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Comparison of Once Through and
Closed Loop Apparatus for Steam Oxidation
Measurements at Ambient and Elevated Pressure
A T Fry, M Serafon, J Banks, D Laing
National Physical Laboratory, Hampton Road, Teddington, Middlesex TW11 0LW, UK
tony.fry@npl.co.uk

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Acknowledgements
The authors would like to acknowledge the Department of Business
Innovation and Science for funding the work reported in this document.
Laboratory scale testing
Advantages
Well controlled
Monitored
Simplifcations allowing parametric studies
Temperature and Pressure control
Disadvantages
Over simplifed
Does not include non steady state factors
Does not reproduce the correct morphology
Relatively short
Frequently used to generate understanding, to characterise and rank material performance.
However results do not always agree as seen in COST 522 and a recent UK-US intercomparison exercise.
Frequently used to generate understanding, to characterise and rank material performance.
However results do not always agree as seen in COST 522 and a recent UK-US intercomparison exercise.
Apparatus
Figure 2: Schematics of the (a) atmospheric rig and (b) the high pressure steam loop.
References
[1] P. J. Ennis and W. J. Quadakkers, The steam oxidation resistance of 9-12%chromium steel,
in Materials for Advanced Power Engineering 2002, (2002).
[2] A. T. Fry, Standardisation in High Temperature Corrosion Testing, in 23rd Annual Conference
on Fossil Energy Materials, Pittsburgh, (2009).
[3] A. T. Fry, M. Serafon and J. Banks, High pressure steam oxidation: Extents and infuences,
in Advances in Materials Technology for Fossil Power Plants, Waikoloa, Hawaii, (2013).
Experimental
Double distilled water/deionised
Deoxygenated by bubbling N
2
Samples in alumina boats or hung from sample holder
Mass change and oxide thickness measurements
Once through
O
2
~ 5-13ppb
Flow rate ~3 ml min
-1
Water fed into furnace
Heats to form steam
Passes over samples
Exits through water trap
Recirculating
O
2
~ 2-5ppb
Flow rate ~9 ml min
-1
Water fed into evaporator to form steam
Passes over samples
Returns to reservoir
Figure 4: Representative micrographs from the exposures
Static Autoclave Once Through Steam Loop
Static steam
Stagnant?
Increase in mass gain
with time and pressure
Defective scale
Flowing steam
Porous scale
Increasing mass and
thickness with time
Flowing steam
Dense scale
Increasing mass and
thickness with time and
pressure
Thinner oxide at 1 bar
Figure 4: Mass change as a function of time
and exposure method and pressure for
Grade 92 steel at 650C in steam.
In comparing the ambient and 1 bar data from the once
through and recirculating steam loop a clear diference
in the mass change and oxide thickness is observed
between the two apparatus (Figure 4).
For tests conducted with dissolved O
2
levels of ~200ppb
there is two fold decrease in the mass change compared
with that of the recirculating loop using dissolved O
2

levels of ~5 ppb.
Improved control of the dissolved O
2
levels in the tube
furnaces shows a decrease in mass gain of 25%.
Previous investigations into the efect of water chemistry
on the oxidation rate did not show such a marked efect
for Grade 92 material, suggesting that the control ofered
by closed loop systems is highly advantageous.
Tests on additional materials show the efect is not
material related (Figure 5).
Figure 6: Results for the intercomparison
with the 1 bar steam loop data
superimposed.
Figure 5: Mass change as a function pressure
for various steels at 650C in steam.
These results may ofer an explanation of the diferences
seen in the results of the COST round robin and an
intercomparison exercise conducted in 2009
[1]
,
[2]
. Within
this small intercomparison three laboratories exposed
grade 92 material to fowing steam in tube furnaces,
where two were at ambient pressure whilst the third was
at 17 bar.
Taking into account the 25% drop in mass gain, with
better control of O
2
this would essentially drop data
points onto the lower curve as shown in Figure 6.
Modelling work not reported here supports these
fndings (Figure 7)
[3]
Figure 7: Modelled internal oxide thickness as a
function of pressure at 650C compared with steam
loop 1 bar data and once though data.