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INSTRUCTION MANUAL

SILICA ANALYZER PCs 2030

Version 2.08

Boom sesteenw eg 930

2610 Antw erpen
Tel : 00 32 (0)3 877 59 75
Fax : 00 32 (0)3 877 59 73
Manual silica Prolytics 2030 1
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Warnings

This instrument conforms to DIN57411 part 1 / VDE 041 part 1 "protective measures for electronic
measuring instruments" and has left the factory in faultless condition. To maintain this condition
and to guarantee harmless operation of the instrument, the user has to observe all warnings and
directives of the manual.

Interruption of the protective grounding line or loosening the ground connection inside or outside
the instrument may lead to dangerous situations. Disconnecting the ground is prohibited.

Disconnect power whenever electronic service is required. Care should be taken when opening or
removing parts of the instrument; connectors may be under tension. Service should be performed
by authorized personnel only.

If proper operation is not possible anymore, the instrument has to be disconnected from all power
lines and measures should be taken to prevent inadvertent operation.

Safe operation is not possible :

- when the instrument has been visibly damaged during shipping or installation
- when the instrument does not function
- after extended storage in unfavorable surroundings
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Contents
1. Introduction
1.1 Priciple of operation 4
1.2 Description of the measuring system 5

2. On-line operation
2.1. Frontpanel functions 5
2.2. Display - submenu 100 : Measurement 6

3. Installation
3.1. On-site requirements 6
3.2. Sample requirements 6
3.3. Electrical installation 6

4. Operation and programmation 7

4.1. Cal/Phot value 8
4.2. Parameters auto analysis 8
4.3. Parameters auto calibration 9
4.4. Start analysis / Reset function 9
4.5. Start calibration / Reset function / Measured standard 10
4.6. Manual test 11
4.7. Service submeu 11
4.8. Programming analog output 11
4.9 Fail alarms 12

4.10 High alarm value 13

4.11 Trend viewing 13
4.12 Time parameters analysis 13
4.13 Time schedule 14

5. Preparing the reagents

5.1. Reagent 1 15
5.2. Reagent 2 (optional) 15
5.3. Reagent3 15

6. Start-up (blank value) 16

7. 7.1 Normal Operation 17

7.2Grab sample 17

8. Maintenance 17

9. Electrical Wiring
9.1 Wiring diagram for user 18

Appendix 1 :Password protection 19

Appendix 2 : Reset factory calibration factor 19
Appendix 3 : Calibration procedure 19
Manual silica Prolytics 2030 3
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1. Introduction
1.1 Principal of operation

The analyzer has a microprocessor based display/control unit and an analytical part.

The heart of the analytical part has a measuring cell, in which a magnetic stirrer to mix the reagents
with the sample and, a 860 nm LED light source with a light detector to measure the intensity of the
formed color (absorbance).

The sample enters the analyzer through a needle inlet valve and an electromagnetic inlet valve to
the measuring cell from where it overflows into the drain. When the measuring cell is rinse out by
the sample, the electromagnetic inlet valve closes and about 25 ml of sample is trapped inside the
cell.

Before the first reagent is added, the light intensity is measured and set to zero absorbance. In this
way sample turbidity and color and light source aging is automatically compensated.

Reagent 1; Ammonium-molybdate reacts with reactive silica and phosphate to form a weak
yellow color. The reaction time is 240/300 seconds.
Reagent 2: Oxalic acid is added to decomplex the phosphate-molybdate compound and to stop
further reaction of the molybdate with the silica. For measurements in de-ionized
water, boiler feedwater without phosphate, condensate and low levels of silica this
reagent is not wanted. (optional)
Reagent 3: Reducing agent converts the weak yellow color in a more intense blue color, which
is very suitable for low ppb measurements. The reaction time is 300/360 seconds.

At the end, the absorbance/extinction is measured and converted to concentration value.

The sample cell is flushed at the end of the analysis with fresh sample and the analyzer is ready for
a new measurement.

For the calibration another electromagnetic valve just after the needle inlet valve is activated to
rinse and fill the measuring cell with a standard solution (recommended 250 ppb). The absorbance
measured with the standard solution is than equaled to its concentration value. The calculated
conversion factor is shown on the display and used to calculate the concentrations in the sample.
.
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1.2 Schematic drawing of the measuring system

Note : This is a schematic drawing. The flow detector can also be an overflowvessel at the
top, near the standard reagent bottle
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2. On-line operation

2.1. Frontpanel functions

On the frontpanel one can see four LED 's with the following functions :
ANALYSIS, CALIBRATION, HIGH ALARM, FAIL ALARM

ANALYSIS Analysis is in progress

CALIBRATION Calibration is in progress

HIGH ALARM High limit value

FAIL ALARM - No sample

- No standard
- Photometer error
- No reagent
- Dirty cell

Select/Return The SELECT-key is used to enter and leave a „highlighted“ program menu.
In a program menu the SELECT-key is used to enter and leave „highlighted“
program sub-menu parameters.
In the sub-menu parameters the SELECT key is used to confirm a parameter
change.

ARROW keys The ARROW (up and down) keys are used to move the „highlight“ bar to the
different menu items. When the „highlight“ bar is not on the display, it is on
the corresponding one level up.
The ARROW-keys are also used to change parameters (confirm with Select-
key)

ANALYSIS CALIBRATION HIGH ALARM FAIL ALARM

NO FUNCTION SELECT/ KEY

RETURN
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DECREMENT KEY INCREMENT KEY

2.2 Display - submenu Measurement

By selecting the submenu 100 : Measurement one gets the principal display menu

The first line displays the last measured concentration in a sample.

The second line displays the calibration factor.
The Cal factor must be between 0.700 – 1.300
(The 3.3 is no more valid !)

3. Installation

3.1. On-site requirements

Sample inlet : 1/8" NPT-F or 6mm

Drain : 3/4" NPT-F or hose nozzle ending in a atmospheric drain.
AC power supply : 110-230 VAC, 50/60 Hz

Outputs : 1 analog output (4-20 mA, 600 Ohm)

1 RS232-C, RS422, Profibus(optional)
1 Alarm - contact, 250 VAC, 1A
1 Fail - contact, 250 VAC, 1A

3.2. Sample requirements

Parameter

Flow 50 ml/min - 200ml/min during washing cycle

Sample pressure: 0.3 - 3 bar
Temperature: 5 - 45C

3.3. Electrical installation

Warning !

Always turn off AC power before manipulating electrical parts.

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4. Operation and programming

For viewing the main menu with the program possiblities, one has to press the
SELECT/RETURN key.

Press SELECT/RETURN

Measurement : Toview last SiO2 value and calibration factor

Cal/Phot value : To view photometer extinction, standard solution, offset, cal.

factor

Par. Autoanalyse : Selecting the frequency of analysis, the washing time for
an analysis, On/Off and STORE

Par. Autocal : Selecting the frequency of calibration, the silica value of

the calibration solution, the blank value, On/Off and STORE

Start analysis : START immediately an analysis or RESET to stop

Start calibration : START immediately a calibration or RESET to stop and sets

the calibration factor to default value. Shows the measured
value of the standard using the previous calibration factor.

Manual test : For activating or de-activating the valves, pumps and stirrer.

Service : To view the last measured potentials of the photometer.

4-20 mA output : Programming the analog output range. Shows the current
output in mAmps.

Fail alarms : To view and acknowledge (delete)the error messages

High alarm : Programming the high alarm value

Trend To view the last 100 measured values update every 15 min

Time parameters To program the pump and reaction times, these values are
entered in the factory. Do not change them unless you are
specifically instructed to do so.

Time schedule To view the remaining times for the next calibration/analysis
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4.1 Submenu : Cal/Phot value

Select in the "level 1 data" menu 101 : Cal/Phot value and the following screen will be
viewed.

This is only a display menu and none of the parameters can be changed here.

The actual photometer output is measured in mV and monitoring helps for solving problems.

The cal(ibration) values are the concentration of the standard solution, which can be changed
in the submenu 103 : Par. autocal.

The blanc is value of impurities coming from the reagent in ppb. The blank value is
measured in 0.0 ppb sample. (Change under 103 : Par. autocal)

The factor is an indication for the response of the photometer. This value is calculated
after each calibration. The cal factor must be between 0.7 -1.3.

4.2 Parameters auto analysis

For changing parameters, move the cursor („highlight“ bar) to the line of the parameter and
press SELECT/RETURN. The line starts blinking and value is changed using the ARROW
keys. Press the SELECT/RETURN key to confirm the new value.

The standard frequency time for an analysis is set to 20 min, but can be changed from 1 to
900 min.

The rincing/washing time is standard set to 60 sec.

This is the time when the inlet valve will be activated just before and after an analysis or
calibration. This parameter must be long enough to remove any remains of the previous
analysis.

The status indicates if the auto analysis function is active or not. With the ARRROW keys
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and the SELECT/RETURN key ON or OFF can be selected.

After changing the parameters, the changes have to be confirmed in the STORE function.
Press SELECT/RETURN on the STORE line, the line starts blinking and select with the
ARROW keys YES/OK and press SELECT/RETURN.

To return to the main menu, move the cursor line off the display and press the
RETURN/SELECT key.

4.3 Parameters for auto calibration

Select the 103 : Par. autocal submenu and the following screen will be shown.

In this submenu the frequency of calibration is selected in hours.

The concentration of the standard must be entered here. We recommend to use 250 ppb.
The blank value can be changed.

The status indicates if the auto calibration function is active or not. With the ARRROW
keys and the SELECT/RETURN key ON or OFF can be selected.

After changing the parameters the changes have to be confirmed inthe STORE function.
Press SELECT/RETURN on the STORE line, the line starts blinking and select with the
ARROW keys YES/OK and press SELECT/RETURN.

To return to the main menu, move the cursor line off the display and press the
RETURN/SELECT key.

4.4 Start analysis / Reset function

In the 104 : Start analysis submenu an analysis of the sample is started. Select START
ANALYSIS with the SELECT/RETURN key and to choose YES/OK with the ARROW
keys and press the SELECT/RETURN key.
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The reset function is used to stop an analysis. Select the RESET line and choose
YES/OK with the ARROW keys and press SELECT/RETURN.

NOTE : After RESET the inlet valve is activated according to the rinsing time

4.5 Start calibration / Reset function / Measured standard

In the 105 : Start calibration submenu the user can start a calibration by selecting START
CALIBRATION with the SELECT/RETURN key and to choose YES/OK with the
ARROW keys and again pressing the SELECT/RETURN key.

The reset function is used to stop a calibration. Select RESETl and choose
YES/OK with the ARROW keys and press SELECT/RETURN.

The measured concentration in the standard solution, based on the previous calibration
factor is shown in the last line. This value has been used to calculate the new calibration
factor.

NOTE : With the RESET the inlet valve will be activated according to the rincing time
.

4.6 Manual test

With the 106 : Manual test submenu one can activate/desacitvate pumps, valves and stirrer.
In the start-up procedure (paragraph 6) these operation functions are used.

With the SELECT/RETURN and the ARROW keys one can change :
Inlet valve off into Inlet valve on
Reagent 1,2 and 3 off into Reagent 1,2 and 3 on (start pump 1,2 and 3)
Cal. Valve off into Cal valve on
Stirrer off into Stirrer on

WARNING: ONLY ACTIVATE THE PUMPS WHEN SAMPLE IS RUNNING

THROUGH THE ANALYZER, TO DILUTE AND RINSE OUT THE
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CONCENTRATED REAGENT.

WARNING: MAKE SURE THAT ALL THE FUNCTIONS ARE RESET TO OFF !

4.7 Service submenu

The 107 : Service submenu views the photometer outputs after the addition of the different
reagents. The difference between Eo and E3 is used to calculate the silica concentration.
The data are also the base for error messages.
Eo < 4000 mV Dirty cell
Eo < 50 mV Photom. error
Eo =/> E3 No Reagent

The first set of data from a 2 pump system gives 214 ppb. Other typical sets are next to it.

105: Service . 9.82 ppb 103,7 ppb

Eo = 7.320,2 mV 7330,1 7327,4
E1’ = 7.036,1 mV 7.308.2 7113.1
E1 = 7.034,4 mV 7.306,6 7.110,6
E2 = 6.956,8 mV 7.297,7 7.135,7
E3’ = 4.473,7 mV 7.117,2 5.639,8
E3 = 4.471,1 mV 7.119,7 5.637,4

Eo value : Background value

E1' value : Photometer reading at 90% of the reaction time of the reagent 1.
E1 value : Photometer reading at 100% of the reaction time of the reagent 1.
E2 value : Photometer reading at 100% of the reaction time of the reagent 2.
E3' value : Photometer reading at 90% of the reaction time of the reagent 3.
E3 value : Photometer reading at 100% of the reaction time of the reagent 3.

4.8 Analog output

The analog output can be programmed through the submenu 108 : Analog output.

The start value is the value at 4 mA, the end value is the value at 20 mA.
With the SELECT/RETURN key and the ARROW keys, the default values of 0 and 500 ppb
are changed.

In the last line shows the actual output in mA.

The maximum load for the mA signal is 600 Ohm
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4.9 Fail alarms

When a failure is detected, the right LED on the controller will lighten on and the fail relay is
activated.
In any display the top line will also give the message FAIL ALARM

The relay and fail message will remain activated unless the user acknowledge the fail message
in the submenu 109 : Fail alarms

The message is confirmed selecting the acknowledge line and with the SELECT/RETURN
key, go to Yes/ok and press SELECT/RETURN key.
All the messages are deleted until a next failure is detected.

Explanation of the fail alarms Actions

No sample Check the sample flow

No standard Check the standard solution level.

Check the cal. Valve through manual test

Photom. Error Check the Extinction in 101 : Cal/Phot value

Lower than 50 mV, replace lamp - receiver

No reagent Check reagent level or renew reagent

Dirty cell Remove top plate by loosing the screws and

clean the interior glass cell with a tissue or
5 ammonia solution.

Note : When the reagent tube(s) is|(are) blue, it is recommend to immerse the tube(s) in
5% ammonia solution. Start the reagent pump(s) and pump the ammonia solution in
the measuring cell for 15 minutes.
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4.10 High alarm value

An high alarm value (default 500 ppb) is available and is changed by using the
SELECT/RETURN key and the ARROW keys.

In case of an high alarm the LED on the controller will lighten up, the high alarm relay is
activated and in the top line of any display the message HIGH ALARM will be shown.

4.11 Trend viewing

In the submenu 111: Trend the user can look at the last 100 measurements updated every 15
minutes.

The vertical scale is in % of programmed mA output range.

4.12 Time parameters for analysis

In the submenu 112 : Time parameters, the pump and chemical reaction times can be viewed
and changed. The values are already updated during factory calibration and the user should first
consult a specialist before changing these times.

After changing the time parameters, the entries have to be stored before they become active
(similar for calibration and analysis parameters).
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4.13 Time schedule

In the submenu 113 : Time schedule

Shows the selected mode of auto analysis and auto calibration (ON or OFF).
Next the remaining time until the next calibration or analysis.
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5. Preparing the reagents

GENERAL WARNING: WEAR PROTECTIVE PLASTIC GLOVES AND CLOTHING.

WEAR PROTECTIVE EYEGLASSES.

USE HIGH PURITY WATER AND PLASTIC CONTAINERS.

5.1 Reagent 1

The preparation of this reagent releases heat. Rinsing the bottle with cold water is necessary or add
the sulfuric acid in small portions.

It is recommended to designate 2 liter plastic bottles for each reagent for preparation.

1. Fill a 2 liter reagent storage bottle with about 1.2 liter ultra pure water
2. Add 200 gram sulfuric acid H2SO4 (100%, analytical grade)
in small portions to prevent overheating. (110 ml H2SO4 = 200g)
3. Add 80 grams of ammonium molybdate (Merck 1182)
slowly while keeping the solution in motion.
4. Keep shaking the solution until all is dissolved.
5. Fill up with pure water to 2 liter mark.

5.2 Reagent 2 (Used in three pumps system optional)

1. Fill a 2 liter reagent storage bottle with about 1.5 liter ultra pure water
2. Add 40 gram of oxalic acid slowly while keeping the solution in motion.
3. Fill up with pure water to 2 liter mark.
4. Keep shaking the solution until all is dissolved.

5.3 Reagent 3
1. Fill a 2 liter reagent storage bottle with about 1.5 liter ultra pure water
2. Add 160 gram of Potassium Disulfite (Merck 5057)
slowly while keeping the solution in motion.
3. Add 40 gram of 4-methylaminophenol sulfate
(Photo-Rex Merck 7299) slowly while keeping the solution in motion.
4. Fill up with pure water to 2 liter mark.
5. Keep shaking the solution until all is dissolved.

Our reagent packs are delivered without sulfuric acid. All other reagents are in powder form and
require only to be dissolved in the prescribed amount on the plastic container.
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6. START-UP.

During start-up, the reagent bottles first have to be filled and the analyzer has to be prepared to
analyze the sample.

1. Program the analyzer to meet your requirements.

2. Fill reagent bottles. Take care that the bottles are vented to air.
3. Go into MANUAL TEST
4. Activate the inlet valve and adjust the sample flow to be 50 - 100 ml/min.
5. Activate, one after the other, each pump for about 10 minutes to fill the pump tubing.
6. Close (de-activate) the inlet valve
7. Select START ANALYSIS and select start - Yes/ok and the first analysis will be
performed.
8. After a few analysis and good rinsing/washing a calibration can be performed

Note :
- Rinsing time in PAR. AUTOANALYSE should be long enough for good washing !
- Always switch off all pumps, valves and stirrer when leaving the MANUAL TEST
menu.

A blank determination (SiO2 in the reagent) can be performed by using a 0.0 ppb SiO2 solution in
the standard bottle and start a grab sample. Measurements will be shown in the menu.

Precautions should be taken into account by trying to determine a blank value.

The best way is to flow a zero SiO2 sample through a small additional mixed bed.
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7 Operation
7. 1 Normal operation
Under normal operation the electromagnetic inlet valve and the electromagnetic calibration valve
are deactivated. The calibration valve is only activated during the first rinsing step of the
calibration cycle.
and the inlet valve is activated when an analyze or calibration cycle is started.

When the analyzer is in stand-by mode the sample flows through the 2 electromagnetic valves into
the drain. To reduce sample consumption, the outlet from the valve to the drain may be closed.

Check the analyzer on a regular basis for reagent content.

A flow detector will detect no flow at the beginning of an analysis.

7.2 Grab Sample.

It is possible to measure the silica content of a different sample point using the standard bottle.
1. Rinse the standard bottle well.
2. Fill the standard bottle with 1 liter of sample
3. Place the bottle in its place in the analyzer.
4. Go in menu to GRAB SAMPLE, select START change to YES/OK, cal valve will open
automatically. 3 values will be shown in the same menu for 1 liter of sample.
5. Remove the grab sample from the bottle and replace with standard.

8. Maintenance

Weekly: Check reagent levels, refill and fill the reagent tubing as explained in start-up

3 month Clean measuring cell and reagent tubing with 5% ammonia solution.
Place reagent tubing in ammonia solution and run the pumps for 15 minutes.
Open inlet valve to remove the ammonia from the measuring cell.
Perform star-up procedure

Yearly : Replace pump tubing when reagents have to be refilled/replaced.

1. Go to the MANUEL TEST menu.

2. Loosen the clip of the pump by turning it.
3. Remove upper plastic cover
4. Remove tubing from pump
5. Replace pump tubing of the pump collars
6. Place new tubing in pump by sliding the tube collars
in place. Do not twist the tubing.
7. Replace plastic cover and fasten clip system
8. When all pumps are done, perform the start-up procedure.
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9. Electrical Wiring

1 Ground -
2 Neutral -
3 220 VAC -
6 IR led + brown) Amplifier (red) red
7 IR led - (white) Amplifier (red) blue
8 Detector + (brown) Amplifier yellow
9 Detector - (white) Amplifier green
13 Inlet valve - 24 VDC
14 Inlet valve Amplifier (black) blue
15 Calibration valve Amplifier (black) red
16 Calibration valve + 24 VDC
17 Pump 1 ( -24 VDC) -
18 Pump 1 (+ 24 VDC) -
19 + VDC stirrer (brown) -
20 - VDC Stirrer (white) -
21 + mA output Z40
22 - mA output Z39
24 Flow detector Z35
25 Flow detector -
27 Pump 3 (+24VDC) Z37
28 Pump 3 (-24 VDC) -
29 Potential free input start analysis + 24 VDC
30 Potential free input start analysis Z36
31 NC High value (250 VAC, 1A)
32 C High value (250 VAC, 1A)
33 NO High value (250 VAC,1A)
34 NO fail alarm contact (250 VAC, 1A)
35 C fail alarm contact (250 VAC, 1A)
36 NC fail alarm contact (250 VAC,1A) |

Fail alarm contact : inversed operation, no power means 36 open !

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Appendix 1 : Password protection

All menus with parameters which can be changed are protected by a password.
The factory password is 99.

Go to 101 : Password <Enter>

Go to Password and Introduce 99 <Enter>

Now all menus are displayed in the Main menu.

For changing the password

Go to 102 : Change password

Introduce a new password and acknowledge with yes/ok

The factory password can always be reinstalled by the 101 : Password menu and acknowledge
<Reset factory password>

For quitting the availability of the parameter menus :

Go back to 101 : Password and set the password to a value different from the password.

Eg : if the password is 99, set it to whatever.

Appendix 2 : Reset Factory calibration factor

Go to :
Menu 107 : Cal menu

The cal menu is updated with an extra line :

1: Start cal
2: Reset factor
3: Reset cal

The RESET FACTOR resets the standard factor of 1.242.

Appendix 3 : Calibration procedure

If you are measuring values below 50 ppb, we recommend you to calibrate the analyzer with 250 or
200 ppb. (Be aware 1000mg Si = 2140 mgSiO2)
Put the solution in the calibration bottle and start the calibration.
To verify the calibration one could start an analysis while activating the cal valve by hand so that
the cal solution enters the reaction chamber. The value which will be displayed will be within 5%
of the actual value.
Preparing a solution with half the concentration of the cal solution and repeat the same as explained
above will give a value which will be within 5% of the actual value.
If this is not the case then the reagents or standards should be checked or replaced.