Operator ManualPOLYMETRON 9210

221=192=010 - Revision J - 20/11/2007

SILKOSTAT 9210

i

Notice for readers

The information contained in this manual was as complete and exact as possible at the time of printing. If the behaviour of this product during its use is different from that described in the documentation, it is perhaps because your manual is out of date. In this case, please contact your Hach Ultra Analytics agent immediately to remedy the problem. If the instrument is used in a way not specified by the manufacturer, the protection ensured by the instrument could be compromised. Hach Ultra Analytics reserves the right to make modifications and changes to the equipment and software comprising the product described in this manual. Thank you.

Restriction of Hazardous SubstancesNote:The following only applies to exports of the product into the People’s Republic of China.

Marking

Products contain toxic or hazardous substances or elements.

Environment Protection Use Period Marking (years).

Toxic or Hazardous Substances and Elements

Part NameLead (Pb)

Mercury (Hg)

Cadmium (Cd)

Hexavalent Chromium

(Cr VI)

Polybrom Biphenyls

(PBB)

Polybrom Diphenyls

(PBDE)

Transmitter box X

CPU PCB (with battery) O O

Power PCB O O

RS 485 O

Profibus O

PCB CAN O

PCB Local controller O

PCB Measure O

PCB Pumps O

PCB Mixer O

PCB Channel O

O: Indicates that this toxic or hazardous substance contained in all homogeneous material for this part is below the limit requirement

X: Indicates that this toxic or hazardous substance contained in at least one of the homogeneous materials used for this part is above the limit requirement

SILKOSTAT 9210

ii

Safety Precautions Please read this entire manual before unpacking, setting up, or operating this instrument. Pay particular attention to all danger and caution statements. Failure to do so could result in serious injury to the operator or damage to the equipment. To ensure the protection provided by this equipment is not impaired, do not use or install this equipment in any manner other than that which is specified in this manual. Use of Hazard Information If multiple hazards exist, this manual will use the signal word (Danger, Caution, Note) corresponding to the greatest hazard. DANGER Indicates a potentially or imminently hazardous situation which, if not avoided, could result in death or serious injury. CAUTION Indicates a potentially hazardous situation that may result in minor or moderate injury. NOTE Information that requires special emphasis. Precautionary Labels Read all labels and tags attached to the instrument. Personal injury or damage to this instrument could occur if not observed. This symbol, if noted on the instrument, references the

instruction manual for operation and / or safety information.

This symbol, if noted on the instrument, marks the wiring connection point for Protective Earth.

This symbol, if noted on the product, indicates the need for protective eye wear.

Electrical equipment marked with this symbol may not be disposed of in European public disposal systems after 12 August of 2005. In conformity with European local and national regulations (EU Directive 2002/96/EC), European electrical equipment users must now return old or end-of life equipment to the Producer for disposal at no charge to the user. Note: For return for recycling, please contact the equipment producer or supplier for instructions on how to return end-of-life equipment for proper disposal. Important document. Retain with product records.

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SILKOSTAT 9210

iii

Power Connections. on page 20. Wiring the Instrument for Power on page 17.

Reagents preparation on page 23. Maintenance on pages 9 and A2.

Maintenance The integrity of electrical connections and protection instruments of the system should be checked periodically. All necessary measures should be taken to remedy any inadequate condition.

Service and repairs None of the instrument’s components can be serviced by the user. Only personnel from Hach Ultra Analytics or its approved representative(s) is (are) authorised to attempt repairs to the system and only components formally approved by the manufacturer should be used. Any attempt at repairing the instrument in contravention of these principles could cause damage to the instrument and corporal injury to the person carrying out the repair. It renders the guarantee null and void and could compromise the correct working of the instrument and the electrical integrity or the CE compliance of the instrument. If you have any problems of installation, starting or using the instrument please contact the company that sold it to you. If this is not possible, or if the results of this approach are not satisfactory, please contact the manufacturer’s Customer Service.

Hach Ultra Analytics 6 route de Compois – CP212 CH-1222 Vesenaz Geneva

Tél. + 41 22 855 91 00 Fax + 41 22 855 91 99

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SILKOSTAT 9210

CONTENTS Page

1. Presentation of the instrument............................................................................................................... 5 Operation ................................................................................................................................................... 6 Calibration.................................................................................................................................................. 6

2. Technical specifications ......................................................................................................................... 7 Specifications............................................................................................................................................. 7 Dimensions of the analyser...................................................................................................................... 10

3. Installation .............................................................................................................................................. 13 Unpacking ................................................................................................................................................ 13 Inspection................................................................................................................................................. 13 Pre-installation ......................................................................................................................................... 13 Presentation of the analyser .................................................................................................................... 14 Positioning the canisters .......................................................................................................................... 15 Connecting the sample ............................................................................................................................ 16 Connecting the evacuation (drain) tube................................................................................................... 16 Mains power connection .......................................................................................................................... 17 RS485 connections (optional extra)......................................................................................................... 19 User signals connections ......................................................................................................................... 20

4. Starting-up.............................................................................................................................................. 23 Reagent preparation ................................................................................................................................ 23

Reagent concentrations (by type).................................................................................................. 23 Reagent preparation (makes 2 litres) ............................................................................................ 23 Calibration solution ........................................................................................................................ 24

Positioning the canisters .......................................................................................................................... 25 Using the menu........................................................................................................................................ 27 Language programming........................................................................................................................... 28 Time and date programming.................................................................................................................... 28 Starting up the analyser ........................................................................................................................... 29 Starting a measurement........................................................................................................................... 30

5. Analyser programming.......................................................................................................................... 31 Analyser configuration flow chart............................................................................................................. 31 User Interface .......................................................................................................................................... 32

Main display................................................................................................................................... 32 Definition of the display screen 2 (Disp2) ...................................................................................... 33 Definition of the display screen 3 (Disp3) : alarms ........................................................................ 34 Definition of the display 4 (Disp 4) : trend curve............................................................................ 35 Modification of a value................................................................................................................... 35

Main menu ............................................................................................................................................... 36 Calibration menu............................................................................................................................ 37

Execution primary sub menu ................................................................................................. 38 Execution manual sub menu.................................................................................................. 39 Programming sub menu (automatic execution) ..................................................................... 40 Calibration parameters sub menu.......................................................................................... 42 Calibration historic sub menu................................................................................................. 42 Manual – automatic calibration results sub menu.................................................................. 43

Maintenance menu ........................................................................................................................ 45 Start up sub menu.................................................................................................................. 45 Reagents refill sub menu ....................................................................................................... 46 Adjust volumes....................................................................................................................... 46 Tubes priming ........................................................................................................................ 47 Extended stop sub menu ....................................................................................................... 47

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SILKOSTAT 9210

Tubes cleaning sub menu...................................................................................................... 48 Measure / Photometer test sub menu.................................................................................... 48 Measure / Photometer test sub menu.................................................................................... 49 Pumps-others sub menu........................................................................................................ 49 Solenoid valves sub menu ..................................................................................................... 50 Relays sub menu ................................................................................................................... 50 Logical inputs sub menu ........................................................................................................ 50

Measure Menu............................................................................................................................... 51 Measuring mode sub menu ................................................................................................... 51 Grab sample sub menu.......................................................................................................... 52 Historic sub menu .................................................................................................................. 52 Programming.......................................................................................................................... 53 Read ..................................................................................................................................... 53 ADC values sub menu ........................................................................................................... 53

Alarms Menu.................................................................................................................................. 54 Alarms parameters 1 to 6 sub menu...................................................................................... 54 Warning alarm sub menu....................................................................................................... 56 System alarm sub menu ........................................................................................................ 56

mA outputs menu........................................................................................................................... 58 Outputs affect 1 to 6 sub menu.............................................................................................. 58 Special prog sub menu .......................................................................................................... 60 Test sub menu ....................................................................................................................... 60

Communication menu.................................................................................................................... 61 Choice of the measure sequence menu........................................................................................ 61

Channel activation sub menu................................................................................................. 61 Sequence sub menu .............................................................................................................. 62

Service menu................................................................................................................................. 63 Time sub menu ...................................................................................................................... 63 Display sub menu .................................................................................................................. 63

Customize ......................................................................................................................... 64 Service / Code sub menu....................................................................................................... 64 Soft issues sub menu............................................................................................................. 64 Default / values sub menu ..................................................................................................... 65 Adjust mA sub menu.............................................................................................................. 65 Factory sub menu .................................................................................................................. 66

Solenoid valves................................................................................................................. 66 Pumps............................................................................................................................... 67 Measure ............................................................................................................................ 67

Configuration sub menu......................................................................................................... 67 6. Maintenance and exploitation............................................................................................................... 69

Reagent refills .......................................................................................................................................... 69 Prolonged stopping .................................................................................................................................. 71 Restarting after a prolonged stopping...................................................................................................... 72 Tube cleaning .......................................................................................................................................... 73

7. Troubleshooting..................................................................................................................................... 75 Possible sources of the problem.............................................................................................................. 75 Possible solutions .................................................................................................................................... 76 Typical measurement values during calibration....................................................................................... 78

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SILKOSTAT 9210

Appendix A : Spare parts of the 9210 SILKOSTAT ....................................................................................A1 Appendix B : Safety Precautions .................................................................................................................B1 Appendix C : Table of user’s configuration................................................................................................C1 Appendix D : Pressure range change..........................................................................................................D1 Appendix E : Preparation of the tubes for insertion in the “fast” connections..................................... E1

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SILKOSTAT 9210

1. Presentation of the instrument Figure 1

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SILKOSTAT 9210

Operation The 9210 can analyse up to six different samples. The sample to be analysed circulates in a fast loop permitting rapid renewal of the sample. Adjustment of the flow is carried out with the help of a needle valve (2). At the beginning of the analysis, the sample is introduced into the measurement cell (4) with the help of a solenoid valve (5).

The 1st reagent is added with the pump (9). The silica contained in the sample now reacts with the molydate and forms the silicomolybdic complex. The reagent time is relatively long.

Oxalic acid is then added to avoid the interference of phosphates and to intensify the colour.

The silicomolybdic complex is reduced to a blue molybdenum complex by means of ferrous ions. A photometric measurement is carried out at the end of the reaction.

Figure 2 Working principal 1 - Overflow tank with level detector 2 - Flow adjustment valve 3 - Sample input 1 to 6 4 - Photometric measurement cell 5 - Measuring solenoid valve

6 - Mixing motor 7 - Magnetic bar 8 - Drain 9 - Reagent pump

10 - Calibration solution canister 11 - Calibration pump 12 - Photometer 13 - Drain pump of measurement cell

Calibration In order to ensure correct functioning, the analyser should be calibrated periodically. The zero is realised chemically and internally in the analyser. The system slope is controlled in comparison to a standard solution of known concentration.

8

10

3

3

3

3

3

3

18

47

5

11

13 12

9

2

6

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SILKOSTAT 9210

2. Technical specifications

Specifications Measurement range (two different versions) : - 0 – 1000 ppb - 0 – 5000 ppb

This instrument complies with the following standards :

Number of channels 1 – 6

Measurement cycle < 10 min / channel

Sample pressure 0.2 to 6 bar (3 to 87 psi)

Temperature 5 - 50 °C (41 – 122°F)

Sample flow 10 to 20 l / hour

CONNECTIONS

Sample admission tube PE ∅ 4/6

Sample evacuation tube PE ∅ 12/17 silicone

CONDITIONS OF USE

Ambient temperature 5 to + 45°C (41 to 113°F)

- use inside - fluctuations ± 10 % of the power

supply voltage - overvoltage category 2 - degree of pollution 2 (according

to CEI 664)

Altitude ≤ 2000 m

Relative humidity 10 to 80 %

WEIGHT

Panel analyser without canister Cabinet analyser without canister Full canisters

13 kg 65 kg 8 kg

- Immunity to electromagnetic interference

EN 50082-2 et EN 50082-1

- Electromagnetic emissions EN 50081-1 et EN 50081-1

- Low voltage standard IEC61010-1

SAMPLE

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SILKOSTAT 9210

ANALYSIS

Value measured dissolved SiO2

Measurement field 0 – 1000 ppb 0 – 5000 ppb

Repeatability ± 2 % or ± 0,5 ppb ± 2 % or ± 2 ppb

Detection limit 0,5 ppb 2 ppb

INPUTS / OUTPUTS

Alarms Number : 8

Functions : - 6 threshold relays / lack of sample / active channel

- System alarm 3 contacts

- 1 warning relay

Cut-off power : 30 VDC, 0.5 A maximum

Logic inputs Number : 12

Remote clearance Inhibition of samples

Serial input interface RS 485, Modbus communication protocol

Outputs 4 / 20 mA

Number : 8

4/20 mA / 0/20 mA programmable. Galvanically insulated

Maximum charge of 800 ohms

MATERIALS & PROTECTIONS

Transmitter Aluminium with polyester paint

Panels and other boxes Polystyrene

Protection transmitter box IP 65

Protection cabinet (optional) IP 54

Cabinet front door Plexiglas

Cycle time ∼ 10 minutes per channel

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SILKOSTAT 9210

MAINTENANCE

Calibration Chemical zero, slope with calibration solution

Maintenance No particular maintenance is necessary. Cleaning can be done with a soft non-aggressive cloth.

Reagent consumption Approx. 1 l per month and per reagent

Calibration solution consumption Approx. 200 ml / calibration

Time safeguard lithium battery CR 1220 (3 V)

Caution :

There are risks of explosion if the replaced battery does not correspond to the correct model.

Do not throw away used batteries in the dustbin. Send to a recycling centre.

TRANSMITTER

MAINS POWER SUPPLY

Display

• Programming by menu.

• Concentration of 6 samples.

• Analyser status.

• Alarms.

• Trend curves.

• Concentration historic

• Calibration parameters historic (date, slope and offset).

Mains • 100- 240 VAC 50 - 60 Hz.

• automatic switching.

• Max. consumption: 80 VA.

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SILKOSTAT 9210

Dimensions of the analyser

Figure 3 Dimensions of the analyser – Panel version

A : Mains power supply cable gland, drilled 11, ∅ 5 to 10mm, 100…240V, 50-60Hz, 25VA

B : Field bus cable gland, drilled 13, ∅ 6 to 12mm

C : 5 to 7 mm cable gland

* Alarm signals : 30V, 0.5A max.

* Logic inputs : Inhibition on channels 1 to 6, acknowledgement of alarm signals

* Analogue outputs : 0-20 mA or 4-20 mA

D : Samples inlets, (channels 1 to 6), QR coupling for semi-rigid tubing, ∅ 6mm

5 to 50 °C (40 ° to 120 °F), P 0.2 to 6bar (3 to 87 PSI)

E : Drain tube : silicon tubing, ∅ 12 x 17mm, at atmospheric pressure

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SILKOSTAT 9210

Figure 4 Dimensions of the analyser – Cabinet version

A : Cable gland, 5 to 7mm

* Mains power supply cable gland, drilled 11, ∅ 5 to 10mm, 100…240V, 50-60Hz, 25VA

* Field bus cable gland, drilled13, ∅ 6 to 12mm * Alarm signals : 30V, 0.5A max. * Logic inputs : Inhibition on channels 1 to 6, acknowledgement of alarm signals * Analogue outputs : 0-20mA or 4-20mA

B : Samples inlets (channels 1 to 6), QR coupling for semi-rigid tubing, ∅ 6mm

5 to 50°C (40° to 120°F), P 0.2 to 6 bars (3 to 87 PSI)

C : Drain tube : silicon tubing, ∅ 12 x 17mm, at atmospheric pressure.

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SILKOSTAT 9210

3. Installation

Unpacking

The instrument should be unpacked with care. Be careful not to mislay the accessories during unpacking.

Caution :

Assembly should not be carried out by non-qualified personnel.

The power supply should not be connected until the installation has been completed and checked.

Inspection The instrument has been tested and checked at the factory before shipping, however it is advisable to carry out a visual inspection to be sure that it has not suffered any damage. Damaged packaging could mean the presence of damage not immediately visible. Keep the packaging in case of complaints. For any missing parts or accessories, please contact your distributor.

Pre-installation Before installing the analyser, think about the following precautions:

• Place the analyser close to a sample point. The sample should be homogenous and representative. This will allow the response time to be reduced. The temperature of the sample should be between 5 and 50°C. The pressure of the sample should be between 0.2 and 6 bar and remain relatively stable. The solution should be free of particles. The sample lines should be in PE/PTFE/FEP (∅ 4 x 6 mm).

• Avoid any location with a corrosive atmosphere or subject to liquid spills.

• Chose a dry and dust-free location.

• The ambient temperature of the analyser should not exceed 45°C. If the temperature is below 5°C, the analyser should be installed in a heated cabinet.

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SILKOSTAT 9210

Presentation of the analyser

Figure 5 Analyser front panel

Figure 6 Analyser rear panel

1- Monec transmitter box 2- Sample level detector 3- Overflow vessel 4- Sample 1 to 6 flow adjustment valves 5- Photometric measurement cell

6 - Local controller box 7 - Measurement solenoid valve 9 - Measurement box 10 - Sample inlet valves 11 - Drain

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SILKOSTAT 9210

Positioning the canisters A canister holder is supplied with the analyser, it is fixed as shown in the figure below.

Figure 7 Canister replacing

In all cases, respect the maximum height between the measurement cell and the canister.

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SILKOSTAT 9210

Connecting the sample Use new pipes for connecting the installation

• exterior ∅ : 6 mm imperatively (or ¼'') • Material : polyethylene or PTFE or FEP • Pressure : 0,2 to 6 bars • Temperature : 5 to 50°C

At this stage of the installation, make sure that the flow valves (2) are all closed.

The connection of pipes is done by insertion into the quick release connections found under the sampling block.

Figure 8 Direct sample connections

1

3

2

Connecting the evacuation (drain) tube The connection of the pipe is located on the bottom of the analyser and is carried out by the user with the help of a 12 x 17 mm pipe delivered with the instrument. It should be at atmospheric pressure and not be looped.

Caution :

Evacuation should be free of any mechanical constraints, and free of any counter-pressure.

1- Solenoid valve 2- Solenoid valve flow adjustment screw 3- Sample input 1 to 6

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SILKOSTAT 9210

Mains power connection

Figure 9 Layout of electronic boards in the datalyt box

The electrical installation should be carried out by duly qualified personnel. A supply voltage of 100-240 VAC is acceptable without changing the configuration. The power supply terminals can be removed from their housing to make connection easier.

For safety reasons, it is imperative to respect the working procedure below :

• Use a three-wire power lead (line + neutral + earth) sized for supplying the required power.

• The instrument should be connected to the mains via a circuit-breaker or fuse whose value should be less or equal to 20 A. It should be located in proximity and be identified.

• This connection should cut-off the phase and the neutral when electrical problems occur or when the user wishes to intervene inside the instrument. On the other hand, the earth conductor should always be connected.

Danger :

No intervention should be carried out on the instrument without first switching off the power.

1

2

3

4

1 - Mains power connection terminals 2 - Real time clock backup battery 3 - RS 485 (or equivalent) communications module 4 - Internal communications and low voltage power supply connector (for

additional electronics modules).

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SILKOSTAT 9210

The connection of mains is found in the transmitter box.

To gain access :

• Unscrew the 4 screws from the front panel.

• Rotate the front panel.

• Remove the shielding plate.

• Run the cable through the transmitter gland.

• Remove the terminals and screw up the wires.

Figure 10 Position of mains connection and the fuse

Fuse T2 AL – 250 V

according to CEI 127

In mains N

L

earth neutral line

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SILKOSTAT 9210

Figure 11 Shieldied plate of the 9210

RS485 connections (optional extra)

• Unscrew the 4 fixing screws from the front panel and turn it round.

• Run the cable through the transmitter gland.

• connect RX/TX+ and RX/TX- (connector is on the optional board figure 3.5 item 3).

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SILKOSTAT 9210

User signals connections This box is found on the back of the SILKOSTAT on the top (see figure 6).

Unscrew the 4 screws of the cover to gain access to the terminals.

Note :

The cable glands mounted on the “local controller box” should be perforated with a screwdriver before being used.

To ensure a good seal, the external diameter of cables should be between 5 and 7 mm.

Figure 12 “Local controller” connections

+

+

1

+ +

++

+

FIX2

+

Vcc

TDO

TCK

TMS

TDI

GN

D

Rel

12

Rel

11

Vout 1Vout 2Vout 3Vout 4Vout 5Vout 6Vout 7Vout 8Vout 9Vout 10Vout 11Vout 12Iout 1

Iout 2Iout 3Iout 4Iout 5Iout 6Iout 7Iout 8

In 1

In 2

In 3

In 4

In 5

In 6

In 7

In 8

In 9

In 1

0In

11

In 1

2P

t 100

Hea

ter

Mix

er

Rel

10

Rel

9R

el 8

Rel

7R

el 6

Rel

5R

el 4

Rel

3R

el 2

Rel

1

Danger :

The relay outputs can only supply power in very low safety voltage (30 VAC Or 42.4 Vdc maximum) and limited to 0,5 A.

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SILKOSTAT 9210

Connections Function Max. voltage

Max. current

Mixer control 24 Vac 1 A

Heater control 24 Vdc 1 A

Cell temperature measurement 5 Vdc 1 mA

Re1 to Re6 User relay of threshold 1 to 6 30 Veff ou 0,5 A Re7 to Re10 Not used in this application 42.4 Vdc resistive Re11 Warning alarm charge Re12 System alarm (NO and NF switch are available) In1 to In6 Inhibition input (channels 1 to 6)

For input In1, use terminals “in” and "-“ . Terminals « + » and « out » are not used.

5 Vdc 5 mA

In7 to In10 Input not used in this application In11 Remote acknoledgment of alarms In12 Level sample detector Iout1 to Iout6 Analog output 0-20 or 4-20 mA (channels 1 to 6) 24 Vdc 23 mA Iout7 Analyser status Iout8 Not used in this application Vout1 Sampling electrovalve control 30 Vdc 1 A Vout2 to Vout7 Sample selection electrovalves control (channels 1 to 6) Vout8 Calibration pump Vout9 to Vout11 Reagent pump P1 to P3 Vout12 Drain pump

Note :

The system alarm relay (12) is in the positive safety position for informing in case of a cut-off or an analyser error.

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SILKOSTAT 9210

4. Starting-up

Reagent preparation

Danger :

Read the precaution and security appendix and wear protective goggles and clothes before use chemical products.

Reagent concentrations (by type)

Reagent 1 - Molybdate reagent

• Sodium dihydrate molybdate 50 g/L

• Concentrated sulphuric acid 45 mL/L

Reagent 2 - Oxalic reagent

• Oxalic acid dihydrate 40 g/L

Reagent 3 - Reducing reagent

• Concentrated sulphuric acid 12.5 mL/L

• Ammonium ferrous (II) sulphate hexahydrate 20 g/L

Reagent preparation (makes 2 litres)

Reagent 1 - Molybdate reagent

Sodium dihydrate molybdate, Na2MoO4.2H2O, >99%, neat (analytical quality)

(FLUKA# 71756, MERCK# 106521 or equivalent) 100 g

Concentrated sulphuric acid, H2SO4, 95-97%, neat (analytical quality)

(FLUKA# 84721, MERCK# 100731 or equivalent) 90 mL

1) Fill a 2-litre graduated flask to 2/3rds capacity with demineralised water (with the lowest possible silica content). Add the sodium dihydrate molybdate whilst stirring the solution.

2) Continue to stir until the molybdate is completely dissolved (<5minutes).

3) Still stirring, slowly add the concentrated sulphuric acid in 3 or 4 parts (measured out from a test tube).

4) Keep stirring until completely dissolved (<5minutes).

5) Make up the volume to the gauge line (2 litres).

6) Leave to cool before transferring to the 2-litre container provided for this reagent.

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SILKOSTAT 9210

Reagent 2 - Oxalic reagent

Oxalic acid dihydrate, C2H2O4.2H2O, >99.5%, neat (analytical quality),

(FLUKA# 75700, MERCK# 100495 or equivalent) 80 g

1) Fill a 2-litre graduated flask to 2/3rds capacity with demineralised water (with the lowest possible silica content). Add the oxalic acid whilst stirring the solution.

2) Keep stirring until completely dissolved (<5minutes).

3) Make up the volume to the gauge line (2 litres).

4) Transfer to the 2-litre container provided for this reagent.

Reagent 3 - Reducing reagent

Concentrated sulphuric acid, H2SO4, 95-97%, neat (analytical quality)

(FLUKA# 84721, MERCK# 100731 or equivalent) 25 mL

Mohr's Salt = Ferrous (II) ammonium sulphate hexahydrate, (NH4)2Fe(SO4)2,6H2O, >99%, neat (analytical quality)

(FLUKA# 09720, MERCK# 103792 or equivalent)

40 g

1) Fill a 2-litre graduated flask to 2/3rds capacity with demineralised water (with the lowest possible silica content). Add the concentrated sulphuric acid whilst stirring the solution (measured out from a test tube).

2) Still stirring, add the ferrous ammonium sulphate hexahydrate.

3) Keep stirring until completely dissolved (<5minutes).

4) Make up the volume to the gauge line (2 litres).

5) Leave to cool before transferring to the 2-litre container provided for this reagent.

Calibration solution

CONCENTRATED SOLUTION

Use of Titrisol (Merck) cartridge

Dillute one cartridge of Titrisol Merck 109947 solution into one litre of demineralised water will give a concentration of 1000 mg/litre of Si, ie, 2139 mg/litre of SiO2.

Dillute this solution, 100 times, ie, 10 ml in one litre. This will give a concentration of 10 mg/litre of Si, ie, 21.39 mg/litre SiO2.

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SILKOSTAT 9210

CALIBRATION SOLUTION

By diluting an appropriate volume of the concentrated solution (at 21.39 mg/litres) with demineralised water, various calibration solutions with a known concentration of SiO2 may be prepared :

Suggestion for calibration solution preparation (for 2 litres)

ml of concentrated solution 21.39 mg/l

calibration solution ppb Si

calibration solution

ppb SiO2

Instrument Measuring range

10 50 107 0-200 ppb 20 100 213.9 0-200 ppb 25 125 267.4 0-500 ppb 50 250 534.8 0-1000 ppb

Positioning the canisters

Reagent tubings are tagged as 1 to 3. They come with an analyser and are fed through the special stoppers on the reagent canisters. One end of these pipes is fitted with a chemically inert, PVC strainer that is used to position the pipes in the bottom of the canisters. Before starting analyser, it is necessary to connect each cap on its canister : • Tubing N° 1 on the reagent canister R1: Sodium molybdate and

sulphuric acid. • Tubing N° 2 on the reagent canister R2: Oxalic acid reagent.

• Tubing N° 3 on the reagent canister R3: Sulphuric acid and ferrous

ammonium sulphate.

Screw the cap on the canisters. Then, check that the strainer is resting in its proper position at the bottom of the canister. Put the canister on the canister-stand to have cap towards interior as shown figure 7

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SILKOSTAT 9210

In the panel version, the canister-stand must be under the analyser panel. In the cabinet version, it is in the back part of the cabinet.

Note : The canisters must not be placed more than 40 cm from the lower part of the down of the panel to have a good reagent injection in the cell.

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SILKOSTAT 9210

Using the menu

Sample 1 14:00 10.00 ppb

Last calibration Sample 5 P:date Sampling O:date DISP2 START MENU

Esc

Modification of a value

The highlighted digit may be modified with the key . Each digit can be modified by pressing ENTER. Repeat both operations for each digit.

On the first digit : possibility to display the sign "-"

On the others digits : possibility to display the sign "."

Note : If you do not use the keyboard for at least 10 minutes, the instrument returns to the measuring mode except for the calibration and maintenance mode.

An access code may be required for the calibration, programming and service menu (see CODE menu).

Name of last measured sample (here : sample 1)

Current time (XX:XX).

Concentration of last measured sample.

Unit concentration.

Sample is being analysed : SAMPLE 5. Analysis status : sampling, conditioning, measure … Bargraph indicates the state of the cycle.

Display of the last calibration, date and hour.Default values for dates and hours are 09/09/09 00/00/00.

Function key ESC : cancels a data input or goes back to the

previous screen Enter : validate and go to the next step : function keys

Access to Programming mode.

Go to display 2.

Start / stop the analyser.

10

10

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SILKOSTAT 9210

Language programming

SERVICE TIME AFFICHAGE CODE SOFT ISSUE DEFAUT VALUES ADJUST mA CONFIGURATION FACTORY select

Esc

Access to the menu :

• Press the "MENU" key.

• Choose "SERVICE" menu with the "select" function key and validate by "Enter".

• Choose "DISPLAY" menu with the "select" function key and validate by pressing "Enter".

DISPLAY LANGUAGE : F CONCENTRATION : ppb/ppm CUSTOMIZE Select

Esc

Choice of the language, measures units and samples customize.

Use the key to change the selected digit and press the "Enter", key to validate the modification and select the next digit.

Languages available are :

• French : F • English : GB • German : D • Spanish : Sp • Italian : I

Unit choice is ppb or µg / l.

Time and date programming

TIME DAY : Monday DATE (JJ MM AA) : 09/05/01 TIME : 14:43:16 Select

Esc

Access to the menu :

• Choose the sub menu "TIME" in the menu "SERVICE" and validate by pressing "Enter".

• Use the key to change the selected digit and press the "Enter" function key to validate the modification and select the next digit.

DISPLAY

Note : See menu "customize" for the customization of the name of the measuring channels.

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SILKOSTAT 9210

Starting up the analyser

START UP Adjust flow Sample x OK

Esc

Adjustment of the samples flow

This adjustment is used to set up the flow-rates for the various channels. The sampling solenoid valve is open during this stage and agitation is continuous. The flow rate may be set by adjusting the screws on the front panel so as to fill the overflow vessel and guarantee a slight overflow.

The "Enter" key allows to access to the next sample.

x : n° of the sample (1 to 6).

START UP Pumps priming Verify immersion OK

Esc

Pumps priming :

Imerge the different reagent tubings in the canisters.

Press OK when pipes of the different pumps are full of reagent. Go back to "maintenance" menu.

MAINTENANCE DEMARRAGE REAGENTS REFILL EXTENDED STOP TUBES CLEANING PHOTOMETER TEST PUMPS-OTHERS SOLENOID VALVES RELAYS LOGICAL INPUTS Select

Esc

Access to the menu :

• Stop the analyser if it is analysing with the help of START/STOP function key.

• Press the "MENU" key.

• Choose "MAINTENANCE" menu with the "select" function key and validate by pressing "Enter".

• Choose "START UP" sub menu, press "Enter".

This menu allows two choices :

START UP

Caution : Don’t completelly unscrew the flow adjust screws. There is no stop screw, so it will provoke a sample leak

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SILKOSTAT 9210

Starting a measurement

Sample 1 14:00 10.00 ppb

CAL Sample 5 P : 02/02/02 Sampling 14:30:00 Z : 03/02/02 14:30:00 DISP2 START MENU

Esc

With the help of the "Esc" function key, go back to the main screen and press "START" key.

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SILKOSTAT 9210

5. Analyser programming

Analyser configuration flow chart

MENUCALIBRATION

CALIBRATION PROGRAMMINGEXECUTION PRIMARY EXECUTION MANUAL PARAMETERS HISTORIC

PROGRAMMING EXECUTION MANUAL OFFSET INTERVAL : xxx h

AUTOMAT SLOPE CAL. : YES / NO CAL. SOL : xxx,x ppb AUTOMAT CAL: NO

EXECUTION ZEROEXECUTION SLOPE EXECUTION ZERO+SLOPE

MAINTENANCE MAINTENANCE START UP

REAGENTS REFILL TUBES CLEANING EXTENDED STOP PUMPS-OTHERS SOLENOID VALVES RELAYS PHOTOMETER TESTLOGICAL INPUTS

REAGENTS REFILL ADJUST VOLUMES ADJUST VOLUMESTUBES PRIMING BOTTLES FULL : yes/no

REAGENT 1 VOL : x.xx l REAGENT 2 VOL: x.xx l REAGENT 3 VOL: x.xx l REAGENT 4 VOL: x.xx l

PUMPS PUMP 01 : off/on PUMP 04 : off/on Drain : on/off Mixer : on/off Heater : on/off

SOLENOID VALVES .

VALVE 01 : off/onVALVE 07 : off/on

RELAYS RELAY 01 : off/on RELAY 12 : off/on

.

MEASURE MEASURE MEASURING MODE GRAB SAMPLE HISTORIC ADC VALUES

PROGRAMMINGMODE : NormalCYCLE : IN LOOP

HISTORICPROGRAMMINGREAD

PROGRAMMINGFROM : xx/xx/xx AT : xx:xx:xx CH : A11 ALARMS : yes ALARMS ALARMS

ALARM 1 ALARM 2 ALARM 3 ALARM 4 ALARM 5 ALARM 6 WARNING ALARM SYSTEM ALARM

ALARM XMOD : limitAFFECT : Channel 1LIMIT : xxx.x ppb DIRECTION : DownHYSTERESIS : xx%RELAYS : NO/NC

WARNING ALARMALARM : yes/no ACCEPT : manual RELAYS : NO/NC

SYSTEM ALARM ALARM : yes/no

mA OUTPUTS mA OUTPUTS AFFECT SPECIAL PROG. TEST

AFFECTOUTPUT 1OUTPUT 2OUTPUT 3OUTPUT 4OUTPUT 5OUTPUT 6

OUTPUT XAFFECT : Channel x TYPE: 0-20 MODE : Linear LOW : xxx.x ppb UP : xxx. ppb

SPECIAL PROG. MAINTENANCECALIBRATION GRAB SAMPLE SYSTEM ALARM WARNING ALARM

CALIBRATION MODE : Last

TESTVALUE : xx mA

COMMUNICATION COMMUNICATION N° : xx BAUD : 300/600/1200/2400/4800/9600 PARITY : no/even/odd BIT STOP : 1/2

SEQUENCE SEQUENCECHANNEL ACTIVATIONSEQUENCE

CHANNEL ACTIVATION CHANNEL 1 : On / Off

CHANNEL 6 : On / Off SERVICE SERVICE ...

TIME DISPLAY CODE SOFT ISSUES DEFAULT VALUESADJUST mA FACTORY

TIMEDAY : xxxxxDATE : JJ/MM/AATIME : xx/xx/xx

DISPLAY LANGUAGE : F/GB/D/Sp/I CONCENTRATION : ppb-ppm / ug-mg/l CUSTOMIZE

CODE

PROGRAMMATION: xxxCALIBRATION : xxxx SERVICE : xxxx mA ADJUST

CONFIGURATION OUTPUT 1

OUTPUT 8...

…

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SILKOSTAT 9210

User Interface The interface consists of 5 keys and a graphic backlet display screen providing a display of the data, operational settings and trend curves.

Informations are available from several screens.

Main display

Sample 1 14:00 10.00 ppb

Last calibration Sample 5 P : 02/02/02 Sampling 14:30:00 Z : 03/02/02 14:30:00 DISP2 START MENU

Esc

10

Name of last measured sample (here : sample 1)

Current time (XX:XX).

Concentration of last measured sample.

Unit concentration.

Sample is being analysed : SAMPLE 5. Analysis status : sampling, conditioning, measure … Bargraph indicates the state of the cycle.

Last slope and offset calibrations, date & time.

Function key ESC : cancels a data input or goes back to the

previous screen Enter : validate and go to the next step : function keys

Programming mode.

Go to display 2.

Start / stop the analyser.

10

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SILKOSTAT 9210

Definition of the display screen 2 (Disp2)

Sample 1 : XXX XX:XX:XX Sample 6 : XXX XX:XX:XX Extern :

DISP3

Esc

Last measures with next indications:

.

.

.

.

.

.

.

.

.

.

.

.

.

.

.

.

Sample name.

The last concentration value of the sample.

Time when last measurement was performed

Function key Disp3 (alarms) allows to access to the display 3.

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SILKOSTAT 9210

Definition of the display screen 3 (Disp3) : alarms

ALARM S1 : OK . . S6 : OK W : disable : OK DISP4

Esc

This screen displays the alarms status as well as the following indications :

• S1…S6 : Threshold function with the following parameters,

* OK : Alarm condition is not met.

* Sample X > XXX : Alarm is actived and the alarm condition is clearly mentioned. For example, the sample X measurement exceeds xxx ppb.

* Disable: Alarm function is disactivated.

• W : Warning alarm.

• : System alarm.

• DISP4 : Go to the display 4.

The following table indicates the different messages which may appear in case of default.

Displayed message (english)

Description Category

Reset mod. Measure Reset of the measure module System Reset module LC Reset of the local controller module. System Error lc Local controller module error System Err. measure mod. Measure module error System Com error CAN communication error System Table error Error during table transmission System Task error Task execution error System Measure error Measurement error Warning Reference error LED light ajustment problem Warning Extinction error Black current problem Warning Meas.time over Maximum cycle time for the measure

has been exceeded Warning

Cal.time over Maximum cycle time for calibration has been exceeded

Warning

No sample No sample available System Sample x missing Sample x missing Warning Reagent < 250 ml Low level of the reagent left (2.5 days

before no reagent alarm) Warning

Calib < 300 ml Low level of the calibration solution (1 calibration left before no calibration solution alarm)

Warning

No reagent Empty reagent canisters <150 ml System Slope drift Slight drift of slope calibration

parameter (Confirmation zone) Warning

Zero drift Slight drift of zero offset calibration parameter (Confirmation zone)

Warning

Zero error Zero calibration major error System Slope error Slope calibration major error System Sample x < C Sample concentration x is lower than

C Threshold

Sample x < 0 ppb Sample concentration x is negative Warning Sample x > 1000 ppb ou > 5000 ppb

Sample concentration over range Warning

Reference error The reference measurement lies outside its limiting values

Warning

.

.

.

.

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SILKOSTAT 9210

Definition of the display 4 (Disp 4) : trend curve

Sample 4 (X) 30/08/01

Esc

Function key :

• Main : Return to the main screen.

• Graph+ : Visualisation of the 6 curves associated with the 6 analogue outputs.

Modification of a value

The highlighted digit may be modified with the key . Each digit can be modified by pressing ENTER. Repeat both operations for each digit.

On the first digit : possibility to display the sign "-"

On the others digits : possibility to display the sign "."

Note :

If you do not use the keyboard for at least 10 minutes, the instrument returns to the measuring mode except for the calibration and maintenance mode.

An access code may be required for the calibration, programming and service menu (see CODE menu).

Main Graph+

This screen allows to display the trend curves.

Constant time scale which corresponds to 24 hours.

concentration scale equals to analogue output programmed scale.

Sample name.

Number of the associated output.

Date of the trend curve.

0 24

5,00

0,00

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SILKOSTAT 9210

Main menu

Sample 1 14:00 10.00 ppb

CAL Sample 5 P = 02/02/02 Sampling 14:30:00 Z = 03/02/02 14:30:00 DISP2 STOP MENU

Esc

Sample 1 14:00 10.00 ppb

CAL Sample 5 P = 02/02/02 Sampling 14:30:00 Z = 03/02/02 14:30:00 ARE YOU SURE ? YES / NO

Esc

Sample 1 14:00 10.00 ppb

CAL ANALYSER P = 02/02/02 STOPPED 14:30:00 Z = 03/02/02 14:30:00

DISP2 STOP MENU

Esc

You have 2 possibilities to access to the programming menu :

• Access to the menus which are not protected by a code :

Simply press "MENU".

• Access to the menus which are protected by a code :

Press "STOP" key.

Confirm by "YES" key.

Press "MENU"

Once the programming operation is completed and if the analyser is stopped, press "START" to restart it.

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SILKOSTAT 9210

Calibration menu

CALIBRATION PROGRAMMING EXECUTION PRIMARY CAL EXECUTION MANUAL CAL PARAMETERS HISTORIC Select

Esc

To get a good precision from the instrument, you should calibrate it on a regular basis.

Calibrations allow to adjust :

• ZERO of the system.

• SLOPE of the system.

• Both ZERO and SLOPE of the system.

The ZERO calibration is performed by the SILKOSTAT/chemically.

In order to avoid the use of water free of SiO2, the SILKOSTAT carries out a measurement without a colorimetric reaction.

The slope of the system is calibrated with a known concentration of SiO2 standard solution.

Three types of calibration are available :

• Primary calibration.

• Manual execution.

• Automatic execution.

MENU CALIBRATION MAINTENANCE MEASURE ALARMS mA OUTPUTS COMMUNICATION SEQUENCE SERVICE Select

Esc

"MENU" allows to access to the programming of the instrument.

This screen allows to choose between different programming sub-menus.

Press the "Select" function key to select the programming menu you wish to have access to and press "Enter" to validate the choice.

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SILKOSTAT 9210

Execution primary sub menu

CALIBRATION PROGRAMMING EXECUTION MANUAL CAL PARAMETERS HISTORIC Select

Esc

A primary calibration is carried out when operating the instrument for the first time and is used as a reference for the following calibrations. Generally, it should be carried out only after a consequent modification.

It allows to fix the zero and slope reference.

All the results of the further manual or automatic calibrations will be compared to the zero and slope references set by this calibration.

A more important shift will allow to detect an error calibration which will be signified by an error message.

This calibration can be realized only in the manual way.

• Access to the main "MENU".

• Choose "CALIBRATION" menu with the "select" function key and validate by pressing "Enter".

• Choose "EXECUTION PRIMARY" sub menu and validate by pressing "Enter".

The slope calibration is going on, followed by the zero.

PRIMARY CALIBRATION Slope calibration Cal sol sampling CALIBRATION

Esc

The upper bar indicates the type of calibration : primary, manual or automatic.

Press "Esc" if you want to quit the calibration menu : and go back to the "CALIBRATION" menu.

The calibration stages are displayed as follow :

• Sample preparation. • Conditioning • Measure. • Rinse.

A bargraph indicates the calibration state.

At the end of the calibration, results are displayed on screen.

EXECUTION PRIMARY CAL

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SILKOSTAT 9210

PRIMARY CALIBRATION Default values : S = 760.0 O = 0.0 Primary calibration S = XXX O = XXX

Esc

Primary calibration results:

S = value of the slope (ppb / Abs)

O = value of the zero shift in milli-Abs

The default values show a general idea of standard values according to the range (0-1000 or 0-5000 ppb).

Execution manual sub menu

CALIBRATION PROGRAMMING EXECUTION PRIMARY CAL PARAMETERS HISTORIC Select

Esc

Choice of the calibration.

Access to the menu :

• Press "MENU" key.

• Choose "CALIBRATION" menu with the "select" function key and validate by pressing "Enter".

• Choose "EXECUTION MANUAL CAL" with the "select" function key and validate by pressing "Enter".

CALIBRATION EXECUTION ZERO EXECUTION SLOPE EXECUTION ZERO + SLOPE Select

Esc

This screen allows a manual calibration of the SILKOSTAT 9210.

Press "select" key.

Choose "EXECUTION ZERO" or "SLOPE” or "ZERO + SLOPE" sub-menu and validate by pressing “Enter" key.

EXECUTION MANUAL CAL

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SILKOSTAT 9210

Programming sub menu (automatic execution)

CALIBRATION EXECUTION PRIMARY EXECUTION MANUAL PARAMETERS HISTORIC Select

Esc

The calibration of the zero and the slope can be carried out automatically at adjustable frequencies.

• Press "CALIBRATION" menu.

• Sub-menu "PROGRAMMING" and validate by pressing "Enter".

• Choose "PROGRAMMING" sub-menu and validate by pressing “Enter”.

PROGRAMMING OFFSET INTERVAL : 200 h CAL. SOL.: 010.0 ppb AUTO. CAL. : Non Select

Esc

This screen allows to program the zero calibration frequency, the calibration concentration solution and to choose an automatic calibration or manual calibration. The following table indicates the zero calibration frequency controlled in terms of the minimum concentration of the samples.

PROGRAMMING

Sample minimum concentration Zero frequency control < 5 ppb 24 hours

5 < x < 50 ppb 48 hours > 50 ppb > 72 hours

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SILKOSTAT 9210

PROGRAMMING OFFSET INTERVAL : 200 h CAL.: 010.0 ppb AUTO SLOPE CAL. : Yes BASE : Day WEEK : SMTWTFS HOUR : 15:00:00 Select

Esc

OR

In case of an automatic slope calibration, this screen allows to adjust the frequency.

• When the "BASE" menu is selected, the "WEEK" menu allows to choose the calibration day (s).

Ex : SMTWTFS, daily calibration. SM*W*FS, calibration every day except Tuesday and Thursday.

"HOUR" menu allows to adjust the hour to start calibration.

PROGRAMMING OFFSET INTERVAL : 200 h CAL. : 010.0 ppb AUTO SLOPE CAL.. : Yes BASE : Hour INTERVAL : XXXX Select

Esc

When the hour base is chosen , the "INTERVAL" menu allows to adjust the periodicity of the calibration slope.

The required slope calibration frequency is about 1 week (168 hours).

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SILKOSTAT 9210

Calibration parameters sub menu

MANUAL / AUTOMATIC CALIBRATION

Default values : S = 760.0 O = 0.00 Primary calibration : S = 694.0 01/01/01 O = 0.00 01/01/01 Last calibration : S = 694.0 01/01/01 O = 0.00 01/01/01

Esc

This screen allows to visualize the primary calibration parameters and the last calibration parameters.

Calibration historic sub menu

HISTORIC 31/08/00 auto 09:18:01 O = -5 19:28:51 O = -5 02/09/00 manu 10 :01 :05 O = -4 S = 560 12/09/00 manu 15 :01 :05 o = -6 S = 561 Select

Esc

This screen allows to visualize the calibrations historic with the following information :

• Date and hour.

• Type : manual or automatic.

• Slope (S) and offset (O).

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SILKOSTAT 9210

Manual – automatic calibration results sub menu

At the end of a manual or automatic calibration, the analyser compares the results with the primary calibration master.

According to the calibration results, you can validate, restart or quit the calibration.

There are 3 zones :

S : (%) 20 % 50 % 150 % 180 %

Rejection zone Confirmation zone Zone ok Confirmation

zone Rejection zone

O : (mAbs) - 50 - 30 30 50

XXX Primary calibration : S = XXX XX:XX:XX O = XXX XX:XX:XX Last calibration S = XXX XX:XX:XX O = XXX XX:XX:XX C = XXX XX:XX:XX Actual calibration S = XXX O = XXX Calibration OK OK

Esc

Zone ok

Normal variations around the reference values. The new parameters are considered.

In automatic mode, the analyser returns to its measurement cycle.

In manual mode, validate with OK and restart the instrument (START).

P:XXXXX DD:MM:YY slope

Z:XXXXX DD:MM:YY offset

C:XXXXX DD:MM: concentration of the sample solution just measured, calculated using the calibration values from the "Last calibration".

Prim

ary

calib

ratio

n m

aste

r

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SILKOSTAT 9210

XXX Primary calibration : S = XXX XX:XX:XX O = XXX XX:XX:XX Last calibration S = XXX XX:XX:XX O = XXX XX:XX:XX C = XXX XX:XX:XX Actual calibration S = XXX O = XXX Calibration error Conf Cancel

Esc

Confirmation zone

Abnormal gap compare to the reference. So it allows to have correct results and a warning is displayed. In automatic mode, the analyser returns to the measure mode with the previous parameters.

In manual calibration, you must confirm (Conf) or cancel (Annul) the new parameters.

XXX Primary calibration : S = XXX XX:XX:XX O = XXX XX:XX:XX Last calibration S = XXX XX:XX:XX O = XXX XX:XX:XX C = XXX XX:XX:XX Actual calibration S = XXX O = XXX Calibration error Cancel Remake

Esc

Rejection zone

Parameters are abnormal. There is material problem or an important error like bad calibration solution preparation. (see troubleshooting).

In automatic mode, the analyser stops and emits an alarm system.

In manual mode, you can cancel (turn to the measure with previous parameters) or restart a calibration.

Note : The reference measurement lies outside its limiting values. In auto mode, where the calibration has not been made correctly, the analyser takes one measurement and then recalibrates. After 3 successive faulty calibrations, the 9210 waits for the next programmed date.

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SILKOSTAT 9210

Maintenance menu

Note :

When one of the maintenance procedure is released, the analyser automatically stops

Don’t forget to restart the instrument when maintenance operations are realized.

Start up sub menu

MAINTENANCE START UP REAGENTS REFILL EXTENDED STOP TUBES CLEANING PHOTOMETER TEST PUMPS / OTHERS SOLENOID VALVES RELAYS LOGICAL INPUTS Select

Esc

This screen allows to choose the proposed maintenance help procedure :

Start up

• Starting procedure.

Reagents refill

• The procedure is applicable to each reagent refill.

Extended stop

• Allows to condition the instrument before an extended stop.

Tubes cleaning

• In case of reagent tubings clogging.

Photometer test : Check the photometer.

Pumps, Solenoid valves, relays, others

• Working test of this devices.

Logical inputs

• Logical inputs test.

START UP Adjust flow Sample X OK

Esc

This screen allows to adjust the sample flows

Adjust the first sample flow with the help of the screws placed in the front panel of the face (see figure 3.4 item. 2) to have a perpetual overflowing in the top of the overflow vessel.

Press OK to go to the next sample.

Warning : Do not unscrew completely the flow rate set screw. It has no stop and may get out of its housing and provoke a sample leak.

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SILKOSTAT 9210

Reagents refill sub menu

Adjust volumes

START UP Pump priming OK

Esc

Pump priming :

Press OK when the pump tubing are full of reagent. The display goes back to the menu “Maintenance”.

REAGENTS REFILL ADJUST VOLUMES TUBING DRAINING CANISTERS FULL yes/no Select

Esc

Every reagent and calibration solution renewal, access this menu for.

This menu allows to choose between :

ADJUST VOLUMES : the 4 canisters volumes are displayed and can be modified.

TUBES PRIMING : start the priming / renewal procedure of the reagents in the tubes. "Esc" allows to return to the previous screen or to stop the procedure.

CANISTERS FULL : choose this option each time than canisters are full. The volumes of the 4 canisters are automatically programmed with 2 litres.

ADJUST VOLUMES REAGENT VOL 1 : 2.00 λ REAGENT VOL 2 : 2.00 λ REAGENT VOL 3 : 2.00 λ REAGENT VOL: 2.00 λ Select

This menu allows to visualize the volumes of the reagent canisters and the calibration solution. You eventually can adjust these volumes. The «FULL CANISTERS » menu put these volumes to 2 litres.

The analyser controls the calibration solution and reagent consumption and emits alarm system according to the level of the canisters.

Warning Alarm system

Reagents < 250ml < 150ml Esc

Cal solution < 300ml

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SILKOSTAT 9210

Tubes priming

Note :

It is recommended to calibrate the zero after each reagent refill.

Extended stop sub menu

REAGENTS REFILL Please wait…

Esc

The tubes priming is going on ; the reagent pumps and the calibration solution are running at the same time than the mixing motor and the drain.

REAGENTS REFILL ESC = quit

Esc

At the end of the tubes priming you can quit the procedure by pressing "ESC".

After the pump operation, check visually the tubings are full. If it is not the case, return to the menu "pump".

EXTENDED STOP

Put tubes in demineralised water

Accept with OK

OK

Esc

This screen shows the procedure to follow in case of a long stop (1 or more than a week).

Provide 250 ml of demineralised water.

Press "OK" to start each stage of the procedure.

Follow the instructions and validate each stage with "OK".

At the end of the stop, restart the analyser with the help of the MAINTENANCE / START UP menu.

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SILKOSTAT 9210

Tubes cleaning sub menu

TUBES CLEANING

Put tube R1 in NH4-OH solution

Accept with OK

OK

Esc

Tubes cleaning procedure in case of depositing.

Have ready a beaker containing 250ml of demineralised water and a second beaker containing 100ml of ammonia at 10% of normal commercial concentrations by volume, ie, approximately 3% v/v. Immerse tubing R1 in the ammoniac solution.

Press "OK" for the cleaning and press "Esc" to stop and come back to the previous screen.

Follow the instructions and validate by "OK".

TUBES CLEANING Put pumps tubes In demineralised water Accept with OK.. OK

Esc

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SILKOSTAT 9210

Measure / Photometer test sub menu

Pumps-others sub menu

PHOTOMETER TEST Dark current : 0.008 Reference : 3.50 Led current : 9000 Measure : 3.10 Absorbance : 52.7 Bck ref meas

Esc

With this menu, technicians can verify the good running order of the photometer.

The mixer is operating and the transfer valve is open.

Displayed parameters Dark current : Measurement value which corresponds to the

emitter LED. Reference : reference signal after LED current adjustment. Led current : current of the LED. Measure : Continuous photometric measure signal. Absorbance : Absorbance in milli-Abs. Function key Bck : allows to begin the measure which corresponds to the

switching off of the LED. Ref. : allows to adjust the led current and to measure the

reference voltage.

Mes : starts the continuous photometric measure.

MAINTENANCE Pump 01 > OFF Pump 02 OFF Pump 03 OFF Pump 04 OFF Drain OFF Mixer OFF Heater OFF Select On Off

Esc

This screen allows to test the good running order of the pumps, the mixer, the drain and the heater.

Utilize the "Select" key to control an element and press the "On" key to operate it or "Off" key to stop it.

The following table shows the nominal flow rates for each pump :

Pumps 01 Reagent 1 1,5ml/mn Pumps 02 Reagent 2 1,5ml/mn Pumps 03 Reagent 3 1,5ml/mn Pumps 04 Cal. solution 10l/h

Page 50

SILKOSTAT 9210

Solenoid valves sub menu

Relays sub menu

Logical inputs sub menu

MAINTENANCE

Solenoid valve 01 > OFF Solenoid valve 02 OFF Solenoid valve 03 OFF Solenoid valve 04 OFF Solenoid valve 05 OFF Solenoid valve 06 OFF Solenoid valve 07 OFF Select On Off

Esc

This screen allows to test the correct operating of the solenoid valves.

Utilize the "Select" key to select a valve and press the "On" key to operate it or "Off" key to stop it.

Press "Esc" to come back to the previous screen.

• Solenoid valves 01 to 06 : sample solenoid valves ( measuring channel 01 to 06).

• Solenoid valves 07 : measure solenoid valves (sample transfer from overflow tank to measuring cell.).

MAINTENANCE Relay 01 > OFF Relay 02 OFF Relay 03 OFF Relay 04 OFF Relay 05 OFF Relay 06 OFF Relay 07 OFF Relay 08 OFF Relay 09 OFF Relay 10 OFF Relay 11 OFF Relay 12 OFF Select On Off

Esc

This screen allows to operate or to stop the relays.

Utilize the "Select" key to select a relay and press the "On" key to operate it or "Off" key to stop it.

LOGICAL INPUTS

I/O 0 0 0 0 1 1 2 4 6 8 0 2 ------------------------- Status * 1 * 1 * * * * * * *

ESC : exit

Esc

This screen displays the status of the logical inputs and allows to test the good running order of the inputs In1 to In12.

Status : 1 : short circuited input

* : open input

Note : See the relays functions on page 21.

Example : in the above example, measurements on channels 3 and 6 are inhibited.

The analyser goes directly to the next channel

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SILKOSTAT 9210

Measure Menu

Measuring mode sub menu

MEASURE MEASURING MODE GRAB SAMPLE HISTORIC ADC values Select

Esc

This screen allows to accede to the measure parameters ; the mode and the cycle of measure, the historic, the external sample measure (manual analysis) and the photometer parameters (ADC values).

The measure historic allows to visualize the data during 5 days.

PROGRAMMING MODE : Normal CYCLE : In loop INTERVAL : XXX mn Select

Esc

OR

This screen allows to program the measuring mode.

If the interval cycle is selected, the analysis are made every 10 minutes.

INTERVAL : XXX mn, you must adjust the measuring cycle time.

Example : if 030 mn is displayed, the instrument does a measure every 30 minutes.

PROGRAMMING MODE : Normal CYCLE : In loop Select

Esc

If the « In loop » cycle is chosen , measures are made one after one without waiting time.

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SILKOSTAT 9210

Grab sample sub menu

Historic sub menu

GRAB SAMPLE Please wait…

Esc

Allows to carry out the measure with a grab sample.

Before measuring, take 200 ml of the sample to analyse.

The analyser begins to rinse the measuring cell.

GRAB SAMPLE Fill sample About 200 ml OK

Esc

The analyser complains the sample to analyse :

• Remove the level probe of the overflow vessel (figure 3.1, item 2), refill with the sample in 3 or 4 times.

• Replace the level probe.

• Press "Ok" to operate the measure.

To return to the programming, wait the end of the measure (display of the results and « terminate » message).

"Esc" key allows to stop the measure and comes back to the previous screen.

HISTORIC PROGRAMMING READ Select

Esc

This screen allows to read the stored data (concentration and alarm values).

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SILKOSTAT 9210

Programming

Read

ADC values sub menu

PROGRAMMING FROM : 01/01/01 AT : 00/00/00 CH : all ALARMS : yes Select

Esc

Allows to choose the date and the time when the historic will be displayed and the measure channels desired.

• CH : all or individually (1 to 6)

• ALARMS (yes or no) : display of the « system » and « warning » alarms .

HISTORIC 18/05/01 13:30 # 1 12.6 13:40 # 2 103 Select

Esc

"READ" allows to read the historic.

Use the scroll up key to choose the data format.

Date : day/month/year.

Hour, sample n° (#n) and concentration or default.

ADC VALUES PRIMARY CALIBRATION ref : meas : S : XXXX XXXX O : XXXX XXXX LAST CALIBRATION Ref: meas : S : XXXX XXXX O : XXXX XXXX LAST MEASUREMENT ref : meas : XXXX XXXX

Esc

This screen displays the parameters of the photometer for the primary calibration, the last calibration and the last measurement.

The information stored in this menu must be utilized only at the end of the diagnostic in case of incorrect operation.

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SILKOSTAT 9210

Alarms Menu

Alarms parameters 1 to 6 sub menu

Value Description

MODE − Limit − Active

channel − Level

sample.

Allows to choose the type of relay : threshold (limit) , active channel or level sample.

AFFEC Channel 1 to 6 Allows to assign the alarm (1 to 6) to the measure channel of our choice.

LIMIT XXXX Allows to adjust the limit value (ppb)

DIRECTION − Up − Down

Allows to adjust the relay direction interlocking

HYSTERESIS XX % Allows to adjust the hysteresis in %

RELAYS N.O N.C

Relay type

N.O : normally open N.C : normally closed

ALARMS ALARM 1 ALARM 2 ALARM 3 ALARM 4 ALARM 5 ALARM 6 WARNING ALARM SYSTEM ALARM Select

Esc

This screen allows to assign alarms and parameters to each relay.

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SILKOSTAT 9210

ALARM 1 MODE : Limit AFFECT : Channel 2 LIMIT : 100.0 ppb DIRECTION : Up HYSTERESIS : 00 % RELAY : N.O Select

Esc

OR

If MODE = Limit (concentration threshold)

Example :

• Affects the alarm contact 1 to channel 2

• Adjust of the threshold value 100.0 ppb.

• Relay activating direction towards up (when C > 100 ppb).

• No hysteresis : 00 %.

• Relay type N.O. (normally open)

ALARM X MODE : active channel RELAY : NO Select

Esc

OR

If MODE = Active channel

The alarm N°X is activated when the sample N°X is analysing.

Choice N.O (normally open) or N.C (normally closed).

ALARM X MODE : level sample RELAY : NO Select

Esc

If MODE = Level sample

The alarm N°X is activated when the sample N°X is absent.

Choice N.O (normally open) or N.C (normally closed).

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SILKOSTAT 9210

Warning alarm sub menu

System alarm sub menu

NB:

The alarm system can only be acknowledged manually, either by holding down the <Enter> key or, remotely, by using the digital input, In 11, on the I/O card (see Section 3, figure 3.12).

WARNING ALARM ALARM : yes ACCEPT : Manual RELAY : N.O Select

Esc

Allows to adjust the « WARNING » alarm parameters.

ALARM 1 ALARM : yes RELAY : N.O Select

Esc

Allows to adjust the system alarm

Value Description

ALARM Yes No

Warning alarm in operating or not.

Manual

Press enter to accept the alarm (manual).

ACCEPT

Auto Automatic accept of the alarm (disappear when the alarm disappear).

RELAY

N.O

N.C

Type of relay

"Normally not excited (contact closed between 1 and 2 contact open between 3 and 4).

" Normally excited (contact open between 1 and 2 contact closed between 3 and 4)

Value Description

ALARM Yes No

Activates / Deactivates the warning

RELAY

N.O

N.C

Type of relay

"Normally not excited (contact closed between 1 and 2 contact open between 3 and 4).

" Normally excited (contact open between 1 and 2 contact closed between 3 and 4)

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SILKOSTAT 9210

The following table shows the different alarms : • Warning : the analyser emits a warning at the display and on the warning

relay. • System alarm : the analyser locks the system alarm relay, displays a

message ant stops.

Displayed message

(english) Description Category

Reset mod. Measure Reset of the measure module System Reset module LC Reset of the local controller

module. System

Error lc Error of the local controller module

System

Err. measure mod. Error of the measure module System Com error Error CAN communication System Table error Error during transmission the

table System

Error task Error of the task execution System Measure error Error of the measure Warning Reference error Curent del adaptation problem Warning Extinction error Extinction del problem Warning Meas.time over Cycle time of the measure is

very long Warning

Cal.time over Cycle time of the calibration is very long

Warning

No sample No sample here System Sample default x Short sample x Warning Reagent < 250 ml Low level of the reagent Warning Cal.sol < 300 ml Low level of the calibration

solution Warning

Low reagent Empty reagent canisters <150 System Slope drift Confirmation zone Warning Zero drift Confirmation zone Warning Zero default Rejection zone for the zero

calibration System

Offset zero Rejection zone for the slope System Sample x < C Sample concentration x is < to

threshold C Warning

Sample x < 0 ppb Sample concentration x is negative

Warning

Sample x > 1000 ppb ou > 5000 ppb

Sample concentration too high Warning

Reference error. Incorrect reference measurement

Warning

Page 58

SILKOSTAT 9210

mA outputs menu

Outputs affect 1 to 6 sub menu

mA OUTPUTS AFFECT SPECIAL PROG TEST select

Esc

This screen allows to access to the analogue outputs parameters.

AFFECT OUTPUT 1 OUTPUT 2 OUTPUT 3 OUTPUT 4 OUTPUT 5 OUTPUT 6 Select

Esc

This screen allows to select an output and to display its parameters.

AFFECT : Allows to assign the output (1 to 6) to the channel desired.

SPECIAL PROG: Allows to program 0/4-20mA outputs in special cases.

TEST : Allows to test the correct operating of the analogue outputs.

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SILKOSTAT 9210

The following curve indicates the result of the 4-20 current in terms of the scale programming type and the first, middle and end value of the scale.

OUTPUT 1 to 6 AFFECT : X TYPE : 0-20 MODE : Linear LOW : 000.0 ppb UP : 01.00 ppm Select

Esc

OR

OUTPUT 1 to 6 AFFECT : Channel 1 With output 1 TYPE : 0-20 MODE : Linear FIRST : 000.0 ppb MIDDLE : 000.0 ppb END : 000.0 ppm Select

Esc

This screen displays the parameters of each 6 output.

If the dual mode is chosen, you must program the concentration value corresponding to the middle of the scale.

Concentration

•

12 / 10 mA

END FIRST

•

Current 0..20mA/4..20m

4 / 0 mA

20 / 20 mA

•

MIDDLE

Linear

Dual

AFFECT : Choice of the measure channel. The concentration of this channel will be carried over the output X.

TYPE : 0-20 mA or 4-20 mA, choice of the analogue output scale.

MODE : Linear or dual (see curve)

FIRST : First scale value.

MIDDLE : Middle scale value.

END : End scale value.

Page 60

SILKOSTAT 9210

Special prog sub menu

Test sub menu

SPECIAL PROG CALIBRATION GRAB SAMPLE SYSTEM ALARM WARNING ALARM Select

Esc

MAINTENANCE MODE : Last Select

Esc

OR

This screen allows to program the status of the output n°7 during special events :

• Maintenance. • Calibration. • Grab sample analysis. • System alarm. • Warning alarm.

With the help of the CHOICE function, choose the event for which the output n°7 can be programmed.

Storage : The output n°7 is not modified.

SPECIAL PROG

MODE : Preset VALUE : XXX mA Select

Esc

Preset : The analogue output n° 7 is set to the programmed value in the VALUE parameter between 0 and 21 mA.

Note :

In case of system alarm, all the analogue outputs (1 to 7) are fixed to the preset value.

According to the programmed choice selected in the menu mA outputs / special prog / system alarm.

TEST VALUE : 00 mA

Esc

Allows to test all the loops 0.20 and 4.20.

The scroll up key allows to adjust the current value generated by each output between 0 and 21 mA.

(See paragraph Service/mA adjustment).

MAINTENANCE

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SILKOSTAT 9210

Communication menu

Choice of the measure sequence menu

Channel activation sub menu

COMMUNICATION N : 00 BAUD : 9600 PARITY : No STOP BIT : 1

SWAP WORD : No

Select

Esc

This screen allows to adjust the communication parameters like RS 485 of the SILKOSTAT. The communication protocol is MODBUS-JBUS.

Utilize the scroll up key to change the selected digit and press the « Enter » key to validate and go to the next digit.

SEQUENCE CHANNEL ACTIVATION SEQUENCE Select

Esc

The "SEQUENCE" menu allows to run or stop the different measurement channels and to set up the analysis samples order.

CHANNEL ACTIVATION

CHANNEL 1 : On CHANNEL 2 : Off CHANNEL 3 : On CHANNEL 4 : On CHANNEL 5 : Off CHANNEL 6 : On Select

Esc

The « CHANNEL ACTIVATION » allows to run or to stop the measurement channel.

Select : allows to choose the channel.

: allows to run / stop a channel

Enter : allows to validate a choice.

N° : Monec number (0 … 33).

Baud : Transmission speed in bauds (300, 600 1 200, 2 400, 4 800, 9 600).

Parity : odd, even, no.

Stop bit: 1 or 2

Swap word Allows to reverse the send order of the data.

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SILKOSTAT 9210

Sequence sub menu

SEQUENCE

SEQUENCE : 123562141131 Delete

Esc

The "SEQUENCE" menu displays the configured sequence and allows to change it.

The sequence is set up on 12 steps.

Utilize the scroll up key to change the number of the channel as the channel number as possible.

The "Delete" key replaces the digit by the symbol "*". This symbol indicates the inhibition of the step in the sequence.

Press "Enter" to validate and go to the next digit.

Sequences examples:

1) 1 2 3 4 5 6 * * * * * *

4 5 6 3 2 1 * * * * * *

These two sequences allow to analyse samples (1 to 6) in different order.

2) 12 12 12 12 12 12

or 12 ** ** ** ** **

or 1* 2* ** ** ** **

These 3 sequences are the very same and allow to analyse alternately the samples 1 and 2.

Page 63

SILKOSTAT 9210

Service menu

Time sub menu

Display sub menu

SERVICE TIME DISPLAY CODE SOFT ISSUES DAFAULT VALUES mA ADJUST FACTORY Select

Esc

This screen gives access to the parameters of the 9210 SILKOSTAT hardware.

TIME DAY : Monday DATE (JJ MM AA) : 09/05/01 TIME: 14:43:16 Select

Esc

This screen allows to change the date and the time of the instrument.

DISPLAY LANGUAGE : F CONCENTRATION : ppb/ppm CUSTOMIZE Select

Esc

This screen allows to change the programming language, the concentration unit and to customize the samples displays (you can name the samples).

Languages : choice of the message language

• French : F

• English : GB

• German : D

• Spanish : Sp

• Italian : I

The unit choice is ppb / ppm or µg / mg/l

Page 64

SILKOSTAT 9210

Customize

CUSTOMIZE Ch 1 : anion1 Ch 2 : anion2 Ch 3 : mixed bed Ch 4 : ball Ch 5 : condens Ch 6 : vapour Select

Esc

Allows to choose the letter

"Enter" allows to validate this letter and go to the next character.

Note

Customizing a sample name is possible with the lower-case letter “a...z”, with the upper-case letters “A...Z”, numbers “0...9” and punctuation signs.

Service / Code sub menu

Soft issues sub menu

CODE PROGRAMMATION : 0000 CALIBRATION : 0000 SERVICE : 0000 Select

Esc

Use this screen to enter the analyser's calibration or service menu programming access codes. These codes are independent of one another.

Enter 0000 if there is no access code.

SOFT ISSUES SILKOSTAT XX I/O Module XX Module Colo. XX

Esc

This screen displays the different software issues installed on the different electronic boards of the 9210 SILKOSTAT.

Page 65

SILKOSTAT 9210

Default / values sub menu

Adjust mA sub menu

DEFAULT VALUES Loading

Default values ? YES

Esc

This screen allows to load default values. (See appendix C). Note :

This operation will erase all the parameters (calibration, 4…20 mA scale, alarms, sequence,…), and the default values will be loaded and will erase the measurement values and the historic alarms.

ADJUST mA OUTPUT 1 OUTPUT 2 OUTPUT 3 OUTPUT 4 OUTPUT 5 OUTPUT 6 OUTPUT 7 OUTPUT 8 Select

Esc

Select the output with the "Select " key and validate by the "Enter" key to display the next screen.

Each 4…20 mA output can be individually calibrated on 2 points.

Connect a mill ammeter to the 1 to 8 outputs.

ADJUST mA 4 mA VALUE : 0000 - +

Esc

OR

Utilize the "-" and "+" key to adjust the current value to 4 and 20 mA, validate (press “Enter” ) and press “Esc” to come back to the previous screen.

ADJUST mA 20 mA VALUE : 0000 - +

Esc

Page 66

SILKOSTAT 9210

Factory sub menu

Solenoid valves

FACTORY CODE : 0000

Esc

FACTORY CHANNEL NUMBER : X SOLENOID VALVES PUMPS MEASURE CONFIGURATION

Esc

This menu enables to adjust the channel number between 1 and 6, the operating and waiting time of the sample valves, pumps and measurement parameters.

SOLENOID VALVES Ton SAMPLE : XXX Toff SAMPLE : XXXs SOL. CAL. Ton : XXX SOL. CAL. : Toff : XXXs

Esc

Adjustment of the opening time of the sample solenoid valves and calibration solution pump (Ton) and waiting after action (Toff).

Note : Personal constructor menu. An access code is required to enter . Switch off the instrument to have access.

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SILKOSTAT 9210

Pumps

Measure

Configuration sub menu

PUMPS PUMP 1 Ton : XXX PUMP 1 Toff : XXXs PUMP 2 Ton : XXX PUMP 2 Toff : XXXs PUMP 3 Ton : XXX PUMP 3 Toff : XXXs

Esc

Ton : number of impulses.

Toff : waiting time.

MEASURE RANGE : XXX LINEAR COEFF. : XXX WAITING TIME : XXXs MEASURE TIME : XXXs ZERO CONC : XXX NEGATIVE VAL. : XXX FILTER : XXX HEATER : XXX

Esc

CONFIGURATION MAINS FREG : 50 Hz REFERENCE FREQ : 0020 BLACK FREQ : 0020 Select

Esc

This screen allows to change the frequencies

MAINS FREG.: 50 Hz or 60 Hz (it depends on the country frequency).

REFERENCE FREQ : Current frequency adjustment of the LED-level reading.

BLACK FREQ : Current frequency measurement of the black-level reading.

RANGE Select the measuring range between 0-1000 ppb or 0-5000 ppb

LINEAR COEFF. Correctness coefficient of the non-linearity (the sub-menu is displayed only if the range 0-5000 ppb is chosen).

WAITING TIME Waiting time before measure

MEASURE TIME Measure time

ZERO CONC reserved

FILTER reserved

NEGATIVE VAL. Choice to display the negative values

HEATER Heating on/heating off

Page 69

SILKOSTAT 9210

6. Maintenance and exploitation A periodical maintenance will allow to have a good running and an exact analysis. Verify the level of the calibration solution and the reagents and refill if it is necessary.

Reagent refills The analyser monitors the reagents and calibration solution consumption. Messages are displayed when the canister levels are low.

Messages Signification Relays on

Reagent < 250ml Low reagent level (range < 10 days)

Warning (Re 11)

Cal. Sol < 300ml Calibration low level (range < 2 calibration)

Warning (Re 11)

Short reagent Reagent canister volume < 150ml

System (Re 12)

Short cal. Calibration solution canister volume < 150ml

It is necessary to program the new canister volume at each refill for a good detection of the short reagent.

• Stop the instrument "STOP".

• Refill the reagent canisters.

• Press the "MENU" key.

• Choose the "MAINTENANCE" menu.

• Choose the "REAGENTS REFILL" menu.

• Choose CANISTERS FULL to program all the canisters

volumes to 2 litres.

REAGENTS REFILL ADJUST VOLUMES TUBES PRIMING CANISTERS FULL yes/no Select

Esc

ADJUST VOLUMES : the 4 canisters volumes are displayed and can be modified.

TUBES PRIMING : start the priming / renewal procedure of the reagents in the tubes. "Esc" allows to return to the previous screen or to stop the procedure.

CANISTERS FULL: choose this option each time than canisters are full. The volumes of the 4 canisters are automatically programmed with 2 litres.

Page 70

SILKOSTAT 9210

Note :

It is recommended to calibrate zero after each reagent refill.

ADJUST VOLUMES REAGENT 1 VOL : 2.00 λ REAGENT 2 VOL : 2.00 λ REAGENT 3 VOL : 2.00 λ SOL CAL VOL : 2.00 λ Select

• Or ADJUST VOLUMES to visualize or program another value than 2 litres.

This menu allows to visualize the volumes of the reagent canisters and the calibration solution. You eventually can adjust these volumes. The «FULL CANISTERS » menu put these volumes at 2 litres.

The analyser controls the calibration solution and reagent consumption and emits system alarm as the level of the canisters is going too low.

Warning Alarm system

Reagents < 250 ml < 150 ml Esc

Calibration solution

< 300 ml

REAGENTS REFILL Please wait…

Esc

• Choose REAGENTS REFILL to start the reagents refill procedure.

The tubes priming is going on ; the reagents pumps and the calibration solution are running at the same time than the mixing motor and the drain.

REAGENTS REFILL ESC = quit

Esc

At the end of the tubes priming you can quit the procedure by pressing "ESC".

Page 71

SILKOSTAT 9210

Prolonged stopping In case of an extended stop longer than 1 week, it is recommended to clean the tubes and the measuring cell.

Provide 250 ml of demineralised water.

Submerge the 3 tubes in the beaker and start the rinsing operation:

• Stop the instrument by pressing "STOP".

• Press the "MENU" key.

EXTENDED STOP Put tubes in

demineralised water

Accept with OK OK

Esc

• Choose the "MAINTENANCE" menu.

• Choose the sub menu "EXTENDED STOP".

The measuring cell is empty.

Disconnect the instrument.

Replace the reagents tubes in their canisters.

In case of an extended stop over 6 weeks, you must throw the reagents and prepare another set for the restart.

Note : Don’t reverse the tubes.

Page 72

SILKOSTAT 9210

Restarting after a prolonged stopping • Connect the analyser to the main.

• Start the instrument by pressing "START".

• Press the "MENU" key.

• Choose the "MAINTENANCE" menu.

• Choose the sub menu "START UP".

MAINTENANCE / START UP

START UP Adjust flow Sample 1 (to 6) OK

Esc

This screen allows to adjust the samples flow.

Set the flow-rate for the first sample using the adjusting screws on the front panel (see Figure 3.3, serial 4) in such a way that a constant overflow takes place over the top of the overflow vessel.

START UP PIPE START Verify immersion OK

Esc

This screen enables to prime the pumps.

After the pump operation, check visually the tubings are full. If it is not the case, return to the menu “pump ".

Warning : Do not unscrew completely the flow rate set screw. It has no stop and may get out of its housing and provoke a sample leak.

Page 73

SILKOSTAT 9210

Tube cleaning

Cleaning procedure of the reagent tubings in case of deposit. Use a beaker with 250 ml of demineralised water and a beaker with 100 ml of 10% ammoniac, about 3%. Immerse the tubing R1 in an ammoniac solution. Press « OK » to launch the cleaning and « esc » to stop the procedure and to come back to the preceding menu. Follow the instructions and press « OK » at each step

The procedure is the following :

• Rinse the tube with demineralised water.

• Clean with a 10% ammonia solution.

• Rinse again the tube with demineralised water.

During these stages :

In special cases you must clean the reagents tubes. Follow the procedure to clean the tubes with demineralised water and a 10% ammonia solution (NH4-OH) and rinse with demineralised water. During the cleaning the sample runs into the cell with the mixer running.

TUBES CLEANING Put pumps tubes In demineralised water Accept with OK.. OK

Esc

TUBES CLEANING Put pumps tubes

in demineralised water Accept with OK OK

Esc

Page 75

SILKOSTAT 9210

7. Troubleshooting

Possible sources of the problem The list gives you an idea to inspect different parts of the 9210 SILKOSTAT when it doesn’t normally run.

Problem

Possible cause

Problem

N°

The system doesn’t run

Start / Stop Datalyt

1

The measure is not stable, too high or too low.

Cal Tubes Photometer Valves Pump

5 3 8 4 2

Wrong calibration

Pump Tubes Valves Cal solution Calibration program Reagents Photometer

2 3 4 6 7 7 8

The photometer doesn’t run or doesn’t correctly measure.

Photometer

8

Page 76

SILKOSTAT 9210 - MANUEL D'UTILISATION

Possible solutions Problem

Symptom

Solution

Analyser stopped

• System alarm : Rectify the problem according to the

displayed message (see System Alarm Messages). • Start up the analyser (START key).

1. START / STOP

Mains power cut off

• Connect the analyser to the mains power. • Verify the fuse.

Doesn’t run

• Test the pump : in the MAINTENANCE / PUMP menu

start pumps one after one and verify than their flow is about 1,5ml / mn (30 pulses).

• Change the pump.

2. PUMP

Irregular

• The analyser may have been stopped without tubes

cleaning. Send water in the pump during its work. • Change the pump.

Defective tube

Change the tube

3. TUBES

Clogged tube

Change the tube

Solenoid valves leak

Remove, test and clean.

The solenoid valves can’t open

Sticked collar, must be clean

4. SOLENOID VALVES

The solenoid valves can’t close

Locked spring ; necessary cleaning

Dirty

Disconnect the samples from the sample block.

5. CAL.

Diminution of the flow

Verify and adjust the flow (10 l/h), change the sample tube if it is clogged.

Page 77

SILKOSTAT 9210

Problem

Symptom

Solution

6. CALIBRATION

Wrong configuration of the calibration solution concentration

Reprogram the calibration solution concentration (SiO2)

Wrong concentration of the standard solution

Prepare a new standard solution.

Wrong laboratory analysis of the calibration solution concentration

Verify the SiO2 concentration of the laboratory calibration solution.

Wrong chemicals products or olds or contaminated

Wrong purity ? New supplier ? Clean the reagents bottles.

Reagents canisters connected in a wrong order.

Verify the flow of the circuit "MAINTENANCE/PUMPS-OTHERS" menu.

Reagents tubes connected in a wrong order.

Verify the flow diagram

Wrong concentration

Prepare a new reagents batch

Wrong chemical products or old or contaminated

Wrong purity ? New supplier ?

7. REAGENTS

Wrong reagents proportional

Verify the good running order of the pumps.

Bacterial developpement in reagent R3 (greenish deposit)

Add 40 ml of sodium benzoate at 1 g/l

White deposit in the reagent tubing R1 Immerse the tubing in an ammoniac solution according to the procedure described in the menu MAINTENANCE/TUBING CLEANING

8. PHOTOMETER

Wrong or irregular measure

• Verify the photometer "MAINTENANCE /

PHOTOMETER TEST " . In this menu measurement values of reference and measurement during the last calibration of the measurement cycle appears. The typical values of these values are in the following table.

• Is there an error message ?

Page 78

SILKOSTAT 9210 - MANUEL D'UTILISATION

Typical measurement values during calibration These values are given as an indication and are dependant on the ambient temperature. The real values may deviate from more than one volt without having an effect on the measurements.

Version 0…1000 ppb Sample concentration Reference (mV) Measure (mV)

107 ppb 3500 2515 214,9 ppb 3500 1754 267,4 ppb 3500 1472 534,8 ppb 3500 603

Version 0…5000 ppb Sample concentration Reference (mV) Measure (mV)

1000 ppb 3500 1400 3000 ppb 3500 300

Page A1

SILKOSTAT 9210

Appendix A : Spare parts of the 9210 SILKOSTAT

DESCRIPTION Part Number

Accessories / Options :

0,5 – 6 bar adaptation kit for six sample selection solenoid valves

09210=A=0100

9210 Instruction manual in English 621=192=010

9210 Instruction manual in French 621=092=010

9210 Instruction manual in German 621=292=010

9210 Instruction manual in Italian 621=492=010

9210 Instruction manual in Spanish 621=592=010

Spare parts - Electronics

User’s interface / Interface board 09200=A=5000

CPU board with display for Monec E9200, non programmed 09200=A=1001

CPU board with display for Monec E9200, programmed for SILKOSTAT

09200=A=1010

CPU board with display for Monec E9200, programmed for PHOSPHAMAT

09200=A=1011

Power supply board for Monec E9200 09200=A=2000

RS485 board (MODBUS) + Manual 09125=A=0485

92XX Internal bus communication module 09200=A=5500

2 wires interconnection cable (per m) 370=302=034

4 wires interconnection cable (per m) 370=304=034

7 wires interconnection cable (per m) 370=307=034

Analogue board 92XX 820 nm 09210=A=1500

Analogue board 92XX 525 nm 09210=A=1510

Analogue board 92XX 540 nm 09210=A=1520

Spare parts – Sampling

4x6 mm PE tubing (per m) 151575,00006

Sampling solenoid valve, NPS 1.6 (0.2-2 bars) 689=118=016

Sampling solenoid valve, NPS 0.8 (0.5-6 bars) 689=118=008

O-ring, 4 x 1 356099,05040

Sampling flow-rate adjustment screw 09210=A=0105

Sample level sensor for 921 X 09210=A=0250

SILKOSTAT 9210

Page A2

DESCRIPTION Part Number

Viton O-ring 38 x 2 mm 356099,35380

Sampling solenoid valves (overflow vessel) 689=118=024

Spare parts – Photometric cell

Connection board for 921 X mixer/heater 09210=A=1234

Complete mixer for 921X analysers 09210=A=0400

Teflon coated magnetic stirrer 226=003=013

Heating element 09097=C=0560

Pt100 temperature sensor 359000,40780

Fibre optics for 9210 Silkostat 921X 09210=A=0500

Mirror for 9210 Silkostat 921X 09210=C=0340

PG21 tap PA black 425=210=022

Spacer ring for 921X mirror 09210=C=0330

O-ring Viton 22x1 mm 356099,05220

Square cover for 921 X photometric cell 09210=C=0310

Spare parts – Reagents and calibration

Chemical kit for silkostat 9210 09210=C=7000

PE tubing Ø 1.6x3.2 mm (per m) 590=050=060

PTFE tubing Ø 0.8x1.6 mm (per m) 151065.08699

PE tubing Ø 4x6 mm (per m) 151575.00006

Reagent pulse pump 695=114=001

Calibration / flush pump 695=004=004

2 litres PE cap 495=020=001

Strainer 09210=A=0600

Connection for PE tube, Ø 4 x 6 589=011=040

Connection for PE tube, Ø 1.6 x 3.2 589=010=015

Caution :

The chemical products kit of the SILKOSTAT is compounded with all the reagents except the sulphuric acid for 6 weeks.

!

Page B1

SILKOSTAT 9210

Appendix B : Safety Precautions

HEALTH AND SAFETY INFORMATIONS

PRODUCT : OXALIC ACID

The health and safety information on oxalic acid is as follows :

Name :

OXALIC ACID 1. dihydrate Formula : 1. (COOH)2. 2H2O 2. anhydrous Formula : 2. (COOH)2.

CAS N°144-62-7

PHYSICAL PROPERTIES

MELTING POINT 1. 101 °C 2. 190 °C

SOLUBILITY IN WATER About 14%

FIRE AND EXPLOSION HAZARD Decomposition products include carbon monoxide (highly flammable and toxic) and carbon dioxide.

HEALTH HAZARD Classification of risk – Harmful Harmful in contact with skin Harmful if swallowed Harmful if inhaled Minimum letal dose (LD50) = 275 mg/Kg

SAFETY PRECAUTIONS

EYES Irrigate thoroughly with water ; obtain medical attention

LUNGS Remove exposure, rest and keep arm ; obtain medical attention

INGESTION Wash out thoroughly with water ; give plenty of water of drink ; obtain medical attention

CHEMICAL HAZARDS AND STABILITY STABILITY Stable

SPECIAL HAZARDS Mixtures with sodium chlorite can explode on the addition of water.

WASTE DISPOSAL Dissolve or mix the material with a combustible solvent and burn in a chemical incinerator equipped with an after burner and scrubber. Dispose in safe manner consistent with Local Authority chemical waste regulations. For guidelines on disposal consult the requirements of the Control of Pollution Act (1974) and the Control of Pollution (Special Wastes) Regulations (1980 S1 1709).

SILKOSTAT 9210

Page B2

PROTECTIVE MEASURES

RESPIRATOR Dust mask or positive pressure hood – if handling large quantities.

GLOVES Rubber or plastic

EYE PROTECTION Goggles

SPILLAGE HANDLING

SMALL SPILLAGE Mop up with plenty of water and run to waste, diluting greatly with running water.

LARGE SPILLAGE Transfer to salvage canister and treat residue as for small spillage.

The information on this sheet is believed to be correct at the time of collation. The details should be reviewed periodically and should be checked for special uses.

Page B3

SILKOSTAT 9210

HEALTH AND SAFETY INFORMATION

PRODUCT : SULPHURIC ACID (98%)

The health and safety information for sulphuric acid is as follows :

Name :

SULPHURIC ACID Formula : H2 SO4

Hazard class : 8 UN N° : 1830

CAS N° 7664-93-9

PHYSICAL PROPERTIES

MELTING POINT 10 °C

BOILING POINT 330°C

SPECIFIC GRAVITY 1,8

MISCIBLE WITH WATER

FIRE AND EXPLOSION HAZARD May evolve toxic fumes in a fire.

HEALTH HAZARD Classification of risk – Corrosive. Causes severe burns to eyes and skin. If indigested causes severe internal irritation and damage. Dilute acid irritates the eyes and skin and can cause burns and dermatitis. Minimum lethal dose, D50 = 2140 mg/Kg, par voie orale.

Occupational exposure standard, long term exposure limit (8 hours TWA) mg-3 : Keep out of reach of children.

SAFETY PRECAUTIONS-FIRST AID

EYES Irrigate immediately and thoroughly with plenty of water at least of 10 minutes. Obtain medical attention.

LUNGS Remove from exposure, rest and keep warm, or if exposure has been great, obtain medical attention.

MOUTH Wash out mouth thoroughly with water ; give plenty of water to drink ; obtain medical attention.

SKIN Drench the skin thoroughly with water and give plenty of water to drink. Obtain medical attention.

SILKOSTAT 9210

Page B4

CHEMICAL HAZARDS AND STABILITY

Reacts vigorously with evolution of heat. Never add water to this product. Will react violently with the following : • Acetonitrile. • Perchlorates. • Nitro-organic compounds. • Alkali metals. • Potassium permanganate • Metal halogenates. Avoid contact with bases.

PROTECTIVE MEASURES

Wear chemical-resistant gloves (nitrile), safety goggles or face shield and use fume cupboard. For large quantities use approved breathing apparatus, plastic apron and sleeves and wear boots. Ensure that safety shower and eye bath are available in the locality.

SPILLAGE HANDLING Wear appropriate protective clothing. Cover the spillage with soda ash. If local regulations permit, cautiously add plenty of water and mop up while diluting with more water and run to waste. Wash site of spillage thoroughly with water. Otherwise cover with dry lime, sand or soda ash and place in covered canisters. Arrange removal by disposal company. Ventilate area and wash spill site with water after material removal is complete. If material has entered drains it may be necessary to inform the Local Authorities.

WASTE DISPOSAL

Dispose in safe manner consistent with Local Authority chemical waste regulation. For guidelines on disposal consult the requirements of the Control Pollution Act (1974) and the Control of Pollution (special wastes) Regulations (1980 SI 1709).

The information on this sheet is believed to be correct at the time of collation. The details should be reviewed periodically and should be checked for special uses.

Page B5

SILKOSTAT 9210

HEALTH AND SAFETY INFORMATION

PRODUCT : SODIUM HEXAFLUOROSILICATE

The health and safety information on this product is as follows :

SODIUM HEXAFLUOROSILICATE (sodium fluorosilicate , disodium hexafluorosilicate disodique)

Formula : Na2SiF6 Hazard class : 6.1No. UN : 2674 CAS N° 16893-85-9

PHYSICAL PROPERTIES White granular powder

Density (20 °C) approx. 2,7 g cm-3

Slightly soluble in water (6g 1-1 to 20°C)

FIRE AND EXPLOSION HAZARD When heated to decomposition it may emit hydrogen fluoride.

HEALTH HAZARD Classification of risk – toxic.

Avoid contact with skin.

Avoid contact with eyes.

Keep locked up.

Keep out of reach of children.

Toxic by ingestion and skin contact

Toxic by inhalation

Irritating to skin and eyes, may cause damage if exposure is prolonged.

Occupational exposure standard, long term exposure limit (8h TWA) 2,5 mg m-3

SAFETY PRECAUTIONS – FIRST AID If the casualty feels unwell, seek medical advice and show label where possible.

EYES Rinse immediately and thoroughly with water for at least 10 minutes. Obtain medical attention.

LUNGS Remove from exposure, rest and keep warm. In severe cases, or if exposure has been great obtain medical attention.

MOUTH Wash out mouth thoroughly with water and give plenty of water to drink. Obtain medical attention.

SKIN Wash skin thoroughly with water and give plenty of water to drink. Obtain medical attention.

CHEMICAL HAZARD AND STABILITY Contact with acids liberates toxic gas.

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Page B6

PROTECTIVE MEASURES (as appropriate to quantity handled)

RESPIRATOR Dust respirator.

VENTILATION Extraction hood.

GLOVES Rubber or plastic.

EYE PROTECTION Goggles or face shield.

OTHERS MEASURES Plastic apron, sleeves, boots – if handling large quantities.

SPILLAGE HANDLING

PRECAUTIONS Wear appropriate protective clothing.

Mix with sand, transfer carefully to canister and arrange removal by disposal company. Wash site of spillage thoroughly with water and detergent.

For large spillages liquids should be contained with sand or earth and both liquids and solids transferred to salvage canisters. Any residues should be treated as for small spillages.

If material has entered surface drains it may be necessary to inform Local Authorities, including fire services flammable.

WASTE DISPOSAL Dispose in safe manner consistent with Local Authorities or national chemical Waste Regulation. For guidelines for disposal in the UK consult the requirements of the Control of Pollution (special wastes) regulations (1980 SI 1709).

The information in this sheet is believed to be correct at the time of callation. The details should be reviewed periodically and should be checked for special uses.

Page B7

SILKOSTAT 9210

HEALTH AND SAFETY INFORMATION

PRODUCT : FERROUS AMMONIUM SULPHATE HEXAHYDRATE

The table below shows the health and safety (MSDS) data for Ferrous ammonium Sulphate:

PRODUCT IDENTIFICATION

PRODUCT NAME FERROUS AMMONIUM SULPHATE HEXAHYDRATE

CAS No. (CE) 7783-85-9 233-151-8

FORMULA (NH4)2Fe(SO4)2, 6H2O

MOLECULAR WEIGHT 392,14 AMU

ALTERNATIVE NAMES Ferrous ammonium sulfate hexahydrate * Ammonium ferrous sulfate, hexahydrate * Iron ammonium sulfate hydrate * Sulphuric acid, ammonium iron (2+) salt, hexahydrate

PHYSICAL PROPERTIES

FORM Solid

COULOUR Greenish blue

ODOUR Nil

MELTING POINT 100°C

DENSITY 1.86 g/cm³

FIRE AND EXPLOSION HAZARD

Non-combustible. Likelihood of dangerous vapours being given off if close to a fire. In fire situations it may form nitrogen oxides and sulphur oxides.

HEALTH RISKS

SPECIFIC ENVIRONMENTAL AND HEALTH HAZARDS Irritant for the eyes, respiratory tract and skin.

SAFETY MEASURES

EYES – SKIN Flush copiously with water. Remove any contaminated clothing

RESPIRATORY TRACT Avoid continued exposure, breathe in fresh air; seek medical attention.

IF SWALLOWED Drink plenty of water, provoke vomiting, and seek medical advice.

CHEMICAL RISKS AND STABILITY

STABILITY Conditions to avoid - high temperatures

CONDITIONS TO AVOID Sensitive to air, sensitive to light.

PRODUCTS TO AVOID Powerful oxidising agents and acids.

SILKOSTAT 9210

Page B8

DANGEROUS DECOMPOSITION PRODUCTS

• Iron oxides.

• Ammonia.

• Sulphur oxides.

PREVENTIVE MEASURES

HANDLING Safe Handling Instructions: Do not breathe the dust. Avoid contact with the eyes, skin or clothing. Avoid prolonged or repeated exposures.

EXPOSURE LIMITS

UK:

Source - category - value OEL - LTEL - 1 mg (Fe)/m³ OEL - STEL - 2 mg (Fe)/m³

BREATHING EQUIPMENT Use dust-masks or over-pressure breathing gear if dust formation is likely.

GLOVES Essential.

Wear chemical resistant gloves (nitrile rubber, NBR).

EYE PROTECTION Protective glasses/goggles are essential.

OTHER

Wear protective clothing and work in a well-ventilated area.

Remove any contaminated clothing and wash hands thoroughly after working with the product.

DISPOSAL MEASURES

Contact a specialist waste disposal organisation where disposal of this product is required. Dissolve, or mix, the product with a combustible solvent and burn in a chemical incinerator fitted with post-combustion and scrubber systems. Observe all applicable local, national and international environmental regulations.

FIRST AID MEASURES

FOLLOWING INHALATION In the event of inhalation, seek clean air. Where breathing has stopped, apply artificial respiration. Where breathing is difficult, give oxygen.

FOLLOWING CONTACT WITH SKIN In the event of skin contact, wash the skin immediately using soap and plenty of water.

FOLLOWING CONTACT WITH THE EYE In the event of contact with the eyes, rinse out immediately with plenty of water for at least 15 minutes.

FOLLOWING INGESTION (IF SWALLOWED) If swallowed, rinse out the mouth with water if the patient is still conscious. Call medical assistance.

Page B9

SILKOSTAT 9210

FIRE FIGHTING - EXTINCTION METHODS

SUTABLE EXTINGUISHERS Water spray. Carbon dioxide, dry chemical powder or suitable foam.

SPECIAL RISKS Specific Danger(s): Gives off toxic fumes if burnt.

SPECIAL PROTECTIVE EQUIPMENT NEEDED FOR FIRE FIGHTING

Wear individual breathing apparatus and protective clothing to prevent any contact with the eyes or skin.

The information contained in this document is reviewed at regular intervals and checked for special cases.

SILKOSTAT 9210

Page B10

HEALTH AND SAFETY INFORMATION

PRODUCT : SODIUM MOLYBDATE DIHYDRATE

The health and safety information for Sodium Molybdate Dihydrate is as follows :

Name :

SODIUM MOLYBDATE DIHYDRATE Formula: Na2MoO4.2H2O

CAS N° 10102-40-6

PHYSICAL PROPERTIES

MELTING POINT 687°C

SOLUBILITY IN WATER 840 g/L

FIRE AND EXPLOSION RISK No information available

HEALTH RISKS Not hazardous according to Directive 67/548/EEC

SECURITY MEASURES

EYES Rinse immediately with plenty of water, keeping the eyelids open as much as possible

LUNGS In case of inhalation, remove from exposure and move to fresh air immediately.

INGESTION Drink plenty of water. If feeling unwell seek medical aid

CHEMICAL DANGER AND STABILITY

STABILITY Stable

SPECIFIC RISKS No information available

DISPOSAL Observe all federal, state, and local environmental regulations for disposal of chemical products

PERSONAL PROTECTION

RESPIRITORY Wear appropriate breathing apparatus due to the formation of dust

GLOVES Not necessary

EYES Wear appropriate safety goggles

MEASURES TO TAKE IN CASE OF ACCIDENTAL SPILLAGE

PERSONAL Avoid inhalation of any dust

ENVIRONMENT Do not dispose of in any standard waste disposal systems such as sinks or sewers

CLEANING Vacuum or sweep up material and place into a suitable disposal container. Avoid generating dusty conditions.

The information listed above must be reviewed periodically and should not be considered a substitute for the MSDS for this product.

Page B11

SILKOSTAT 9210

HEALTH AND SAFETY INFORMATION

PRODUCT : 9210 R1 REAGENT

PRODUCT AND COMPANY IDENTIFICATION

SUBSTANCE Product code : R1

Name of product : 9210 R1 Reagent

SUPPLIER Manufacturer Name : HACH SAS Address : 29 rue de Bures 14670 Troarm Phone : (33) 02.31.15.37.10 Fax N° : (33) 02.31.15.37.30 Emergency : (33) 02.31.15.37.35 (Unit of production) : (33) 01.45.42.59.59 (N° ORFILA)

COMPOSITION / INFORMATION ABOUT THE COMPONENTS

CHEMICAL PROPERTIES Preparation

HAZARDOUS COMPONENTS

CAS NUMBER SOLUTION QUANTITY CLASSIFICATION 213-653-7 10102-40-6 7664-93-9

Water Sodium molybdate Sulphuric acid

90 % 5 % 5 %

C ; R35 ; S26 -30 - 45

IDENTIFICATION OF HAZARDS

Product not considered as dangerous according to the 67/548/CEE directive

FIRST AID

SKIN CONTACT Rinse affected area with plenty of water. Remove contaminated clothing. Swab with polyethylene glycol 400

EYE CONTACT Immediately flush eyes with plenty of water with eyelids open for 10 minutes. Get medical aid if necessary

IF SWALLOWED IN LARGE QUANTITIES Give plenty of water to drink. In case of indisposition, take medical advice. Do not try to neutralize

FIRE FIGHTING MEASURES

EXTINGUISHING MEANS Adapt the extinguishing agent to the products stored in the immediate vicinity

SPECIFIC HAZARDS Non combustible. Risk of forming hydrogen if in contact with light metals

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Page B12

MEASURES IN CASE OF SPILLAGE

PRECAUTIONS FOR PEOPLE Avoid contact with skin and eyes

ENVIRONMENT PROTECTION Do not pour in sewers or rivers

CLEANING Collect in specific containers. Clean soiled materials

HANDLING AND STORAGE

PRECAUTIONS TO TAKE Avoid contact with metals

USEAGE ADVICE Respect conditions of use

STORAGE RECOMMENDATIONS Store in hermetically sealed containers

EXPOSURE CONTROLS / INDIVIDUAL PROTECTION

RESPIRATORY PROTECTION Required if steam / aerosol

HAND PROTECTION Wear latex gloves

EYE PROTECTION Safety glasses are recommended

OTHER PROTECTION Acid-proof clothing

HYGIENE MEASURES Wash hands after contact

PHYSICAL AND CHEMICAL PROPERTIES

FORM Liquid

COLOR Light yellow

ODOR Odorless

pH < 1

STABILITY AND REACTIVITY

CONDITIONS TO BE AVOIDED Heating

SUBSTANCES TO BE AVOIDED Metals, base, acid

DANGEROUS BY-PRODUCTS In case of fire, see FIRE FIGHTING MEASURES – SPECIFIC HAZARDS above

TOXICOLOGICAL INFORMATION

ACUTE TOXICITY CL50 (oral, rat) : 3250 mg/Kg

IN THE EVENT OF SKIN CONTACT Causes burns

IN THE EVENT OF EYE CONTACT Causes burns

IF SWALLOWED IN LARGE QUANTITIES Strong pains with nausea, vomiting and diarrhea

Page B13

SILKOSTAT 9210

ECOLOGICAL INFORMATION

ECOTOXIC No specific indications

OTHER ECOLOGY-RELATED INFORMATION In the event of proper handling and use, there is no risk of ecological problems.

Injurious on aquatic life, by pH modification

DISPOSAL CONSIDERATIONS

PRODUCT There are as yet no uniform regulations concerning the disposal of chemicals and their residues within the European Union.

The chemicals and their residues must be considered as special waste; their disposal is regulated by each EEC member state.

We advise you to contact the competent authorities (administration or specialist waste disposal companies) that will inform you of the disposal measures to take

PACKAGING Disposal in accordance with prevailing legislation. Contaminated containers must be processed in the same manner as the chemical itself.

Unless specifically regulated, non-contaminated containers may be disposed of as household waste, or be recycled

TRANSPORT INFORMATION

Not subject to transport provisions

REGULAR INFORMATION

LABELLING TO EEC DIRECTIVES N° CE : 231-211-8

HAZARDOUS PRODUCT IDENTIFICATION

C Corrosive

« R » Sentences 35 Causes burns

« S » Sentences 26 - 30 - 36/37/39-45 If in contact with the eyes, flush eyes immediately with plenty of water.

Wear protective clothes, gloves, goggles and a face protection device. In case of accident or feeling faint, contact a doctor

OTHER INFORMATION

Updated version : November 2005 Issue A

SILKOSTAT 9210

Page B14

HEALTH AND SAFETY INFORMATION

PRODUCT : 9210 R2 REAGENT

PRODUCT AND COMPANY IDENTIFICATION

SUBSTANCE Product code : R2

Name of product : 9210 R2 Reagent

SUPPLIER Manufacturer Name : HACH SAS Address : 29 rue de Bures 14670 Troarm Phone : (33) 02.31.15.37.10 Fax N° : (33) 02.31.15.37.30 Emergency : (33) 02.31.15.37.35 (Unit of production) : (33) 01.45.42.59.59 (N° ORFILA)

COMPOSITION / INFORMATION ABOUT THE COMPONENTS

CHEMICAL PROPERTIES Preparation

HAZARDOUS COMPONENTS

CAS NUMBER SOLUTION QUANTITY CLASSIFICATION 213-653-7 6153-56-6

Water Oxalic acid

95 % 5 %

Xn ; R21/22

IDENTIFICATION OF HAZARDS

Injurious on contact with skin or by ingestion

FIRST AID

SKIN CONTACT Rinse affected area with plenty of water. Remove contaminated clothing.

EYE CONTACT Immediately flush eyes with plenty of water with eyelids open

IF SWALLOWED IN LARGE QUANTITIES Give plenty of water to drink. In case of vomitting, take medical advice.

FIRE FIGHTING MEASURES

EXTINGUISHING MEANS Adapt the extinguishing agent to the products stored in the immediate vicinity

SPECIFIC HAZARDS Non combustible. Risk of forming hydrogen if in contact with light metals

Page B15

SILKOSTAT 9210

MEASURES IN CASE OF SPILLAGE

PRECAUTIONS FOR PEOPLE Avoid contact with skin and eyes

ENVIRONMENT PROTECTION Do not pour in sewers or rivers

CLEANING Collect in specific containers. Clean soiled materials

HANDLING AND STORAGE

STORAGE RECOMMENDATIONS Store in hermetically sealed containers

EXPOSURE CONTROLS / INDIVIDUAL PROTECTION

RESPIRATORY PROTECTION Required if steam / aerosol

HAND PROTECTION Wear nitrile gloves

EYE PROTECTION Safety glasses are required

HYGIENE MEASURES Wash hands after contact

PHYSICAL AND CHEMICAL PROPERTIES

FORM Liquid

COLOR Colorless

ODOR Odorless

pH < 1

STABILITY AND REACTIVITY

CONDITIONS TO BE AVOIDED Strong heating

SUBSTANCES TO BE AVOIDED Bases

DANGEROUS BY-PRODUCTS No available information

TOXICOLOGICAL INFORMATION

ACUTE TOXICITY DL50 (oral, rat) : 7500 mg/Kg

IN THE EVENT OF SKIN CONTACT Slight irritation

IN THE EVENT OF EYE CONTACT Slight irritation

IF SWALLOWED IN LARGE QUANTITIES Injurious

SILKOSTAT 9210

Page B16

ECOLOGICAL INFORMATION

ECOTOXIC Biologic : Fish CL50 : 325 mg/l (anhydrous liquid)

OTHER ECOLOGY-RELATED INFORMATION Damage :

DCO : 0.18 g/g (compared to the pure substance)

DThO : 0.18 g/g (compared to the pure substance)

DBO : 0.16 g/g (compared to the pure substance)

Do not pour in sewer or in the rivers.

DISPOSAL CONSIDERATIONS

PRODUCT There are as yet no uniform regulations concerning the disposal of chemicals and their residues within the European Union.

The chemicals and their residues must be considered as special waste; their disposal is regulated by each EEC member state.

We advise you to contact the competent authorities (administration or specialist waste disposal companies) that will inform you of the disposal measures to take

PACKAGING Disposal in accordance with prevailing legislation. Contaminated containers must be processed in the same manner as the chemical itself.

Unless specifically regulated, non-contaminated containers may be disposed of as household waste, or be recycled

TRANSPORT INFORMATION

Not subject to transport provisions

REGULAR INFORMATION

LABELLING TO EEC DIRECTIVES

HAZARDOUS PRODUCT IDENTIFICATION

Xn Injurious

« R » Sentences 21/22 Injurious in contact with skin or if ingested

« S » Sentences 36/37 Wear protective clothes and appropriate gloves

OTHER INFORMATION

Updated version : November 2005 Issue A

Page B17

SILKOSTAT 9210

HEALTH AND SAFETY INFORMATION

PRODUCT : 9210 R3 REAGENT

PRODUCT AND COMPANY IDENTIFICATION

SUBSTANCE Product code : R3

Name of product : 9210 R3 Reagent

SUPPLIER Manufacturer Name : HACH SAS Address : 29 rue de Bures 14670 Troarm Phone : (33) 02.31.15.37.10 Fax N° : (33) 02.31.15.37.30 Emergency : (33) 02.31.15.37.35 (Unit of production) : (33) 01.45.42.59.59 (N° ORFILA)

COMPOSITION / INFORMATION ABOUT THE COMPONENTS

CHEMICAL PROPERTIES Preparation

HAZARDOUS COMPONENTS

CAS NUMBER SOLUTION QUANTITY CLASSIFICATION 213-653-7 7783-85-9 7664-93-9

Water Ammonium iron (III) sulphatesSulphuric acid

96 % 2 % 2 %

C ; R35 ; S26 -30 - 45

IDENTIFICATION OF HAZARDS

Product not considered as dangerous according to the 67/548/CEE directive

FIRST AID

SKIN CONTACT Rinse affected area with plenty of water. Remove contaminated clothing. Swab with polyethylene glycol 400

EYE CONTACT Immediately flush eyes with plenty of water with eyelids open for 10 minutes. Get medical aid if necessary

IF SWALLOWED IN LARGE QUANTITIES Give plenty of water to drink. In case of indisposition, take medical advice. Do not try to neutralize

FIRE FIGHTING MEASURES

EXTINGUISHING MEANS Adapt the extinguishing agent to the products stored in the immediate vicinity

SPECIFIC HAZARDS Non combustible. Risk of forming hydrogen if in contact with light metals

SILKOSTAT 9210

Page B18

MEASURES IN CASE OF SPILLAGE

PRECAUTIONS FOR PEOPLE Avoid contact with skin and eyes

ENVIRONMENT PROTECTION Do not pour in sewers or rivers

CLEANING Collect in specific containers. Clean soiled materials

HANDLING AND STORAGE

PRECAUTIONS TO TAKE Avoid contact with metals

USEAGE ADVICE Respect conditions of use

STORAGE RECOMMENDATIONS Store in hermetically sealed containers

EXPOSURE CONTROLS / INDIVIDUAL PROTECTION

RESPIRATORY PROTECTION Required if steam / aerosol

HAND PROTECTION Wear nitrile gloves

EYE PROTECTION Safety glasses are required

OTHER PROTECTION Acid-proof clothing

HYGIENE MEASURES Wash hands after contact

PHYSICAL AND CHEMICAL PROPERTIES

FORM Liquid

COLOR Colorless

ODOR Odorless

pH < 1

STABILITY AND REACTIVITY

CONDITIONS TO BE AVOIDED Strong heating

SUBSTANCES TO BE AVOIDED Metals, base, acid

DANGEROUS BY-PRODUCTS In case of fire, see FIRE FIGHTING MEASURES – SPECIFIC HAZARDS above

TOXICOLOGICAL INFORMATION

ACUTE TOXICITY DL50 (oral, rat) : 7500 mg/Kg

IN THE EVENT OF SKIN CONTACT Causes burns

IN THE EVENT OF EYE CONTACT Causes burns

IF SWALLOWED IN LARGE QUANTITIES Strong pains with nausea, vomiting and diarrhea

Page B19

SILKOSTAT 9210

ECOLOGICAL INFORMATION

ECOTOXIC No specific indications

OTHER ECOLOGY-RELATED INFORMATION In the event of proper handling and use, there is no risk of ecological problems.

Injurious on aquatic life, by pH modification

DISPOSAL CONSIDERATIONS

PRODUCT There are as yet no uniform regulations concerning the disposal of chemicals and their residues within the European Union.

The chemicals and their residues must be considered as special waste; their disposal is regulated by each EEC member state.

We advise you to contact the competent authorities (administration or specialist waste disposal companies) that will inform you of the disposal measures to take

PACKAGING Disposal in accordance with prevailing legislation. Contaminated containers must be processed in the same manner as the chemical itself.

Unless specifically regulated, non-contaminated containers may be disposed of as household waste, or be recycled

TRANSPORT INFORMATION

Not subject to transport provisions

REGULAR INFORMATION

LABELLING TO EEC DIRECTIVES N° CE : 23-211-8

HAZARDOUS PRODUCT IDENTIFICATION

C Corrosive

« R » Sentences 35 Causes burns

« S » Sentences 26 - 30 - 36/37/39-45 If in contact with the eyes, flush eyes immediately with plenty of water.

Wear protective clothes, gloves, goggles and a face protection device. In case of accident or feeling faint, contact a doctor

OTHER INFORMATION

Updated version : November 2005 Issue A

SILKOSTAT 9210

Page B20

LITHIUM BATTERY SAFETY PRECAUTIONS

The lithium battery on the Datalyt Microprocessor p.c.b does not constitute a serious hazard providing the following instructions are observed :

NEVER : Attempt to recharge the battery.

Crush, puncture, open or dismantle the battery.

Store or operate equipment above the temperature specified.

Short-circuit the battery.

Dispose of the battery in a fire.

Try to repair faults on the control p.c.b.

In the event of a p.c.b fault or battery leakage :

ALWAYS : Wear suitable protective clothing.

Remove the equipment to a well ventilated area.

Contact your local agent.

Refer to Health and Safety Notes on Lithium batteries.

Page C1

SILKOSTAT 9210

Appendix C : Table of user’s configuration User’s configuration

Order Function Default/Values Possible values Selected values Date

CALIBRATION / PROGRAMMING offset interval Frequency 24 h 1…6

cal. sol Concentration 214 ppb Xxxxx auto. cal Auto calibrate No yes/no

base Day Day/hour week Mtwtfs Calendar Mtwtfs hour 00:00:00 Hours

MAINTENANCE/REAGENTS REFILL Reagents vol. 1 Used reagent volume 2,00 l Xx Reagents vol. 2 Used reagent volume 2,00 l Xx Reagents vol. 3 Used reagent volume 2,00 l Xx Reagents vol. 4 Used reagent volume 2,00 l Xx

MEASURE/MEASURE MODE Cycle Interval interval/in loops

Interval 15 mn xx hour/minute ALARMS / ALARM 1

Mode Limit limit/active channel/level sample. Affect Channel 1 Conc Limit 1000 ppb Xxx

Direction Low low/high Hysteresis 0% Xx

Relay N.O. N.O./N.C. ALARMS / ALARM 2

Mode Limit limit/active channel/level sample. Affect Channel 2 Conc Limit 1000 ppb Xxx

Direction Low low/high Hysteresis 0% Xx

Relay N.O. N.O./N.C. ALARMS / ALARM 3

Mode Limit limit/active channel/level sample. Affect Channel 3 Conc Limit 1000 ppb Xxx

Direction Low low/high Hysteresis 0% Xx

Relay N.O. N.O./N.C. ALARMS / ALARM 4

Mode Limit limit/active channel/level sample. Affect Channel 4 Conc Limit 1000 ppb Xxx

Direction Low low/high Hysteresis 0% Xx

Relay N.O. N.O./N.C.

SILKOSTAT 9210

Page C2

User’s configuration

Order Selected values Selected values Possible values Selected values Date

ALARMS / ALARM 5 Mode Limit limit/active channel/level sample. Affect Channel 5 Conc Limit 1000 ppb Xxx

Direction Low low/high Hysteresis 0% Xx

Relay N.O. N.O./N.C. ALARMS / ALARM 6

Mode Limit limit/active channel/level sample. Affect Channel 6 Conc Limit 1000 ppb Xxx

Direction Low low/high Hysteresis 0% Xx

Relay N.O. N.O./N.C. ALARMS / WARNING ALARM

Alarm Yes yes/no Accept Manual Manual/automatic Relay N.O. N.O./N.C.

ALARMS / SYSTEM ALARM Alarm Yes Oui/non Accept Manuel Manual/automatic Relay N.C. N.O./N.C.

mA OUTPUTS/ AFFECT / OUTPUT 1 Affect Channel 1 Channel 1…Channel 6 Type 0-20 mA 0/20 mA ou 4/20 mA Mode Linear Linear / dual Low 0 ppb XXX

Middle 100 ppb XXX Up 1 ppm XXX

mA OUTPUTS/ AFFECT / OUTPUT 2 Affect Channel 2 Channel 1…Channel 6 Type 0-20 mA 0/20 mA ou 4/20 mA Mode linear Linear / dual Low 0 ppb XXX

Middle 100 ppb XXX Up 1 ppm XXX

mA OUTPUTS/ AFFECT / OUTPUT 3 Affect Channel 3 Channel 1…Channel 6 Type 0-20 mA 0/20 mA ou 4/20 mA Mode Linear Linear / dual Low 0 ppb XXX

Middle 100 ppb XXX Up 1 ppm XXX

Page C3

SILKOSTAT 9210

User’s configuration

Order Selected values Selected values Possible values Selected values Date

mA OUTPUTS/ AFFECT / OUTPUT 4 Affect Channel 4 Channel 1…Channel 6 Type 0-20 mA 0/20 mA ou 4/20 mA Mode Linear Linear / dual Low 0 ppb XXX

Middle 100 ppb XXX Up 1 ppm XXX

mA OUTPUTS/ AFFECT / OUTPUT 5 Affect Channel 5 Channel 1…Channel 6 Type 0-20 mA 0/20 mA ou 4/20 mA Mode Linear Linear / dual Low 0 ppb XXX

Middle 100 ppb XXX Up 1 ppm XXX

mA OUTPUTS/ AFFECT / OUTPUT 6 Affect Channel 6 Channel 1…Channel 6 Type 0-20 mA 0/20 mA ou 4/20 mA Mode Linear Linear / dual Low 0 ppb XXX

Middle 100 ppb XXX Up 1 ppm XXX

mA OUTPUTS / SPECIAL PROG / MAINTENANCE Mode Last Last/preset/live Value if preset mode selected : 0 mA Xx

mA OUTPUTS / SPECIAL PROG / CALIBRATION Mode Last Last/preset/live Value if preset mode selected: 0 mA XX

mA OUTPUTS / SPECIAL PROG / GRAB SAMPLE mode Last Last/preset/live Value if preset mode selected: 0 mA XX

mA OUTPUTS / SPECIAL PROG / SYSTEM ALARME mode Last Last/preset/live Value if preset mode selected: 0 mA XX

mA OUTPUTS / SPECIAL PROG / WARNING ALARME mode Last Last/preset/live Value if preset mode selected: 0 mA Xx

COMMUNICATION N n° of Monec 0 0 à 33

Baud Speed communication 9600 300,600,1200,2400,4800,9600 Parity No No, odd, even

Stop bit 1 1 or 2 Swap word Word send order No Yes/no

SILKOSTAT 9210

Page C4

User’s configuration

Order Selected values Selected values Possible values Selected values Date

SEQUENCE / CHANNEL ACTIVATION Channel 1 On on / off Channel 2 On on / off Channel 3 On on / off Channel 4 On on / off Channel 5 On on / off Channel 6 On on / off

SEQUENCE / PROGRAMMING Sequence Sequence programming 123456123456 123456*

SERVICE/TIME Day Day of the week Monday Monday … Friday Date Date of the day 01/01/01 Time Hour 09:25:55

SERVICE/DISPLAY Language GB F/GB/D/SP/I

concentration Ppb ug/l / ppb SERVICE/CUSTOMIZE

Sample 1 name Sample 1 a…..z and 0…..9 Sample 2 name Sample 2 a…..z and 0…..9 Sample 3 name Sample 3 a…..z and 0…..9 Sample 4 name Sample 4 a…..z and 0…..9 Sample 5 name Sample 5 a…..z and 0…..9 Sample 6 name Sample 6 a…..z and 0…..9

SERVICE / CONFIGURATION Mains freq. 60 Hz 50/60 Hz

Reference freq. 0 Xx Freq. noir 9999 Xx

SERVICE/ FACTORY Channel number X 1 to 6

SERVICE/ FACTORY/SOLENOID VALVES Sample N Open time adjust 3 xx

Toff sample Close time adjust 180 s xx s Cal. Sol. N Open time adjust 3 xx

Toff cal. sol. Close time adjust 180 s xx s SERVICE/ FACTORY/ PUMPS

Pump 1 Ton Impulses number 5 Xx Pump 1 Toff Waiting time 240 s xx s Pump 2 Ton Impulses number 5 Xx Pump 2 Toff Waiting time 15 s xx s Pump 3 Ton Impulses number 5 Xx Pump 3 Toff Waiting time 60 s xx s

SERVICE/ FACTORY/MEASURE Type Choice of the range

0-1000 or 0-5000 ppb 0-1000 ppb 0-1000 ppb

0-5000 ppb

Linear coeff. Coefficient of non-linearity 0 0---XXX Waiting time Before the measure 1 s xx s

Measure time Extended measure 10 s xx s Conc. zero Reserved 0 ppb

Filter Reserved 50 mV Heating Heating activation Yes Yes/no

Negative values Display or no display of the negative values

no Yes/no

Page D1

SILKOSTAT 9210

Appendix D : Pressure range change

The battery of the input solenoid valves works with pure water sample. The pressure range is about 0,2 to 2 bars. If the pressure is about 0,5 to 6 bars, it is required to change the solenoid valves collar (see figure 1 item 6). So a « High pressure » kit contains 6 collars (0,8 diameter) and a TORX key.

Figure 1 Mounting of the solenoid valves

1 Hold down screw of the solenoid valves

2 Order coil

3 Body fixing screw

4 Solenoid valves main part

5 Flow direction

6 Solenoid valves collar

7 Seal

8 Calibration steel block

9 Sample output

10 Undeceiver

SILKOSTAT 9210

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To change the solenoid valves collar, proceed as follows : • Unscrew the 2 superior screw (1) of the solenoid valves. • Move the solenoid valves coil • Unscrew the 2 screws (3) of the main part fixing (4). • Move the collar (6) of the body (4). • Change the 2 O-rings (7) of the collar (6). • Replace the joints to the new collar. • Put the collar in position on the steel block (8) in the good direction.

Place the undeceiver (10) in the indicated position in terms of the cal output (9).

• Replace the main part (4) in position ; mark NC (5) and sample

output (9) must be placed in the same side. • Re-screw the fixing screw (3). • Replace the coil (2) and tighten with help of the 2 screws (1).

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SILKOSTAT 9210

Appendix E : Preparation of the tubes for insertion in the “fast” connections Figure 1 Slot marking

• Locate the slot to realise (see the table below)

Tube length 6 mm 1/4’’ 5/16’’

L 7,3 ± 0,5 0,33 ± 0,02 0,36 ± 0,02

Figure 2 Fasten the knurl

• Place the tube in the tube-cutter and set the knurl on the mark. • Fasten the knurl a quarter turn.

• Turn the tool around the tube and check the presence of a slot all

around the turn. • Remove the tube-cutter.