Hydrogen/Oxygen determinator

The ROH600 determines the hydrogen and oxygen content of an inorganic sample
using a self contained electrode furnace for fusion.
Hydrogen and oxygen are measured by infrared detection as water,carbon dioxide
and carbon monoxide in an oven consisting of four IR cells.
Analysis begins by placing a sample into the loading head and placing an empty
graphite crucible on the lower electrode.After pressing the loader button the
electrodes close and atmosphere is purged from the crucible.High current passes
through the crucible generating heat,which drives off gases trapped in the
graphite.This process is called outgassing.Next, a sample is dropped from a loading
mechanism into the crucible.The oxygen released from the sample combines
combines with the carbon from the crucible to form carbon monoxide and small
amounts of carbon dioxide.Hydrogen in the sample gas is released as hydrogen gas.
Sample gases pass from the furnace to the to the CO and CO2 detectors.From there,
sample gases pass through heated copper oxide wire which converts carbon
monoxide to carbon dioxide and hydrogen to water.The sample gases then pass
through the H2O and low CO2 IR cells.The hydrogen result is measured by the
H2O IR cells and the oxygen result is measured by a combination of the two carbon
dioxide and carbon monoxide IR cells.

Barometric pressure:
Since atmospheric pressure directly affects gas volume,it is important to input the
correct barometric pressure in order to obtain the most accurate results during gas
dosing.
For gas dosing the units of atmospheric pressure is taken to be “mm” of mercury.
mm of Hg=25.4*inches of Hg

Pressure varies inversely with altitude.When entering the barometric pressure the
value should be obtained from a local,known accurate source.

Operation pressure/760*reported barometric pressure at 0 feet=adjusted pressure

(from table) at atmosphere

eg.Barometric pressure is reported as 750 mm of Hg at sea level(0 feet), but

operation altitude is 1000 feet.Adjust the reported sea level pressure to operation
level pressure .
ans:733mm of Hg/760 mm of Hg* 750 mm of Hg=723 mm of Hg
In this eg.,the barometric pressure to be entered into the instrument is 723 mm
of Hg.

*Calibration curve:
After the blank is defined, a calibration curve needs to be defined. Several standards
need to be selected that will cover the operating range of the analyte concentration
for the samples of unknown anlyte concentration.At least three replicates of each
standard should be analysed.Care must be taken to accurately compensate for
trapped atmosphere,atmospheric blank, with each analysed standard.If the
calibration curve is constructed using more than one sample type,the atmospheric
blank must be determined for each standard.This can be accomplished by analyzing
the same sample mass encapsulated and in an open container dissolving in water,or
palletizing the sample.The difference in the results is the atmospheric blank

The area under the peak is calculated and stored as a raw area,Ar.The current
blank area,Ab, is subtracted from the raw area,Ar, of the standard to yield the
area,A.
A=Ar-Ab.

The area A,is adjusted for instrument drift by multiplying by the drift factor.Each
time a calibration is performed the drift factor is reset to 1.0.The units of the
area,A ,are then adjusted to reflect absolute amount of analyte by multiplying by
the sensitivity factor.

Aadj =A*sensitivity factor*drift factor

The resultant adjusted area , Aadj ,of the standards are plotted against the known
grams analyte*100 of the analysed standards.The bestfit line,linear,quadratic or
cubic is determined and taken as the calibration curve for the method.The default
calibration curve has slope of 1 and travels through the origin.
In general, the line that is to be selected is the line that yields the lowest RMS
error.However,if none of the calibration stds. are very low in analyte
concentration,then linear fixed at origin should be selected.This should only be done
if the samples of unknown analyte concentration do not fall in the range of very low
analyte concentration.
If however, the samples of unknown concentration mostly falls into the very low
analyte concentration range,the 1/certified weighting should be selected.This type of
weighting helps off set a natural bias to higher concentration stds. during the least
squares fitting process.

Aadj is now taken through the calibration curve to yield grams analyte*100

grams analyte*100 = adjusted area*slope+intercept

This is then generally converted to the % to be reported.

%analyte = ( grams analyte*100 / sample mass )- atmospheric blank

The instrument is now ready to give accurate results over the caliubrated range for
each calibrated cell.

Calibration curve types:

3 types of curves:linear,quadratic and cubic
2 types of intercepts:fixed at origin and determined by the regression.
These curves and intercepts are used to create the best calibration for a selected
group of samples.
To establish the appropriate calibration curve for each method ,perform a series of
analysis using calibration standards at various concentration levels.(eg:
50,100,150,200ppm etc depending on sample and element concentration).Perform 3
to 5 for each mass.The plot that appears on the calibration screen indicates the
measured milligrams of element in relation to the theoretical (or ideal) milligrams of
the element for each mass.

*Linear calibration:
Analyte=(b)(area)+a
where,
b is software calculated coefficientthat dictates the slope of the line and a is the
intercept.All points used for calibration should rest close to or on this line.

*Quadratic calibration:

Analyte=(c)(area)^2+(b)(area)+a

where,
b is software calculated coefficientthat dictates the slope of the line and a is the
intercept.All points used for calibration should rest close to or on this line.c is
software calculated coefficient that fine tunes the slope of the line, allowing it to
curve and provide a better fit for the chosen standards.

*Cubic calibration:

Analyte=(d)(area)^3+(c)(area)^2+(b)(area)+a
where,
d is is also software calculated coefficient that further fine tunes the slope of the
line,allowing it to curve in two different directions and provide abetter fit for the
chosen standards.