Professional Documents
Culture Documents
Pardue,
Michael F. Burke,
and Jack R. Barnes
Purdue University
Lafayette, Indiana 47907
= cAT(k./k,
- 1)
(1)
With the weight percent of the solute being proportional to the percent area of the recorded peak, it is
now necessary to determine the area beneath each
component peak. Several graphical methods have
been suggested; however, the most accurate is that
described by Cremer and Muller (5), which shows the
area beneath a Gaussian (bell shaped) peak to be best
approximated by multiplying the peak height by the
width a t half height.
Volume 44, Number 7 7, November 1967
695
Figure 1.
Figure 2.
Direct Reading Integrator. A block diagram representmg the functions of the instrument is illustrated
in Figure 2. The signal resulting from a chromatographic peak is connected a t E;. and compensated for
detector response by the sensitivity compensator. The
signal is then integrated with respect to time and the
integrated signal for each peak is stored. After all
the peaks of a chromatogram have been processed in
this manner, the sum of all the stored integrals is
measured and adjusted until a reading of 1.000 is observed on the digital voltmeter (om). Each individual integral is then sequentially measured and the
digital voltmeter presents the data in the form of
weight percent for each component.
The circuit layout illustrated in Figure 3 contains
components which perform the functions described
below.
put in the input circuit so that the input current is proportional to the signal voltage. The output voltage is
then given by
DYM.
Figure 3.
SWI
SWZ
SWI
SWa
Single-pole-single-throw switch
Four.pole-six-position rotory switch
Four-pole-single-throw rotory switch
Normallv ooen wsh-bullon swibh
RI-R; 10K ten'turn poientiometer
Rs
1K 10% resirtor
1 OOK ten turn potentiometer
RD
C L - 6Mylor, 2/rf. ZOO-w.v.d.c. capacitors (Goodoll)
O.A. Heath Model EUW-IOA operational amplifier (Heath Co., Benton
Harbor, Michigan)
FOL Unit No. 1 of above system in the follower position
tector response so that the same weight of each material results in the storage of equal charges on the c a
pacitors. This function is performed by a bank of five
10-turn, 10-kilohm potentiometers (RI,
etc.) used in
the input to the integrator. These potentiometers are
switched, by a set of contacts on the resistor-capacitor
(RC) selector switch (SWJ into the integrator circuit
one a t a time to receive the integration signal arising
from the individual peaks.
Integration. The operational amplifier (O.A.) is one
section of a Heath Model Em-1OA operational amplifier system (Heath Co., Benton Harbor, Mich.)
stabilized with a Phibrick K2-P chopper stabilizer (8)
(Philbrick Researchers, Boston, Mass.). This ampliier is connected in the conventional integrator configuration (Fig. I), with capacitor in the feedback to
accumdate and store the integrated signal. After each
peak, the selector switch is set to a new RC combination
for integration of the signal for the next component.
It should be noted that each potentiometer is always
associated with the same capacitor. The capacitors
must be closely matched in capacitance value and must
be made with very low-leakage dielectric. Those used
in this work are 10% tolerance Mylar, 2-pf 200-wvdc
(Goodall) matched to within +0.5% by smaller parallel
capacitors.
When the INT-READ switch (ST3) is placed in the
READ position, a 1K resistor (Re) is placed in the feedback loop of the amplifier to prevent i t from limiting.
Cmnputation. The integrals are summed by connecting the capacitors in series a t the input of amplifier
No. 1 in the follower configuration. The high input
impedance of the follower prevents drainage of charge
from the capacitors during readout. The output
from the follower is sampled by a ten turn, 100 kilohm
potentiometer. This potentiometer is adjusted to divide the output giving a reading of 1.000 v on the digital
voltmeter representing 100.0%. Leaving the potentiometer a t this setting, each capacitor is switched individually into the input to the follower and the output voltage, representing percent of that component,istabulated.
Digital Readout. A DigiTec Model 201 (United
Systems Corp., Dayton, Ohio) digital voltmeter with a
2.000-volt full-scale range is used to convert the analog data into digital data.
Procedure
Determination of Relative Response Factors
697
Table 1.
Disc
Dinct
Reading Int.
Heptane
Octane
Decane
0.92 i 0.02
0.96 f 0.02
1.000
0.910 i 0.015
0.949 10.010
1.I100
Table 2.
Actual
D/,
.
Heptane
Octane
Decane
32.0
33.6
34.4
Direct
Readine Int.
Disc
Manual
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