U.S. patent number 3,609,324 [Application Number 04/796,782] was granted by the patent office on 1971-09-28 for method and apparatus for measuring the purity ratio of intermediate products in sugar manufacture.
This patent grant is currently assigned to Carl Zeiss-Stiftung. Invention is credited to Horst Loffler, Meinrad Machler.
United States Patent |
3,609,324 |
Machler , et al. |
September 28, 1971 |
METHOD AND APPARATUS FOR MEASURING THE PURITY RATIO OF INTERMEDIATE
PRODUCTS IN SUGAR MANUFACTURE
Abstract
The proportion of sucrose in the whole of the dissolved
substances of intermediate products in sugar manufacture is
measured by: measuring the refractive index n of a sample of an
intermediate product, measuring the polarimetric rotation .alpha.
of the same sample and then combining these measurements in the
relationship .alpha. /n- n.sub.o to produce a "purity quotient"
(n.sub.o being the refractive index of pure water.) The numerical
value of this quotient varies with the temperature of the sample.
Therefore the temperature of the sample is maintained constant
within a certain range and an additional temperature correction is
effected. In a preferred form of apparatus for performing the
measuring method, the result of the calculation of the quotient is
reproduced in both analog and digital form respectively for
controlling automatic process control computers and for actuating a
device for indicating the measurements in visible form.
Inventors: |
Machler; Meinrad (Ellwangen,
DT), Loffler; Horst (Oberkochen, DT) |
Assignee: |
Carl Zeiss-Stiftung (Heidenheim
on Brenz, Wurrtemberg, DT)
|
Family
ID: |
5688057 |
Appl.
No.: |
04/796,782 |
Filed: |
February 5, 1969 |
Foreign Application Priority Data
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Feb 10, 1968 [DT] |
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P 16 98 292.6 |
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Current U.S.
Class: |
702/25; 436/55;
356/73; 422/50 |
Current CPC
Class: |
G01N
33/143 (20130101); Y10T 436/12 (20150115) |
Current International
Class: |
G01N
33/02 (20060101); G01N 33/14 (20060101); G01n
021/00 (); G01n 021/40 () |
Field of
Search: |
;235/151.35,151.12
;356/114,115,116 |
References Cited
[Referenced By]
U.S. Patent Documents
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3468607 |
September 1969 |
Sloane et al. |
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Foreign Patent Documents
Primary Examiner: Botz; Eugene G.
Claims
What is claimed is:
1. A method for measuring the proportion of sucrose in the total of
dissolved substances of intermediate products in sugar manufacture
comprising measuring refractometrically the refractive index n of a
sample solution of an intermediate product which is to be measured,
measuring polarimetrically the angle of rotation .alpha. of said
sample, and combining these measurements and the known refractive
index n.sub.o of pure water in the quotient
.alpha./(n-n.sub.o).
2. The method of claim 1 in which the difference between the
refractive indices n and n.sub.o is directly measured
refractometrically and in which this difference and the
polarimetrically measured angle of rotation .alpha. are in the form
of electric quantities, and in which the respective electric
quantities are combined electrically to produce an electric signal
representing the quotient .alpha./(n-n.sub.o).
3. The method of claim 2 in which the electric signal representing
said quotient is produced in analog and in digital form, whereby
said analog form is available for the application to control the
operation of a process control computer and said digital form is
available for operating an indicating device for reproducing said
quotient in visible form.
4. The method of claim 1 in which said sample is diluted before
measurement.
5. The method of claim 1 in which said quotient .alpha./(n-n.sub.o)
is produced in the form of an electric quantity and in which said
quotient is electrically multiplied by a factor F in order to
relate said quotient to the conventional purity quotient
(Pol/Brix).sup.. 100.
6. The method of claim 1 in which the difference between the
refractive indices n and n.sub.o is directly measured
refractometrically and in which this difference and the
polarimetrically measured angle of rotation .alpha. of the sample
solution are reproduced in the form of electric quantities, and in
which the respective electric quantities electrically produce an
electric signal representing the quotient .alpha./(n-n.sub.o),
further comprising measuring the temperature of the sample
solution, reproducing electrically a temperature factor, and
multiplying said quotient by said factor electrically in order to
correct the influence of the temperature of the sample solution on
said quotient.
7. The method of claim 2, in which the electrical signal
representing said quotient is produced in analog form.
8. The method of claim 2, in which the electrical signal
representing said quotient is produced in digital form.
9. The method of claim 1, in which the difference between the
refractive indices n and n.sub.o is measured refractometrically,
and in which said combining step combines said last-mentioned
measurement and said polametric measurement.
10. The method of claim 9, in which a temperature measurement is
made on the sample solution, and in which said combining step
combines said temperature measurement with said quotient to correct
the influence of the temperature of the sample solution on said
quotient.
11. The method of claim 1, in which said measurements are made
concurrently.
12. The method of claim 1, in which the sample solution is
continuously flowing and in which said measurements are
continuously made on separate like divisions of the sample flow,
the first-mentioned measurement being a refractometric measurement
of the difference between the refractive indices n and n.sub.o in
one of said flow divisions, the second-mentioned measurement being
made in another of said flow divisions.
13. The method of claim 1, in which said measurements are made at
the same temperature.
14. Apparatus for measuring the proportion of sucrose in the total
of dissolved substances in liquid intermediate products in sugar
manufacture, comprising a mixing device, first conduit means
connected to said device for supplying to said device a sample flow
of one such intermediate product having an unknown sucrose content,
second conduit means connected to said device for supplying a flow
of pure water to said device, refractometric means including a
measuring cell connected to the output of said device and
accommodating mixed liquid discharge thereby, polarimetric means
including a measuring cell connected to the output of said device
and accommodating mixed liquid discharged thereby, said
refractometric means producing an electrical signal output
proportional to the difference between the refractive index n of
the sample liquid and the refractive index n.sub.o of pure water,
said polarimetric means producing an electrical signal output
proportional to the angle of rotation .alpha. of the sample liquid,
and quotient-calculating means electrically responsive to said
signal outputs and producing an output indicative of the quotient
.alpha./(n-n.sub.o).
15. Apparatus according to claim 14, in which said cells have
separate and like connections to the output of said mixing device,
whereby they are simultaneously subjected to like but divided flows
of diluted sample liquid.
16. Apparatus according to claim 15, in which heat-responsive means
producing an electrical signal output is positioned at the output
of said mixing device, said heat-responsive electrical signal
output being connected in temperature-correcting relation to said
quotient-calculating means.
17. Apparatus according to claim 14, in which said conduits each
include a pump, said pumps having a common drive.
Description
The present invention relates to a method and apparatus for the
automatic continuous measurement of the purity ratio of
intermediate products in sugar manufacturing.
In the manufacture of sugar, crude juice is first obtained from the
raw material. In the case of sugar beets this is done by extraction
from washed and chipped beets with hot water. In the case of
sugarcane, the juice is squeezed out by roll crushers.
The crude juice thus obtained is purified-- for example, by means
of the lime-carbon dioxide method-- to remove a major portion of
the nonsugar substances. The resulting thin juice is evaporated in
an evaporator station to a thick juice, which contains about 60 to
65 percent dry substance.
The thick juice flows into the sugarhouse where it is boiled to
massecuite, which is a thick mixture of light crystals and dark
syrup. The massecuite is cooled in mash troughs and then
centrifuged. The mother syrup which is separated by this step is
called runoff.
After this separation, and particularly in the production of white
sugar, a washing medium (for example, water) is sprayed on the
sugar layer in the centrifuge to remove the syrup particles
adhering to the sugar crystals. In this process sugar is also
dissolved and the wash syrup resulting from a repeated
centrifugation has a high sugar content. The centrifuged wash syrup
is thereafter further concentrated by boiling.
The runoff, or mother syrup from the boiled and centrifuged
massecuite, is again boiled, cooled, centrifuged, and washed in a
successive stage.
Depending on the type of factory (raw sugar or white sugar
factory), the crystallization and the separation of the sugar are
effected in at least two or three successive stages. Runoffs and
wash syrups are recycled through the various boiling and
centrifuging stages in various ways until molasses, which is a
runoff that can no longer be crystallized, is obtained.
For an economical manufacture of sugar it is important to keep the
power consumption in the various boiling stages at a minimum and to
control the process so that molasses with a low sucrose content is
obtained. To this end it is necessary to measure the various
intermediate products (runoffs, wash syrups, and charges of the
various boiling stages), giving particular attention to the
proportion of pure sucrose in the total of nonhydrous substances.
This proportion in percentages is indicated by the so-called purity
quotient, which is frequently called the "quotient" for short.
The purity quotient is usually written in the form (Pol/Brix).sup..
100, where Pol denotes the sucrose concentration in degrees S,
determined polarimetrically according to the ICUMSA method
(International Commission for Uniform Methods of Sugar Analysis).
Brix denotes the refractometrically determined total dry substance
content in degrees Brix according to the international sugar scale
in the version of 1936, which is still used today.
Since the knowledge of the purity quotient is of paramount
importance for the processing of the intermediate products, the
determinations of the quotient represent a major part of the work
done in the laboratory of a sugar factory.
The expenditure in time and energy for the determination of the
quotient is relatively great, because the material to be measured
requires certain preparations. Since the quantities degrees S and
degrees Brix are not equidimensional, the temperature for the
measurement is fixed, according to definition, at 20.degree. C. For
measuring the quantity degrees Brix, the sample material is diluted
in the proportion 1:1 before measurement, then measured at
20.degree. C., and the result is then multiplied by the factor 2.
For measuring the quantity degrees S, 26 grams of the sample
material are diluted to make 100 ml. of solution. The nonsugar
substances contained in the latter solution are then precipitated
with lead acetate, then the solution is filtered and measured
polarimetrically at 20.degree. C.
Due to the preparatory operations the time required for a quotient
determination is about 20 minutes. Moreover, this conventional
method of quotient determination cannot be fully automated.
Efficient sugar production requires that the proportion of sucrose
in the total of nonhydrous substances-- that is, the purity
quotient-- in various intermediate products be measured as rapidly,
accurately and automatically as possible. But, improvement in this
regard is not possible using the conventional method of quotient
determination.
It is, therefore, an important object of this invention to provide
an improved method for measuring the purity ratio of the
intermediate products in the sugar manufacture, and to provide such
a method which is rapid, accurate and which is adapted to being
performed automatically.
According to the invention, the angle of rotation .alpha. of a
sample liquid is determined polarimetrically and the refractive
index n of the same sample liquid is determined refractometrically.
From these quantities, and from the known refractive index n.sub.o
of pure water, is then formed the quotient .alpha. /(n- n.sub.0 )
which defines the proportion of sucrose in the total of nonhydrous
substances.
The invention will now be described in detail with reference to the
accompanying drawings in which:
FIG. 1 is a graph in which the specific rotations .alpha. arc
plotted against the refractive indices n for four samples, each
having a different sucrose content, and
FIG. 2 is a schematic diagram of apparatus for measuring the purity
quotient in accordance with the invention.
As can be gathered from the graph FIG. 1 every sample yields a
straight line whose slope is characteristic of the purity of the
sample. All these lines start from the value n.sub.o as the
specific rotation .alpha. is zero at sucrose concentration zero,
while the refractive index n has the value n.sub.0 , n.sub.o being
the refractive index of pure water. This means that the purity can,
indeed, be described by the new expression .alpha.
/(n-n.sub.o).
The expression .alpha. /(n-n.sub.o) is free of
concentration-dependent coefficients of measure and is, therefore,
independent of the concentration of the sample. .alpha., which is
the function of the difference between two refractive indices,
namely the indices of the levorotatory and of the dextrorotatory
polarized light, thus has a different temperature dependence than
the pure refractive index n for nonpolarized light. It is,
therefore, necessary to relate the determination of the quotient
.alpha. /n-n.sub.o) to a constant temperature. This temperature
can, however, be selected at random, in contrast to the
conventional quotient determination which is only exact at
20.degree. C. In the case of temperature deviations from the
selected reference value, it is possible to make the correction by
simple mathematics, or by an automatic correction device in the
measuring apparatus.
Since the sample for the measurement of the quotient .alpha.
/(n-n.sub.o) does not require special preparation, and since the
values for .alpha. and n can be measured rapidly and with great
accuracy, the quotient can likewise be measured rapidly and with
great accuracy. The method of this invention thus contributes to
the efficiency of the conventional discontinuous
sugar-manufacturing process and in addition provides the basis for
an automated, or partly automated continuous manufacturing
method.
The quotient .alpha. /(n-n.sub.o) can be related in a simple manner
to the purity quotient Pol/Brix.sup.. 100 ; it is only necessary to
multiply the quotient .alpha. /(n-n.sub.o) by a factor F, which
takes into account the polarimetric path length, the measuring
temperature, and other quantities. The factor F can be determined
mathematically, but empirical determination by measuring a pure
sucrose solution, which has according to definition a purity
quotient of 100 is preferable. The information content is however,
not increased by relating the quotient .alpha./(n-n.sub.0)to the
purity quotient (Pol/Brix.sup.. 100. The information gain
apparently achieved by said relating is the possibility to make a
direct comparison with the values obtained by the conventional
method. This is not necessary for factory control.
In a preferred manner of using the method of this invention the
quotient .alpha. /(n-n.sub.o) is obtained by translating the angle
of rotation .alpha. and the refractive index n into electric
quantities and forming the quotient .alpha./Cn-.sub.0) electrically
from these quantities and from a corresponding input value for
n.sub.0 . Also, the quotient thus determined can be multiplied
electrically by the proportionality factor F.
The quotient .alpha. /(n-n.sub.o) can be used, before or after
multiplication by the factor F, for the automatic regulation or
control of the sugar-manufacturing process. It is advantageous to
produce said quotient in both analog and digital form, the analog
form being particularly suited to being fed directly into a process
computer for automatic operation control. The digital form is
particularly suited for actuating an indicating device for
reproducing the quotient in visible form.
It has been found expedient to dilute the sample liquid before the
measurement in order to avoid crystallization, and this can be
accomplished automatically.
The measurement of the angle of rotation .alpha. and of the
refractive index n can be effected either simultaneously by
parallel flow of the sample to be measured or successively by
connecting the measuring points in series.
In the automatic formation of the quotient .alpha. /(n-n.sub.o) it
is advantageous to measure the temperature on the material
constantly and to automatically correct for the influence of the
temperature on the quantities .alpha., n and n.sub.0 .
Referring now to FIG. 2, magnetic valves 1, 2, 3, 4, and 5 are
arranged respectively in five feedlines for different samples.
These valves are actuated selectively according to a preset program
which is controlled, for example, by a process computer. The
various feedlines for the samples open into a common conduit 6,
having a pump 7 therein, and connected to a mixing device 11. A
pure solvent, such as water, is also supplied to the mixing device
11 through another conduit 8 having a pump 9 therein. The pumps 7
and 9 are driven by a common motor 10 so that the same amount of
solvent is always added to a given amount of sample liquid. The
mixing device 11 is driven by the motor 12 and may be designed as a
circulating pump.
From the device 11 suitable conduits 35, 13 at the same time carry
some of the diluted sample liquid into a measuring cell of a
polarimeter 14 and the rest into the measuring cell of a
refractometer 15. The temperature of the conduits 35, 13 and of
said measuring cells is controlled, so that there is no temperature
drop between the measuring points.
The polarimeter 14 is so constructed that it shows the measured
value of the angle of rotation .alpha. in digital form at 16. At
the same time it produces the measured value in its analog form as
an electric voltage tapped by a precision potentiometer 17.
The refractometer 15 measures the deviation of the refractive index
n of the sample liquid from the refractive index n.sub.o of pure
water. It produces the measured value n-n.sub.o in its analog form
as an electric voltage tapped by a precision potentiometer 18.
The electric voltages produced by the measuring instruments 14, 15
are processed in a calculating device 19 which calculates the
quotient .alpha./Cn-n.sub.o electrically. The device 19 contains
resistances 20, 21 connecting one end of the output network (viz
resistor 26) in series with one end of the potentiometer 17; device
19 also includes a resistance 22 connecting the other end of the
output network (viz resistor 29) in series with one end of the
potentiometer 18. The tap of the potentiometer 17 is connected to
resistance 23 while the tap of potentiometer 18 is connected to
resistance 24. Resistances 23 and 24 are both connected to an
amplifier 25 the amplification factor of which may be one, and the
amplifier output is connected to the resistor 29 end of the output
network. The midconnection of the output network is grounded, as
are also the remaining ends of the potentiometers 17, 18. Values of
the quotient .alpha./(n-n.sub.o of less than 50 do not occur in
practice, so that it is reasonable to suppress them for the
recording. By means of the resistances 26, 27, 28, 29 this
suppression is effected so that the output voltage at 30 is zero
for the quotient 50 and only quotients of more than 50 produce an
electrical voltage at the output 30.
By means of the resistances 26, 27, 28, 29 it is also possible to
approximate the quotient .alpha./(n-n.sub.o by means of a
correction factor F to the value of the quotient (Pol/brix).sup..
100 conventionally determined. The factor F may be adjusted by
adjusting the resistances 26 and 29.
It is another object of the calculating device 19 to compensate for
the temperature coefficient of the quotient. For this purpose a
thermistor 31 is connected into the conduit leading the sample
liquid from the device 11 to the measuring instruments 14, 15. This
thermistor is connected in series to the resistances 20, 32 which
are arranged within the calculating device 19. By means of
thermistor 31 and resistances 20, 32 a temperature coefficient is
produced which corrects automatically the influence of the
temperature of the sample liquid on the quotient
.alpha./(n-n.sub.o).
For automatic regulation or control of the sugar-manufacturing
process an appropriate process control computer (not shown) would
have its input connected to the output 30 of the calculating unit
19.
In the embodiment illustrated, an analog-digital converter 33 is
connected between the calculating unit 19 and an indicating device
34 which shows in digital form the quotient
calculated in the unit 19. Alternatively, the analog digital
converter 33 could be omitted and the indicating device 34 could be
replaced by an indicating device adapted to show the quotient in
analog form.
* * * * *