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Training

dew point and hydrogen measurement in


the
float bath atmosphere
with DSS70A Vaisalainstrument
and Messkonzept instrument
Herzogenrath, Feb. 2014
P. Vehres

Projekt Chemistry of the float bath


Theory
Where comes H2O and O2 in the atmosphere from?

Taken from a presentaion of Dr Andreas Kasper : Theorie O_H_S float

For dew point important processes/


compounds in the float bath
O2

> come in through leaks in the side sealing

O2

> from a reaction with SO3 (glass) and H2

H2

> from mixed gas

H2O > come in with the mixed gas


H2O > from reaction with SO3 (glass) and H2
H2O > from reaction with Sn and O2
The measured dew point is normally -10C to -50C
concentration O2 0.000 000 000 000 000 000 000 001atm
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Aim of dew point and hydrogen measurements


o The dew point is a deciding indicator for the quality of the float
atmosphere and the mixed gas
o A WCM-Project is launched to reduce the hydrogen concentration in
the float bath,
save money
optimize the process
a control of the float bath atmosphere is needed
o With a known dew point and a known hydrogen concentration the
oxygen concentration in the float bath atmosphere can be
calculated
Low oxygen concentration reduces the risk of dross formation
Low oxygen limits SnO evaporation ( Top Tin)

Regular control of the dew point and the hydrogen


concentration in the float atmosphere helps to solve
problems and to save money
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Measurements of dew point (DP) and


hydrogen concentration (H2)
Overview
Float
bath

Slab in
window

Glass
pipe

PTFE tube

DP measurement
DSS70A / DM70

H2 measurement
sensor / recording system

Measurements of dew point (DP) and


hydrogen concentration (H2)
DP and H2 measurement is an extractive analysis.

Measurement point, slab with quartz


glass tube and PTFE tube

Registration
system for H2

Messkonzept
measurement
system for H2

Vaisala DSS70A
(extraction system DP)

Vaisala DM70 (Sensor DP)


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Quartz Glass and PTFE tube


o HRDC use a quartz glass pipe: 800 mm long,
inner 6 mm, outer 10 mm
o HRDC use a PTFE tube with inner 4 mm and
outer 6 mm

The sample PTFE tubing should


be as short as possible
o inner (ID) glass = outer (OD) PTFE tube
Make sure that you have a gas leak free connection
between quartz glass tube, PTFE tube and sensor
Important : No contamination with O2 !!!
.
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Set up quartz glass tube


1.
Take the quartz glass tube and a
big silicon tube, length ca. 5 cm
ID silicon tube big = OD glass tube

10mm

10mm

2.
Slip 1.5 cm of the silicon tube over
the quartz glass tube

Set up PTFE tube


10mm

1.
Take the PTFE tube and a small
silicon tube (length ca. 1 cm)
OD PTFE = ID silicon small
OD silicon small = ID silicon big

2.
Slip the small silicon tube over the
PTFE tube

10mm

Connect quartz glass tube and PTFE tube


10mm

1.
Quartz glass tube and PTFE tube are
ready to connect
ID Glass = OD PTFE tube
2.
Put PTFE tube inside the glass tube
and slip big silicon tube over small
silicon tube

10mm

PTFE tube inside the glass tube

3.
Close gas leak free
with PTFE ribbon
>
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Build a slab to put in a side sealing window as


a guidance
If the slab is set in side sealing
window the metal tube at the
atmosphere side must always face
upwards direction roof.
Explication:
The slab is the guidance for a long glass tube,
which is required to extract the atmosphere.

200 mm

Angel must be so that one end of a


glass tube is located in the float
bath atmosphere

Slab in a side sealing window.


o For all kind of window build at least 1
slab
o Try with a tube, which has the size of
your glass tube, if it doesnt touch the
wall or tin

For measurements exchange the glass in the


windows for the slab and seal with mortar
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Put the quartz glass through the slab

1. Implement the glass tube through the slab into


the atmosphere of the float
2. Seal the hole with kerlane / wool so that the
glass tube cant move
3. Make sure that you dont touch the wall or the tin

Make sure that you do not extract tin


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Measurements without a slab !


How to build a gas leak free connection to the
float bath atmosphere ?
Put a quartz glass tube in an
existing pipe in the side sealing
Seal the hole with kerlane / wool

Put a PTFE tube 1cm in an existing


pipe in the side sealing, use silicon
tubes and PTFE ribbon to connect gas
leak free
(same procedure as used to connect glass
and PFTE tube, see above)

Make sure that you do not extract tin


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Measurements with DSS70A Vaisala and


H2-Sensor Messkonzept
Please read the instruction / manuals of the
instruments before you start the measurements
Please make sure that the instruments are ready
to use (refer manual)
Connections
1. Connect gas inlet of the DSS70A with
PTFE tube (coming from the float atmosphere)
2. Connect gas outlet of DSS70A with gas
inlet of Messkonzept sensor
3. Connect DSS70A with
DM70
4. Connect Messkonzept sensor
with reading system
Eventually take notes.

gas outlet DP to gas


inlet H2
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gas inlet

Start measurements
Please read the instruction / manuals of the instruments before you
start the measurements
Start measurement by following the instruction in the suitcase DSS70A
1. Make sure that the pump is switched off.
2. Lift the flow meter to a vertical position
3. Close the sample value
4. If you measure in the float bath atmosphere you
measure a non-pressurized system
5. Connect the sampling PTFE-tube (atmosphere) gas leak free to the IN
fitting
6. Turn on the pump
7. Adjust the sample flow rate to a value of 1L/minute
8. Turn on the DM70 sensor and set all the needed parameter
9. Turn on the Messkonzept system + recording system
10. Control after 5 at least minutes that you not extract tin

Wait until the reading has stabilized (minimum 45 minutes)


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Handling DM70
Please read the instruction / manuals of the
instruments before you start the measurements
Starting the measurement
1. Press the Power On/ Off button
2. Go to the Recording / Viewing menu, set the recording of the reading
for the dew point every 30 second.
3. Let the instrument auto calibrate
4. The internal purge will take some minutes
The measurement will take minimum 45 minutes.
You can note the values in order to control if you reach stable
values (DP < 2C)
After the measurement
Connect the DM70 with a computer, save the readings
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Stop Measurements
Please read the instruction / manuals of the
instruments before you stop the measurements
Please make sure that the instruments are ready
to use (refer manual)
Stop
1. Stop measurement by following the instruction
in the suitcase DSS70A
2. Stop Messkonzept system
3. Disconnect gas inlet of the DSS70A from
PTFE tube
4. Disconnect gas outlet of DSS70A from gas
inlet of Messkonzept sensor
5. Disconnect DM70 from DSS70A

Gasinlet
Gas outlet
DP to gas
inlet H2

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GOOD LUCK FOR THE


MEASUREMENTS

If you have any problems please contact me


petra.vehres@saint-gobain.com
0049 2406 91 1205

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