PROTOC 200
TOC Analyzer
ba43200e01 11/00
Operating Manual
0 - 2
Status at printing Our policy of continuous development ensures the advanced
technology and high quality standard of our equipment. As a result, this
operating manual may not correspond exactly to your equipment.
Furthermore, errors in the contents cannot be ruled out. Please be
aware that the information, figures and descriptions in this manual
cannot be used as the basis for legal claims.
Copyright
© Weilheim 2000, WTW GmbH & Co. KG
Reproduction – including excerpts – only upon express written consent
of WTW GmbH & Co. KG, Weilheim.
Printed in Germany.
PROTOC 200 Contents
0 - 3
1 Overview . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5
2 Safety . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7
2.1 Intended use . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7
2.2 Non-intended use . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7
2.3 Use of safety symbols . . . . . . . . . . . . . . . . . . . . . . . . . . . 7
2.4 General safety instructions . . . . . . . . . . . . . . . . . . . . . . . . 8
2.5 Hazards . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9
3 Installation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 11
3.1 Scope of delivery . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 11
3.2 Preparing solutions . . . . . . . . . . . . . . . . . . . . . . . . . . . . 11
3.2.1 Reagent solution . . . . . . . . . . . . . . . . . . . . . . . . 11
3.2.2 Standard solution . . . . . . . . . . . . . . . . . . . . . . . 12
3.2.3 Cleaning solution . . . . . . . . . . . . . . . . . . . . . . . . 13
3.3 Prerequisites for installation . . . . . . . . . . . . . . . . . . . . . . 14
3.4 Installation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 15
3.4.1 Wall assembly . . . . . . . . . . . . . . . . . . . . . . . . . . 15
3.4.2 Sample conditioning . . . . . . . . . . . . . . . . . . . . . 18
3.4.3 Electrical installation . . . . . . . . . . . . . . . . . . . . . 19
3.4.4 Connecting the carrier gas . . . . . . . . . . . . . . . . 21
3.4.5 Connecting the outlet . . . . . . . . . . . . . . . . . . . . 22
3.4.6 Connecting the reagent solution . . . . . . . . . . . . 22
3.4.7 Connecting the standard solution . . . . . . . . . . . 23
3.4.8 Connecting the cleaning solution . . . . . . . . . . . 23
3.5 Initial commissioning . . . . . . . . . . . . . . . . . . . . . . . . . . . 24
3.6 Checklist for commissioning the equipment . . . . . . . . . . 27
3.7 Commissioning . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 27
4 Operation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 29
4.1 Operation basics . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 29
4.2 Calibration . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 30
4.3 Shutting down the system . . . . . . . . . . . . . . . . . . . . . . . 32
5 Setup . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 33
5.1 Controller function . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 33
5.2 Sensor setup menu . . . . . . . . . . . . . . . . . . . . . . . . . . . . 34
5.2.1 Overview . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 34
5.2.2 Selecting the units . . . . . . . . . . . . . . . . . . . . . . . 34
5.2.3 Changing the calibration point . . . . . . . . . . . . . . 35
5.2.4 Setting the measuring range . . . . . . . . . . . . . . . 36
5.2.5 Cleaning . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 37
5.2.6 Zeroing . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 38
5.2.7 Calibration . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 39
5.2.8 Purging . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 40
Contents PROTOC 200
0 - 4
5.3 Alarm setup menu . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 41
5.3.1 Overview . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 41
5.3.2 Setting the nominal alarm values . . . . . . . . . . . . 42
5.3.3 Setting up the access code . . . . . . . . . . . . . . . . 43
5.4 Display settings . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 44
5.5 Controller setup . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 45
5.5.1 Overview . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 45
5.5.2 Setting the date/time . . . . . . . . . . . . . . . . . . . . . 46
5.5.3 Configuring the analog output . . . . . . . . . . . . . . 46
5.5.4 Setting the output voltage/current range . . . . . . 47
5.5.5 Serial interface (option) . . . . . . . . . . . . . . . . . . . 48
6 Maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 49
6.1 Weekly maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . 49
6.2 Six-monthly maintenance:
Replacing all pump tubes . . . . . . . . . . . . . . . . . . . . . . . . 49
6.3 Replacing individual pump tubes . . . . . . . . . . . . . . . . . . 51
7 What to do if... . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 52
7.1 The display responds slowly or not at all to the
calibration solution or sample . . . . . . . . . . . . . . . . . . . . . 52
7.2 Calibration and/or zeroing does not function . . . . . . . . . 52
7.3 Unstable readings . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 53
8 Technical data . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 55
8.1 Dimensions and weights . . . . . . . . . . . . . . . . . . . . . . . . . 55
8.2 Connections . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 56
8.3 Outputs . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 57
8.4 Miscellaneous . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 58
9 Appendix . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 59
9.1 Flow diagram . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 59
9.2 Socket connections for the analog output . . . . . . . . . . . . 60
PROTOC 200 Overview
1 - 5
1 Overview
View of equipment
Figure 1-1PROTOC 200 Analyzer
Figure 1-2PROTOC 200 Controller
Overview PROTOC 200
1 - 6
Function The PROTOC 200 is used to continuously measure organic carbon
content (TOC = total organic carbon) in aqueous samples. The mea-
surement procedure consists of the following steps:
l A reagent is added to the sample. The reagent contains sodium per-
sulfate and nitric acid or ortho-phosphoric acid.
l The sample and reagent mixture is sparged with a carrier gas (usu-
ally compressed air or nitrogen). This removes inorganic carbon and
dissolved carbon dioxide. The remaining liquid contains only organic
carbon compounds.
l The remaining liquid is pumped into the reaction vessel.
l A strong ultraviolet light source in the reaction vessel promotes oxi-
dation of the organic carbon compounds by the persulfate. This pro-
cess produces carbon dioxide gas.
l Carrier gas flows in through the reaction vessel base and transports
the carbon dioxide through a gas drying system and on to an infra-
red carbon dioxide detector. The amount of carbon dioxide pro-
duced is directly proportional to the organic carbon content of the
sample.
The PROTOC 200 can also be used to determine the total carbon con-
tent (TC = total carbon). The sample and reagent mixture is pumped di-
rectly into the reaction vessel without prior sparging.
The measuring signal is transmitted to the controller. The controller is
equipped with a signal output used in the control of external processes.
The PROTOC 200 is calibrated by passing a standard solution through
the analyzer. The standard solution contains a known quantity of car-
bon. The IR detector is adjusted until the analyzer displays the correct
reading. Solenoids switch between the sample and the standard solu-
tion.
Measurement output Measuring signals can also be output to external equipment (e.g. re-
corder, PC) via a 4 - 20 mA or 0 - 10 VDC (selectable) analog output.
PROTOC 200 Safety
2 - 7
2 Safety
This chapter contains general instructions to be followed during the in-
stallation, operation and maintenance of the equipment. It is absolutely
essential that users read this chapter prior to working with the equip-
ment. Always keep this operating manual in the vicinity of the equip-
ment!
2.1 Intended use
The intended use of this analyzer comprises
l determining TOC and TC in aqueous samples
l measuring surface water.
The intended use of the analyzer only covers the operation and running
as described in this operating manual.
2.2 Non-intended use
Non-intended use includes all methods of operating and running this
equipment that exceed the scope of operation as described in this op-
erating manual regarding the analyzer or individual components.
2.3 Use of safety symbols
Warning
Denotes information that must be followed in order to avoid serious per-
sonal injury or death.
Attention
Denotes information that must be followed in order to avoid slight per-
sonal injury or damage to equipment or the environment.
Note
Denotes tips regarding the equipment and its use to simplify operation.
Note
Denotes references to information in other sections of this operating
manual or other documents.
Safety PROTOC 200
2 - 8
2.4 General safety instructions
Function and operating
safety
The analyzer left the factory in perfect condition. Perfect function of the
equipment and operating safety can only be ensured if the environmen-
tal conditions and connection specifications stated in Chapter 8 T
ECH-
NICAL DATA, are met.
Perfect function and operating safety of this equipment can only be en-
sured if standard safety precautions as well as the special safety in-
structions in this operating manual are observed when using the
equipment.
Warning
Failure to comply with the instructions and safety notes in this operating
manual may lead to personal injury to operating personnel!
Warning
All maintenance and repair work that goes beyond the activities de-
scribed in Chapter 6 M
AINTENANCE, may only be carried out by techni-
cally qualified personnel authorized by the WTW company.
Technical condition The operator/user is obliged to continuously monitor the general tech-
nical condition of the analyzer (externally visible flaws and damage,
and changes in operational behavior).
Safe operation If it appears that the equipment cannot be safely operated, it must be
shut down and protected against inadvertent operation!
For example, the equipment cannot be safely operated when it:
l appears to have been damaged during transportation,
l has been stored improperly,
l shows visible signs of damage, or
l is not operating correctly.
Please contact the supplier in case of doubt.
Operating personnel The PROTOC 200 was developed for use in the environmental and in-
dustrial sectors. We assume that, through occupational training and ex-
perience, equipment operators are familiar with the safety precautions
required when handling chemicals.
PROTOC 200 Safety
2 - 9
Operator obligations The operator of the analyzer must ensure that the following laws and
guidelines are adhered to when handling hazardous substances:
l EG guidelines for industrial safety
l National laws regarding industrial safety
l Accident prevention regulations
l Safety data sheets of the chemicals and consumable substances
used.
2.5 Hazards
Warning
Touching electric components inside the analyzer during operation
may cause life-threatening injury due to electric shock. Switch off the
lamp before removing the lamp shield. Electric components may only
be serviced by trained and technically qualified personnel.
Warning
The source materials for preparing the reagent solution are highly cor-
rosive. Furthermore, sodium persulfate powder is inflammable when it
comes into contact with combustible substances. Observe the safety
data sheets provided by the chemical manufacturer and strictly comply
with the precautionary measures described therein.
Warning
The cleaning solution is corrosive and irritates skin and eyes. Avoid any
contact when handling the cleaning solution. Observe the safety data
sheets provided by the chemical manufacturer and strictly comply with
the precautionary measures described therein.
Attention
The pump motor contains a high-speed rotating fan. Touching the fan
during operation may cause severe injury to fingers. Never operate the
pump without first installing the finger guard.
Attention
The light source in the reaction vessel emits ultraviolet light during op-
eration. Direct exposure may lead to eye injury. Only operate the UV
lamp with the shield mounted on the reaction vessel. Never operate the
UV lamp outside of the reaction vessel.
Safety PROTOC 200
2 - 10
PROTOC 200 Installation
3 - 11
3 Installation
Attention
The equipment may only be erected, installed and set up by trained and
technically qualified personnel after careful study of this operating man-
ual.
The manufacturer reserves the right to reject warranty claims if these
requirements are not complied with.
3.1 Scope of delivery
Please check the packing list included to ensure that all parts listed
have been received.
3.2 Preparing solutions
3.2.1 Reagent solution
For operation, the analyzer requires a sodium persulfate solution that
has been acidified with nitric acid (preferred) or phosphoric acid.
Use only high quality concentrated nitric acid or phosphoric acid to pre-
pare the reagent solution. Water for dilution should be deionized or dis-
tilled. Tap water may be used for applications in the higher measuring
ranges (from 200 ppm upwards).
Warning
The starting materials used in the preparation of reagent solutions are
highly corrosive. Furthermore, sodium persulfate powder is inflamma-
ble when it comes into contact with combustible materials. Observe the
safety data sheets provided by the chemical manufacturer and strictly
comply with the precautionary measures described therein.
Warning
The oxidation reagent contains sodium persulfate. The reagent is cor-
rosive and irritates skin and eyes. Avoid any contact when handling the
reagent. Wear suitable protective gloves and goggles.
Installation PROTOC 200
3 - 12
The table lists the quantities of chemicals that are required:
Prepare the reagent solution as follows:
Preparing the reagent
solution
Note
A higher acid concentration in the reagent solution is required for appli-
cations in which the proportion of inorganic carbon (inorganic carbon =
IC) to the TOC is very high (IC > 50, TOC < 10), or for applications that
have a high pH value. We recommend doubling the acid quantities in
the above table, i.e. 200 ml acid to 20 liters water.
Note
The reagent solution has a shelf life of several weeks.
3.2.2 Standard solution
You will need a standard solution of known carbon concentration to cal-
ibrate the analyzer. Usually a supply of the standard solution with 1000
ppm carbon is prepared.
Prepare the standard solution as follows:
Preparing the standard
solution
Concentra-
tion
Sodium
persulfate
Water for
dilution
Acid
2.5 % 500 g 20 liters 100 ml
5 % 1 kg 20 liters 100 ml
10 % 2 kg 20 liters 100 ml
1 Fill a clean 5 or 10 liter container half full with water.
2 Add the sodium persulfate and dissolve it completely. Add
more water if required.
3 Add the acid.
4 Transfer the solution to the reagent container and fill it to the
required level with water.
1 Ensure that the accessories and the container are free from or-
ganic contamination.
PROTOC 200 Installation
3 - 13
Note
The concentrated stock solution has a shelf life of 4 to 6 weeks if refrig-
erated.
Note
If higher concentrations are required, prepare the solution with a multi-
ple of the weight specified above.
3.2.3 Cleaning solution
You will need a cleaning solution to clean the analyzer plumbing sys-
tem. The type of cleaning solution required depends on the application
and is specified upon ordering.
2 Weigh out 2.125 g reagent grade, anhydrous potassium hydro-
gen phthalate (C8H5O4K) and transfer it to a 1l graduated
flask.
3 Add distilled or deionized water.
4 Add 1 ml reagent grade, concentrated phosphoric acid.
5 Top up to the 1l mark with water.
6 Mix thoroughly.
7 Label the bottle with the contents and preparation date and
store it in a refrigerator.
8 Dilute the standard solution as required for calibration.
Installation PROTOC 200
3 - 14
3.3 Prerequisites for installation
Location l The equipment is not designed for outdoor use.
l The equipment should be installed as close as possible to the loca-
tion where the sample is taken to avoid any changes to the sample
en route to the analyzer and to minimize the inlet lag time.
l The analyzer should be protected against strong vibrations (as may
be caused by large motors, pumps, etc.) since these may negatively
affect performance.
l There must be an open and pressure-free drain.
PROTOC 200 Installation
3 - 15
3.4 Installation
3.4.1 Wall assembly
Attention
Do not shorten the tubes included; their full length is required for fas-
tening the swage locks.
Figure 3-1PROTOC 200 dimensions (given in mm)
Mounting the analyzer
and controller
Dimensions and space
requirements
1 Attach the analyzer securely to the mounting wall using the 4
wall fixtures. Bear in mind that the unit must be accessible from
all sides.
2 Attach the controller fixture to the mounting wall; if possible, it
should be mounted close to the analyzer.
3 Place the controller onto the wall fixture.
4 Space requirements for the controller are shown in the dimen-
sioned views in Figure 3-1. Figure 3-2 presents a typical wall
assembly with the required drilled holes.
Installation PROTOC 200
3 - 16
Figure 3-2Typical wall assembly with drilled holes (dimensions in mm)
203
101.5
ca.1800
647
457
min. 200
Analyzer
Controller
24
Typical wall assembly
5 Connect the analyzer power cable to Connection A
(see Figure 3-3).
6 Connect the controller to Connection B
(see Figure 3-3) on the analyzer.
PROTOC 200 Installation
3 - 17
Connections
Figure 3-3Connections
Warning
The solution flowing from the drain contains acid and oxidizing sub-
stances. It causes severe injury to eyes and skin upon contact. Avoid
any direct contact with the draining liquid. Wear suitable protective
gloves and goggles.
Connection Function
A Power supply
B Signal output to controller
C Carrier gas inlet
D System outlet
E Sample inlet
F Standard inlet
G Reagent inlet
H Outlet opening
I Ventilation
J Dryer and U-tube ventilation
K Cleaning liquid inlet
L Cleaning liquid outlet
Installation PROTOC 200
3 - 18
3.4.2 Sample conditioning
The PROTOC 200 Analyzer configuration depends on:
l the measuring objective
l the physical arrangement around the equipment
l the nature of the sample
The particle size in the sample to be analyzed should be less than 100
micrometers. Appropriate filtering should be employed which takes the
following into account:
l PROTOC 200 performance depends upon the integrity of the sam-
ple. Each individual installation may require its own unique sample
processing system.
l Ideally, the sample intake into the PROTOC 200 at the sampling lo-
cation will be many times larger than the intake actually required for
measurement. This serves to shorten the time the sample takes to
reach the analyzer (lag time), i.e. to avoid any change in the sample
en route to the analyzer. It also improves the functioning of sample
conditioning and allows the use of prefabricated pumps and tubes.
l Some applications require a cleaning cycle in which the sample flow
tube in the analyzer is rinsed with a cleaning solution. This serves to
prevent blockage due to the build-up of fine particles or to remobilize
deposits or grease.
1 Install the pumping or filtering system suitable for the applica-
tion and connect it to the sample inlet (see Connection E, Fig-
ure 3-3). The sample should not be flowing at this point.
PROTOC 200 Installation
3 - 19
3.4.3 Electrical installation
Warning
It is essential that the analyzer be correctly earthed.
Electrical work may only be carried out by technically qualified person-
nel.
Prior to connecting the equipment, ensure that the data of the mains
power socket correspond to the specifications stated in the T
ECHNICAL
D
ATA section of this manual. The mains power socket must have a
ground cable connection.
Figure 3-4IR detector
1 Before connecting the equipment, ensure that the IR detector
switch (1) located in the analyzer is set to OFF.
1
Installation PROTOC 200
3 - 20
Figure 3-5Lamp switch
Figure 3-6Pump switch and main switch
2 Ensure that the lamp switch (2) is set to OFF.
3 Ensure that the pump switch (3) is set to OFF.
4 Plug in the analyzer power cable.
5 Switch on the main switch (4).
6 Switch on the IR detector (1). The warm-up period begins.
7 Make the remaining connections during this period.
2
4
3
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