PROCEDURE FOR THE AUTOMATIC CONTROL OF A MANUFACTURER OF CHROMATOGRAPHI PROCESS

The invention relates to a method for automatically controlling an industrial process chromatographic, wherein at least two substances, e.g. glucose and fructose, are fractionated chromatographically arise and with for the collection of sufficient purity, while at least one further group must be re-supplied to the process, and wherein the polarization angle and the concentration of the resulting fractions measured constantly in the process, the registered measured values to a program-controlled computer automatically supplied and the groups

AufspürnngReinheitswerte

for the groups are distributed in accordance with the predetermined measured, wherein the flow rate and the temperature of the additionally constantly in the process and the instantaneous and/or the average purity of the resulting fractions, taking into account the flow rate and the temperature is calculated fractions. Zur fractionation or for separating two or three substances to chromatographic separation columns can in various ways be monitored by means of the method of measurement the separation of the various components, which are based on the physical and chemical properties of the components. Such properties are, for example, the density, the viscosity, the refractive index, the PH-value, the conductivity and

Polarisationserscheinungen

in optically active substances. Therefore, the separation efficiency depends from the selection of the flow rate and the amount and selectivity of the

Fraktionierungsprozesses

and concentration of the original solution for the

Destlllieraufsätze

ab. Inadequate separate fractions are supplied as we know, recycled to the process. Generally is required to be able to effective control of the separation process the measurement of the concentration of the complete substance and the concentrations of the components. The analysis of the components-concentrations depends on many factors, not least from the temperature guided.

Bereehnungen

are necessary to determine the components with sufficient accuracy far-reaching, since the measured properties are linear functions of, for example, the concentration or the temperature on the part. GB-PS No 1 in the, 095, 210 is described, such as the concentrations of the various components of glucose-

Fruktese

in aqueous solution (of fish

opticalrotation

) and of the refractive index by means of the are determined

Polarisierungswinkels

. But it is difficult, a reliable method for the direct automatic control with any of the known methods to obtain, if the measured characteristics caused by concentration and temperature are under to relax after. In addition have, for example, in glucose and fructose (the

Polarisierungswinkel

)

Polarimeterablesungen

the opposite sign. As a result, the concentration of fructose and/or the glucose in the fractionated sugar solution can not individually by one of the mentioned measurements are expressed, but what is strictly necessary for controlling the

Fraktionierungsprozesses

. The invention has made the problem is, to create a process, by means of which an industrial of chromatographic process, wherein at least two substances are fractionated chromatographically arise and with for the collection of sufficient purity, while at least one further substance must be re-supplied to the process is automatically controllable in such a way that the aforesaid difficulties properly be remedied. This problem is solved according to the invention thereby that in a number of steps is outlined a

Reinheitskurve

, the outlined

ReinheitskurveReinheitswerten

be compared with the measured points of the and the measured value is selected as a basis for further

Vorzeichnung

" if it lies in the vicinity of the corresponding mapped out point, and the drawn-out point is selected in accordance with, if the measured value significantly deviates from said marked out point. A detailed explanation of the invention follows from the following description with reference to the drawings; 1 a block diagram of an automatically controlled industrial Fig. it show

ehromatographischen

process according to the invention, 2 a schematic representation of a preferred embodiment of a device for automatically Fig. control the process from Fig. 1, Fig 3A .3A -3D the relationship between the

Polarisierungswinkel

, and the purity of the fructose 3C 3B

Glukoseund

fructose-concentrations the and the consequent

Schließprogramm

3A 3D for the distributing valves in accordance with the curves of opening and of, 3C 3B and, an alignment chart for representing the effect of the temperature on the 4 Fig. determination of fructose, and Fig. 5 to 8 flow diagrams of computer programs, which for calculating the unit and overturn of said groups, the

Glukosefraktion

,

Fruktosefraktion

Group and the are used the be recirculated. The 1 as an example is represented in Fig.

Invertzuckerlösung

by a controlled industrial chromatographic separation process according to the invention a 10----fed--12-a valve feed line-. The actuation of the valve is controlled by an associated valve control -12-----13--2 under control of the digital computer control system of Fig., wherein the latter is to be explained later. 13a and 13b has two output terminals----

Ventüsteuerung

This, to the digital-to-input -2 are connected and the control of the system and "A" from Fig. "off"-positions of the valve--12--Show. A input terminal--13c--the valve control is connected to the output control of the system from Fig. 2. In accordance with the signal at the input terminal 13-13c-----opens or closes the valve control----12--these

Ventüsteuerung

the valve, wherein the output terminals 13a and 13b----deliver signals, which reflect the state of the valve--12--. In

Ventü

--12--flows through the the open state in a 14--

lnvertzuckerlösungSpeisetank

--the. This

Speisetank

--14-15 and 16-----two Level measuring device has, which are coupled with the 2

Digltal

-input-and by means of the system of controlling the Fig. the actuation of the valve control--13--control 2 Fig.. If

InvertzuckerlösungSpeisetank

--14--in particular, the sum of the drops below a predetermined level, from the 16--states Level measuring device--, so this Level measuring device generates a signal, which brings the computer of the system from Fig. 2 thereto, automatically

VentüsteuerungVentü

--12----the 13--to open over the, so that new

InvertzuckerlösungSpeisetank

flow to the can. If

Speisetank

--14--on the other hand the solution rises over a predetermined level in the, 15--states by the Level measuring device--, so this generates a signal 15----Level measuring device, through which again

Ventüsteuerung

--13--the via the computer and the 12--Closing

Ventü

--. From

Speisetanks

--14--the discharge opening of the valve 18----a conduit leads to a, which is controlled by an associated valve control----19. Like the valve control--13----18--two output terminals has the valve control 19a and 19b----, "A" and "off" indicating the position of the valve 18-----, as well as an input terminal 19c----, which is connected with the digital-to-Computers-control according to Fig. 2. Depending on the input terminal 19c -19-------the valve control signal fed, the 19------18 opens

Vcntilsteuerung

--or it closes the valve. This valve--18--the is-

Speisetank

Through 14-----20--connected with an inlet opening a separation column. This separation column has a second inlet conduit--22--, through which when the valve is closed--18-24--water is fed via a valve---. This valve--24-25--associated with-a valve control is--ES, 25a and 25b which has two

Ausgangsklcmmen

----, "A" and "off" indicating the position of the valve 24-----, as well as an input terminal 25o----, which is coupled with the digital-to-Computers-control according to Fig. 2. 24----18 and the valves actuated computer control The alternately in accordance with a program, whereby a selected amount of

Invertzuckerlösung

first on the valve 18--20------during a certain period of the separating column is fed, whereupon during a second time period the distillation column via the valve 20------24--water is supplied. In this separation column is separated chromatographically

Invertzuckerlösung

20----glucose and fructose in the. In

Invertzuckerlösung

be fed alternately from above and the process to the surface of the water in the distillation column or the column arranged resin layer. This

Destillier4S

A cap--20--or the column may be constructed in generally known construction

igendwle

appropriate, so that it needs to be not described in detail here. Such a conventional separation column is, for example, in the 1 GB-PS No, 095, 210 described. In of the separating column 20-28-is-----a-above the resin layer disposed Level measuring device, which-the H he or the level of the dilute

InvertzuckerlösungDestillieraufsatzes

monitored within the. Depending on the level of the solution within the

Pegelaufsatzes

, as drawn up by this Level measuring device--28--states, via the valves 18 and 24 is alternately

Invertzuckerlösung

and water----20----of the separating column the supply of water is fed or

Invertzuckerlösung

and switched off. In of the separating column 20----be mentioned, as has already been, glucose and fructose, as a result, glucose

Destillieraufsatzes

be obtained separately and at the bottom of the, a glucose-fructose-mixture, fructose and almost pure water. The regularly resulting solutions are supplied via a polarimeter--30--, a concentration meter adapted to--34--, and a temperature gauge 36--a forward power Speedometer--38----40--three distribution valves, 42 and 44--. The Polarimeter--30--, for example the Type

Bendix

143 C, constantly

Polarisierungswinkel

(of fish

opticalrotation

) and measures the signal corresponding to an analog-to-digital converter provides this angle a, which forms an integral part of the control according to Fig. 2. The concentration meter adapted to----34, for example the Type Va! mer

Dens

Air, 46 via a le pressure-stream-is-with the analog-to-digital converter---2 connected from Fig. converter of the system. For example, the Minneapolis Honeywell Co converter provides pressure-stream-Such. The Flow-Speedometer--36--, for example the Type Foxboro D/P transmitter -13A--, provides a pressure signal to one converter--48--constantly, which converts this signal to the pressure signal and the analog-to-digital converter in a

Stromslgnal

Fig. of the system consisting of 2. The temperature gauge 38----

schließüch

,

Rosemund

PT 100, for example, the type, constantly supplies a signal, indicating the temperatures of the solutions exiting from the separation column--20--, and this leads to the analog-to-digital converter of the system from Fig. 2. The temperature measurement may possibly be unnecessary, leaving the separation column--20--if the solutions have the same temperature. If these temperatures, however, vary, the measurement must be carried out, since the temperature variations

Polarhneterablesungen

, as will be explained below, influence.

Verteilerventfle

--However, the operation of the 40, 42 and 44--is through associated

Ventflsteuerungen

-50, 52 and 54--under the control of the computer control 2 represented in Fig., will be controlled as below to describe,. This valve controls have output terminals--50a, 50b; 52a, 52b; 54a0 54b--, "A" and "off"-indicating respectively the positions of the valves--40, 42 and 44--2 are connected with the digital-to-computer control of Fig. and. The valve controls have also input terminals--50c, 52c and 54c--, which are connected with the system 2 represented in Fig.. Depending on, which performs

Programmtefl

the computer 2 from Fig., receives at least one of the valve controls--50, 52 or 54--a trigger signal, whereby its associated valve is opened. In the valves--40, 42 and 44--glucose or a glucose-fructose-(G shall enter into force) (P) or mixture. Fructose (F) so from. The emerging solutions are distributed in various containers, i.e. each include a container for one of the three different solutions, so as to be further treated possibly. As Fig. 2 shows, the apparatus 1 schematically represented for the automatic control of the process has a central digital

datenverarbeitendes

Apparatus in Fig. 60----, for example, the Nokia Type

PPC

6520,2, which via a cable--61------u with an output-controller, 6537

PPU

the Type Nokia for example ss, and via a cable 63----64----with a analog-to-digital converter, for example, the Nokia Type 6533 PPD is connected. The cable 63----60----connects the data processing apparatus also with a digital input controller--u--, for example, the Nokia Type

PPU

6531, and 68----with a Manipulation desk, for example the Type

NoklaPPU

6542,1. The cable connects with the output control device--62--further comprises Manipulation desk--68--. The Finally 2 illustrated apparatus has in Fig. 70----a telex, 71 and 72 via the cables--60------is connected with the data processing apparatus. As the inscriptions at the output terminals of the output-control--62--show, this provides--62--under the program control of the computer output control signals, which control the actuation of the valves--12, 18, 24, 40, 42 and 44--. The

PolarimeterablesungenPolarisierungswinkel

indicating the, the

Konzentrationsablesungen

, the measured values for the flow rate and the temperature measurement values from the separation column--20--emerging solutions are fed to the analog-to-digital converter--64----60--digits the central data processing apparatus and as fed. As already mentioned, the temperature measurement is not required, when the temperature of the solution leaving from the separation column remains constant. However, where a temperature variation occurs, the action must be taken into account by this fluctuation

Polarimeterablesung

a correction program runs on the is based on the alignment chart, 4 represented in Fig.

welche5

. The positions of the feed valves--12, 18 and 24--indicating signals, i.e. the signals--13a, 13b; 19a, 19b; 25a and 25b------42 are supplied to the digital input control within a cable 66----40--

8teilungen

the distributing valves and the, 42 and 44--signals indicating, d.h.--50a, 50b; 52a, 52b; 54a and 54b within a cable--74----are fed to the corresponding input terminals of the control--66--. Finally, the signals are, 14----

Speisetanks

Show

Pegelhöhe

which the within the 15 and 16 and are supplied by the

Pegelanzeigern

------28--is and which, from the sent to the separation column--2 Level measuring device fl

geieferte

signal within a cable 76--------66-

Elngangsklemmen

the digital input control three other-. The output-control--62--the corresponding decoded instructions, which are received from the digital data processing apparatus--60--to be sent to the input terminals--13c, 19c and 25c; 50c, 52c and 54c--the controls for the valves--12, 18, 24, 40, 42 and 44--control signals. .1o Building, the methods of operation and the connection of the individual components of the system are generally usual, and therefore need not here from Fig. 2 to be described in detail. The invention is based not on the connection of such components to each other also, but rather in the measurement of the

Polarisatiouswinkels

, the concentration, the flow rate and the temperature of the solutions and exiting from the separation column--AD----60 in the feed of the measured values in the data processing apparatus--. As be described further below in detail will be, this data processing apparatus controls the instantaneous and/or average purity and calculated upon reaching predetermined

Reinheitswerte

the distribution of the various groups according to a predetermined programme (F, P and G). Fig .3A

Polarisationswinkels

A as a function of time shows the change of the. Fig .3B

Glukoseund

.3C

Fruktosekonzentrationen

as a function of time and Fig shows the shows, as the purity of the fructose

Destillleraufsatz

--20--in the solution leaving from the varies as a function of time. Fig .3D (1) di shows optimum

öffnungsundSchlleßzelt

of the 40----glucose-distributor valve, Fig .3D (2) and 3D (3) the optimal

öffnungsund

closing times (P) or 42----show said recirculation valve (F)-44----fructose of the distributor valve. Fig .3D (4) shows the state of rest in the separation process, when all are closed

Verteflerventfle

. The alignment chart 4 shows the temperature to the determination of the effect of Fig.

Fruktosereinheit

. It A represents the angle of rotation on a 2.5 mm with a length of

Lichtbahn

, measured at the

Quecksilberlinie

, the concentration (g/100 valley) carbon atoms. The fructose-concentration in the sugar solution depends on the concentration and

Polarimeterablesung

and the (at + 60 °C) occurs from the following empirical formula: F = 62.85C + 5 x 10-3 February 2010

sCs

"

sC2

+ 2 May 2010".-4.10aA 1.4325C + 4.37CZ.10-s + 10 where sC: F = the fructose concentration of the solution (= F-purity) in % of the drying material, carbon = (g/100 valley) concentration, A =

Polarisierungswinkel

(in angular degrees, as measured at a wavelength of 546 pm, length of the 2.5 mm

Lichtbahn

). A corresponding equation is also establish which codes for glucose purity. Since the temperature remains constant at a running process in industrial degree never completely, the

TemperaturkorrakturComputerpregramm

contains a. The recognisable by equation approach can be a linear form, which is suitable for process control (at + 60 °C): F = 43509-2734.2-This equation corresponds to the general shape: F = k-k 2 A the constants k1 and k2 of the measuring conditions such as temperature, wavelength of the light used in the alignment chart in the polarimeter

Lichtbahn

Fig. 4 and depend on the length of the.

Trennprogramms

is the control of the separating process, the distribution of the purpose of the separation column--20--emerging from the solution into three fractions--G, P and F--. The summary and calculation of necessary data for the reports can also be incorporated into the

Trennprogramm

. The process computer, i.e. the data processing hub--60--(Fig .2) distinguishes in sufficiently short intervals, for example every half minute, the concentration, the

Polarimeterablesung

, the temperature and the flow rate of the separating column on. It

Toleranzkontrolle

is a for measured values (wherein Checking that the measured values lie generally within the calibration curve), wherein inaccurate results of not be adopted. From the separation column--20--The distribution of the solution leaving the solution is determined on the basis the F-purity. The groups are glucose (G), the (P) and (F) fructose be recycled mixture. The limit values of the fractions shall mean the F-value and the concentration. For Determining the F-purity there are various methods. When utilizing the instantaneous F-value as an operating parameter for the transfer of glucose Running

zurück2uführenden

mixture and to be recirculated on the basis of the instantaneous mixture from the fructose F-values. Fructose and glucose is determined either by the between The limit F-value or the

Kon2entration

, as the case may be, which is achieved first of said predetermined values. Another method for controlling the separation process is the use of the average F-purity than distribution parameter. The desired average

Reinheitswerte

both for the fructose as for the glucose are added. During the distribution of calculated after each measurement is the average F-purity

Glukosefraktion

the F-purity. If the time the overturning (changeover) to be recycled in the approaches Group, the F increases-value (the purity of the glucose is being phased out) on is carried out until the set value is reached and the turning upside down. In the control system is also a set value for the instantaneous F-purity provided, so as to prevent passes contains that solution, too much fructose 2 which, in the purely fractional glucose. If the turning upside down of glucose in the mixture to be recycled is based on the instantaneous F-

Reinheitswert

, the glucose a smaller average F-purity as the adjusted has-Group average F-

Reinheitswert

. The Determination overturn of said using the average F-

Reinheitswerteszurückzuführendcn

mixture in fructose can not be carried out in the same way as a parameter, since the average purity of the fructose-Group only then is known, when the phase is completed and the mixture at the start of the phase in fructose the tilting to be recycled. Therefore, a set value for the instantaneous F-purity is provided in addition to the average F-purity. After F-Group calculated the computer 60--the average purity of the F-solution--and corrected if necessary the limit value, wherein the correction is carried out always in such a way that the average always remains at the set value purity of the fructose. The limit on a maximum allowed number and it is be recirculated has glucose-mixture an equal minimum permissible number for the fructose-mixture provided to be recycled, under which the computer cannot exceed the border should require, albeit the average F-purity this. £in serious mistake

Relnheitswert

may even be caused by a small error in the calculated, when the computer--60--the above-mentioned formulae used. If

VerteilungsgrenzenReinheitswerte

has been established only by the control of the, directly from the measured values were calculated, from the separation column--20--so the can from the computer--60--imprecise be distributed solutions expiring. To is programmed to prevent this calculated is received, the computer 60----so that he

Reinheitskurve

each new point of the, which, for example, at intervals of one minute, previously. The from the measured values is then compared to the predicted and the more precise value calculated point selected. The new value of the is precalculated

Reinheitskurve

from the computer, for example, specifying the four points of the curve are adopted in the foregoing and following formula used: X yi-

kX

2 No 342897 So that the curve of the actual curve due to projecting as close as possible can follow formula precalculated, the asymptotes have a slight displacement of, for example, with respect to the origin of said precomputed

Kuve

5%. This means that in practice, for example, derived from the pre-yielding 10596 or -5% is value. Percentages outside the range 0 to 100%, however, in the computer program are eliminated. Comparing

beriicksichtigt

predicted from the measured values of the dot by the calculated at this point the slope of the curve, the computer also. Bigger deviations between the measured and the predicted purity rather than at the portions of the curve are permitted at steep parts of the curve, which have only one

allmäh

]

inhe

pitch. lo The difficulty in the circumference with the fructose-glucose-border is therein that both the Po

arimeterabiesung

Registering measurement scales affixed at the extreme lower ends of the as the concentration measurements. Generally the percent error are the measurement scales affixed within these areas greater. Consequently, can have extremely large fluctuations of the measured values calculated

Reinheitswerte

the on either side of the actual value, and a single such an inaccurate control operation can cause extremely faulty bod value. Therefore the turning upside down is not based on a single point of the the Group

initliertReinheitskurve

or a concentration measurement, but it that will be made more, for example three, such measurements, certain to succeed for has been reached that of border. worth. Except the previously described security measures

Standardzeitdauer

a fraction is taken into account as a parameter and the for the distribution of the fraction. If the measured or calculated values state that is a fraction completed, and a new should be started, but that the measured time from the beginning of the group is shorter than the specified standard time, so no change will take place on the report-telex--70--rather than and (Fig .2) the error report is printed out. The Drain

chema

the computer programs for calculating the purity and overturn of said group, the calculation of glucose-Group, the calculation of the fraction and the calculation of the fructose-Group is recirculated into the Fig. 5 to 8 represented. In these flow diagrams indicated symbols have following meaning The: A C V T Q

GPORGPQRPFQRFGQRFGOR

£G P F 3s Q (MIN) ON

PolarisierungswinkelFGCR

C, -concentration, -flow rate, -temperature, -F-purity, Q = f (A, carbon, T)-

vorausbereehnete

purity, -glucose, -

zurüokzuführende

Group, -fructose, -average experimental value of G-purity, -Tilting Limit By Means Of Calculation, determined from the instantaneous purity G-P in the range. -

Kippffrenze

, determined from the instantaneous purity in the range P-F, -Tilting Limit By Means Of Calculation, determined from the instantaneous F-G purity in the range, -average experimental value of the purity of the F-Group, -Tilting Limit By Means Of Calculation, determined from the concentration in the range F-G, -minimum concentration during separation, -fixed

Standarddauer

a fraction, can take place before a tipping to the next group. Also the invention has been described with reference to a specific execution if such are above but a wide variety of modifications and changes possible For, as anyone skilled in the art familiar with some of them. Is, for example, the data processing device can be programmed in such a way--60--that it the amount of dry material in the groups

Ausgangsberichte

calculated and further comprises printing out the. The Apply on a large degree to the invention can be for the production control method, since any number of separation columns in multiple utilization thereof can be controlled by a computer. changes. All such modifications, and therefore also comprises 8 The invention locking 342897 No