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User Manual Ammonia Analyzer
SIWP-Z0-MAN-0004-0085B 02

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Vendor Logo Vendor Document Document Title: Rev: 02


number:
User Manual Ammonia Analyzer
1092 User Manual
Envirolyzer II - Ammonia Date:
R2
10/08/17
SOHAR IWP
NOTES:

(1) Purchase order nº as shown on purchase order

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User’s Manual
EnviroLyzer® Ammonia
Series of on-line Ammonia analyzers

Serial number: 012.1092.1704.050


User’s Manual
EnviroLyzer® Ammonia
Series of on-line Ammonia analyzers

© 2014 – AppliTek NV – Printed in Belgium

All rights reserved. No part of this manual may be reproduced, stored in a retrieval system or
transmitted in any form or by any means - electronic, mechanical, photocopying, recording or
otherwise - without the prior written permission of AppliTek NV.

The content of this document is entirely a non-binding external opinion. AppliTek NV nor any
of its employees can be held liable for damages to people, third parties, goods and assets,
that may result from implementing the content.
CONTENTS
Preface – Documents and safety ................................................................................................ 8
Installation of the analyzer – Overview ................................................................................. 9
1. Installation of the analyzer ............................................................................................... 10
1.1 Dimensions of the analyzer ....................................................................................... 10
1.2 Location and ambient conditions ............................................................................... 11
1.3 Mounting instructions ................................................................................................ 11
2. Power and signals ............................................................................................................. 11
2.1 Power ......................................................................................................................... 11
2.2 Signals ....................................................................................................................... 12
3. Utilities ............................................................................................................................. 13
3.1 Overview ................................................................................................................... 13
3.2 Sample feed ............................................................................................................... 13
3.3 Rinse feed .................................................................................................................. 13
3.4 Drain .......................................................................................................................... 13
3.5 Overflow .................................................................................................................... 14
3.6 Reagents & Calibration/validation solutions feed ..................................................... 14
3.7 Instrument air ............................................................................................................. 14
4. Power up & components test ............................................................................................ 15
4.1 Analyzer design ......................................................................................................... 15
4.2 Wet chemical components ......................................................................................... 16
4.3 Analog output ............................................................................................................ 19
4.4 Analog input .............................................................................................................. 20
5. Analyzer method .............................................................................................................. 22
5.1 Specifications............................................................................................................. 22
5.2 Analysis ..................................................................................................................... 22
5.3 Calibration ................................................................................................................. 23
5.4 Cleaning ..................................................................................................................... 24
5.5 Prime.......................................................................................................................... 24
6. Reagent preparation....................................................................................................... 25
6.1 Reagent consumption ............................................................................................. 25
6.2 Storage and quality of chemicals and solutions ..................................................... 25
6.3 Reagent A solution ................................................................................................. 26
6.4 Reagent B solution ................................................................................................. 27
6.5 Calibration standard solution ................................................................................. 28
6.6 Cleaning solution ................................................................................................... 28
7. Start-up of the analyzer .................................................................................................... 29
7.1 Access ........................................................................................................................ 29
7.2 Prime the reagents ..................................................................................................... 29
7.3 Method navigation ..................................................................................................... 30
7.4 Calibration ................................................................................................................. 35
7.5 Cleaning ..................................................................................................................... 35
7.6 Time List.................................................................................................................... 36
7.7 Data and results ......................................................................................................... 37
7.8 Analyzer settings ....................................................................................................... 38
7.9 Start-up the analyzer for on-line measurement.......................................................... 39
8. Maintenance ..................................................................................................................... 40
8.1 Check for leaks and abnormal conditions.................................................................. 40
8.2 Check for alarms ........................................................................................................ 40
8.3 Prepare reagents and fill the reagent containers ........................................................ 40
8.4 Run the calibration program ...................................................................................... 41
8.5 Replace duckbills ....................................................................................................... 41
8.6 Replacement of the peristaltic pump tubing .............................................................. 41
8.7 Replace dispenser piston ........................................................................................... 42
8.8 Replace dispenser valve............................................................................................. 42
8.9 Shutdown of the analyzer for a longer period ........................................................... 43
9. Troubleshooting ............................................................................................................... 43
10. Spare Parts ..................................................................................................................... 43
Addendum ................................................................................................................................ 44
Addendum 1: Analysis Procedure ............................................................................................ 44
1.1 Ammonia – Method 1 – Analysis .............................................................................. 44
1.2 Ammonia – Method 1 – Cleaning ............................................................................. 45
1.3 Ammonia – Method 1 – Priming ............................................................................... 46
Addendum 2: Configuration..................................................................................................... 47
2.1 Digital Outputs .......................................................................................................... 47
2.2 Digital Inputs ............................................................................................................. 47
2.3 Analog Inputs ............................................................................................................ 47
2.4 Analog Outputs .......................................................................................................... 47
2.5 Dispensers .................................................................................................................. 47
2.6 Results ....................................................................................................................... 48
2.7 Results Calibration .................................................................................................... 48
2.8 Results Calculation .................................................................................................... 48
2.9 Results Analog output ............................................................................................... 49
2.10 Results Stream output ............................................................................................ 49
2.11 Result Alarms......................................................................................................... 49
2.12 Results Graph ......................................................................................................... 49
2.13 Alarm and message table ....................................................................................... 49
2.14 Group DO............................................................................................................... 49
Addendum 3: Alarms and signals ............................................................................................ 50
3.1 Alarms ....................................................................................................................... 50
3.2 Signals ....................................................................................................................... 50
Warranty ................................................................................................................................... 51
Preface – Documents and safety
Thank you for purchasing this high quality analytical instrument. The analyzer is designed for
installation in industrial environments and intended for professional use. On delivery the
analyzer does not offer readily available end-user functionality. The analyzer needs to be
installed and configured by competent staff prior to use by the end user. Information about
the exact specifications, necessary connections, utilities and maintenance schedules is given
in the accompanying GENERAL SAFETY BOOK (8 languages).

General safety instructions


AppliTek and/or its affiliates use their best efforts to deliver a high quality analytical
instrument and reliable software packages. AppliTek nor its affiliates cannot be held
responsible for any damage that may result from the incorrect use of the software and
hardware, use outside the scope of the analyzer’s specification, misinterpretation of the
safety instructions, errors or deliberate modifications made to the analyzer; in addition, any
warranty issued by AppliTek becomes void.

• Knowledge of the basic safety regulations is essential for the safe handling and
disruption-free operation of the unit. Therefore, please read the entire manual before
setting up the analyzer. Pay attention to danger and caution statements;
• These operating instructions contain the most important guidelines necessary in order
to safely oversee the unit’s operation;
• All persons working on the unit should take note of these operation instructions, and
especially those relevant to safety;
• Protect the analyzer from impacts causing corrosion or preventing components from
working properly;
• Have faulty parts of the analyzer replaced immediately;
• Spare parts must comply with the technical requirements determined by AppliTek;
• When malfunctioning, take the analyzer out of operation. Repair the malfunctions
immediately. Failure to do so could result in serious injury to persons or damage to
the equipment;
• On top of this, all rules and regulations pertinent to accident prevention, which are
applicable at the measuring site, are to be followed.
• It is the operator’s responsibility to allow only those persons to work on the unit who
are familiar with the regulations concerning safe handling and have been informed
how to work with the instrument;

Safety devices
Before any initialization of the unit, all safety devices must be properly mounted and
functional. Safety devices can only be removed:

• During maintenance and repair work by trained personnel or when the unit has been
disconnected from the electrical mains.
• After the unit has been safeguarded against renewed operation.

Electrical dangers
Work on the unit’s power supply and electronics can only be carried out by a qualified
electrician. The mains switch must be switched off during work on electrical components.

8
Installation of the analyzer – Overview

9
1. Installation of the analyzer

1.1 Dimensions of the analyzer

10
1.2 Location and ambient conditions
The analyzer is designed for installation at indoor environmental conditions. Install the
analyzer where the temperature is maintained as stable as possible between 10 and 30 °C
(range 4°C) and is not subject to sudden temperature changes.

The analyzer should be installed as close as possible near the sampling point. If this is not
the case, a fast loop sampling system has to be installed because a long distance between
the analyzer and the sampling point will increase the response time of the analyzer.

Do not mount the analyzer in direct sunlight! This can affect the visibility of the screen
and the analyzer, its components and reagents.

Other points of attention are: - humidity: 5 – 95 % non-condensing


- avoid corrosive atmospheres

Variation of these conditions can seriously affect the analyzer results and damage the
analyzer and its components!

1.3 Mounting instructions


The analyzer is designed for wall mounting and intended for permanent installation. Make
sure the location is easy accessible. The dimensions of the analyzer are given on the
previous page. The indicated footprint is a strict minimum and doesn’t take into account the
space needed for tubing and cables.

The analyzer has four mounting holes for screws M8x10mm at the back of the cabinet.
These bolts are fastened into/onto the supporting structure from the inside of the electrical
cabinet at the back.

This analyzer has to be installed by qualified technical personnel to ensure adherence


to all applicable electrical plumbing requirements.

2. Power and signals

2.1 Power
First open the electrical cabinet door by pulling the two levers and unhook them. Make
provisions for removing power to the analyzer during servicing. The AC power cable enters
on the left side of the cabinet at the back through the upper left cable gland. The terminals for
the power and ground are located at the upper left hand corner of the cabinet at the back, as
you face the unit. Connect your wiring to the upper side of the terminals. Connect the AC
feed as follows:

- The protective ground at the yellow/green terminal block.


- The hot/line (L) and neutral (N) wire are to be connected at the circuit breaker.

Terminal North American wire color European wire color


Protective Ground (PE) Green Green/yellow
Hot/line (L) Black Brown
Neutral (N) White Blue

11
2.2 Signals
External 24Vdc power supply

Note: If additional AO, DI or DO connections are required, extra terminals will be present.

Connections:

AO1-AO2: Analog Outputs


4-20mA, active current, loop
powered from the analyzer
max. load 500R

FCT1-FCT5: Free ConTacts


(digital output)
Relay output, contact loading
max. 24VDC/0,5A

PCT1-PCT4: Power ConTacts


(digital outputs)
24VDC/0,5A output

INP1-INP4: INPut
(digital input)
24VDC, to trigger with external
potential free contact

CONTACT INPUT/OUTPUT NAME 24VDC, only to be


AO1 AO1 Result Ammonia used for external
FCT1 DO25 Malfunction control (max load 1A)
FCT2 DO26
FCT3 DO27
FCT4 DO28
FCT5 DO29
PCT1 DO21
PCT2 DO22
PCT3 DO23
PCT4 DO24
INP1 DI1
INP2 DI2
INP3 DI3
INP4 DI4

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3. Utilities

3.1 Overview
Consumption/ Consumption/28 days
Comment Connection
analysis (1 analysis/20 min)
Atmospheric
Sample ~30 ml ~60 L 1/8”
pressure
Atmospheric
Rinse water ~40 ml < 85 L 1/8”
pressure
Atmospheric
Dilution water ~12 ml < 30 L 1/8”
pressure
Vent / / Free 1/4”
Atmospheric
Reagents See Chapter 6 See Chapter 6 1/8”
pressure

3.2 Sample feed


The sample feed to the analyzer must be at atmospheric pressure if the analyzer uses a
peristaltic pump for sampling. The sample feed to the analyzer must be higher than the
sample flow in the analyzer. It is recommended to use a small overflow vessel (next to the
analyzer) from which the analyzer will take fresh sample. Thus the sample in the overflow
vessel should be continuously refreshed. If the size of the solids present in the sample is too
high, it is recommended to filter the sample.

Connection: 1/8” OD tubing (PFA)


Location: Bottom side of the analyzer

The analyzer is not designed for use with samples that are explosive or flammable. If a
solution other than water is used, this solution should be tested to test the
compatibility with the instrument!

3.3 Rinse feed


The rinse solution should be on atmospheric pressure. The rinse solution (de-mineralized
water) has to be connected to the rinse valve.

Connection: 1/8” OD tubing (PFA)


Location: Bottom side of the analyzer

3.4 Drain
The analyzer needs a drain to discharge both sample and reagents after analysis. A floor or
sink drain is satisfactory, but it must be unrestricted and located at a lower level than the
analyzer so that gravity will carry away the liquid. The drain must have a vent to the
atmosphere and the drain tube from the analyzer must not be submerged. Pay attention that
the drain line is never blocked. A water connection is also recommended so that the drain
sink and piping is regularly flushed with clean water in order to avoid clogging due to
crystallization. Steepness of the draining pipe must be sufficient.

Drain piping: recommended diameter of 32 mm,

Connection: 1/4” OD tubing (PFA)

13
Location: Bottom side of the analyzer

Although the chemical reagents are diluted, the user has to check that the external
drain/overflow system is appropriate for reagents and corrosive wastes! Used
reagents shall be treated for disposal according to national or local regulations!

3.5 Overflow
The analyzer needs an overflow tube in order to drain the analysis compartment in case of
leakage of sample fluids, reagent fluids (and combination of both) in the compartment. A floor
or sink drain is satisfactory, but it must be unrestricted and located at a lower level than the
analyzer so that gravity will carry away the liquid. The overflow tube from the analyzer must
not be submerged. Pay attention that the overflow line is never blocked. Steepness of the
overflow pipe must be sufficient.

Connection: 1/4” OD tubing (PFA)


Location: Bottom side of the analyzer

3.6 Reagents & Calibration/validation solutions feed


Connections have to be made between the reagent containers and the dispensers, the micro
pumps and the cleaning valve. The calibration/validation solutions can be connected to the
REF1/REF2 selection valve.

Connection: 1/8” OD tubing


Location: Bottom or left side of the analyzer

Although the chemical reagents are diluted, the user has to check that the external
drain/overflow system is appropriate for reagents and corrosive wastes! Used
reagents shall be treated for disposal according to national or local regulations!

Remark : Reagents are not supplied for start-up and commissioning.

3.7 Instrument air


The instrument air must be dry and dust free (according to ISA-S7.0.01-1996). The minimal
pressure of the instrument air necessary for the analyzer is 1 bar (100 kPa or 15.5 psi).
Instrument air is used for purging the analyzer in order to prevent corrosion by corrosive
gases such as chlorine gas from outside the analyzer.

Remark : If no corrosive gases are present, instrument air is not needed. AppliTek is not
responsible for corrosion if instrument air is not used.

Connection: 1/4” OD tubing (PFA)

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4. Power up & components test
The analyzer and its components must be tested before the unit can be put into online
service. Make sure that all necessary connections were made before testing the following
components. Switch on the analyzer by means of the circuit breakers lever in the electrical
compartment and (if present) the external power switch.

When connecting the power of the analyzer, the software is started up. First, the initial
startup screen appears. While this screen is visible, the parameters are loaded (loading of
methods, configuration …) and the dispensers are initialized. Next, the MAIN screen
becomes visible automatically.

Initial startup screen MAIN screen

4.1 Analyzer design

15
4.2 Wet chemical components
Menu path:
→ F2

In the Visualization (F2) submenu, the wet chemical components (reagent pumps, stirrer,
dispenser…) can be controlled manually. Press the icons on the screen to control the
components. A control panel appears on the right side of the screen. By use of this panel,
the chemical components can be controlled. Check if these components are working
properly.

1. Stirrer

Press the stirrer icon. Switch the stirrer


ON/OFF by pressing the ‘ON/OFF’ button. It
is also possible to turn the stirrer ON for a
specified time. Fill in the time (in seconds)
and press the ‘Start’ button.

16
2. Drain pump

Press the pump icon. Switch the pump


ON/OFF by pressing the ‘ON/OFF’ button. It
is also possible to turn the pump ON for a
specified time. Fill in the time (in seconds)
and press the ‘Start’ button.

The ‘Group’ function is implemented for


safety reasons. If for example a valve must be
opened before a pump is started, the group
action can be used, if programmed.

3. Sample pump

Press the pump icon. Switch the pump


ON/OFF by pressing the ‘ON/OFF’ button. It
is also possible to turn the pump ON for a
specified time. Fill in the time (in seconds)
and press the ‘Start’ button.

The ‘Group’ function is implemented for


safety reasons. If for example a valve must be
opened before a pump is started, the group
action can be used, if programmed.

When the sample enters because one or


more valves are switched, it is necessary to
switch these valves on before the sample
pump is started. Press the icon of the
corresponding valve. Switch the valve
ON/OFF by pressing the ‘ON/OFF’ button. It
is also possible to turn a valve ON for a
specified time. Fill in the time (in seconds)
and press the ‘Start’ button.

Next, press the sample pump and start the


sample pump.

17
4. Micropump

Press the micropump icon. Fill in the number


of pulses. Press ‘Pulse’ to start the
micropump. Press the ‘Stop’ button to stop
the micropump.

5. Dispenser

Press the dispenser icon.


Press the ‘Dose’ button to dose a certain
volume into the analysis vessel.
Press the ‘Fill’ button to fill the dispenser.
Press the ‘Empty’ button to empty the
dispenser.
Press the ‘Recycle’ button to recycle the
dispenser. The volume of the dispenser is
dosed into the reagent container.
Press the ‘Extract’ button to take a certain
volume from the analysis vessel.
Press ‘Stop’ to stop any action of the
dispenser.

6. Rinse pump

Press the pump icon. Switch the pump


ON/OFF by pressing the ‘ON/OFF’ button. It
is also possible to turn the pump ON for a
specified time. Fill in the time (in seconds)
and press the ‘Start’ button.

The ‘Group’ function is implemented for


safety reasons. If for example a valve must be
opened before a pump is started, the group
action can be used, if programmed.

Components that are not visible on the visualization screen can be controlled in the DO
submenu.

18
Menu path:

Select the digital output by use of the Edit


(E) button.

The value of the digital output can be toggled


manually with the ‘ON/OFF’ button. After
entering an activation time (seconds), the
‘START’ button can be pressed to activate
the digital output. The digital output will then
be active during the inserted number of
seconds. After entering a number of pulses,
the digital output will give the set number of
pulses.

Press ‘Stop’ to stop any action of the DO.


Press the arrow keys at the top of the screen
to select another DO.

Press ‘Back’ to quit the screen.

4.3 Analog output


Menu path:

Press the EDIT (E) button to control the


selected analog output.

Use a multimeter to check if the analog


output signal is working.

19
Insert a value by use of numeric keyboard
and confirm. Press Accept to update this
value.

Check if this value corresponds to the value


the multimeter is giving.

Check the ‘Installation Manual’ to make the


right connections.

4.4 Analog input


Menu path:

Check if all analog inputs are responding


correctly.

Press the EDIT (E) button to control the


selected analog input.

20
4.4.1 Photometer
The calibration of the photometer is
performed in demineralized water (media 1)

Put the sensor on 9V by use of the screw on


the right side of the photometer block.

Press enter to start calibration


Put sensor in media 1 and enter
Stabilizing, press enter to continue
Update calibration data

The ABS value is now put on 0 mAU.

When the analyzer is started for the first


time, or when the software is updated, the
dark value of the analyzer needs to be set.

Cover the light path of the photometer


Write down the value for the voltage

This value needs to be adjusted in the


configuration of the analyzer

21
5. Analyzer method

5.1 Specifications

Method: Colorimetric

Wavelength: 630 nm

Parameter: Ammonia

Range: 0 – 1 mg/L N-NH3


0 – 10 mg/L N-NH3 (by internal dilution)

Minimum detection limit: 0.005 mg/L NH₃

Precision: < 5 % of full scale range (on standard solutions)

Analysis time: < 20 minutes

Sample requirements: Atmospheric pressure, flow rate between 10 and 30 ml/minute,


sample temperature between 5 and 60 °C

Stream selection: Channel1: Stream 1 (Sample valve)


Channel9: REF1 (REF1 valve)
Channel10: REF2 (REF2 valve)

5.2 Analysis

The analyzer uses a colorimetric measurement for the detection of ammonia in the 0 – 1
mg/L NH₃.

The colorimetric determination of ammonia in water is based on the reaction of the


ammonium-ions with hypochlorite and a thymol component which forms a highly intensive
colored complex. This reaction takes place in a strong alkaline medium (pH>10). Sodium
nitroprusside is added as a catalyst to accelerate the reaction. Sodium tartrate is added to
prevent metal-hydroxide precipitation.

The analysis vessel is cleaned with fresh sample. Before the sample is analyzed, it is diluted
by an internal dispenser dilution system. After bringing the sample into the analysis vessel, a
precise sample volume is aspirated by the dispenser. The excess of sample is drained and
the analysis vessel is rinsed with demineralized water. Afterwards, the dispenser doses the
exact volume of sample and a volume of demineralized water in the analysis vessel.

22
Dispenser and sample loop are filled Dispenser tubing in contact with The analysis vessel is drained
With DI water (= start position) sample is purged by dosing an and then the dispenser is
amount of sample (~ 3 ml - moved downwards to extract
normally) an airgap (0.1 ml)
SIZE 17 SIZE 17
48 48 SIZE 17
48 M 48
48 M
48
48 48
48 M
SAMPLE
SAMPLE SAMPLE
SAMPLE SAMPLE
SAMPLE

SIZE 17 SIZE 17
SIZE 17
48 M 48 M
20-50
48 M
20-50
ml 20-50
RINSE
RINSE ml RINSE
RINSE ml RINSE
RINSE

STIRRER
SIZE 17
STIRRER
SIZE 17 Airgap SIZE 17
STIRRER
48 M 48 M 48 M
DRAIN
DRAIN DRAIN
DRAIN DRAIN
DRAIN

Dilution DI Dilution DI Dilution DI


water STEP 1 water STEP 2 water STEP 3
The analysis vessel is now filled Drain of the excess of sample and The dispenser is now filled with DI
with sample and the dispenser is extraction of the second airgap. water
moved downwards to extract a After draining of the sample the
certain amount of sample vessel is rinsed with DI water (2 x)
SIZE 17 SIZE 17
SIZE 17
48 48 48 48
48 M 48
48 M
48 48 M

SAMPLE SAMPLE SAMPLE


SAMPLE
SAMPLE
S A M P L E

SAMPLE
DI water
S A M P L E

SIZE 17 SIZE 17 SIZE 17


20-50 48 M 20-50 48 M 20-50 48 M
ml
Airgap 1 ml ml
RINSE
RINSE RINSE
Airgap 1 RINSE
R I N S E

RINSE
Sample Airgap 1 RINSE R I N S E

SIZE 17 SIZE 17 SIZE 17


STIRRER
Sample STIRRER Sample STIRRER
48 M
48 M 48 M
DRAIN
DRAIN Airgap 2 DRAIN
DRAIN
Airgap 2 DRAIN
DRAIN

Dilution DI Dilution DI
Dilution DI
water STEP 4 water STEP 5 water STEP 6

After sampling and dilution, the initial absorbance value is measured at 630 nm. Next, reagent
A and reagent B are added to the sample solution. After respecting a stirring period of 900
seconds – performed to obtain complete color development – the final absorbance value is
determined. With the obtained absorbance values, the ammonia concentration is calculated
according to Beer’s law.

Note:
The Lambert-Beer law states that the absorbance (A) is proportional to the concentration of the
absorbing molecules, the length of light-path through the solution and the molar absorptivity
coefficient.

A = Am * L * C

Am is the wavelength-dependent molar absorptivity coefficient


L is the length of the light-path through the solution
C is the analyte concentration

5.3 Calibration
The automatic calibration procedure measures a REF1 or 0 mg/L NH3 solution (channel 9)
and a REF2 or 10 mg/L NH3 solution (channel 10) to adapt the slope and offset factors by
means of a two point calibration.

23
5.4 Cleaning
The cleaning procedure should prevent any build-up of chemicals in the analyzer. To obtain
an effective cleaning procedure one has to test the cleaning solution and the cleaning
interval for each application. Perform the selected cleaning solution and interval for a trial
period, check then the effectiveness of the procedure and change if necessary.

5.5 Prime
The prime procedure can be used when starting up the analyzer or after a shutdown of the
analyzer: the reagent tubings are flushed with fresh reagent solution and the sample tubing
and the analysis vessel are flushed with fresh sample.

24
6. Reagent preparation
Warning:
Some of the chemicals used are corrosive or harmful! All
! operating personnel should wear protective gloves, goggles
and acid-proof clothing! Check the MSDS before starting to
handle the chemicals.

The information in this document is based on the present state of our knowledge and is
applicable to the products with regard to appropriate safety precautions. It does not guarantee
any of the properties of the products. AppliTek shall not behold liable for any damage resulting
from handling or from contact with any product described in this manual.

6.1 Reagent consumption

In the tables below, the products that are needed to prepare the reagents are listed. The
product name, the formula, the molecular weight, the CAS No. and the amount needed to
prepare 1 liter of the reagents is given. Check the consumption of the reagents (28 days) to
adapt the volumes needed.

Consumption/28 days Recommandable


Product Consumption
(1 analysis/ 20min) container
Reagent A solution ~ 1.0 ml / analysis ~2L Glass – 2.5L
Reagent B solution ~ 1.0 ml / analysis ~2L Glass – 2.5L
Calibration solution
~ 30 ml N.A. N.A.
REF1
Calibration solution
~ 30 ml N.A. N.A.
REF2

6.2 Storage and quality of chemicals and solutions

Quality of chemicals:
All chemicals should be of ACS grade or better. We recommend the use of pro analysis
chemicals.

Quality of water:
Reagent grade, ammonia-free de-ionized water must be used to prepare the chemical
solutions and for rinse purposes.

Waste treatment:
Used reagents shall be treated for disposal according to national or local regulations.

Contamination due to vapors:


Contamination due to atmospheric nitrogen (example: ammonia vapors) can significantly
influence the analysis results. To minimize this contamination, reagent A and reagent B
should be stored at low temperature (< 6 °C) for longer periods (more than 1 week).

25
6.3 Reagent A solution

Product Formula MW (g/mol) CAS No. 1 liter solution


Sodium Hydroxide NaOH 40.00 1310-73-2 40 g
Sodium hypochlorite
NaOCl 74.44 7681-52-9 40 ml
solution (6 – 14%)
Di-sodium tartrate
C4H4Na2O6.2H2O 230.08 6106-24-7 62 g
dehydrate

Sodium hydroxide

Hazard statement(s):
H314: Causes severe skin burns and eye damage.

Precautionary statement(s):
P280: Wear protective gloves/ protective clothing/ eye protection/ face protection.
P305 + P351 + P338: IF IN EYES: Rinse cautiously with water for several minutes. Remove contact
lenses, if present and easy to do. Continue rinsing.
P310: IF exposed or if you feel unwell: immediately call a POISON CENTER or
doctor/physician.

Sodium hypochlorite solution (6 – 14%)

Hazard statement(s):
H314: Causes severe skin burns and eye damage.
H400: Very toxic to aquatic life.

Precautionary statement(s):
P273: Avoid release to environment.
P280: Wear protective gloves/ protective clothing/ eye protection/ face protection.
P305 + P351 + P338: IF IN EYES: Rinse cautiously with water for several minutes. Remove contact
lenses, if present and easy to do. Continue rinsing.

Di-sodium tartrate dihydrate

Not a hazardous substance or mixture according to Regulation (EC) No. 1272/2008. This substance is
not classified as dangerous according to Directive 67/548/EEC.

Preparation:
Dissolve 40 g sodium hydroxide (NaOH) and 62 g di-sodium tartrate dihydrate
(Na2C4H4O6.2H2O) in 500 ml demineralized water and add 40 ml sodium hypochlorite
solution (NaOCl with 6 – 14 % active chlorine). Dilute to 1 liter with demineralized water.

Note1: The minimum amount of active component of bleach should be > than 6% (60 g/l)
To determine this activity:
1) Dilute the bleach with factor 100 (1 ml bleach solution in 100 ml bidest. Water)

26
2) Take 20 ml of this sample
3) Add 1 ml of a 1M Nitric Acid solution
4) Add approx. 3 g of potassium iodide to this sample. The sample will turn into a yellow-
brown color.
5) Titrate with 0.01M thiosulfate until the solution turns colorless again.
6) Calculate the amount of active Cl2 component:
Gram Cl2/l 100

Note2: If the reagent is stored in a completely closed (brown) bottle, the reagent can be
stored for one month (fridge).

This solution is stable for 2 weeks.

6.4 Reagent B solution

Product Formula MW (g/mol) CAS No. 1 liter solution


Sodium salicylate HOC6H4COONa 160.00 54-21-7 80 g
Na2[Fe(CN)5NO] ·
Sodium nitroprusside
2H2O 297.96 13755-38-9 1g
dihydrate

Sodium salicylate

Hazard statement(s):
H302: Harmful if swallowed.
H315: Causes skin irritation.
H319: Causes serious eye irritation.
H335: May cause respiratory irritation.

Precautionary statement(s):
P261: Suspected of damaging fertility or the unborn child.
P305 + P351 + P338: IF IN EYES: Rinse cautiously with water for several minutes. Remove contact
lenses, if present and easy to do. Continue rinsing.

Sodium nitroprusside dihydrateAmmonium hydroxide solution

Hazard statement(s):
H301: Toxic if swallowed.

Precautionary statement(s):
P301 + P310: If swallowed: immediately call a POISON CENTOR or doctor/physician..

Preparation:
Dissolve 80 g sodium salicylate (C7H5NaO3) and 1 g sodium nitroprusside dihydrate
(Na2[Fe(CN)5NO].2H2O) in 500 ml demineralized water and dilute to 1 liter with
demineralized water.

27
This solution is stable for 2 weeks at ambient temperature.

Note1: If the reagent is stored in a completely closed (brown) bottle, the reagent can be
stored for one month (fridge).

6.5 Calibration standard solution

Product Formula MW (g/mol) CAS No. 1 liter solution


Ammonium Chloride NH4Cl 53.49 12125-02-9 3.141 g

Ammonium Chloride

Hazard statement(s):
H302: Harmful if swallowed.
H319: Causes serious eye irritation.

Precautionary statement(s):
P305 + P351 + P338: IF IN EYES: Rinse cautiously with water for several minutes. Remove contact
lenses, if present and easy to do. Continue rinsing.

Preparation:
1000 mg/L NH₃ stock solution
Prepare a stock solution of 1000 mg/L NH₃: Dissolve accurately 3.141 g ammonium chloride
in 300 ml de-ionized water using a volumetric flask of 1000 ml. Fill op to 1 liter with de-ionized
water.

10 mg/L NH₃ standard solution – REF2


Prepare a standard solution of 10 mg/L NH₃: take accurately 10 ml of the 1000 mg/L NH₃
stock solution and transfer into a volumetric flask of 1000 ml. Add de-ionized water up to the
mark grade.

0 mg/L NH₃ standard solution – REF1


Prepare a standard solution of 0 mg/L NH₃. Use de-ionized water.

6.6 Cleaning solution

The cleaning procedure should prevent any build-up of chemicals in the analyser. To obtain
an effective cleaning procedure one has to test the cleaning solution and the cleaning
interval for each application. Perform the selected cleaning solution and interval for a trial
period, check then the effectiveness of the procedure and change if necessary.

28
7. Start-up of the analyzer

7.1 Access
Menu path:
→ F1 → User → Enter Access password

Press the black box next to ‘User:’ to change the userlevel by use of the corresponding
password.

Depending on the userlevel some menus are accessible and some are not. Normally, when
the analyzer is started up, the ‘Automatic’ userlevel appears. This level is also used in
online situations. The analyzer is locked, which means that the METHOD (F4) and CONFIG
(F5) menu are not accessible. If modifications of the software are needed, higher userlevels
can be used. The access to certain crucial parameters is only given if the ‘Administrator’
password is used. Enter the password by pressing the ‘Enter Access password’ button.

Default passwords:

User Password
Automatic -
User1 a
User2 b

7.2 Prime the reagents


Menu path:
→ F1 → 1.Method → Priming

Select the method with the navigation buttons at the bottom of the MAIN (F1) screen. The
method screen appears.

29
If all wet chemical components are working properly, the reagents can be connected to the
analyzer. Press the ‘Priming’ button to fill up all tubings to the analysis vessel with reagent
Make sure there is no air present in the tubings. Also, make sure there is no air present in
the dispenser, the tubing to the dispenser and the tubing from the dispenser to the analysis
vessel.

7.3 Method navigation


Follow the procedure below to start the method. It is recommended to run the method
several times and to make sure the measurements are stable before a calibration of the
analyzer is performed. Make sure all flushing times are set correctly before the analyzer is
started for on-line measurement.

Menu path:
→ F1 → 1.Method

Select the method with the navigation buttons at the bottom of the MAIN (F1) screen. The
method screen appears.

Menu path:
→ F1 → Method → Playlist → Automatic sequence

Press the Playlist button. Press the Automatic sequence button and insert the desired
module, channel and number of analysis. Press Accept to confirm. Press Back to quit the
window without saving the changes.

Start parameters:

Module: Analysis, Preconditioning, Cleaning, Priming, Init, and Exit.


CH: Automatic sequence or channel 1 to 10
# Runs: Insert the number of runs of the module (0 = Continuous analysis)
Comment: Add a comment concerning the analysis (Optional). This comment will also be
displayed in the data table.

30
7.3.1 Single stream analysis
- Module: select Analysis
- CH: insert the number of the stream
(Sample = stream 1 – 8; REF1 = stream 9; REF2 = stream 10)
- #Runs: insert the desired number of runs (=1 for single stream analysis)

- Continuous analysis: insert 0 as #Runs in the method main screen


- Fixed number of analysis: insert the desired #Runs in the method main screen

For example:
- The third sample stream needs to be analyzed
- Insert ‘3’ as channel (CH) and 1 as #Runs

7.3.2 Single stream analysis with cleaning


- Module: select the desired module (Analysis or Cleaning)
- CH: insert the number of the stream
(Sample = stream 1 – 8; REF1 = stream 9; REF2 = stream 10)
(For cleaning, always use channel 1)
- #Runs: insert the desired number of runs (=1 for single stream analysis)

Repeat for each stream that needs to be analyzed.

- Continuous analysis: insert 0 as #Runs in the method main screen


- Fixed number of analysis: insert the desired #Runs in the method main screen

31
For example:
- There one streams that need to be analyzed. After 10 analysis, a cleaning is needed.
- Insert ‘Analysis’ as Module, ‘1’ as channel and ‘10’ as #runs
- Insert ‘Cleaning’ as Module, ‘1’ as channel and ‘1’ as #runs
(For cleaning, always use channel 1)

7.3.3 Multiple stream analysis


- Module: select Analysis
- CH: insert the number of the stream
(Sample = stream 1 – 8; REF1 = stream 9; REF2 = stream 10)
- #Runs: insert the desired number of runs (=1 for single stream analysis)

Repeat for each stream that needs to be analyzed.

- Continuous analysis: insert 0 as #Runs in the method main screen


- Fixed number of analysis: insert the desired #Runs in the method main screen

For example:
- There are five streams that need to be analyzed.
- Insert ‘1’ as channel and 1 as # runs
- Insert ‘2’ as channel and 1 as # runs
- Insert ‘3’ as channel and 1 as # runs
- Insert ‘4’ as channel and 1 as # runs
- Insert ‘5’ as channel and 1 as # runs

7.3.4 Multiple stream analysis with cleaning


- Module: select the desired module (Analysis or Cleaning)
- CH: insert the number of the stream
(Sample = stream 1 – 8; REF1 = stream 9; REF2 = stream 10)
(For cleaning, always use channel 1)
- #Runs: insert the desired number of runs (=1 for single stream analysis)

Repeat for each stream that needs to be analyzed.

- Continuous analysis: insert 0 as #Runs in the method main screen


- Fixed number of analysis: insert the desired #Runs in the method main screen

32
For example:
- There are two streams that need to be analyzed. Next, a cleaning is needed.
- Insert ‘Analysis’ as Module, ‘1’ as channel and ‘1’ as #runs
- Insert ‘Analysis’ as Module, ‘2’ as channel and ‘1’ as #runs
- Insert ‘Cleaning’ as Module, ‘1’ as channel and ‘1’ as #runs
(For cleaning, always use channel 1)

7.3.5 Start the method


Menu path:
→ F1 → 1.Method1 → Playlist → Start

7.3.6 Stop the method

Menu path:
→ F1 → 1.Method1 → Stop

Press the ‘Stop’ button. The method will be finished and the analyzer will stop (status will
change from ‘Run’, to ‘Stopped’ and then ‘Ready’).

33
Menu path:
→ F1 → 1.Method1 → Abort

Press the ‘Abort’ button to stop the method immediately after confirmation.

Menu path:
→ E-Stop

In case of emergency, all methods can be stopped directly by pressing the E-STOP button
(SOFTWARE emergency stop) at the bottom of the screen.

7.3.7 Remote control


Menu path:
→ F1 → 1.Method1 → Is Master

Press the ‘Is Master’ button. The following instruction screen appears. Press ‘Toggle’ to put
the analyzer in ‘Is Slave’ position. If the method is in this position, it is impossible to start the
method manually. The method can only be started remotely i.e. by a digital input, by Modbus
communication, by a sequence…

Press Abort to stop the method. Press the ‘Is Slave’ button to put the analyzer in ‘Is Master’
position again.

34
7.4 Calibration
Once the analysis results are stable, the analyzer can be calibrated.

Menu path:
→ F1 → Method → Calibrate

Press the ‘Calibrate’ button. The calibration procedure will start automatically after
confirmation. The ‘Chloride’ method starts from the submenu ‘calibration’.

The calibration procedure consists of following steps:

- Number of runs (REF1): 3x


- Number of runs (REF2): 3x

The number of runs is programmable in the Configuration (F5) menu (See Configuration
Manual for more information).

Press the ‘Calibration history’ button to get an overview of the previous calibration data.

7.5 Cleaning
Menu path:
→ F1 → Method → Cleaning

To clean the analyzer (the analysis vessel) press the ‘Cleaning’ button. The cleaning
subroutine will be executed and the analyzer is stopped.

When the analyzer is on-line, the cleaning procedure starts after the Analysis subroutine is
finished. The analyzer is started again for on-line measurements after the Cleaning
subroutine is finished.

35
7.6 Time List
Menu path:
→ F1 → Method → Time list

Press the Time list button to configure the time list. An overview of the configured time tables
is displayed. Scroll through the list by use of the arrow keys.

Press the Edit (E) button to configure the selected time table. Every time table can be turned
ON or OFF by pressing the toggle (T) button.

Make sure the ‘Direct’ button is selected to guarantee the proper functioning of the Time list.
Press Back to quit the screen.

7.6.1 Configuration of the time list


Only a configured time list can be used. Make sure the time list is turned ‘ON’ and the
‘Direct’ button is selected.
Refer to the Configuration manual for additional information about the configuration of the
time list. Press Accept to confirm. Press Back to quit the screen.

Example:
An automatic calibration on stream 1 of
method 1 is needed, every day at 12 o’clock.

- HH: 12
- Channel: 1
- Start function: Calibration
- Index: Method1

36
7.7 Data and results
Menu path:
→ F3 → Database

The analysis results of every method are displayed in the ‘Database’ submenu. A method
can be selected by use of the arrow keys at the right side of the screen. Press the Edit (E)
button to view the result for the selected method. The arrow keys on the right side of the
screen can be used to scroll through the list.

The file can be exported to a memory stick by pressing the ‘Export’ button. The data are
exported to a CSV-file that can be opened for example in EXCEL.

Menu path:
→ F6

The course of a titration can be followed in the F6 submenu. Select the titration algorithm by
use of the dropdown menu. The graph can be appointed by use of the alphanumeric
keyboard. The screen can be copied to an USB stick by pressing the Export button. Press
the orange arrow key to view the titration data table. The titration algorithm can be selected
by use of the dropdown menu.

37
7.8 Analyzer settings
Adjustments to the analyzer configuration are made in the Configuration (F5) menu. We
recommend you to read the instructions very carefully before making adjustments to the
analyzers configuration: the functioning of the analyzer may be disturbed!

For more information about the analyzer settings, refer to the Configuration Manual.

7.8.1 Adaptation of intervals


Menu path:
→ F5 → Software → CH Interval

The time set in a channel interval is channel dependent. Change this time in order to
extend/reduce for example the flush time of the sample through the analysis vessel.

Repeat for every channel (sample stream) if necessary.

7.8.2 Adaptation of constant values


Menu path:
→ F5 → Software → Constants

Constant values are used in the calculation of the results. Change these values if necessary.

7.8.3 Adaptation of Sample Group DO times


Menu path:
→ F5 → Software → Group DO → E (Edit)

Group actions are implemented to run several actions simultaneously. Be careful when
changing the ‘group DO’ settings, the functioning of the analyzer may be disturbed.

38
Select the ‘group DO’ by use of the arrow keys and press the Edit button to change the
settings.

The times are entered in millisecond (ms). To avoid problems with analyzer functioning, only
change the time with the greatest value. Press Accept to save the settings. Test the changes
before starting the analyzer for on-line measurements.

7.8.4 Adaptation of algorithms


Menu path:
→ F5 → Software → Algorithms

Settings for algorithms are configured in the AppliTek lab with standard solutions.
Depending on the problems that occur in the field, other settings need to be adapted.

For more information about the algorithm settings, refer to the Configuration Manual.

7.9 Start-up the analyzer for on-line measurement


The analyzer is now set-up and ready to go online. Make sure all analyzer components are
working properly and all settings are correct before the analyzer is started.

39
8. Maintenance
Task Daily Weekly Monthly Quarterly Annually
Check for leaks and abnormal
X X X X X
conditions
Check for alarms X X X X X
Prepare reagents and fill the
X X X
reagent containers
Run the calibration program (X) (X) X
Replace the duckbills X
Replace all peristaltic pump
X X
tubing
Replace all pinch valve tubing X
Replace all tubing X
Replace valve and piston of the
X
dispensers

Perform a regular inspection of the analyzer to ensure proper performance.

8.1 Check for leaks and abnormal conditions


It is recommended that the instrument and preconditioning system is inspected visually on a
regular basis in order to guarantee the correct functioning of the system and to check the
integrity of the output.

• Check all the components in the analysis compartment, the outside connectors and tubings
for leaks.
• Confirm sample flow by checking the constant delivery of the sample
• Check the liquid levels in the reagent and standard solution containers
• Check if all the components in the analyzer cabinet are functioning (pumps, valves,
dispensers, photometer/electrode and stirrer). The photometer/electrode can be checked
by checking if the measurement values are normal. If not, double-check by performing a
calibration.
• Check the air pressure.

8.2 Check for alarms


Check the alarm page on the touch screen PC for alarms.

8.3 Prepare reagents and fill the reagent containers


Use reagents supplied by AppliTek or a qualified company or prepare them yourself by
following the instructions in chapter 6. Refill the reagent containers with the fresh made
reagents or use supplied reagents. Make sure that the tubings reach the bottom of the
reagent containers.

Never pour the fresh reagents in containers with old reagents!


Dispose the old reagents before pouring new reagent into its specific container.

Note:
• The consumption of the standard solutions depends on the frequency of the calibration
cycle programmed.

40
• The consumption of the cleaning solution depends on the frequency of the cleaning cycle
programmed.

8.4 Run the calibration program


Refer to chapter 7.4 if analysis results are not as expected.
Refer to chapter 7.6 to program the automatic calibration procedure.

8.5 Replace duckbills


• Open the electrical cabinet of the analyzer.
• Disconnect the micropump and remove the old duckbill valves. Keep in mind their original
position.
• Place the new duckbill valves in the same position as the previous duckbills. Be careful the
duckbills are tightened well when reconnecting the micropump.

8.6 Replacement of the peristaltic pump tubing


• Unfasten the wingnuts that fix the peristaltic pumps onto the electric motor coupler.
• Remove the pump head.
• Separate the front pump half from the back half. Hold the pump axle and the back pump
half together (1a).
• Remove the tubing. Keep in mind the length of both endings coming out of the pump head.
• Cut new tubing of the same size at the same length of the old one.
• Assemble the tube in the exact same way the old one was placed and push it down the
back pump half in front of the pump axle rollers. Then twist the pump axle a bit while you
keep pushing the tubing down so it is pressed between the pump housing and the pump
axle rollers (1b +1c).
• Join the two pump halves and make sure the tubing is not squeezed between the two
halves (1d).
• Place back the pump head and align the pump axle with the motor axle by pushing it
against the motor axle while turning the pump axle with a screwdriver.
• Fasten the wingnuts.
• Activate the pump and check if it is running properly.

41
8.7 Replace dispenser piston
• Flush the dispenser piston with DI water (to remove the reagent).
• Empty the dispenser.
• Put the dispenser in the middle position (first fill and then dose 2.5 ml).
• Remove the piston pin at the base.
• Carefully unscrew the piston from the luer lock fitting while pulling down slowly.
• Replace the old piston with a new one. Screw the piston onto the fitting while pushing
upwards slightly.

8.8 Replace dispenser valve


• Clean the dispenser with DI water (to remove the reagent).
• Fill the dispenser with air (remove the DI water).
• Power down the analyzer.
• Remove tubing and piston.
• Remove the valve by loosening the two screws on the valve.
• Install the new valve by aligning the D-coupler on the valve stem with the D-hole in the
encoder.
• Rotate the valve body so that the luer lock fitting is oriented towards the bottom of the
pump.
• Gently put the valve in place ensuring the locating pins on the frame side of the valve body
in the holes and replace the screws.
• Power up the analyzer and refill the dispenser with reagent.
• Start the analyzer and check for leaks.

42
8.9 Shutdown of the analyzer for a longer period
If the analyzer is stopped for a longer period (more than 1 day), it is recommended to rinse
the sample tubing, the reagent tubing, the dispensers and the analysis vessel with de-
mineralized water or a cleaning solution. In order to increase the lifetime of the electrodes, it
is recommended to take out the electrodes and store them with the original electrode cap. To
prevent evaporation of the electrolyte in the electrode, the electrode cap has to be filled with
electrolyte. Storage of the electrodes in de-mineralized water will significantly decrease the
lifetime of the electrodes.

9. Troubleshooting
If analysis results are unstable the following items should be checked:

a) Micropumps: make sure the reagents are dosed correctly and that no air is present in the
tubings

b) Peristaltic pumps: check if the drain, Rinse and sample pump are working correctly

c) Valves: make sure the sample/REF1/REF2/Clean valves are working correctly

d) Stirrer: check if there is a magnetic stirrer bar in the analysis vessel and if the solution is
stirred during analysis

e) Dispenser: Make sure the dispenser piston is filled with liquid and that no air is present in
the tubings

f) Check the positioning of the tubings inside the analysis vessel


• The drain tubing must be positioned at the back side of the analysis vessel and in
the ringlets.
• The dispenser tubing must be positioned in the liquid after sampling, but not in
front of the light path.
• Other tubing should be positioned above the liquid level.

g) Check the reagents. Prepare a new set of reagents when the reagent containers are
empty. Flush/Prime all tubing before performing a measurement.

10. Spare Parts


See Material Date Sheet with corresponding analyzer serial number.

43
Addendum

Addendum 1: Analysis Procedure


Remark:
Adjustments to the methods are made in the METHOD (F4) menu. We recommend you to
read the ‘Configuration Manual’ carefully before making adjustments to the method: the
functioning of the analyzer may be disturbed.

1.1 Ammonia – Method 1 – Analysis


Nr Step Name Interval Volume Pulses
1 PROGMOD1: Analysis
2 Streamselection ON 50 ms
3 Stirrer ON 50 ms
4 Dilution Fill 3s
5 DP CCW Interval 30 s
6 ABS Meas. 5s
7 ABS drain Calc. 1s
8 SP CW ON 50 ms
9 DP CCW ON 50 ms
10 Flushing Variable: Flushing
11 SP CW OFF 50 ms
12 Dilution Dose 15 s 2 ml
13 Waiting 5s
14 DP CCW OFF 50 ms
15 Airgap 3s 0.1 ml
16 Sample Group 9000 ms
17 Drain Group 16000 ms
18 Sample Group 9000 ms
19 Streamselection OFF 50 ms
20 ABS Meas. 5s
21 ABS sample Calc. 1s
22 Sample Detection Calc. 1s
23 Waiting 15 s
24 Sub procedure 0 0s
25 Dilution Extract 15 s 1 ml
26 Drain Group 16000 ms
27 Airgap 3s 0.1 ml
28 Dilution Fill 1s
29 Rinse Group 10000 ms
30 Drain Group 16000 ms
31 Rinse Group 10000 ms
32 Drain Group 16000 ms
33 Stirrer ON 50 ms
34 Dilution Empty 35 s

44
35 Stirrer OFF 50 ms
36 Waiting 5s
37 ABS Meas. 5s
38 ABS1 Calc. 1s
39 Stirrer ON 50 ms
40 Reagent A pulses 19 s 19p
41 Reagent B pulses 19 s 19p
41 Waiting 900 s
42 Stirrer OFF 50 ms
43 Waiting 5s
44 ABS Meas. 5s
45 ABS2 Calc. 1s
46 N-NH3 Calc. 5s
47 Write to database 1s
48 Drain Group 16000 ms
49 Rinse Group 10000 ms
50 Drain Group 16000 ms
51 Rinse Group 10000 ms
52 Drain Group 16000 ms
53 Waiting Variable: Waiting
54 Sub procedure 1000 0s
55 N-NH3 Calc. 1s
56 Write to database 1s
57 Streamselection OFF 50 ms
58 Waiting 1s

1.2 Ammonia – Method 1 – Cleaning


Nr Step Name Interval Volume Pulses
60 PROGMOD3: Cleaning
61 Clean ON 50 ms
62 DP CCW Interval 30 s
63 Sample Group 9000 ms
64 Drain Group 16000 ms
65 Sample Group 9000 ms
66 Clean OFF 50 ms
67 Stirrer ON 50 ms
68 Waiting 60 s
69 Stirrer OFF 50 ms
70 Drain Group 16000 ms
71 Rinse Group 10000 ms
72 Drain Group 16000 ms
73 Waiting 1s

45
1.3 Ammonia – Method 1 – Priming
Nr Step Name Interval Volume Pulses
74 PROGMOD4: Priming
75 DP CCW ON 50 ms
76 Reagent A pulses 1s 150p
77 Reagent B pulses 30 s 150p
77 Dilution Fill 1s
78 Clean ON 50 ms
79 SP CW ON 50 ms
80 Waiting 15 s
81 Clean OFF 50 ms
82 REF2 ON 50 ms
83 Waiting 15 s
84 REF2 OFF 50 ms
85 REF1 ON 50 ms
86 Waiting 15 s
87 REF1 OFF 50 ms
88 SP CW OFF 50 ms
89 Dilution Empty 1s
90 Waiting 45 s
91 Dilution Fill 1s
92 Waiting 60 s
93 Dilution Empty 30 s
94 DP CCW OFF 50 ms
95 Rinse Group 10000 ms
96 Drain Group 16000 ms
97 Rinse Group 10000 ms
98 Drain Group 16000 ms
99 Waiting 1s

46
Addendum 2: Configuration
See also ‘Material Date Sheet’ with corresponding analyzer serial number.

Software V 3.06.70

2.1 Digital Outputs


Nr Name
1 SP CW
2 SP CCW
3 DP CW
4 DP CCW
6 Stirrer
7 Reagent A
8 Reagent B
12 REF1
13 REF2
14 Clean
15 Rinse
16 Sample
25 Malfunction

2.2 Digital Inputs


Nr Name
1 INP1
2 INP2
3 INP3
4 INP4

2.3 Analog Inputs


Nr Name
1 ABS

2.4 Analog Outputs


Nr Name
1 Result Ammonia

2.5 Dispensers
Nr Name Speed Steps Volume
1 Dilution 45 6000 10

47
2.6 Results
Nr Name Unit
1 Sample Detection N.A.
2 ABS drain mAU
3 ABS sample mAU
4 ABS1 mAU
5 ABS2 mAU
6 NH3 ppm

2.7 Results Calibration


Name A1 Min A1 Max A1 A0 Min A0 Max A0
NH3 0.01012 -1000 1000 -0.13625 -1000 1000

Name Conc. Ref1 Runs Ref1 Conc. Ref2 Runs Ref2


NH3 0 3 10 3

2.8 Results Calculation


Sample Detection
1 M1 - M2
2 IF R1 < 100 THEN Set alarm byte: 1 Value: 1
3 IF R1 >= 100 THEN Set alarm byte: 1 Value: 0
4 IF R1 < 100 THEN go to subprocedure 1000
5 IF R1 >= 100 THEN go to subprocedure 0
6 R1 End of calculation

ABS drain
1 M1 End of calculation

ABS sample
1 M2 End of calculation

ABS 1
1 M3 End of calculation

ABS 2
1 M4 End of calculation

N-NH3
1 M4 - M3
2 R1 write to calibration
3 R1 * Factor a1
4 R3 + Factor a0
5 R4 Low Limit = 0
5 R4 End of calculation

48
2.9 Results Analog output
Result Channel Analog output Value 4mA Value 20mA
NH3 1 Result Ammonia 0 10

2.10 Results Stream output


Result Channel TAG
NH3 1 1
9 REF1
10 REF2

2.11 Result Alarms


Result Channel Low value High value
NH3 0 -5 00,5

2.12 Results Graph


Result Channel Low value High value
NH3 0 0 10,5

2.13 Alarm and message table


Nr Type Apply Function Message Reset
0 Alarm Global Emergency stop E-stop/Reinitialize the dispensers ! Automatic
1 Alarm Global Direct alarm No sample detected Automatic
2 Alarm Global Calibration failure Calibration error Automatic
3 Alarm Global Sensor Sensor ABS error Automatic
4 Alarm Global DispenserDilution Dispenser dilution error Automatic

2.14 Group DO
Action DO1 Status DO2 Status Time (ms)
Sample 1 SP CW On Stirrer Off 2000
2 SP CW On Stirrer On 6000
Drain 1 DP CCW On Stirrer On 5000
DP CCW On Stirrer Off 10000
Rinse 1 SP CW On Stirrer Off 2000
2 SP CW On Stirrer On 7000

49
Addendum 3: Alarms and signals

3.1 Alarms
Introduction

All alarms are implemented as follows:

• Closed contact: the alarm is off and the Analyzer is On-line


• Open contact: the alarm is active

Alarm list

• Malfunctioning alarm:

Every alarm activates the malfunctioning alarm output (contact is opened).

o Emergency stop
When the emergency stop is activated, the analyzer shall stop immediately.

o Leak detection
There is a sensor installed inside the analyzer cabinet to detect leaks. When a leak
is detected, the malfunctioning alarm is triggered and the analyzer is stopped
(optional). A message box appears on the main screen.

o Sensor
When there is a problem with one of the sensors, the malfunctioning alarm is
activated. A massage appears in the message or history submenu.

o Titration alarm
When there is a problem during the titration (titration out of time, no inflection
points detected…) the malfunctioning alarm is activated. A massage appears in
the message or history submenu.

• Maintenance alarm:

When the maintenance mode is active after pressing the MAINTENANCE ON/OFF
button, a digital output is activated (maintenance contact is opened) to indicate
remotely that the analyzer is not running on-line. When the maintenance mode is
active, the analyzer is always in the local control mode: the analyzer can only be
started manually.

3.2 Signals
The standard signal is an active 4-20 mA signal.
RS232/MODBUS are optional, but can be programmed and used if the proper remote IO is
installed.

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Warranty
1. Warranties
AppliTek NV/SA warrants that its products are free from defects in materials and workmanship (under
normal conditions of use and service) for a period one (1) year from date of shipment to original
purchaser.

2. Limited warranty and liability


On principle, the “General terms of and conditions of sale and delivery” of the company AppliTek
apply. All warranty and liability claims made for damage to persons or property are invalid when they
prove to have as a cause one or more of the following:

• Operating the unit for reasons other than its designed purpose
• Improper assembly, initializing, operating or maintenance of the unit
• Operating the unit when any safety or protection devices are defect or non-functioning
• Non-adherence of any instruction in the operating manual
• Unauthorized constructional alterations to the measuring unit
• Unauthorized constructional alterations to the utilities (for example instrument air supply).
• Incorrect maintenance of unit components
• Maintenance and repair work improperly carried out
• Catastrophes caused by outside interference, natural disaster, labor unrest, acts of war,
terrorism, civil strife or acts of any governmental jurisdiction.

Warranty also does not cover:


Freight charges on expedited or express shipment of warranted parts or product
Travel fees associated with on-site warranty repair

3. Inspection and claims


Claims for damage in shipment must be filed immediately with delivering carrier. Claims for shortages,
shipping errors or any claim that the goods do not conform with the terms of the contract must be
submitted to the AppliTek NV/SA in writing within five (5) days of receipt. If buyer fails to comply with
the term ‘within 5 days of receipt’, the goods shall be deemed to conform with contract terms, and
buyer shall accept and pay for the goods in accordance with the contract. Buyer waives any right to
revoke acceptance after such five days period. All claims must be accompanied by a copy of the
shipment note.

4. Indemnity for products manufactured according to customer’s requirements


In the event AppliTek NV/SA provides products in accordance with drawings, models or samples
provided by the customer, customer shall indemnify AppliTek NV/SA from any liability, cost or expense
suffered by AppliTek NV/SA as a result of the violation of any law or regulation or the infringement of
any industrial property right or other right of third parties.

5. Notification of product hazards and recall of products


Customer will inform AppliTek NV/SA immediately in writing about any events which indicate any
hazards connected with the product. Upon written notice of the AppliTek NV/SA about hazards in
connection with the products or unfitness for use of the products and recall of products, the customer
will immediately cease using the products for any reason, the customer, as its sole remedy shall be
entitled compensation equivalent to the current value of the used product, but in no event more than
the purchase price. AppliTek NV/SA shall not be liable for buyer’s loss of profit or incidental
consequential or special damages of any kind.

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