94
Figure 8.9 WPA device - beryllium
8.2.7 Vacuum pump

The vacuum pump contains vacuum oil.
Information on vacuum oil is supplied with the product. For disposal instructions, refer
to the Vacuum Pump Instruction Manual.
95
Figure 8.10 Vacuum pump
8.2.8 Foreline trap

The foreline trap container is filled with absorbent activated alumina pellets. These
pellets absorb vacuum oil and water vapor and make sure that it does not go in the
vacuum system.
Information on vacuum oil is supplied with the product. For disposal instructions, refer
to the Vacuum Pump Instruction Manual.
96
Figure 8.11 Foreline trap
97
98
INDEX
A D
Alerts and hazards. . . . . . . . . . . . 23, 28 Detector. . . . . . . . . . . . . . . . . . . . . . . . 48
Alerts and labels. . . . . . . . . . . . . . . . . 12 Flow detector. . . . . . . . . . . . . . . 90, 48
Alumina pellets. . . . . . . . . . . . . . . . . . 73 HiPer Scint detector. . . . . . . . . 90, 49
Analyzing crystals. . . . . . . . . . . . . . . . 47 Scintillation detector. . . . . . . . . 90, 49
Authorized personnel. . . . . . . . . . . . . 11 Sealed gas detector. . . . . . . . . . 90, 48
Direct loading tool. . . . . . . . . . . . . . . . 60
B
Disposal. . . . . . . . . . . . . . . . . . . . . . . . . 89
Beryllium. . . . . . . . . . . . . . . . . . . . . 89, 17
Beryllium. . . . . . . . . . . . . . . . . . . . . . 89
Detector. . . . . . . . . . . . . . . . . . . . . . . 90
Crystals. . . . . . . . . . . . . . . . . . . . . . . . 93
X-ray tube. . . . . . . . . . . . . . . . . . . . . 90
Detector. . . . . . . . . . . . . . . . . . . . . . . 90
Bg.. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8
Foreline trap. . . . . . . . . . . . . . . . . . . 96
C Lead. . . . . . . . . . . . . . . . . . . . . . . . . . 90
CE. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8 Vacuum pump. . . . . . . . . . . . . . . . . 95
Clean. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . WEEE Directive. . . . . . . . . . . . . . . . . 89
Dust removal device. . . . . . . . . . . . 82 X-ray tube. . . . . . . . . . . . . . . . . . . . . 90
Instrument. . . . . . . . . . . . . . . . . . . . . 66 Double independent safety loops. . 21
Collimator mask. . . . . . . . . . . . . . . . . . 46 Dust removal device. . . . . . . . . . . 82, 51
Components. . . . . . . . . . . . . . . . . . . . . 34
E
Analyzing crystals. . . . . . . . . . . . . . . 47
ED core. . . . . . . . . . . . . . . . . . . . . . . . . 50
Collimator mask. . . . . . . . . . . . . . . . 46
Emergency. . . . . . . . . . . . . . . . . . . . . . 15
Counting electronics. . . . . . . . . . . . 49
ESD. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8
Detector. . . . . . . . . . . . . . . . . . . . . . . 48
Dust removal device. . . . . . . . . 82, 51 F
ED core. . . . . . . . . . . . . . . . . . . . . . . . 50 Flow detector. . . . . . . . . . . . . . . . . 90, 48
Goniometer. . . . . . . . . . . . . . . . . . . . 49 PHD test. . . . . . . . . . . . . . . . . . . . . . . 79
HiPer channel. . . . . . . . . . . . . . . . . . 49 Foreline trap. . . . . . . . . . . . . . . . . 73, 96
HiPer small spot mapping. . . . . . . 50
G
Optical path. . . . . . . . . . . . . . . . . . . . 44
Gas systems. . . . . . . . . . . . . . . . . . . . . 75
Primary collimator. . . . . . . . . . . . . . 46
Replace gas cylinder. . . . . . . . . . . . 76
Sample position. . . . . . . . . . . . . . . . 45
Leakage test. . . . . . . . . . . . . . . . . . . 79
Small spot mapping. . . . . . . . . . . . . 50
Maintenance. . . . . . . . . . . . . . . . . . . 75
Tube filters. . . . . . . . . . . . . . . . . . . . . 45
Pressure regulator. . . . . . . . . . . . . . 77
X-ray tube. . . . . . . . . . . . . . . . . . . . . 44
Goniometer. . . . . . . . . . . . . . . . . . . . . 49
Consumable materials. . . . . . . . . . . . 83
Control panel. . . . . . . . . . . . . . . . . . . . 42 H
Cooling system. . . . . . . . . . . . . . . . . . . . . Hazard. . . . . . . . . . . . . . . . . . . . . . . . . . 15
Fill. . . . . . . . . . . . . . . . . . . . . . . . . . . . 67 Earth leakage current. . . . . . . . . . . 20
Water filter. . . . . . . . . . . . . . . . . . . . . 81 Flammable material. . . . . . . . . . . . . 19
Water treatment unit. . . . . . . . . . . . 68 Hot surface. . . . . . . . . . . . . . . . . . . . 20
Counting electronics. . . . . . . . . . . . . . 49 Ionizing radiation. . . . . . . . . . . . . . . 15
Crystals. . . . . . . . . . . . . . . . . . . 93, 19, 47 Toxic material. . . . . . . . . . . . . . . . . . 16
CSE. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8 Beryllium. . . . . . . . . . . . . . . . . . . . . . 17
CSErel, CSE%. . . . . . . . . . . . . . . . . . . . . . 8
99
INDEX
Lead. . . . . . . . . . . . . . . . . . . . . . . . . . 18 Replace. . . . . . . . . . . . . . . . . . . . . . . . . . . .
Hazardous substances. . . . . . . . 89, 16 Gas cylinder. . . . . . . . . . . . . . . . . . . . 76
HiCap sample changer. . . . . . . . . . . . 51 Replace gas cylinder. . . . . . . . . . . . 76
HiPer channel. . . . . . . . . . . . . . . . . . . . 49 Water filter. . . . . . . . . . . . . . . . . . . . . 81
HiPer Scint detector. . . . . . . . . . . 90, 49 Reset. . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
HiPer small spot mapping. . . . . . . . . 50 Xsafe. . . . . . . . . . . . . . . . . . . . . . . . . . 85
HT. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8 RMS. . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8
HT generator. . . . . . . . . . . . . . . . . . . . . . .
S
Does not switch on. . . . . . . . . . . . . 86
Safety aspects. . . . . . . . . . . . . . . . . . . 11
HT indicator. . . . . . . . . . . . . . . . . . . . . 43
Safety class. . . . . . . . . . . . . . . . . . . . . . . 8
HT keyswitch. . . . . . . . . . . . . . . . . 20, 43
Safety guarantee. . . . . . . . . . . . . . . . . 11
I Safety integrity test. . . . . . . . . . . . . . . 65
Installation category. . . . . . . . . . . . . . . 8 Safety measures. . . . . . . . . . . . . . . . . 20
INSTANT POWER OFF button. . . 20, 43 Safety standards. . . . . . . . . . . . . . . . . 12
Instrument is off-line. . . . . . . . . . . . . 85 Sample changer. . . . . . . . . . . . . . . . . . 51
Direct loading tool. . . . . . . . . . . . . . 60
L
Sample cups. . . . . . . . . . . . . . . . . . . 58
Lead. . . . . . . . . . . . . . . . . . . . . . . . . 90, 18
Sample trays. . . . . . . . . . . . . . . . . . . 57
LIGHT ON indicator. . . . . . . . . . . . . . . 43
Alignment incorrect. . . . . . . . . . . . . 87
LLD. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8
Calibrate. . . . . . . . . . . . . . . . . . . . . . . 87
M Layout. . . . . . . . . . . . . . . . . . . . . . . . 57
Maintenance schedule. . . . . . . . . . . . 63 Sample cups. . . . . . . . . . . . . . . . . . . . . 58
Measurement overview. . . . . . . . . . . 55 Sample loading. . . . . . . . . . . . . . . . . . 55
Medium. . . . . . . . . . . . . . . . . . . . . . . . . 51 Direct loading tool. . . . . . . . . . . . . . 60
Motion safety. . . . . . . . . . . . . . . . . . . . 21 Sample cups. . . . . . . . . . . . . . . . . . . 58
Sample trays. . . . . . . . . . . . . . . . . . . 57
O Automatic loading. . . . . . . . . . . . . . 55
OFF button. . . . . . . . . . . . . . . . . . . . . . 42 Manual loading. . . . . . . . . . . . . 55, 58
ON button. . . . . . . . . . . . . . . . . . . . . . . 42 Sample position. . . . . . . . . . . . . . . . . . 45
ON/OFF button. . . . . . . . . . . . . . . . . . 43 Scintillation detector. . . . . . . . . . 90, 49
Optical path. . . . . . . . . . . . . . . . . . . . . 44 Sealed gas detector. . . . . . . . . . . 90, 48
Skill levels. . . . . . . . . . . . . . . . . . . . . . . . 7
P
Application engineer. . . . . . . . . . . . . 8
PHD. . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8
Operator. . . . . . . . . . . . . . . . . . . . . . . 7
PHD test. . . . . . . . . . . . . . . . . . . . . . . . 79
System engineer. . . . . . . . . . . . . . . . . 8
Ports. . . . . . . . . . . . . . . . . . . . . . . . . . . 64
Small spot mapping. . . . . . . . . . . . . . 50
POWER OFF indicator. . . . . . . . . . . . . 42
Smart Manager. . . . . . . . . . . . . . . . . . 52
POWER ON indicator. . . . . . . . . . . . . 42
Spectrometer status screen. . . . 54, 85
Pressure regulator. . . . . . . . . . . . . . . 77
Switch off instrument. . . . . . . . . . . . . 54
Primary collimator. . . . . . . . . . . . . . . . 46
Switch on instrument. . . . . . . . . . . . . 53
PTB. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8
T
Q
TCM. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
Qualified service engineer. . . . . . . . . . 8
Connect. . . . . . . . . . . . . . . . . . . . . . . 64
R Install. . . . . . . . . . . . . . . . . . . . . . . . . 64
R. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8 TCM5400. . . . . . . . . . . . . . . . . . . . . . 64
Radiation level. . . . . . . . . . . . . . . . . . . . 8 Tube filters. . . . . . . . . . . . . . . . . . . . . . 45
Remote support. . . . . . . . . . . . . . . . . 87
U
Remove the panels. . . . . . . . . . . . . . . 66
User responsibilities. . . . . . . . . . . . . . 14
100
INDEX
V
Vacuum oil. . . . . . . . . . . . . . . . 70, 95, 96
Vollschutz. . . . . . . . . . . . . . . . . . . . . . . . 8
W
Water filter. . . . . . . . . . . . . . . . . . . . . . 81
Water treatment unit. . . . . . . . . . . . . 68
WEEE Directive. . . . . . . . . . . . . . . . . . . 89
X
X-ray tube. . . . . . . . . . . . . . . . . . . . . . . 44
X-RAYS lamps. . . . . . . . . . . . . . . . . . . . 20
Xsafe. . . . . . . . . . . . . . . . . . . . . . . . 85, 21
101

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ZETIUM

EDITION NOTICE: 4023 000 43228, September 2021

Malvern Panalytical Ltd. Malvern Panalytical B.V.

Tel. +44 1684 892456 Tel. +31 546 534 444

2.7 Safe use of the instrument. . . . . . . . . . . . . . . . . . . . . . . . . . . . . 21

Chapter 3. System description. . . . . . . . . . . . . . . . . . . . . . . . . . 33

Chapter 4. Operate the instrument. . . . . . . . . . . . . . . . . . . . . . 53

4.2 Switch on the instrument. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 53

Chapter 5. Measure samples. . . . . . . . . . . . . . . . . . . . . . . . . . . . 55

Chapter 6. User maintenance. . . . . . . . . . . . . . . . . . . . . . . . . . . 63

7.2.1 Reset Xsafe. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 85

Chapter 8. Disposal instructions. . . . . . . . . . . . . . . . . . . . . . . . 89

• 9430 054 00101 Zetium (1 kW configuration)

1.2 Intended use

1.3 Recommended skill levels

The skill levels are:

• Does not need in-depth knowledge of X-ray theory or applications.

• Must be able to follow instructions on how to measure samples using applications

• Must have a thorough knowledge of the analysis process.

1.4 Glossary of terms and abbreviations

Term or abbreviation Description

PTB Physikalisch-Technische Bundesanstalt. An independent test

2.1 Introduction to safety aspects

2.1.1 Authorized personnel

2.1.2 Safety guarantee

WARNING ‑ General Hazard

2.1.3 Alerts and labels

Alerts in this manual are shown as follows:

DANGER ‑ Electrical Hazard

(The symbol relates to the specified hazard)

WARNING ‑ Ionizing Radiation

(The symbol relates to the specified hazard)

CAUTION ‑ General Hazard

(The symbol relates to the specified hazard)

2.2 Safety standards

Refer to the applicable standards, normative documents and directives in the

This product is certified by MET Laboratories to meet these standards:

• CSA C22.2 No. 61010-1 - 2012

2.3 Malvern Panalytical's approach

• Specification of the worldwide lowest radiation level: less than 1 µSv/h at 10 cm

2.4 User responsibilities

2.4.1 What to do in case of an emergency

NOTE: If there is an X‑ray exposure incident, calculation of the absorbed dose is

2.5 General hazards

2.5.1 Ionizing radiation

WARNING ‑ Ionizing Radiation

Obey local safety regulations.

2.5.2 Toxic material

Some analyzing crystals can contain poisonous materials.

For more information, refer to the Safety Data Sheets.

Figure 2.1 Hazardous substances label

Some items in the instrument contain beryllium (Be).

WARNING ‑ Toxic Material

Do not touch, swallow or breathe in beryllium.

Disposal of beryllium must obey all applicable local regulations.

Safety Data Sheet: (https://uqr.to/epa4)

Lead (Pb) is used as a protection material against X‑rays.

WARNING ‑ Toxic Material