Endress+Hauser Analytik Jena APUsim User manual

Operating Manual
APUsim
Sample Preparation Unit

Analytik Jena GmbH
Konrad-Zuse-Str.1
07745 Jena Germany
Phone + 49 3641 77 70
Fax + 49 3641 77 9279
Email [e-mail]
Analytik Jena GmbH
Konrad-Zuse-Str. 1
07745 Jena Germany
Phone + 49 3641 77 7407
Email [e-mail]
http://www.analytik-jena.com
11-0606-001-23
B (01/2021)
Analytik Jena GmbH
© Copyright 2021, Analytik Jena GmbH
Manufacturer
Service
General information
Documentation number
Edition
Implementation of the
Technical Documentation

Contents
APUsim 1
Contents
1Basic Information...............................................................................................................3
1.1 Using the APUsim ................................................................................................3
1.2 About this user manual.........................................................................................3
1.4 Warranty and liability ............................................................................................4
2Safety instructions.............................................................................................................5
2.1 General notes .......................................................................................................5
2.2 Warning and information labels at the APUsim....................................................5
2.3 Requirements for the operating personnel...........................................................5
2.4 Safety instructions, transport and installation.......................................................6
2.5 Safety instructions - operation..............................................................................6
2.5.1 General .................................................................................................................6
2.5.2 Safety instructions - Protection against explosion and fire...................................6
2.5.3 Safety instructions - electrical equipment.............................................................6
2.5.4 Handling of samples and reagents.......................................................................7
2.5.5 Safety instructions - service and repair ................................................................7
2.6 Behavior during emergencies...............................................................................7
3Technical data ....................................................................................................................8
4Installation conditions.......................................................................................................9
4.1 Environmental conditions .....................................................................................9
4.2 Energy supply.......................................................................................................9
4.3 Space requirement .............................................................................................10
5Design and operation of the APUsim ............................................................................11
6Commissioning ................................................................................................................14
7Operation ..........................................................................................................................15
7.1 Screen layout......................................................................................................15
7.2 Configuring the parameters for the sample preparation.....................................16
7.3 Automatic sample preparation............................................................................17
7.4 Manual sample preparation for samples with particles ......................................18
7.5 Manual sample preparation with solid phase extraction (SPE-AOX).................19
7.6 Performing a calibration .....................................................................................21
8Maintenance and care .....................................................................................................23
8.1 Maintenance overview........................................................................................23
8.2 Replacing the tube system .................................................................................23
8.3 Replacing the sealing rings in the syringe adapter ............................................25
9Fault removal....................................................................................................................26
10 Transport and storage.....................................................................................................27
11 Disposal ............................................................................................................................27

Contents
2 APUsim

Basic Information
APUsim 3
1 Basic Information
1.1 Using the APUsim
The APUsim sample preparation unit is an automatic adsorption system for the sample prepara-
tion for AOX determination using the column method in accordance with DIN EN ISO 9562 and
DIN 38409/14.
Up to 6 samples can be processed simultaneously with the APUsim. For the adsorption process
the sample volume, rinse volume and dosing speed can be varied. The AOX columns may be of
difference sizes.
The APUsim has been designed for two operating modes:
1. Automatic dosing of sample and rinse solution.
2. Manual dosing of sample and rinse solution.
This operating mode should be preferred for particulate samples.
The sample preparation unit may only be used for the above-mentioned methods of sample
enrichment for AOX determination. Any other use is not as intended! Only the operator is liable
for any damages that result from this.
The operational safety of the sample preparation unit APUsim is only ensured during proper use
according to the information in this user manual.
The intended use also includes the adherence to the installation conditions prescribed by Ana-
lytik Jena which are available from the customer service address stated above.
1.2 About this user manual
This user manual is aimed at qualified specialist personnel with knowledge of sample prepara-
tion for AOX determination. The user manual informs about the design and function of the sam-
ple preparation unit and provides the necessary know-how for the safe handling of the equip-
ment. It further includes notes on the maintenance and service of the equipment and potential
causes and remedies of any faults.
Typographical conventions
Instructions for actions which occur in chronological order are numbered and combined in
action units.
Instructions for actions consisting of only a single step are identified with "".
Lists which are not in chronological order are shown as itemized lists, sub-listings as bullet
points.
The user manual uses the following symbols and signal words to indicate hazards or instruc-
tions. The safety instructions are always placed before an action.

Basic Information
4 APUsim
WARNING
This signal word indicates medium risk hazards. If not avoided, they
can lead
to death or serious injuries.
CAUTION
This signal word indicates low risk hazards. If not avoided, they can
lead to minor or moderate injuries.
ATTENTION
Follow the instructions marked in this way in order to avoid material
damage and
operating errors.
1.4 Warranty and liability
The warranty duration and liability comply with the legal requirements and the provisions in the
general terms and conditions of Analytik Jena.
Deviations from the intended use described in this user manual results in limitations of warranty
and liability during a damage event. Damage to wearing parts is not included in the warranty.
Warranty and liability claims are excluded for personal injury and property damage due to one
or several of the following causes:
use of the sample preparation unit other than intended
improper commissioning, operation and service of the sample preparation unit
modifications of the equipment without prior consultation with Analytik Jena
unauthorized intervention in the equipment
operation of the device with faulty safety equipment or improperly fitted safety and protec-
tion equipment
inadequate monitoring of the equipment components subject to wear
use of other than original spare parts, wearing parts or consumables
improper repairs
faults due to the non-observance of this user manual

Safety instructions
APUsim 5
2 Safety instructions
2.1 General notes
For your own safety and for a trouble-free operation, read this chapter with care before
commissioning the APUsim.
Observe all safety notices contained in the user manual.
Besides the safety instructions in this user manual and the local safety regulations that
apply to the operation of the device the general applicable regulations regarding accident
prevention, occupational health and safety and environmental protection of the respective
country of use have to be observed and complied with. The operator must ascertain the
latest version of these regulations.
References to potential dangers do not replace the work protection regulations which must
be observed.
2.2 Warning and information labels at the APUsim
There are no warning or information symbols attached to the APUsim. The storage bottle for
nitric sodium nitrate rinse solution (pH ≈ 2) and the waste container have been labeled using the
following danger pictogram. Its meaning must always be heeded:
Warning against corrosive substances
Damaged or missing pictograms can cause incorrect actions leading to personal injury or mate-
rial damage! The pictogram must not be removed! A damaged pictogram must be replaced
without delay!
2.3 Requirements for the operating personnel
The APUsim must only be commissioned, operated and serviced by trained personnel
instructed in technical safety. The instruction also includes imparting the contents of this
user manual.
It must be ensured that only authorized personnel works at the device.
The operating personnel must be familiar with the dangers arising from samples to be ana-
lyzed and excipients used. The appropriate protective equipment must be used.

Safety instructions
6 APUsim
2.4 Safety instructions, transport and installation
Only transport the sample preparation unit APUsim in its original packaging! Prepare the
APUsim for transport, i.e. drain the equipment completely and remove all lose parts
To prevent health damage the following must be observed when moving the device in the
laboratory (lifting and carrying):
•For reasons of safety 2 persons are required to transport the device and must position
themselves on both sides of the equipment.
•Because the device does not have carrying handles, grip the device firmly with both
hands at the lower end.
The guide values and statutory limits for lifting and carrying loads without auxiliary equip-
ment must be observed and adhered to.
2.5 Safety instructions - operation
2.5.1 General
The operator of the APUsim must make sure before each commissioning that the condition
of the device is sound. This applies in particular after each modification or extension of the
device or its repair.
During operation unobstructed access to the mains switch and mains socket must always
be ensured.
The APUsim must only be operated if all protective equipment (drainage channel for chem-
icals, plastic cover at the pump units) are in place, properly installed and operational.
2.5.2 Safety instructions - Protection against explosion and fire
The sample preparation unit may not be operated in an explosive environment.
The operating personnel must be familiar with the location of the fire-fighting equipment in
the operating room of the sample preparation unit.
2.5.3 Safety instructions - electrical equipment
Any work on the electronics (behind the device enclosure) may only be carried out by the
customer service of Analytik Jena and specially authorized technicians.
The device must be switched off immediately at the mains switch (on the equipment back-
plate) and the power supply disconnected from the mains socket if there is any interference
with the electric components.
The electrical components must be checked regularly by a qualified electrician. Any de-
fects, such as loose connections, faulty or damaged cables, must be repaired without de-
lay.

Safety instructions
APUsim 7
2.5.4 Handling of samples and reagents
The operator is responsible for the selection of substances used in the process as well as
for their safe handling. This is particularly important for radioactive, infectious, poisonous,
corrosive, combustible, explosive and otherwise dangerous substances.
When handling dangerous substances local safety instructions and guidelines must be
observed. The notes in this user manual do not replace the specific local regulations or the
regulations in the EC safety data sheets of the manufacturers for the auxiliary and operat-
ing materials.
The instructions and notes in the safety data sheet for the preparation and handling of nitric
sodium nitrate solution (rinse solution with pH ≈ 2) and methanol (SPE-AOX) must always
be observed!
Protective goggles and rubber gloves have to be worn when handing reagents.
The operator is responsible for carrying out suitable decontamination should the device be
contaminated externally or internally with dangerous substances.
Splashes, drops or larger spillages of reagents should be removed using an absorbent
material such as cotton wool, laboratory wipes or cellulose.
2.5.5 Safety instructions - service and repair
The APUsim system is usually serviced by the customer service department of Analytik
Jena GmbH or its authorized and trained specialist personnel.
Independent servicing can maladjust or damage the device. Therefore, the operator may
generally only carry out the tasks listed in chapter "Maintenance and care" p. 23.
The exterior of the APUsim may only be cleaned with a damp, not dripping, cloth after the
device has been switched off.
Any service and repair work at the device may usually only be carried out in the switched-
off condition (unless stated otherwise).
Only use original accessories and original replacement parts from Analytik Jena.
2.6 Behavior during emergencies
During situations of danger or accidents the APUsim must be switched off immediately from the
mains switch at the equipment backplate and the mains plug be disconnected from the mains
socket.

Technical data
8 APUsim
3 Technical data
General characteristics
Designation/type APUsim
Basic device dimensions (W x H x D) 450 mm x 600 mm x 205 mm
Mass app. 20 kg
Procedural data
Number of samples AOX 6
Sample volume 5 – 100 mL, 1 mL step
Rinse volume 0 – 100 mL, 1 mL step
Dosing rate 1 – 6 mL/min., 0.5 mL/min step
Particle handling capacity < 1 mm
Operation internal control module
Stirring function none
Syringe volume max. 100 mL
Electrical variables
Operating voltage 24 V via external power supply
Power consumption 50 W max.
Current consumption 2.1 A max.
Grid voltage of external power supply 100 – 240 V
Interference suppression
(electromagnetic compatibility)
in accordance with the provisions of EN 55022
class A
Environmental conditions
Temperature +10 to +40 °C
Humidity Max. 90 % at +30 °C
Air pressure 0.7 – 1.06 bar
The requirements for the environmental conditions are identical for the operation and the stor-
age of the APUsim. Use a desiccant when storing the APUsim to prevent damage from conden-
sate forming.

Installation conditions
APUsim 9
4 Installation conditions
4.1 Environmental conditions
The APUsim may only be operated in closed rooms. The location must have the appearance of
a chemical laboratory.
it must be devoid of dust, drafts, vibrations and caustic fumes. Smoking is prohibited in the
room where the APUsim is operated.
Do not place the APUsim near sources of electromagnetic interference.
Avoid direct sunlight and heater radiation on the APUsim. Air conditioning is recommended
at the location. The cool air emanating from the air conditioning unit should not be directed
at the device.
The following requirements are placed on the climatic conditions in the operating room:
Temperature range +10 to +40 °C
Humidity Max. 90 % at +30 °C
Air pressure 0.7 bar to 1.06 bar
Summary 1 Environmental conditions for operation
The requirements for the environmental conditions are identical for the operation and the stor-
age of the APUsim. Use a desiccant when storing the APUsim to prevent damage from conden-
sate forming.
4.2 Energy supply
WARNING
Observe the mains connection!
During electrical installation, observe the VDE (German Association for Electrical Engineers)
electrotechnical guidelines and local regulation requirements!
The mains supply must be correctly earthed.
The APUsim is operated on single-phase alternating current.

Installation conditions
10 APUsim
Switching-on conditions
Voltage 24 V via external power supply
Power consumption 50 W max.
Current consumption 2.1 A max.
Grid voltage of external power supply 100 – 240 V
Interference suppression
(electromagnetic compatibility)
in accordance with the provisions of
EN 55022 class A
Overview 2 Power supply
4.3 Space requirement
Height 600 mm
width 450 mm
Depth 205 mm
Mass app. 20 kg
Overview 3 Space requirement and mass
During operation unobstructed access to the mains connection at the equipment backplate must
always be ensured. A safety distance of at least 10 cm to other equipment or walls should be
maintained.

Design and operation of the APUsim
APUsim 11
5 Design and operation of the APUsim
1 Display
2 Control knob
3 Rinse tube
4 Storage bottle for rinse solution
5 Drainage channel
6 AOX columns (here: duplex columns)
7 Sample tube
8 Service flap with tube pump
9 Start button (for the 1st pump unit)
10 Syringe for sampling
Figure 1 Design of the APUsim
The sample preparation unit APUsim is an automatic adsorption system for the sample prepara-
tion for AOX determination based on the column method.
Up to six samples can be processed simultaneously with the APUsim. For the adsorption pro-
cess the sample volume, rinse volume and dosing speed can be varied.
The APUsim features three pump units with two channels each, controlled separately by the
internal control software. The parameters for sample preparation can be configured individually
for each pump unit. The two channels of a pump unit must be operated using identical configu-
rations. They are frequently used for duplicate measurements.
Figure 2 shows the sample path through the sample preparation unit: The samples are filled into
the plastic syringes. The three tube pumps then automatically pump the samples across the
AOX columns. After adsorption has completed, the residual sample runs via the drainage chan-
nel to the waste container. After the valve has been switched over, the dosing pump rinses the
AOX columns with the pre-configured volumes of nitric rinse solution and thereby prepares
them for the AOX determination.

Design and operation of the APUsim
12 APUsim
Figure 2 Tube diagram
The sample preparation unit ensures a high particle handling capacity up to 1 mm. The tube
pumps and their tube system (internal diameter 2 mm) are robust against clogging. No sample
passes through the change-over valves, only clear rinse solution (see Figure 4 p. 13). This pro-
tects the valves against particles and they cannot get clogged up.
With samples with high particle loads incompletely dissolved parts of the sample may sediment
in the syringe and are thus not included in the AOX determination. In this case, the manual pro-
cedure (see "Manual sample preparation for samples with particles" p. 18) is recommended.
In the sample preparation unit up to five AOX columns can be used per channel. Generally, two
AOX columns (duplex columns) are used and filled with disposable tubes of 50 mg active car-
bon. If two AOX columns are not sufficient for the complete adsorption, three columns (triplex
column) must be used. Since the drainage channel is adjustable in height, columns of different
sizes can be used in the APUsim.
With a high particle load a pre-column filled with a suitable filter material (e.g. ceramic wool,
quartz wool) can be screwed upstream of the AOX columns. The pre-column separates parti-
cles and prevents the system from clogging during the sample preparation.
The backplate of the APUsim contains the electrical connections for the external power supply
and mains switch. The rating plate is also attached there. The rating plate also contains the
electrical connection data:
1 Manufacturer
2 CE marking
3 Serial number of the device
4 Disposal instructions (Do not dispose of
as domestic waste!)
5 Warning: Only use direct voltage power
supplies with positive polarity
6 Voltage, max. power and current con-
sumption
7 Device type
Figure 3 Rating plate

Design and operation of the APUsim
APUsim 13
Figure 4 Tube diagram

Commissioning
14 APUsim
6 Commissioning
CAUTION! Prevent any unauthorized interference!
The device may only be assembled, installed and repaired by the service engineers from Ana-
lytik Jena or by technical personnel authorized and trained by Analytik Jena.
ATTENTION
The APUsim must be switched off prior to each installation!
Connecting or disconnecting electrical plug-in contacts might damage the sensitive electronics.
The first commissioning of the APUsim is usually carried out by the customer service depart-
ment of Analytik Jena or persons authorized by Analytik Jena. The presence of all persons des-
ignated for operation of the device during the briefing of the service technician is imperative.
After transport or storage the customer can commission the sample preparation unit inde-
pendently. This installation is being described below.
Prior to commissioning, check that all installation requirements are met at the installation loca-
tion (see section "Installation conditions" p. 9).
1. Insert the drainage channel (5 in Figure 1) into the support rods of the APUsim using the
snap fasteners.
2. Install the waste tube with the tube protection to the drainage channel.
Note: The tube protection prevents the waste tube from kinking.
3. Insert the waste tube into the waste container (volume 5 L).
Note: Lay the waste tube with a constant incline. If required, shorten tube. Otherwise the
waste channel might easily overflow.
4. Fill the storage bottle for the rinse solution (4 in Figure 1) with nitric sodium nitrate solution
(pH ≈ 2).
5. Place the storage bottle into the adapter of the APUsim. Immerse the rinse tube (no. 1) in
the rinse solution.
6. Fill the AOX columns with disposable tubes or quartz containers (with 50 mg active carbon
each). Screw max. 5 AOX columns together. Attach the AOX columns (6 in Figure 1) via
the Luer lock to the respective channel of the APUsim.
7. Slide the drainage channel directly under the column units.
Note: There is a risk of splashing if the drainage channel is located too low under the col-
umn unit.
8. Insert plastic syringes (10 in Figure 1, volume 100 mL) from above into the syringe adapter
of the APUsim. Ensure the tight closure of the connection using the sealing ring.
9. Connect the power supply unit to the equipment backplate. Switch the APUsim on from the
mains switch.
The APUsim is operational.
After commissioning the entire system must be rinsed with distilled water through the plastic
syringes.

Operation
APUsim 15
7 Operation
7.1 Screen layout
By rotating the control knob you can select one of three windows in the display:
Start window
Display of the processing time for each
pump unit
Input window
Parameter configuration:
Sample volume, rinse volume and
dosing speed
Calibration window
Enable the calibration mode
Enter the calculated masses in
50.0 ± 10.0 g.

Operation
16 APUsim
7.2 Configuring the parameters for the sample preparation
The sample preparation unit APUsim has three pump units with two channels each. The pa-
rameters for sample preparation can be configured individually for each pump unit. DIN EN ISO
9562 specifies the following parameters for AOX determination using the column method: Sam-
ple volume 100 mL, rinse volume 25 mL, dosing speed 3 mL/min. Other, customer-specific con-
figurations are possible.
ATTENTION
The APUsim can only dose the correct sample volume if the sample volume in the syringe is
identical to the configured sample volume.
1. Select the input window by rotating
the control knob (2 in Figure 1).
2. Within the window, select the pa-
rameter by rotating the control
knob.
3. Confirm the parameter selection by
pressing the control knob.
The parameter is highlighted
in light blue.
4. Configure the parameter by rotating the control knob.
5. Confirm the configuration by pressing the control knob.
6. Start the desired pump unit by pressing the start button (9 in Figure 1).
The sample preparation starts at the selected pump unit.
During the start the parameter configurations for the selected pump unit are transferred. The
configurations can no longer be modified during the sample preparation.
To operate several pump units with identical parameters, start the desired pump units con-
secutively.
To operate the pump units with different configurations, configure new parameters in the
input window after starting a pump unit, confirm the input and start the corresponding pump
unit(s).

Operation
APUsim 17
Starting or stopping the sample preparation
The start buttons at the pump units (9 in Figure 1) are used to start or stop the sample prepara-
tion. The start window displays the calculated processing time briefly at the start of the meas-
urement. The time then counts down to 00:00. The end of processing is indicated by a signal
tone.
Start button functions
Start the sample preparation
Briefly press the start button. The start button illuminates light
blue.
The time indication in the start
window is running.
The sample preparation starts.
Interrupt the sample preparation briefly.
Briefly press the start button
with the sample preparation
running.
The start button flashes.
The time indication stops. The
pause symbol (II) is shown.
The sample preparation stops.
By briefly pressing the button,
the sample preparation is re-
sumed.
Cancel the sample preparation
Press and hold the start button. The device issues a signal tone.
The start button is no longer il-
luminated.
The time indication is reset to
00:00.
The sample preparation stops.
Note: After canceling the sample preparation the system must be rinsed with rinse solution to
remove the sample residue from the tube system.
7.3 Automatic sample preparation
In the automatic sample preparation the APUsim automatically performs the adsorption of the
samples by the active carbon and the rinse step with NaNO3solution. The sample preparation
must in this case be continued to the end with syringe pistons inserted. Otherwise the system
would aspire air during the rinse setp instead of automatically dosing the rinse solution.
1. Empty the waste container, if necessary.
2. If necessary, fill the storage bottle for the rinse solution with nitric sodium nitrate solution
(pH ≈ 2).
3. Place the storage bottle into the adapter of the APUsim. Immerse the rinse tube (no. 1) in
the rinse solution.
4. Fill the AOX columns with disposable tubes or quartz containers (with 50 mg active carbon
each). Screw the AOX columns together.
5. Attach the AOX columns via the Luer lock to the respective channel of the APUsim.
6. Slide the drainage channel directly under the column units.

Operation
18 APUsim
Note: There is a risk of splashing if the drainage channel is located too low under the col-
umn unit.
7. Fill the plastic syringes with the desired volume of the acidified samples. Insert the syringes
into the APUsim. Ensure the tight closure of the connection using the sealing ring.
8. Switch on the APUsim from the mains switch at the equipment backplate.
The display shows the start window.
9. Configure the sample volume, rinse volume and dosing speed (see "Configuring the pa-
rameters for the sample preparation" p. 16). Configure the sample volume to be identical to
the sample volume in the syringe.
10. Start the desired pump units by pressing the start buttons.
The sample preparation (adsorption, rinsing) takes place automatically.
The processing time is indicated in the start window. It is composed as follows:
Processing time Example
Vsample = 50 mL, Vrinse . = 25 mL, vdosing = 3 mL/min
Sample dosing time 1000 s
+ 10 % dosing time as buffer + 100 s
Rinse solution dosing time 500 s
+ time for dosing 1 mL rinse solution as buffer + 20 s
+ 4 s for valve change-over + 4 s
1624 s ≙27 min 4 s
Display in the start window 27:04
7.4 Manual sample preparation for samples with particles
The manual sample preparation is recommended for samples with high particle loads. Here,
there is a there is a risk that some parts of the sample sediment in the syringe and thus escape
the AOX determination. Unlike with automatic sample preparation, the rinse solution is therefore
dosed manually into the open syringe. The two process steps (adsorption, rinse) are started
individually via the control software.
1. Empty the waste container, if necessary.
2. If necessary, fill the storage bottle for the rinse solution with nitric sodium nitrate solution
(pH ≈ 2).
3. Place the storage bottle into the adapter of the APUsim. Immerse the rinse tube (no. 1) in
the rinse solution.
4. Fill the AOX columns with disposable tubes or quartz containers (with 50 mg active carbon
each). Screw the AOX columns together. Use a pre-column, if necessary.
Note: With a high particle load a pre-column with a suitable filter material can prevent the
system from clogging.
5. Attach units with the AOX columns via the Luer lock to the respective channel of the
APUsim.