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MCS

PRIMACS TOC
ANALYSER

CHAPTER 6: TECHNICAL INFORMATION

Preface:

This chapter gives details of the hardware.


PrimacsMCS TOC Analyser Chapter 6 Technical information 6-1

6 TECHNICAL INFORMATION
The schematic layout of the principal of operation and the main functional
parts of indicating and control elements can be found in this chapter.
The power supply connection is at the back of the cabinet together with the
main power switch and fuses.
6.1 Technical specifications
PrimacsMCS
Frame: Steel and duralomin profiles and sheets
Dimensions: HxDxW : 73 cm x 30 cm x 40 cm
Weight: 20 kg
AC line voltage: 220-240 Volts, 50 Hz
100-120 volts, 60 Hz
Fuses: 3.15 A mA (220-240V)
6.3 A (100-120V)
Carrier gas: Pure OXYGEN (contains CO2 less than 20 vol.
ppm)
Flow rate: 140 ml/min
TC oven: 1100C
IC oven: 125C

IR detector In Formacs:
Measuring range: Dependent on customers requirements
Default measuring range: 1-40 mg C abs.
Output signal: 0 1V DC
Fuse: 0.5 A
Linearity: 2%
Repeatability: Within 2% of full scale
Ambient temperature: 5C to +45C
Warm-up time: About 15 minutes
PrimacsMCS TOC Analyser Chapter 6 Technical information 6-2

Figure 6.1 Gas flow scheme


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6.2 Hardware
6.2.1 A brief description of the analytical procedure.
1. The carrier oxygen enters the PrimacsMCS analyser at the side through
the lower gas connector.
2. The carrier gas (0.2 MPa) enters the analyser and passes the gas flow
controller, where it is adjusted to 140 ml/min.
3. The carrier gas then enters the TC port.
A. TC measurement
1. When the analysis is started the TC sampling port is closed and the
carrier gas flows directly through the TC reactor, while the crucible is
pushed up.
2. The sample is combusted in the reactor at 1100C. All combustion
products join the carrier oxygen and will be converted by the aid of the
catalyst in the top of the reactor into CO2.
3. The gas flow passes the TC condensate trap, where the gas flow is
cooled to room temperature and the condensate is collected in a waste
vessel.
4. The gas flow then passes the complete IC reactor and the IC
condensate trap.
5. The gas flow then passes two delay vessels to postpone the gas entry
in the IRD to a time when the carrier gas flow level is constant.
6. Then the gas flow leaves the PrimacsMCS and enters the Formacs
analyser where it passes the Peltier cooler (see the manual of the
Formacs analyser), where the flow is cooled to 2-4C and the
condensate is drained off.
7. Then the gas flow passes the halogen scrubber (see the manual of the
Formacs analyser), to remove any halogens from the flow.
8. The gas flow then enters the IRD (see the manual of the Formacs
analyser), where the CO2 is analysed in the pre-set range; the signals
are passed on to the computer system for calculation.
9. The gas leaves the analyser at the side of the instrument.
At the end of the analysis (when the message is displayed that a sample
has to be inserted) the crucible has to be moved down and the sampling
port is opened to replace the crucible by a new sample.
In the next part of this chapter the parts described in bolt will be described
more fully.
B. IC measurement
1. When the analysis is started for a measurement the test tube is pushed
up into the screw head of the IC sampling port. The screw head is
tightened and the IC reactor (temperature 125C) is placed around the
tube (if required).
2. Acid is added by means of the dispenser. The reaction is started and
the carrier oxygen flow blows through the test tube. The products of
reaction join the carrier oxygen.
3. The gas flow passes the IC condensate trap, where the gas flow is
cooled to room temperature and the condensate is collected in a waste
vessel.
4. The gas flow then passes two delay vessels to postpone the gas entry
in the IRD to a time when the carrier gas flow level is constant.
5. Then the gas flow leaves the PrimacsMCS and enters the Formacs
analyser where it passes the Peltier cooler (see the manual of the
PrimacsMCS TOC Analyser Chapter 6 Technical information 6-4

Formacs analyser), where the flow is cooled to 2-4C and the


condensate is drained off.
6. Then the gas flow passes the halogen scrubber (see the manual of the
Formacs analyser), to remove any halogens from the flow.
7. The gas flow then passes two delay vessels to postpone the gas entry
in the IRD to a time when the carrier gas flow level is constant.
8. The gas flow then enters the IRD where the CO2 is analysed in the pre-
set range; the signals are passed on to the computer system for
calculation.
9. The gas leaves the analyser at the side of the instrument.
At the end of the analysis (when the message is displayed that a sample
has to be inserted) the heater is pushed down and aside. The tube is
released from the IC sampling port by releasing the screw head bit.
6.2.2 Gas flow controlling parts
The carrier oxygen from the supply gas cylinder has an input pressure of 2-
3 bar (= 200 - 300 KPa on the gas cylinder). The flow is displayed on a
pressure gauge, visible at the front of the analyser.
The proper flow of the carrier gas is set by a flow controller RP32. This is a
downstream controller, controlling the flow according to the pneumatic
resistance of the gas way. The flow is set on 140 ml/min.
6.2.3 High temperature TC reactor
The TC reactor consists of the TC
sampling system and the reactor
tube with heating (see Figure 6.2).
TC sampling system
The PRIMACSMCS analyser uses
the vertical system of sampling of
quartz crucibles. This unique
system allows the comfortable and
fast operation with extremely hot
crucibles and is easy enough to
be reliable. The crucible is placed
into the crucible holder with
handgrip. The crucible can easy
be placed into the holder with the
aid of tweezers. By pushing the
crucible into the TC port by means
of the hand grip the TC port is
closed into the operation position.
During the analysis the port is
sealed by a hand lever. Leakage Figure 6.2 TC reactor
is avoided by an O-ring. The hand
slider is used for vertical pushing of the crucible into the combustion space
of the reaction tube.
The TC reactor tube
The reactor tube consists of two parts: The large ceramic reaction tube (for
solids as well as solids containing much liquid) where the combustion takes
place and the small ceramic reaction insert tube, which is filled with an
oxidative catalyst to complete the reaction.
The small ceramic tube is hanged inside the large ceramic reaction tube
and has holes at the bottom to allow the gas flow pass the catalyst. The
PrimacsMCS TOC Analyser Chapter 6 Technical information 6-5

catalyst is held in its position with the aid of quartz wool plugs. For filling the
tube, see also Chapter 4, Maintenance.
The ceramic tubes are resistant to a max. temperature of 1100C. The
large ceramic tube is placed in the heat sink and sealed with the aid of a
gasket and O-rings. The special coupling (sealed with O-rings) is used as a
gas output in the top of the reactor tube.
The TC reactor is designed for the use of crucibles with a diameter of 22
mm and a height of 15 mm. The ceramic tube has an outer diameter of 31
mm and an inner diameter of 25 mm.
The electrical heating of the reactor tube is insulated with aid of ceramic
material. The temperature of the heating is controlled by a thermocouple
inside the oven. A 30V oven is used. The oven is fixed in its holder together
with a wires terminal and thermocouple. This common holder allows easy
removing the oven for maintenance of the reactor tube; see also Chapter 4,
Maintenance.
6.2.4 Inorganic carbon reactor
The inorganic carbon reactor is shown in Figure 6.4.This reactor consists of
the IC sampling port and the reactor itself.

Figure 6.4 IC reactor Figure 6.3 Schematics IC reactor

The sample in the test tube is pushed into the head and sealed by a screw
nut. This head is a common in/outlet of acid and carrier gas. The heater is
then placed and fixed around the reaction tube.
The reaction is done directly in the test tube after adding of the acid. The
reaction space is heated to 125C. The temperature is controlled by a
thermal switch. The heating temperature is sufficient for boiling of the liquid
in the test tube during the reaction with acid. The acid is added by means of
a dispenser (included with the PrimacsMCS). For the input of acid a tube is
used. The same tube in the axis of the reactor is used as the oxygen input.
The oxygen is used as a purging and mixing gas. It is bubbled through the
mixture of acid and solid powdered (or liquid) sample during the reaction.
The gas carries the reaction products out of the reactor via the straight
union coupling to the condensate trap.
PrimacsMCS TOC Analyser Chapter 6 Technical information 6-6

6.2.5 Condensate traps


The carrier gas with reaction products either from the TC reactor or the IC
reactor enters the condensate traps. These condensate traps catch the first
(major) part of condensate coming from either TC or IC. The carrier gas
descends through the chamber, after which the gas rises as the liquid is
collected in the waste vessel.

Figure 6.6 IC Figure 6.5


Condensate trap Collection vessels

6.2.6 Collection vessels


The system has two collection (delay) vessels that are placed in series.
They are necessary for postponing the gas entry to the IRD to a time when
the carrier gas flow level is constant.

6.2.7 Extra components in Formacs analyser


To facilitate the measurement of different sample gas supplies in the
detector of the Formacs analyser na extra component has to be installed in
the Formacs analyser.
A MCS module has to be placed to keep the different gas ways separated.
PrimacsMCS TOC Analyser Chapter 6 Technical information 6-7

MCS module
The MCS module is mounted in the
IC compartment of the Formacs
analyser (see Figure 6.7). It consists
of two valves. The valves are
switched from one gas way to the
other by means of the software of the
Formacs. Both valves are switched at
the same time. The MCS module is
placed between the IC module and
the Peltier cooler.

Figure 6.7
PrimacsMCS TOC Analyser Chapter 6 Technical information 6-8

6.3 Recommended Spare parts and consumables


Please always quote catalog number when placing an order.
PrimacsMCS TOC Analyser:
Description Catalog no. Quantity
TC-reactor, ceramic tube 2CS22170 1
Ceramc insert tube 2SN22254B 1
Collection vessel (large) 2CS22050 1
IC cup holder 2CA50160 2
O-ring Viton 25 x 2 mm 90039583 10
O-ring Viton 16 x 4 mm 90039564 10
O-ring Viton 34 x 3 mm 90039588 10
O-ring Viton 32 x 2 mm 90039510 10
O-ring Viton 11 x 2.5 mm 90039533 10
O-ring Silicone 29.3 x 4.6 mm 2CA50250 1 set (10)
Tubing PTFE 3.2 x 1.6 mm (OD x ID) 90041454 1m
Ferrule 6 mm 90037901 5
Ferrule 1/8 - SS 90037926 5
Ferrule 6 mm SS 90037917 5
Catalyst, TC-Reactor 2CA10319 50 g.
Quartz Wool, filling 2CA10359 1 (10 g.)
Support disks 90035227 2 p (of 10)
Fuse, slow 5 x 20 VDE 3.15 A* 90028823 2
Fuse, slow 6.3 x 32 CSA 6.25 A* 90029056 1
PE tubing black 6 X 4 mm 90041092 1m
Test tubes + rack 2CA50002 1 set
Quartz crucibles (22 x 15 mm) 2CS22003 1 set

Items marked with a * denote that there is a choice for this item and is
depending on the configuration of the analyser.