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SPECTRO XEPOS

Benchtop XRF Spectrometer

Original operating instructions

Table of Contents
1  Description of instrument .................................................................................... 5 
1.1  Description .......................................................................................................................... 5 
1.2  Function .............................................................................................................................. 5 
1.3  Overview ............................................................................................................................. 6 
1.3.1  Configuration ......................................................................................................... 6 
1.3.2  Instrument (front) ................................................................................................... 7 
 Opening and closing the sample chamber lid ....................................................... 8 
1.3.3  Instrument (back)................................................................................................... 9 
1.3.4  Sample chamber ................................................................................................. 10 
1.3.5  Sample chamber - additional components .......................................................... 11 
1.3.6  Sample tray ......................................................................................................... 11 

2  Safety................................................................................................................ 12 
2.1  Symbols used ................................................................................................................... 12 
2.2  User information................................................................................................................ 13 
2.3  Intended use ..................................................................................................................... 13 
2.4  Prohibited operating conditions ........................................................................................ 14 
2.5  Residual risks.................................................................................................................... 14 
2.6  Radiation protection advice .............................................................................................. 16 
2.6.1  Other countries .................................................................................................... 16 

3  Technical data................................................................................................... 17 

4  Transportation/Setting-up ................................................................................. 18 

4.1  Storage ............................................................................................................................. 19 
4.2  Gas supply (optional) ........................................................................................................ 19 
4.3  Vacuum (option)................................................................................................................ 20 
4.4  Uninterruptible power supply – UPS (option) ................................................................... 21 

5  Operation .......................................................................................................... 23 

5.1  Displays ............................................................................................................................ 23 
5.1.1  Screen – Routine dialog ...................................................................................... 23 
5.1.2  Beam Stop display on the instrument.................................................................. 24 
5.2  Switching on the instrument .............................................................................................. 25 
5.3  Proceed with the start-up test ........................................................................................... 27 
5.3.1  Checking the safety circuits on the sample chamber lid ..................................... 27 
5.3.2  Checking the safety circuit on the filter changer ("Beam Stop").......................... 28 
5.3.3  Initialization of the stepping motors ..................................................................... 29 
5.3.4  Automatic verification of the safety circuits after one month ............................... 30 
5.4  Switching off the instrument .............................................................................................. 31 
5.5  Standby mode ................................................................................................................... 32 
5.6  Measuring procedure ........................................................................................................ 33 
5.6.1  Preparing the measuring procedure .................................................................... 33 
 How to measure different samples ...................................................................... 34 

SPECTRO XEPOS — 19.01.2017 —3

  How to measure cuvettes (powder or liquid) ....................................................... 34 
 How to measure powder pallets .......................................................................... 35 
 How to measure glass or melting pellets ............................................................. 35 
 How to measure large samples ........................................................................... 36 
5.6.2  Proceed with the measurement ........................................................................... 37 
 How to change/remove the sample tray .............................................................. 38 
5.7  Dust protection shutter / beam stabilization vacuum shutter (option) ............................... 39 
 Dust protection shutter......................................................................................... 39 
 Beam stabilization vacuum shutter ...................................................................... 39 

6  Maintenance by the operator ............................................................................ 40 

6.1  Operator maintenance plan............................................................................................... 40 
6.2  Energy channel recalibration (MCA) ................................................................................. 42 
6.3  Standardization (Global recalibration)............................................................................... 43 
6.4  Clean the sample tray ....................................................................................................... 44 
6.5  Clean the sample chamber ............................................................................................... 44 
6.6  Replacing the adhesive film in the discharge reservoir .................................................... 45 
6.7  Replacing the tray pads .................................................................................................... 46 
6.8  Insert the film for the "liquid protect" sample cup .............................................................. 47 
6.9  Replacing the filter mat ..................................................................................................... 49 
6.10  Dust protection shutter / beam stabilization vacuum shutter (option) — Clean O-ring ..... 50 
6.11  Troubleshooting ................................................................................................................ 51 

7  Spare parts and consumables .......................................................................... 55 

8  De-commissioning ............................................................................................ 55 

9  Manufacturer address ...................................................................................... 55 

—4 SPECTRO XEPOS — 19.01.2017

 Description of instrument

1 Description of instrument

1.1 Description
Designation: SPECTRO XEPOS
Model: XEP05
Type: 76004852

1.2 Function
X-rays excite the atoms of the sample, causing them to emit radiation. This
radiation is measured by a semiconductor detector.
To achieve a higher sensitivity, the exciting radiation can be optimized by using X-
ray optical elements or filters.
The instrument comes with a prepared analysis method. Data are already stored
in the instrument's memory. The measured values are compared with these data.
After the measurement is complete, the results of a sample relating to an unknown
composition are displayed on the screen.
The sample material may be solid, liquid or in powder form, see Chapter "How to
measure different samples".

SPECTRO XEPOS — 19.01.2017 —5

Description of instrument

1.3 Overview

1.3.1 Configuration
The instrument is available in various configurations. Depending on the
application/requirement, the instrument is equipped with the following X-ray optics:
 Direct excitation
 Direct excitation and single polarization channel
 Direct excitation and dual polarization channel

Depending on the application / requirement, the following expansions are

available:
 Sample spinner
 Helium flushing
 Vacuum pump
 Active pile-up suppression
 Dust protection shutter / beam stabilization vacuum shutter

—6 SPECTRO XEPOS — 19.01.2017

 Description of instrument

1.3.2 Instrument (front)

3 3

Fig. 1: Front view

No. Component

1 Sample chamber lid

2 Ventilation slots with filter mat

3 Beam stop display Open/closed (Open = red/closed = green)

X-ray display On/Off (On = orange/Off = off),
see also Chapter 5.1.2.

SPECTRO XEPOS — 19.01.2017 —7

Description of instrument

Opening and closing the sample chamber lid

Caution! Risk of crushing injuries!

When closing the sample chamber lid, there is an inherent risk of crushing injuries.
 When closing the sample chamber lid keep the fingers out of the sample
chamber.

1 2

Fig. 2

No. View

1 Sample chamber lid closed

2 Sample chamber lid open

When pressing slightly against the handle, the sample chamber lid can be pushed
back and locked into place. In order to open the cover, slightly press against the
handle and pull on the sample chamber lid.

—8 SPECTRO XEPOS — 19.01.2017

 Description of instrument

1.3.3 Instrument (back)

3 4 5 6 7
Fig. 3: Rear view

No. Component No. Component

1 Type plate with serial number, 5 Power supply connection for

date of production, max. vacuum pump (1000 W max.)
parameters of the X-ray tube

2 PC/Ethernet conviction (using the 6 Power In (max. 1200 W)

LAN cable included in delivery)

3 Helium supply line connection 7 Key-operated switch On/Off

4 Vacuum hose connection

Note
Set up the instrument to ensure the power isolators (switches and power cable)
can be easily reached.

SPECTRO XEPOS — 19.01.2017 —9

Description of instrument

1.3.4 Sample chamber

3
5
4

Fig. 4

No. Component

1 Sample tray locking device

2 Sample tray (different models available)

3 Analysis position (position of the sample during the measurement)

4 Tray handle

5 Tray screw

— 10 SPECTRO XEPOS — 19.01.2017

 Description of instrument

1.3.5 Sample chamber - additional components

3
2 4

5
6

Fig. 5

No. Component

1 Sample tray support

2 Discharge reservoir

3 Sample spinner drive (optional)

4 Dust protection shutter or beam stabilization vacuum shutter (optional)

5 Active pile-up suppression (optional)

6 Tray pad (3 pcs. Installed inside)

7 Tray pad rotation tray (7 pcs., installed outside)

Single sample rotation unit (optional), (not shown for clarity)

1.3.6 Sample tray

The sample trays come in different versions.
 12 sample positions for Ø 40 mm samples with an adapter for Ø 32 mm
samples
 25 sample positions for Ø 20 mm samples
 8 sample positions for rotating samples for Ø 40 mm samples or
6 sample positions for rotating Ø 52 mm samples

SPECTRO XEPOS — 19.01.2017 — 11

Safety

2 Safety
Every user of the instrument must have understood these operating instructions.
This applies in particular to the safety regulations.

2.1 Symbols used

The following symbols are used in these abbreviated operating instructions and/or
on the instrument.
If required, additional important information is available in connection with these
symbols.

Caution! Risk of injury!

Danger! Risk of electric shock!

Caution! Fire hazard!

Caution! Danger of poisoning!

Caution! Risk of crushing injuries!

Caution! Ionizing radiation!

Notice!
Warns of activities or conditions that may adversely affect the safety or function of
the instrument.

Note
Displays information that is important for the correct and safe use of the instrument

— 12 SPECTRO XEPOS — 19.01.2017

 Safety

2.2 User information

 Compliance with all safety instructions is mandatory. It's for your own safety.
 Carry out only operator maintenance work that is described in chapter 6. The
operating personnel is not permitted to proceed with any other maintenance
work. Any further services (e.g. technical maintenance) or repairs must only
be performed by service personnel that are authorized by the manufacturer.
 Comply with all safety instructions and accident prevention regulations at all
times while operating and maintaining the instrument. This regulation is, for
example, DIN EN 61010 or any other comparable national standard.
 The safety measures must be checked following every technical maintenance
or repair activity. This check must be performed according to VBG4/DIN EN
61010 or a comparable national standard.
 Compliance with the maintenance schedule specified by the manufacturer is
mandatory, All maintenance activities must be recorded. This will maintain the
operational safety of the instrument.
 Never tamper with the safety devices! If you feel that a safety device does not
work properly, shut down the instrument immediately! Please contact your
Service Center.
 Only genuine spare parts must be used when repairing the instrument. The
use of non-genuine spare parts will make the CE Declaration of Conformity
null and void.
 The instrument may only be connected to the power supply with a protective
grounding conductor.
 If an instrument is positioned on a sloped surface, it may roll away during the
operation. Secure the instrument while in operation. This applies also when
the instrument is being transported.
 Compliance with the relevant safety regulations when using tools and
operating equipment is mandatory.
 Compliance with the safety instructions when handling and preparing the
samples (material safety data sheet) is mandatory. The contact with certain
metals, plastics, powders, liquids, or other materials can be hazardous to
health.

2.3 Intended use

The spectrometer must only be used to analyse liquid substances or powdery
materials inside special containers (e.g., cuvette, sample cup). Solid samples, e.g.,
metal parts, may be analyzed outside of these containers.

SPECTRO XEPOS — 19.01.2017 — 13

Safety

2.4 Prohibited operating conditions

Do not operate the instrument if one of the following conditions exists:
 If the instrument is faulty or damaged.
 If the ambient conditions do not comply with the specification.

2.5 Residual risks

This instrument has been manufactured in accordance with the state of the art.
Nevertheless, a residual risk cannot be completely excluded.

Danger! Risk of electric shock!

The spectrometer produces electric voltages of up to 60 kV.
 Shut down the instrument immediately if damaged.

Caution! Danger of poisoning!

The ray exit window of the X-ray tube and the detector window contain beryllium.
Vapors or dust of beryllium and its compounds are toxic and hazardous to your
health when inhaled.
 Do not touch this window.
 Should you have broken the beryllium window of the detector, immediately
seal off the measurement window of the spectrometer with adhesive tape.
This ensures that no broken beryllium window pieces can leave the
spectrometer. Switch off the spectrometer and inform the service department
of SPECTRO. The detector and the spectrometer can no longer be used.

Caution! Risk of crushing injuries!

When closing the sample chamber lid, there is an inherent risk of crushing injuries.
 When closing the sample chamber lid keep the fingers out of the sample
chamber.

— 14 SPECTRO XEPOS — 19.01.2017

 Safety

Caution! Ionizing radiation!

This spectrometer operates with ionizing radiation (X-rays). The safety devices
ensure that the spectrometer can be operated only in a safe, closed and shielded
condition.
 Never tamper with the safety devices.
 If you are concerned that the safety devices do not work properly, shut down
the spectrometer immediately. Please contact your Service Center.
 The results of the ambient dose rate measurements are an integral part of the
documentation supplied with the spectrometer (radiation protection
certificate).
 The condition of the beam stop (it cannot be seen from the outside since it is
immediately in front of the X-ray tube) is shown by the combination display
"Beam-Stop / X-Rays ON".
"Green" indicates that the Beam Stop is on, "Red" indicates that the Beam
Stop is open. If the Beam Stop is opened, this always caused the sample
chamber lid to be locked. An orange-colored LED indicates the operation of
the X-ray tube. See also Chapter 5.1.2 on page 24.

Note
If the instrument is in its normal operating mode (standby or measuring mode), it
produces ionizing radiation (X-rays).
The safety circuits in the instrument are designed to ensure the sample chamber
lid is always locked during the measurement.
For your safety, the safety circuits are checked automatically. Therefore, when
starting the software, a message is displayed requesting the opening and closing
of the cover (referred to as Start-up test, see Chapter 5.3).

Automatic safety circuit checks must be carried out at least once a month. If the
device has not been switched off and switched on again at the main switch for one
month, the software prompts you to do so (see also chapter 5.3.4). Three days
before the deadline, a first reminder appears in the status display of the software.

SPECTRO XEPOS — 19.01.2017 — 15

Safety

2.6 Radiation protection advice

Please observe the national safety and approval regulations in force in your
country and state!

2.6.1 Other countries

The operation of the instrument may require official approval in other countries.
Compliance with the national safety and approval regulations in force in your
country and/or state is mandatory! Please contact the responsible local approval
authority.

— 16 SPECTRO XEPOS — 19.01.2017

 Technical data

3 Technical data
Description Value

Instrument height 465 mm (18.3“)

Instrument width 618 mm (24.3“)

Instrument depth 730 mm (28.8“)

Instrument weight 65 kg (143 lbs) approx.

Place of installation Inside of dry, dust-free rooms up to an

altitude of 2,000 m above sea level,
vibration-resistant (not subject to impact
and vibration loads)

Operating voltage range 90 - 253 VAC, 50/60 Hz

Spectrometer power input max. 1,200 W (without PC)

Fuse 16 A (slow-blow)

Temperature range +10 to +35°C (50 to 95°F)

Storage room temperature range -10 to +50°C (14 to 122°F)

Optimal temperature range (within +20°C – +25°C (68 °F – 77 °F)

specifications)

Air humidity 10 to 80% (non-condensing) at 25°C

10 to 75% (non-condensing) at 30 °C

Protection class/contamination class IP20 (DIN 40050), contamination class II

(laboratory environment)

EMC environment Normal laboratory environment

Helium gas flushing (option)

Pressure 1.0 – 3.0 bar; (15 – 44 psi)

Quality ≥ 99.996% (4.6)

Consumption typically 4.5 L per analysis

Vacuum (option)

End pressure/operating pressure < 5 mbar (0.07 psi)

Voltage supply 110 V/230 V (instrument-controlled)

SPECTRO XEPOS — 19.01.2017 — 17

Transportation/Setting-up

4 Transportation/Setting-up
Only instructed personnel may unpack, install, and set up the instrument.

Note! Measurement errors!

 Shocks to the instrument during the measuring process may result in
measurement errors.
 Therefore, shocks to the instrument when taking measurements must
be avoided.
 Avoid mechanical impacts.
 Measurement errors may result from temperature differences inside the
instrument.
 Install the instrument so that it cannot heat up on one side only.

Observe the following information regarding the instrument's installation/transport:

 Use the adjustable legs of the instrument in order to compensate for a slight
unevenness.
 Always transport the instrument in a horizontal position, ensuring its legs are
pointing down.
 Always keep the instrument upright when transporting it! To do this,use your
left and right hand to reach underneath the plastic housing. Remember that
the center point of gravity of in the front of the instrument.
 Save the transport package in case you have to ship the instrument to the
service department at a later date.
 All connections are located at the back panel.
 When setting up the spectrometer, ensure all sides are easy to access
for maintenance and repair purposes, and electrical connections.
 Set up the instrument to ensure the power isolators (switches and power
cable) can be easily reached.
 All necessary cables and hoses are included in the delivery.
 If the instrument is to be moved to another place of installation after set-up,
there is a risk of damaging the instrument. Contact the SPECTRO Service
Department in this matter.

— 18 SPECTRO XEPOS — 19.01.2017

 Transportation/Setting-up

4.1 Storage
Storage conditions:
 The instrument must be stored in a dry place
 Room temperature -10 to +50°C (14°F to 122°F)
 Avoid storing the instrument at very low temperatures.

4.2 Gas supply (optional)

The optional gas flush is performed using helium.
The respective pressure reducer required for the gas supply is integrated in the
instrument.
 Input pressure 1.0 to 3.0 bar; (15 to 44 psi)
Gas is supplied through a PTFE hose included in SPECTRO's scope of supply:
 Dimensions OD/ID = 6/4 mm, length 3 m (~ 10 ft)
This hose is inserted into the rear panel of the spectrometer, see page 9.

SPECTRO XEPOS — 19.01.2017 — 19

Transportation/Setting-up

4.3 Vacuum (option)

In order to connect the vacuum pump, follow the instructions below or refer to the
information provided by the manufacturer (applicable documentation):

1. Check the oil level in the viewing

tube (2).
2. Top up oil or change the oil as
required.
Oil filler plug (1)
Oil drain plug (3)

Fig. 6
3. Install the oil mist filter (1).
 To do this, use the clamp to
fasten the oil mist filter.

Fig. 7
4. Use the vacuum hose to
connect the vacuum pump and
the instrument.
 To do this, fasten the
vacuum hose with the
clamps at both connecting
points.

Fig. 8
5. Use the power cable to connect
the vacuum pump and the
instrument.

 The vacuum pump is now

connected.

Fig. 9

— 20 SPECTRO XEPOS — 19.01.2017

 Transportation/Setting-up

4.4 Uninterruptible power supply – UPS (option)

Note
The first installation of the UPS must be performed by a technician who is
authorized by SPECTRO.
If you would like to retrofit the instrument, please order the retrofitting set:
 Part number 71000229: UPS 230V/50-60HZ + accessories
 Part number 71000230: UPS 110V/60HZ + accessories

Notice! Risk of damage!

 Without a UPS, the X-ray tube may be damaged in case of frequent power
failures.
 When a UPS is available, ensure that the entire power supply system of
the instrument is connected to the UPS.
 Connecting a laser printer to the UPS may destroy the UPS.
 Never connect a laser printer to the UPS.
 If the instrument is equipped with the vacuum option, this UPS must not be
used.
 If possible, ensure to provide an uninterrupted power supply

In case of a power failure, the UPS (Uninterrupted Power Supply) sends a signal
to the instrument. The instrument is then shut down in a controlled manner. In the
case of extended power failures, the computer is shut down after a given amount
of time.

1 2 3 4 5 6

Fig. 10

No. Component No. Component

1 UPS "ON/OFF" switch 4 Automatic circuit breaker 6 A

2 "Turn off alarm signal" switch 5 PC communication port

3 UPS power supply connection 6 Power connection for instruments

SPECTRO XEPOS — 19.01.2017 — 21

Transportation/Setting-up

When changing or reconnecting the UPS, proceed as follows:

1. Connect all components with the UPS (spectrometer, PC, monitor, etc.)
2. Connect the UPS with the power supply.
3. Switch on the UPS.
4. Switch on the components (spectrometer, PC, monitor, etc.)
 The UPS is now installed.

— 22 SPECTRO XEPOS — 19.01.2017

 Operation

5 Operation

5.1 Displays

5.1.1 Screen – Routine dialog

2
3

Fig. 11

No. Display Function

1 Status line Display for information from the program and the
instrument

2 Sample data table Input fields for sample data

3 Sample Display of the sample position, the spectrum, and the

tray/spectrum/result results of the analyses

4 Buttons Buttons for controlling the measurements

SPECTRO XEPOS — 19.01.2017 — 23

Operation

5.1.2 Beam Stop display on the instrument

The Beam Stop shields the source of radiation if the measurement is not active.
Therefore, the sample can be replaced when the X-ray tube is switched on. A
high-voltage generator (HV generator) is used to operate in the X-ray tube. The
displays on both sides of the spectrometer provide information about the
respective operating mode.
The following table illustrates the four display combinations that are possible:

Display "Beam Stop" Display "X-rays ON" Operating condition

(lettering and radiation
symbol)

green light not illuminated  Beam Stop closed

 HV (high-voltage) generator off
 e.g., spectrometer was just
switched on

green light orange light  Beam Stop closed

 HV generator switched on
 e.g., sample replacement, tube
in standby mode

red light not illuminated  Beam Stop open

 HV generator switched off
 This condition may occur during
the start-up test

red light orange light  Beam Stop open

 HV generator switched on
 Measurement mode

— 24 SPECTRO XEPOS — 19.01.2017

 Operation

5.2 Switching on the instrument

Note
When turning on the spectrometer after a long period of downtime, the following
conditions must be taken into consideration:
 If the spectrometer was shut down for more than two days, the X-ray tube
must be run under standby conditions for at least 20 minutes. Start measuring
only after this period.
 If the spectrometer was shut down for more than one month, the X-ray tube
must be run under standby conditions for at least 1 hour. Start measuring only
after this period.
Otherwise, the service life of the X-ray tube will be reduced significantly.
 If the spectrometer is operated inside an air-conditioned room, a constant
ambient temperature must be maintained. If the room temperature was
changed, wait at least 30 minutes before switching on the spectrometer.
Otherwise, the results of the measurements will be falsified.

Note
Ensure that the ambient conditions specified in Chapter "Technical data" are
maintained. If the temperature and/or relative humidity does not comply with the
specifications, the software of the instrument will initiate a warning.

To switch on the instrument, proceed as follows:

1. Turn the key-operated switch on the spectrometer (see figure, page 9, Pos. 7)
into its horizontal position.
2. Switch on the computer.
 The operating system is started.
3. Click on the "XRF Analyzer Pro" button; this will start the routine dialog.
 A login window opens:

SPECTRO XEPOS — 19.01.2017 — 25

Operation

4. Log on to the software.

 A prompt will request you to initiate the start-up test for the safety circuits
(see Chapter "Proceed with the start-up test"). Follow the instructions on
the screen. During the start-up test, the functionality of the safety circuits
will be tested automatically. If the start-up test is not successful, the high-
voltage supply of the X-ray tube cannot be switched on.
5. After the start-up test, all stepping motors are tested. Follow the instructions
on the screen (see Chapter "Initialization of the stepping motors").
 The instrument is switched on. In order to ensure stable measurement
conditions, it is highly recommended to wait 20 minutes before starting the
measurements.

— 26 SPECTRO XEPOS — 19.01.2017

 Operation

5.3 Proceed with the start-up test

While switching on the instrument (see Chapter 5.2), you will be prompted to
initiate the safety circuits start-up test. Follow the instructions on the screen.
During the start-up test, the functionality of the safety circuits will be tested
automatically. If the start-up test is not successful, the high-voltage supply of the
X-ray tube cannot be switched on.

5.3.1 Checking the safety circuits on the sample chamber lid

First, the communication connection of the computer will be established with the
instrument:

If the connection is successful, the software will first check the condition of the
safety circuits. The software checks the condition of the sample chamber lid
(open/closed). If the sample chamber lid is closed, you will be prompted to open it:

If the sample chamber was open when the instrument was switched on, this step
will be omitted and the software will skip this procedure.

SPECTRO XEPOS — 19.01.2017 — 27

Operation

Subsequently, the software will prompt you to close the sample chamber lid:

5.3.2 Checking the safety circuit on the filter changer ("Beam Stop")
Since an electric motor is used to move the assembly, the safety switches on the
Beam Stop are checked autonomously by the instrument's software. During this
procedure, the software displays an appropriate message:

After the safety test was completed successfully, the stepping motors that are
integrated into the spectrometer, are initialized.

— 28 SPECTRO XEPOS — 19.01.2017

 Operation

Alternatively, if the start-up test fails based on a malfunction, the user will be
informed accordingly:

Note
If the start-up test fails, the safety circuits are faulty.
 The high-voltage supply of the X-ray tube cannot be switched on.
 In this case, please contact your Service Center.

5.3.3 Initialization of the stepping motors

During the initial isolation you will be prompted to remove the sample tray from the
sample chamber. If there is no sample tray inside the sample chamber, click on
"OK, Plate Removed".

Follow the instructions on the screen.

Details about the content and the progress of the initialization process can be seen
on the messages.

SPECTRO XEPOS — 19.01.2017 — 29

Operation

If the startup test and the initialization were successful, the high-voltage supply of
the X-ray tube can be activated.
The X-ray tube should be switched to standby mode.
 On the screen dialog click on "Enter HV-Standby".

 After 20 minutes, the spectrometer is stable and ready for measurements.

5.3.4 Automatic verification of the safety circuits after one month

If the device has not been switched off for one month, the software prompts you to
do so. Switch off the device at the key-operated switch and turn it on again after
three seconds, not sooner. Subsequently, connect the device to the software. The
automatic check of the safety circuits starts as described in the chapter 5.3.1.

— 30 SPECTRO XEPOS — 19.01.2017

 Operation

5.4 Switching off the instrument

Notice! Risk of damage!
If the spectrometer is switched on but not used for an extended period of time,
ozone (O3) is generated in the small gap between the X-ray tube and the Beam
Stop. Ozone is an extremely reactive gas and has a corroding effect on the
excitation and sample chamber.
 If the spectrometer is not used for more than one day (weekends, office
holidays) it is recommended to switch off the instrument.
 If you do not work with the system for an extended period of time, the X-ray
tube must be operated in standby mode for at least one hour once a month.
This procedure is also required if the instrument is not to be used afterwards.
To switch off the instrument, proceed as follows:
1. Open the instrument server that is installed on the computer and select
"Shutdown".

2. A security question will be asked. Confirm the question with "Yes".

SPECTRO XEPOS — 19.01.2017 — 31

Operation

3. If at that point the X-ray tube is not switched on, subsequently, the high-
voltage supply will be shut down gradually and automatically.

 The instrument server will be closed.

4. Turn the key-operated switch to its horizontal position.
5. Select the “Start” menu in the Windows user interface and the “Exit”
command.
 The computer is turned off.
 The instrument is switched off.

5.5 Standby mode

(see also Chapter 5.2)
Observe the following instructions regarding the standby mode:
 If the spectrometer was shut down for more than two days, the X-ray tube
must be run under standby conditions for at least 20 minutes. Start measuring
only after this period.
 If the spectrometer was shut down for more than one month, the X-ray tube
must be run under standby conditions for at least 1 hour. Start measuring only
after this period.

— 32 SPECTRO XEPOS — 19.01.2017

 Operation

5.6 Measuring procedure

Note
The sample tray must be assembled outside of the instrument. This reduces the
contamination of the sample chamber. This applies in particular to powder pellets.

5.6.1 Preparing the measuring procedure

Before starting the measurement, proceed as follows:
1. Check the sample chamber and in the sample tray for contaminations. If
necessary, remove the contamination (see Chapter 6.4 and 6.5).
2. Ensure that the proper sample tray is selected or another sample holder unit
is chosen.
 The sample tray defined in the measurement program and the
assembled tray must be the same. Otherwise, the sample will not be
moved to its correct position during the measurement.
3. The samples placed onto the sample tray must not exceed a max. of 1,200 g.
Ensure the weight is evenly distributed.
The maximum sample height must not exceed 45 mm.
4. If necessary, use an adapter for Ø 32 mm sample or a "liquid protect cup".

Adapter for Ø 32 samples "Liquid protect cup"

5. Ensure that only such samples are present on the sample tray that are
measured under the same conditions (air, helium, vacuum).
 The measurement is now prepared.

SPECTRO XEPOS — 19.01.2017 — 33

Operation

How to measure different samples

Note
The sample tray must be assembled outside of the instrument.

How to measure cuvettes (powder or liquid)

Caution! Fire hazard!

When using flammable samples, there is an increased risk of fire.
 Always measure gaseous, highly volatile or flammable samples separately.
This will limit the amount of samples to an amount that will prevent the
spread of fire.

Notice! Damage to instrument!

Escaping liquids can damage the instrument.
 When measuring liquids, always use the "liquid protect cup" with an additional
protective film.
 When measuring liquid samples, the maximum permitted number of cuvettes
on one sample tray is limited to four.

Observe the following instructions when inserting the samples:

 Leave the filled cuvettes outside of the sample chamber for approx. 3 minutes
and then check them for tightness and ensure the film is undamaged.
 If the film is crinkled, the sample with this film must not be measured. In
this case, the sample must be prepared again, using a new cuvette and
film.
If the film is damaged inside the sample chamber, there is an indentation in the
chamber (discharge reservoir) in which the sample material is collected.
Therefore, only measure the liquid and powdery samples while they are in the
following trade positions:
 Standard tray (12 positions à 40 mm): Position 4 to position 9
 Rotation tray (8 positions à 40 mm): Position 3 to position 6
 Tray for small samples (25 positions à 20 mm): Position 7 to position 20

For cuvettes, a filling height of 10 mm it is recommended. Some cuvettes use a

level indicator to display the filling height. To arrive at the correct analysis, in
addition to the filling height, the weighted portion of the sample (or the density, if
known) must be determined and entered into the software.

— 34 SPECTRO XEPOS — 19.01.2017

 Operation

Always measure the following samples with gas flushing or in a diluted condition:
 gassing samples,
 highly volatile samples,
 flammable samples,
 samples with a Cl content of more than 2%.
After completing the measurement of liquid and powdery samples, the
spectrometer will sound a signal. Furthermore, a message on the screen will
prompt you to remove the sample trays with the cuvettes from the sample
chamber.

How to measure powder pallets

We recommend pressing the pellets into 40 mm steel rings. A ratio of
sample/binding agent of 5:1 is recommended (5 g sample + 1 g binding agent).
Samples without a steel ring are measured with an adapter for Ø 32 mm samples.

How to measure glass or melting pellets

Glass or melting pallets can be measured directly on the sample tray, depending
on size, with or without adapter for Ø 32mm samples.

Note
Glass pallets must always be measured on their "own" tray. Prior to the
measurement, all dust must be cleaned off the tray. A contaminated sample tray
will falsify the analysis.

SPECTRO XEPOS — 19.01.2017 — 35

Operation

How to measure large samples

In order to measure large samples, the sample tray and, if necessary, the sample
tray support must be removed.
To do this, proceed with the following steps:
1. Remove the sample tray as described in Chapter "How to change/remove the
sample tray" on page 38.

2. Use an Allen key to loosen the

tray screw (1).
3. Remove the sample tray
support.

Fig. 12
4. If possible, use the single
1
sample holder (1) that is
included with the delivery.

Fig. 13
Three single sample holders are included with each delivery. Additional holders
can be ordered from our SPECTRO Shop. The part number can be found on page
55.
The installation of the sample tray and the sample tray support takes place in
reverse order. During the installation of the sample tray support, tighten the tray
screw until the sample tray support can be rotated.

— 36 SPECTRO XEPOS — 19.01.2017

 Operation

5.6.2 Proceed with the measurement

Caution! Risk of crushing injuries!

When closing the sample chamber lid, there is an inherent risk of crushing injuries.
 When closing the sample chamber lid keep the fingers out of the sample
chamber.

Notice! Risk of damage!

 If sample liquid leaks into the spectrometer, the detector and the excitation
compartment might be damaged significantly.
 Measure the liquid samples in cuvettes in the "liquid protect" sample cup
with protective film.
 Never measure samples in cuvettes in a vacuum.
 When switching on the vacuum pump while the sample chamber is open, the
pump will work without resistance and be destroyed.
 Never switch on the vacuum pump if the sample chamber is open.

To measure the sample, proceed as follows:

1. Place the sample(s) on the sample tray and subsequently insert the sample
tray into the sample chamber.
When measuring large samples, depending on the sample size, use up to
three single sample holders.
2. Close the sample chamber lid.
3. Click on the sample position in the sample data table on the screen.
 For measurements without tray (large samples), always select trade
position 1.
4. Enter the sample data into the sample data table.
5. Start the measurement using the “Start” button.
 The measurement is performed automatically.
6. Perform further measurements if required.
 The measurement is complete.

Note
Measure a reference sample at regular intervals. This will allow you to identify
changes of the measurement results in good time.

SPECTRO XEPOS — 19.01.2017 — 37

Operation

How to change/remove the sample tray

To change or remove the sample tray, proceed as follows:

1. Loosen the locking device of the

sample tray (1) by turning it
clockwise.

Fig. 14
2. Carefully remove the sample
tray.

Fig. 15
3. Install the new sample tray.
 Ensure the red dot of the
sample tray and the red dot
of the tray support are
aligned (2).
4. Close the locking device of the
sample tray by rotating it
clockwise and simultaneously 2
lifting the device slightly.
Fig. 16

 The sample tray has been changed.

— 38 SPECTRO XEPOS — 19.01.2017

 Operation

5.7 Dust protection shutter / beam stabilization vacuum shutter

(option)

Dust protection shutter

The "Dust protection shutter" reduces the risk of contamination of the excitation
chamber during the standby mode while the sample chamber is being cleaned
(see Chapter 6.5) as well as during the removal or insertion of the sample tray into
the sample chamber (see page 38).
Functionality:
During the initialization of the device (see Chapter 5.3.3) and after completion of
the measurement, the dust protection shutter is moved automatically above the
excitation chamber and lowered into it.

Beam stabilization vacuum shutter

Devices that are equipped with the vacuum option (see chapter 4.3) use the
shutter as "beam stabilization vacuum shutter". In addition to reducing the risk of
contamination of the excitation chamber, the chamber is evacuated during the
standby mode. The evacuation of the excitation chamber has two main
advantages:
 The evacuation results in a significantly lower mechanical load on the
beryllium window of the x-ray tube, which increases the service life of the
tube.
 No load of the used crystal due to humidity. This leads to a better stability of
the analyzes.
When measurements are performed in air or using helium flushing, the system
requires at least 60 minutes to return to the state of highest stability and precision.

SPECTRO XEPOS — 19.01.2017 — 39

Maintenance by the operator

6 Maintenance by the operator

Note
In order to ensure the availability and operational safety of the equipment, we
recommend having the system checked for correct operation and performance at
least once per year by specialized technicians. To find contact addresses of
service organizations authorized by SPECTRO go to www.spectro.com

6.1 Operator maintenance plan

Caution! Ionizing radiation!

An X-ray tube is inside the spectrometer.
 Proceed only with the operator maintenance task described in this chapter.
The operating personnel is not permitted to proceed with any other
maintenance work. Any other services (e.g., technical maintenance) or
repairs must only be performed by service personnel authorized by the
instrument manufacturer.

The maintenance intervals specified in the following table are guidelines which
should be observed as a minimum requirement. The maintenance intervals may
vary, depending on the use of the instrument.
To ensure the flawless function of the instrument, proceed with the following
maintenance tasks:

Daily operator maintenance work

Visual inspection. Checking the housing, the sample chamber,

the mechanism of the sample chamber lid
for damage.

Measure the reference samples.

Clean the sample chamber. Use a soft cloth and, if possible, a mild
cleaning agent or pure alcohol, e.g.,
isopropanol, see Chapter 6.5.

Weekly operator maintenance work

Inspection the filter mat (back of the See Chapter 6.9.

instrument) for contamination.

Inspect the shutter O-ring for contamination See chapter 6.10

(option "dust protection shutter / beam
stabilization vacuum shutter”)

— 40 SPECTRO XEPOS — 19.01.2017

 Maintenance by the operator

Monthly operator maintenance work

Energy channel recalibration (MCA). See Chapter 6.2.

Shutting down and rebooting the computer. See Chapter 5.2 and 5.3.

Shutting down and restarting the See note on page 15 and chapter 5.3.4
spectrometer and repeating the start-up test
(testing the safety circuits).

Further operator maintenance work As required

Data backup (complete XAP directory).

Standardizing the instrument (global See Chapter 6.3.

recalibration)

Clean the sample tray. See Chapter 6.4.

Check the adhesive film in the discharge See Chapter 6.6.

reservoir for dirt, replace if necessary.

Replace the tray pads in the sample See Chapter 6.7.

chamber.

Replace the "liquid protect cups" protective See Chapter 6.8.

film.

Clean the sample rotation drive (do not Use a soft brush.
lubricate!).

Vacuum system maintenance (optional). Changing the vacuum oil and cleaning the
oil mist filter. See Chapter 4.3.

SPECTRO XEPOS — 19.01.2017 — 41

Maintenance by the operator

6.2 Energy channel recalibration (MCA)

In order to recalibrate the instrument, proceed as follows:
1. Press the "Recalibration" button.
 The corresponding program window is displayed.
2. Press the "Start MCA only" button and follow the instructions.
 The energy-channel recalibration is performed automatically.

After the measurement is completed, a result window is displayed.

 The spectrometer is recalibrated.

— 42 SPECTRO XEPOS — 19.01.2017

 Maintenance by the operator

6.3 Standardization (Global recalibration)

After a while, the beryllium window of the detector may become smudged. This
may increase the absorption of light elements.
A standardization should only be performed if the results during the measurement
of reference samples is outside of the expected range and other causes, such as
position of the sample or sample preparation, can be ruled out.
Samples for standardizing the instrument are enclosed in the scope of supply.
In order to standardize the instrument, proceed as follows:
1. Press the "Recalibration" button.
 A window opens. Press the "Start Recalibration" button and follow the
instructions.

After the measurement is completed, a result window is displayed.

 The standardization (global recalibration) is completed.

SPECTRO XEPOS — 19.01.2017 — 43

Maintenance by the operator

6.4 Clean the sample tray

To clean the sample tray, proceed as follows:
1. Remove the sample tree from the sample chamber, see page 38 and place
the sample tray on the level, clean surface.
2. Use a small brush to carefully clean the sample tray.
Do not apply any pressure to the sample support surface.
 The sample tray is now cleaned.

6.5 Clean the sample chamber

Note
Any sample material left in the sample chamber must be removed immediately.
To do this, use a soft cloth. If the sample chamber floor is heavily soiled, it should
be cleaned with alcohol, e.g., isopropanol.

Notice! Risk of damage!

Improper cleaning procedures can destroy the beryllium window of the detector.
 Never use a vacuum cleaner or compressed air to clean the sample chamber.

— 44 SPECTRO XEPOS — 19.01.2017

 Maintenance by the operator

6.6 Replacing the adhesive film in the discharge reservoir

There is a double-sided adhesive film available for the discharge reservoir. Dust
and other residues will adhere to the film. (This adhesive film is included in the
scope of supply).
One side of the film is non-permanent adhesive (with a transparent protection
layer). On the other side, there is a permanent adhesive surface (with white
protection layer).
The adhesive film can be ordered from the SPECTRO Shop. The part number can
be found on page 55.
To replace the filter mat, proceed as follows:
1. Remove the old adhesive film (1).
2. Attach the new adhesive film into 1
the discharge groove.
 The protective film is cut on
both sides; that makes its
removal easier.
 Ensure the adhesive film is
attached with the non-
permanent side facing down.
Fig. 17
 Now, the adhesive film is replaced.

SPECTRO XEPOS — 19.01.2017 — 45

Maintenance by the operator

6.7 Replacing the tray pads

Replace the tray pads only if you are prompted by the software to do so or if one
or several tray pads have slipped or are visibly damaged.
The tray pads are included with each delivery. Additional pads can be ordered
from our SPECTRO Shop. The part number can be found on page 55.
To replace the tray pads, proceed as follows:
1. Replace the old tray pads (1, 2) 2 1 2
or the residue and clean the area
on the sample chamber surface
intended for the tray pads. To do 2
this use pure alcohol.
 The tray pads for the rotation 2
drive (2) are only assembled 1
if the optional rotation drive
is available. 2

2 1 2
Fig. 18
2. Remove the new tray pads and
stick them carefully and
accurately onto the marked
surfaces.
3. Subsequently, push the tray pads
downward against the sample
chamber floor.

4. Ensure the tray pads are

positioned in the locations
intended for this purpose.
5. If a tray pad is not placed
accurately on its specified
location, it must be removed and
a new tray pad must be used.
Otherwise, it may not adhere
properly.

Fig. 19
 Now, the tray pads are replaced.

— 46 SPECTRO XEPOS — 19.01.2017

 Maintenance by the operator

6.8 Insert the film for the "liquid protect" sample cup
Parts required for inserting the film:
 XRF film (2)
 Sample cup holder (4)
 Clamping ring (3)
 Tool for removing the clamping
ring (1)

Fig. 20
To insert the film, proceed as follows:
1. Place the parts of the sample cup
holder on a clean surface.
2. Place the film on the narrow end
of the sample cup holder.
3. Place the clamping ring on the
film.

Fig. 21
4. Push the clamping ring down
until the sample cup holder and
the clamping ring are on the
same level.
5. Ensure the film is not crinkled.
Fig. 22

SPECTRO XEPOS — 19.01.2017 — 47

Maintenance by the operator

6. In order to replace the film, push

the tool into the gap between the
sample cup holder and the
clamping ring and push off the
clamping ring.

 The film is now inserted.

Fig. 23

— 48 SPECTRO XEPOS — 19.01.2017

 Maintenance by the operator

6.9 Replacing the filter mat

There is an air filter below the front
side of the instrument.

Fig. 24
The filter mat is included with each delivery. Additional mats can be ordered from
our SPECTRO Shop. The part number can be found on page 55.
To replace the filter mat, proceed as follows:
1. Loosen the cover on the
magnetic locks (1) by pulling 1 1
downward.
2. Remove the old filter mat.

Fig. 25: Bottom view

3. Install the new filter mat.
4. Reinstall the cover.
 Ensure the magnetic lock is
positioned properly.

 Now, the filter mat is replaced.

SPECTRO XEPOS — 19.01.2017 — 49

Maintenance by the operator

6.10 Dust protection shutter / beam stabilization vacuum shutter

(option) — Clean O-ring
To clean the O-ring, proceed as described below:
1. Remove the sample tray and clean the sample chamber (see chapter 6.5).
2. Click the Diagnostic Tools of the "XRF Analyzer Pro" software. Select the
menu item "Shutter" and click the option "Open and deactivate".
3. Inspect the O-ring (2). A dirty O-
ring can contaminate the 1
excitation chamber. If necessary,
clean the O-ring (2).
 While cleaning, ensure the
excitation chamber is not
contaminated. To clean the 2
O-ring (2), use a soft cloth
and possibly isopropanol
(isopropyl alcohol). Do not
apply grease to the O-ring. Fig. 26

4. In order initialize the shutter (1),

select the option "Re-Initialize
Shutter" in the menu
item"Shutter" in the Diagnostic
Tools.

 The O-ring has been changed.

— 50 SPECTRO XEPOS — 19.01.2017

 Maintenance by the operator

6.11 Troubleshooting

Notice! Damage to instrument!

Improper repairs may damage the instrument.
 Do not repair the instrument yourself. Contact your immediate supervisor.

Fault Cause Remedy

The spectrometer cannot The power plug is not Insert the power plug properly.
be switched on. inserted properly.

The UPS (option) is not Connect the UPS to the power

connected to the power supply.
supply.

The UPS (option) is not Switch on the UPS.

switched on.

The computer cannot be The power plug is not Insert the power plug properly.
switched on. inserted properly.

The monitor cannot be The power plug is not Check if the power plug was
switched on. inserted properly. properly inserted.

The keyboard does not The keyboard is not Check the keyboard connection
react. properly connected. to the computer.

The keyboard is defective. Please contact your Service

Center.

The mouse does not The mouse is not properly Check the mouse connection to
convert any entries. connected. the computer.

The mouse is defective. Please contact your Service

Center.

When starting "XRF The spectrometer is not see above

Analyzer Pro", the switched on.
message error
"Connection failed" is The connecting cable is Connect the cable and check the
displayed. not connected or not plug for correct fit.
properly connected to the
spectrometer.

The connecting cable is Connect the cable and check the

not connected or not plug for correct fit.
properly connected to the
computer.

SPECTRO XEPOS — 19.01.2017 — 51

Maintenance by the operator

Fault Cause Remedy

Incorrect start-up test The sample chamber lid is Check if the sample chamber lid
 The X-ray tube not closed. is properly closed.
cannot be switched
on. Faulty safety switches or Please contact your Service
defective X-ray Center.
tube/generator.

Beam Stop defective Please contact your Service

 The stepping motor or Center.
the safety switches are
defective.

When the measurement Faulty safety switches or Please contact your Service
starts, the high-voltage is defective X-ray tube. Center.
shut down again

No spectrum is displayed There is no sample at the Check the sample position on the
when the measurement is measurement position. sample tray or place the sample
started. onto the measurement position.

Defective stop mechanism, Please contact your Service

excitation or detection Center.
system.

The input pulse density Activate the power control in the

(ICR) is too high. measurement method.

During the MCA There is no proper sample Place the MCA sample onto the
calibration, error at the measurement correct position of the sample
messages appear. position or no sample at tray.
all.

Defective detection Please contact your Service

system. Center.

— 52 SPECTRO XEPOS — 19.01.2017

 Maintenance by the operator

Fault Cause Remedy

The analysis results There is no proper sample Place a reference sample at the
of the reference at the measurement measurement position.
sample show great position or no sample at
deviations. all.

When using the vacuum Switch on the vacuum pump, check

system, it was not switched the vacuum hoses.
on or not properly
connected.

The helium supply was not Connect the helium supply and start
connected when the the procedure again.
helium flushing was used.

The "Liquid-Protect" film of Replace the "Liquid-Protect" film of

the sample cup is torn. the sample cup.

Contamination in the Clean the sample chamber, clean or

sample chamber. replace the film holder.

The MCA recalibration Repeat the MCA calibration.

failed previously

Defective stop mechanism, Please contact your Service Center.

excitation or detection
system.

Other malfunctions in the Please contact your Service Center.

system.

Powder from a Apparent contamination. Clean the sample chamber.

cuvette has leaked
into the spectrometer. Clean or replace the film holder.

Additional contamination Please contact your Service Center.

that cannot be accessed.

SPECTRO XEPOS — 19.01.2017 — 53

Maintenance by the operator

Fault Cause Remedy

Liquid from a cuvette Apparent visible Clean the sample chamber.

has leaked into the contamination.
spectrometer. Replace the "Liquid-Protect" film of
the sample cup.

Additional contamination Please contact your Service Center.

that cannot be accessed.

The sample chamber The measurement Wait several seconds until the end of
lid does not open. procedure is not yet the measurement the sample
complete or there is still chamber lit is unlocked or the
residual vacuum in the sample chamber is completely
sample chamber. aerated.

Locking mechanism of the Please contact your Service Center.

sample chamber lid is
defective.

The dust protection The shutter is deactivated. Click the Diagnostic Tools of the
shutter / beam "XRF Analyzer Pro" software. Select
stabilization vacuum the menu item "Shutter" and click the
shutter does not close option "Re-initialize shutter".
the excitation
chamber after The drive mechanism of Please contact your Service Center.
measurement. the shutter is defective.

— 54 SPECTRO XEPOS — 19.01.2017

 Spare parts and consumables

7 Spare parts and consumables

You can find the spare parts and consumables for this instrument under "Support -
Parts Catalogue" (Service – Parts Catalogue) on our website at www.spectro.com.
Part numbers of various consumables:

Article Order number

Adhesive film for discharge reservoir 47720053

Tray pads 47220044

Filter mat 47840301

Reducer ring 32 mm 46902022

Liquid Protection Cup 46101444

4µm Prolene film 78999107

Single sample holder 41236915

8 De-commissioning
Only organizations or persons authorized by the instrument manufacturer shall be
permitted to de-commission the instrument. Please contact your Service Center.

9 Manufacturer address
SPECTRO Analytical Instruments GmbH
Boschstr. 10
D-47533 Kleve
Germany
Tel.: +49.2821.8 92-0
Fax: +49.2821.8 92-22 00
http://www.spectro.com

SPECTRO XEPOS — 19.01.2017 — 55