VOD & RH Application Summary Prima PRO.

doc
Page 1 of 4

VOD & RH APPLICATION SUMMARY

1. PRIMA PRO ANALYTICAL SPECIFICATION

The Prima Pro will be used to analyze H2, CO, N2, O2, Ar and CO2 over the below concentration ranges, over a
process pressure range of 1000 mbar to 0.3 mbar.

Range % mol concentration

H2 0 – 10
CO 0 – 70
N2 0 – 100
O2 0 – 25
Ar 0–4
CO2 0 – 60

PRIMA PRO PERFORMANCE SPECIFICATION

Analytical performance is demonstrated by analyzing calibration bottle 1 over 1 hour following calibration as shown
below:-

% mol concentration Standard Deviation Accuracy

% mol % mol
specified as at or below the specified as at or below the
following values following values
H2 2 0.002 0.01
CO 40 0.03 0.1
N2 10 0.03 0.1
O2 1 0.002 0.01
Ar 42 0.03 0.1
CO2 5 0.01 0.05

Standard deviation, σn-1 = {∑(xi-xm) /(n-1)}

2 1/2

where:-

n refers to the number of measurements to which the statistical determination is to be applied, xi refers to the
individual measurements and xm is the mean value = {x1 + x2 + x3 + .... xn}/n.

Accuracy = difference between mean value and calibrated value.

The analysis is on a normalized basis, i.e. the individual reported component concentrations are adjusted, so that
their sum equals 100%.

The above assumes an analysis time of 5 seconds.

2. CALIBRATION GAS REQUIREMENTS – to be supplied by others

The following calibration gases are required:-

Thermo Fisher Scientific Ion Path, Road Three, Winsford, Cheshire +44(0)1606 548700 www.thermo.com
CW7 3GA, UK +44(0)1606 548711
 VOD & RH Application Summary Prima PRO.doc
Page 2 of 4

Calibration bottle 1 2 3 4
H2 2 mol%
CO 40 mol% 20 mol%
N2 10 mol%
O2 1 mol%
Ar 42 mol% 80 mol% 80 mol%
CO2 5 mol% 20 mol%
He 1 mol% 100 mol%

Notes

1. Typical calibration cylinder sizes are 10-50 litres. Cylinder pressures should be the maximum obtainable up
to 200 bar, consistent with being non-condensing. Double stage regulators with 0-2 bar(g) output stages
should be used in conjunction with the calibration gas cylinders to set the output pressure to the mass
spectrometer calibration panel to 1 bar. It is the responsibility of others to provide calibration gas
cylinders, regulators and pipe-work leading from each cylinder to the calibration panel. It is recommended
that 316 stainless steel tubing be used for connecting the calibration cylinders to the calibration panel.

2. Cal gas 1 should be a gravimetric mix certified to better than 1% relative.

3. Cal gases 2 and 3 should use >99.9% purity.

4. Cal gas 4 should use >= 99.995% purity.

5. Calibration interval is daily with cal gas 1 (quick) and weekly with all four cal gases.

6. Calibration time is <4 minutes for daily quick calibration and <15 minutes for weekly full calibration.

Thermo Fisher Scientific Ion Path, Road Three, Winsford, Cheshire +44(0)1606 548700 www.thermo.com
CW7 3GA, UK +44(0)1606 548711
 VOD & RH Application Summary Prima PRO.doc
Page 3 of 4

3. RECOMMENDED ANALYSIS SET-UP - reference information

Example values of relative sensitivities and fragmentation patterns (actual values will differ but be accurately
calibrated by the instrument using the calibration gases).

H2 CO N2 O2 Ar CO2
Relative sensitivity 0.5 0.01 0.015 0.7 1.2 1.0
2 100
12 100 1
14 1.0 100
32 100
40 100
44 100

The electron energy should be set to 45 eV rather than the more common setting of 70 eV. This is in order to
2+
suppress the formation of CO which is detected at mass 14 and which degrades the accuracy of the analysis of
CO and N2. The base gas should be set as CO2.

4. RECOMMENDED CALIBRATION PROCEDURE - reference information

The gas calibration should be configured as follows, where F= Fragmentation, S = Sensitivity, L = Linearity. Note
backgrounds should be measured with cal gas 4 (100% helium).

Calibration bottle 1 2 3 4
H2 2 mol%
S
CO 40 mol% 20 mol%
L FS
N2 10 mol%
L
O2 1 mol%
S
Ar 42 mol% 80 mol% 80 mol%
S
CO2 5 mol% 20 mol%
L FS
He 100 mol%

5. NOTES ON APPLICATION

RH and VOD are secondary steel-making processes to produce specialty steels and involve degassing. The
process occurs with molten steel under vacuum, which enables reduction of the carbon content to very low levels
(<0.01%) without undesirable oxidation of chromium. The process gas needs to be monitored over the pressure
range of 1000 mbar (atmospheric pressure) down to 0.3 mbar. The Vacuum-Oxygen Decarburization process is
used for making stainless steel. During the VOD process an oxygen lance is used to blow oxygen on top of the melt,
while argon is bubbled up from the bottom. In the Ruhrstahl-Hausen process two legs of the vacuum chamber that
are lowered into the melt. Argon is injected in one leg causing a vigorous boiling and mixing action. The R-H-OB
Process is a variation on the R-H Process in that oxygen is also added for greater decarburization.

Thermo Fisher Scientific Ion Path, Road Three, Winsford, Cheshire +44(0)1606 548700 www.thermo.com
CW7 3GA, UK +44(0)1606 548711
 VOD & RH Application Summary Prima PRO.doc
Page 4 of 4

6. SPECIAL APPLICATION REQUIREMENTS - reference information

INLET
Variable Pressure Inlet for sampling at between 1000 mbar and 0.3 mbar.

SAMPLE CONDITIONING
This application requires a special vacuum sampling conditioning system.

Thermo Fisher Scientific Ion Path, Road Three, Winsford, Cheshire +44(0)1606 548700 www.thermo.com
CW7 3GA, UK +44(0)1606 548711