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Claims  |
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We claim:
1. Process for the determination of grain size distribution of a suspension
of grains in a liquor, where suspended grains of less than 1 micron in
size are made to settle in a settling tank using optical signals obtained
during the settling of the suspension in the settling tank, comprising the
steps of:
circulating the suspension through the settling tank to form a homogeneous
distribution of suspended grains therethrough;
terminating the circulation;
measuring the optical density of the suspension, repeatedly in situ, with a
plurality of light detection means positioned in at least three fixed,
increasingly spaced-apart places along the length of the settling tank,
opposite an equal plurality of similarly spaced-apart light sources; and
determining, from the optical density measurements obtained, the most
probable size of the grains in suspension by means of equalizing
calculations.
2. Process according to claim 1, comprising the further steps of:
measuring the optical density at at least three places at time intervals
ranging from about 0.001 to about 1.0 seconds; and
repeating the measurements for a period of time ranging from about 30 to
about 300 seconds.
3. Process according to claim 2, comprising the further steps of:
adding a standard solution of as dispersing agent to the suspension during
circulation, to adjust the optical density to a value of between 0.5 to
1.0.
4. Process according to claim 3, comprising the further step of:
regulating the temperature of the suspension in the settling tank (1) not
to exceed ambient temperature by more than 2.degree.-10.degree. C.
5. Process according to claim 4, comprising the further steps of:
initially circulating a plain standard solution through the settling tank
(1), prior to circulating the suspension of grains to be measured; and
measuring the the optical density of the standard solution and the dark
current of each measuring device, in at least three places in the settling
tank (1), to determine an initial optical density corresponding to a value
of maximum masking for each measuring device.
6. Process according claim 5, wherein the step of determining the initial
optical density corresponding to the maximum masking, comprises the steps
of:
forming the reciprocal value of the optical density;
multiplying the reciprocal values so formed by the least initial optical
density value measured to obtain correction factors; and
correcting the subsequently measured optical density values the suspended
grains by the correction factors thus obtained.
7. A system for the determination of grain size distribution of grains
suspended in a liquid suspension, the system comprising:
a settling tank (1) for holding the grains in suspension; the settling tank
(1) having:
(a) means for circulating the suspension therethrough; and;
(b) a plurality of at least three measuring heads (2, 3, 4, 5, 6) for
measuring the optical density of the suspension, at various positions in
the settling tank, spaced from each other;
optical means for measuring the optical density of the suspension in the
settling tank;
a computer processing unit;
means applying the measured optical density as an input to the computer
processing unit;
the computer processing uunit determining the grain size distribution from
the measured optical density values;
an overflow rim (1B) fitted about the upper end of settling tank (1); and
a lid (7) having an inner non-reflecting surface fitted at the upper end of
settling tank (1).
8. The system of claim 7, further comprising:
a plurality of at least five measuring heads (2, 3, 4, 5, 6) arranged the
length of the settling tank (1);
the uppermost, first measuring head (6), is positioned under the lid (7),
at a distance of 0.03 to 0.003H therefrom;
the second, next lower, measuring head (5) is positioned at a distance of
about 0.1-0.03H from the first measuring head (6); and
the remaining measuring heads (4, 3, 2) are positioned at increasing
distances from each next adjacent head;
where H represents the height of the settling tank (1).
9. The system of claim 8, wherein the means for circulating the liquid
suspension comprises:
a circulating tank (11);
a first pipe (18) connecting the lowest portion of the circulating tank
(11) to the lowest portion of the settling tank (11);
a circulating pump (14) in the first pipe (18); and
a second pipe (9) through which the liquid suspension from the upper part
of the settling tank (1) is returned to the circulating tank (11).
10. The system of claim 9, further comprising:
a first heat regulating device (20) for maintaining the temperature of the
liquid in the circulating tank (11) at a predetermined level;
a standard solution tank (29), connected to the circulating tank (11) by a
third pipe (26) and;
a remotely controllable first valve (22), in the third pipe (26), for
regulating the flow of standard solution therethrough.
11. The system of claim 10, further comprising:
a second heat-regulating device (33) in the standard solution tank (29) for
maintaining the temperature of the standard solution in the tank (29) at a
predetermined, given level.
12. The system of claim 11, further comprising:
a fourth pipe (10) connected to the settling tank (1), to the circulating
tank (11) and to the standard solution tank (29) for maintaining equal
ambient pressures in the tanks (1, 11 and 29);
a fifth pipe (27,42) connected between the pipe (45) carrying the
suspension to be tested and the circulating tank (11); and
a second controllable valve (24,41) in the fifth pipe (27,42) for
controlling the flow of the suspension to be tested into the circulating
tank (11).
13. The system of claim 12, further comprising:
a feed pump (35), between the circulating tank (11) and pipe (45), to
selectively feed into circulating tank (11), through the fifth pipe
(42,27), either;
the suspension to be tested, flowing in pipe (45), or;
standard solution, from the standard solution tank (29).
14. The system of claim 13, further comprising:
a sixth pipe (28), for providing liquor to flush the circulating tank (11);
a third valve (23), for controlling the flow of liquor to flush the
circulating tank (11);
a seventh pipe (36), connected to the first pipe (18), for draining liquor
from both the circulating tank (11) and the settling tank (1);
a control valve (25), in the seventh pipe (36), to control the flow of
liquid suspension or liquor draining from the tanks (1 and 11); and
a fluid sensor (46), in the seventh pipe (36), for detecting the presence
of any liquid suspension or liquor in the seventh pipe (36).
15. The system of claim 14, further comprising:
a processing and control unit (48); and
a digital data processor;
the digital data processor having as inputs thereto data from the measuring
heads (2, 3, 4, 5, 6), and outputs therefrom applied as inputs to control
the operation of the pumps (14,35) and the processing and control unit
(48).
16. The system of claim 15, wherein the digital data processor further
comprises:
a digital data bus (50), and
an evaluation unit (49);
the digital data bus (50 ) connecting the processing and control unit (48)
to the evaluation unit (49). |
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Claims  |
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Description  |
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BACKGROUND OF THE INVENTION
This invention relates to both the is a process and equipment for the
determination of grain size distribution of particles in suspension.
The known or prior art and equipment processes for the determination of
grain size distribution are characterized by the fact that the measurement
is carried out by drawing samples independent of the technological process
under laboratory conditions. The time required for measurement and
evaluation is fairly long therefore this kind of solution is not suitable
for continuous measurement and process control. The equipment called
"Analysette 20" of the Fritsch-make represents the basis of a process for
the determination of grain size distribution wherein the settling
rate/velocity of particles is determined by photoextinction density
measurement and further on the grain size distribution as a function of
the path of settling. By this instrument the samples taken from the
technological process are similarly treated under laboratory conditions.
The principal part of the unit is a cell filled with suspension sample
which is, after some predetermined time, scanned by a photoextinction
measuring head moved continuously in an opposite direction to the
settling. As a result of movement of the measuring head the extinction of
the smaller particles can be determined after a shorter path of settling
and the measurement can be performed within 15-20 minutes i.e. far before
total settling would be completed. Disadvantage of the solution lies in
the condition that measurement cannot earlier be terminated and evaluated
before measuring a moving head reaches the surface of liquor, at the same
time the accuracy of measurement improves in direct proportion to the
height of the column of liquid which means that higher accuracy is
associated with longer measuring time. Minimum measuring time with this
kind of measurement of result resulting in acceptable results would take
about 15 minutes. This time is too long to apply the solution for direct
control of the technological processes.
A further disadvantage of the known device lies in the condition that the
measuring range of grain size distribution is comparatively small because
measuring time can only be reduced by the reduction of useful height of
the cell thus limiting the upper limit of measuring range and the
interfering effect on the photoextinction measurement of the reflection of
liquor surface in the cell limits the lower limit of measuring range.
Particles exhibiting a settling path less than 1 cm can no longer be
measured by this device, it only provides acceptable measuring results in
the particle range of 1-200 .mu.m.
SUMMARY OF THE INVENTION
For a number of technological processes, e.g. classification, sizing,
grinding, crystallization, settling and agglomeration, a solution for the
measurement of grain size distribution is needed. The results of which
should be useful directly for the contemporary regulation and control of
the process. The invention is based on the recognition that for the
determination of the photoextinction grain size distribution, the optical
density is repeatedly measured at several points in the container holding
the suspension, and the grain size distribution is determined from the
data obtained by the use of a digital data processing unit. This way,
partly the measuring range can be extended, partly the measuring time can
be reduced thus the measuring results may directly be used for the control
of some technological processes.
Accordingly the invention represents a process for the determination of
grain size distribution of particles in suspension in the course of which
the suspension is allowed to settle in a settling tank while the optical
density of the suspension in the settling tank is measured and from this
the grain size distribution is determined.
According to the invention, the suspension is homogenized by circulating it
in the settling tank, then circulating is stopped and optical density is
repeatedly measured at at least three points of different height.
Repeating of measurements should expediently be made at 0.0001-1 second
interwals for 30-300 seconds.
When applying more, preferably five measuring heads along the settling
tank, a settling tank of an appropriate height can partly be used
resulting in the extension of the upper measuring limit, partly the fast
processing of results obtained at given time intervals by the measuring
heads by a microprocessor or microcomputer decreases measuring time
considerably. It is of advantage in practice that measurement by the
measuring heads is made very quickly by the use of change-over-switch for
measuring points according to the given intervals one by one, rather than
all at once. In order to optimize the optical density measurement, a
standard solution is added to the suspension such as to obtain an optical
density of 0.5-1.0, preferably, 0.7-0.9 of the mixture. For standard
solution an aqueous or organic solvent solution of the dispersing reagent
is expediently to be added. Accuracy of measurement may be increased if
the temperature of suspension, respectively the mixture and standard
solution is kept at constant value, preferably at temperatures exceeding
by 2.degree.-10.degree. that of the ambient one.
The measurement can be made more accurate if prior to circulating the
suspension, plain standard solution is circulated first in the settling
tank and the optical density of standard solution and the dark current of
the measuring device is measured. By storing the values thus obtained the
optical density values measured for the suspension can be corrected.
It is of advantage during the process according to the invention to
measure, at the beginning of measurement yet during circulation, the
initial optical density corresponding to the maximum masking at all
places, then to form their reciprocals and multiply the latter by the
least value of initial optical density. Optical density values measured
afterwards could be corrected by the corrected values thus obtained.
Optical density data measured during settling are stored in the corrected
state. Based on the point of time of successive measurements for every
measuring head the corresponding grain size is determined. The grain size
ranges of the neighbouring measuring heads become overlapped, and making
use of this, in the course of preprocessing the measurement data starting
from the lowermost measuring head only those points will be accepted to be
valid which relate to coarser grains than the uppermost measuring head
could have detected. This way, one particular grain size corresponds to
but a single optical density. This reduction of data, according to the
invention, not only reduces the data pairs to be transmitted to get
further processed to their fifth part, but assures the selection of data
pertaining to the longest measured path thus being most accurate. In the
course of preprocessing, the mass proportions are calculated from the data
pairs in a way that the product of the individual grain size and optical
density data pairs is divided by the sum of those products. The mass
proportions determine already the cumulative grain size distribution.
The invention also includes a system for the determination of grain size
distribution of particles in a suspension. The equipment used in the novel
system comprises a settling tank for the suspension, a device for
measuring the optical density of the suspension in the settling tank and a
computing unit for the determination of grain size distribution from the
optical density values measured. According to the invention, the settling
tank in the equipment is equipped with a circulating system for the
suspension, and at least three measuring heads to sense the optical
density are arranged at heights of different spacings along the settling
tank.
It is advantageous to provide the settling tank preferably of tubular shape
with an overflow rim on its upper end and a lid with its inner surface not
reflecting inwards. The lid prevents the upper level in the settling tank
from reflecting and thus interferring. This way, the uppermost measuring
head can directly be arranged below the lid and thus the lower limit of
measurement can substantially be reduced. It is advantageous to arrange
the measuring heads at increasing spacings, for instance in the way that
the uppermost measuring head is located under the lid at a distance of
0.01-0.00H, the second one below the first one at a distance of 0.1-0.03H
and the other measuring heads one by one at still increasing distances,
where H represents the height of the settling tank.
In one operative embodiment the circulating system comprises a circulating
tank, a first pipe coming from the former leading to the bottom part of
the settling tank, a circulating pump built-in in the first pipe and a
second pipe carrying the suspension leaving the upper part of the settling
tank and recycling the substance into the circulating tank. If the
circulating tank is equipped with a temperature controlling device, so
constant temperature of the suspension in the settling tank can be
assured.
It is of advantage if the equipment according to the invention is provided
with a tank holding the standard solution the former being connected by
pipe with the circulating tank. A controllable valve is built in this
pipe. The standard solution is partly used for calibration before
measurement partly for the dilution of the suspension to be measured. In
order to increase accuracy the thermal regulation of the standard solution
tank is also advantageous.
The settling tank, the circulating tank and the standard solution tank are
connected on top by a pressure equalizing pipe. The equipment according to
the invention is suitable for both laboratory measurements and
measurements necessary for controlling a technological process. In the
latter case, the circulating tank is linked up over a controllable valve
with the pipeline of the suspension of the technological process to be
tested. It is expedient to install a charging pump between the circulating
tank and the pipeline of the technological process in order to
alternatively feed suspension from the pipeline or standard solution from
the standard solution tank into the circulating tank. By this method the
required mixing ratio can be adjusted. For flushing the equipment
according to the invention after measurement the circulating tank is
connected over a controllable valve with the pipe of flushing liquor. The
circulating pipe, on its lower section is connected to a drain pipe over a
controllable valve. A liquor sensor is provided in the drain pipe
indicating the condition for the processing and control unit that drainage
has been completed.
With the equipment according to the invention such kind of realization is
practicable where all the measuring heads, pumps and controllable valves
are connected to a single processing and control unit, the latter
comprising also a digital data processor. This processing and control unit
carries out the control of the entire measuring unit and the preprocessing
of optical density data supplied by the measuring heads. It is expedient
to transmit the preprocessed data over a digital bus to an evaluation unit
comprising another digital data processor. Thus the processing and control
unit is capable during the processing time of transmitted data of
controlling the subsequent measuring cycle. The invention is further
explained with reference to the drawings representing the practicable
realization modes, where
BRIEF DESCRIPTION OF THE INVENTION
FIG. 1 shows a block diagram of the various pieces of equipment according
to the invention,
FIG. 2 is a schematic representation of the various interconnections of the
measuring unit of the system according to the invention,
FIG. 3A and 3B is a block diagram of the interconnections of the processing
and control units of the equipment according to the invention,
FIG. 4 shows the block diagram of the evaluation unit of the equipment
according to the invention.
DETAILED DESCRIPTION OF THE PREFERRED EMOBIDENTS
In FIG. 1 measuring heads 2, 3, 4, 5 and 6 are located along settling tank
1. Said heads 2, 3, 4, 5 and 6 are arranged to measure optical density of
the liquor and suspension being held in the settling tank 1. The settling
tank 1 is, at its lower and upper ends connected to a recycling
circulating system comprising a circulating tank 11, a pipe 18 leading
from the bottom of the former to the bottom of the settling tank 1,
further a return pipe 9 leading from the upper section of the settling
tank 1 to the circulating tank 11 and a circulating pump 14 installed in
the pipe 18 between valves 12 and 13. The pipe 18 is connected at its
lower track to the pipe 36 over a controllable valve 25. To indicate the
completion of drainage the pipe 36 is fitted with a liquor sensor 46. To
provide temperature control for the circulating tank 11 a heating device
20 and a temperature sensor 21 is provided. To indicate the filled-up
state a level detector 19 is fitted in the circulating tank 11. The
circulating tank 11 is connected over a controllable valve 22 and by a
pipe 26 with a standard solution tank 29 which for heat control is
similarly fitted with a heating device 33, and a temperature sensor 32,
moreover, for the indication of filled-up state with level detectors 30
and 31. Pipe 45, carrying the suspension to be measured, is connected to
circulating tank 29 by means of controllable valves 24 and 41 and by pipe
42. The pipe 45 is one pertaining to those of the technology or industrial
process being measured, respectively, it may run parallel thereto. The
circulating tank 11 is connected with a pipe 28 to carry the flushing
liquor, e.g. water over a controllable valve 23. The standard solution
tank 29 is connected with a pipe 43 of a feed pump 35 by a pipe 44 and
over a controllable valve 40. The pipe 43 is connected with the pipe track
between the controllable valves 24 and 41. This way the feed pump 35
charges either suspension over the pipe 42 into the circulating tank 11
with the valve 40 closed, or standard solution into the same with the
valve 41 closed. During charging material by the pump 35 the valves 24 and
41, respectively, valves 24 and 41 should alternately be operated. The
settling tank 1, circulating tank 11 and the standard solution tank 29 are
interconnected on their upper part by a pressure equalizing pipe 10.
Control of measuring heads 2, 3, 4, 5 and 6 respectively, reception of
their measured data as well as the control of valves 12, 13, 22, 23, 24,
25 and 40 and 41 further of pumps 14 and 35 is performed by a data
processing and control unit 48. The processing and control unit 48 is
further linked up with the heating devices 20 and 33 used for the
temperature control of the circulating tank 11 and the standard solution
tank 29, and the temperature sensors 21 and 32 as well. Similarly, the
processing and control unit 48 receives the signals of level detectors 19,
30 and 31. The processed data are transmitted by the processing and
control unit 48 via a bus 50 to an evaluation unit 49.
An advantageous and more detailed realization mode of measuring unit 47 of
the equipment according to FIG. 1 is shown in FIG. 2. In FIG. 2 the
settling tank 1 is a vertical tube having a bottom inlet portion in the
shape of a frustum of a cone in order to provide uniform flow pattern. At
the upper end of settling tank 1, however, the liquor suspension flows
over an overflow rim 1B and returns from liquor collecting channel 8 over
a pipe 9 into the circulating tank 11. There is a lid 7 on top of the
settling tank 1, its inner surface having a mat black finish, e.g. it is
made of a rough plate covered with platinum black on its bottom side, in
order to avoid the reflection caused by the upper surface of liquor in the
settling tank 1 which would interfere with the extinction measurement.
This way, the uppermost measuring head 6 can be located quite near to the
lid 7, e.g. about 0.005H away from it, where H is approximately the height
of the settling tank 1. The distance between the measuring heads 6 and 5,
in the example is about 0.05H, that between the measuring heads 5 and 4 is
about 0.195H, that between the measuring heads 4 and 3 is about 0.25H and
that between the measuring heads 3 and 2 is about 0.5H. The lowermost
measuring head 2 is located at a distance of about 0.05H from the bottom
of the settling tank 1, however, the height of the inlet part 1A is about
0.02H. In this operative embodiment the value for H comes to about 1
meter. The settling tank 1 is provided with heat insulation in order to
avoid heat convection and is located in a lightshielded shaft enabling the
extinction measurement. An exemplary realization of the measuring heads 2,
3, 4, 5 and 6 is given in FIG. 3A.
In FIG. 2 the pump 14 is a diaphragm pump equipped with a bellow-shaped
diaphragm 14A, a piston 16A and a magnetic core 16 moving together with
the former being displaced by an operating coil 15 against a spring 17.
The operating coil 15 is supplied with changeable frequencies. On both
sides of the pump 14 there are silicon-rubber membrane valves 12 and 13
installed. The valve 12 opens on the suction effect of the pump 14, the
valve 13 opens on the delivery action of the same. The feed pump 35 is of
the similar design fitted with magnetic core 38, piston 38A, operating
coil 37 and spring 38. In this case, however, the operating coil 37
operates the piston 38A by a long stepped impulse. By this operation the
valves 24 and 41 are synchronously controlled while the charging of
suspension coming over the pipe 42 takes place, respectively the similar
happens to valves 24 and 40 if the standard solution coming over the pipe
44 is charged. It can be seen in the figure that all the valves 22, 23,
24, 25, 40 and 41 are electromagnetically operated by the corresponding
operating coils 22A, 23A, 24A, 25A, 40A and 41A. For aeration purposes the
standard solution tank 29 is provided with a pipe stub leading to the
atmosphere. The latter is covered by a cap provided with a filter insert.
There is a liquor sensor 46 provided for which is indicating the
completion of discharge being for instance an oscillometric measuring
condenser due to flammable solution or suspension possibly used.
Signal transmitting and control lines leading to the processing and control
unit 48 have not been indicated in FIG. 2. Those are shown in FIGS. 3A and
3B representing an operative embodiment of the processing and control unit
48. FIGS. 3A and 3B constitute a single figure where the lines 88, 89, 90,
91, 92, 93, 94, 95 and 96 are connected to the corresponding lines 88A,
89A, 90A, 91A, 92A, 93A, 94A, 95A and 96A.
Power supply for the processing and control unit 48 is provided by the
power supply unit 51 assuring a noise-suppressed power fitted with
alternating or direct current output terminals.
With all the outputs there is a possibility to report the short or open
circuit of interconnected functional units and to give an alarm signal.
The identity number of defective unit is indicated by the photodiode. The
power supply voltage output lines are drawn in dashed lines. The central
unit of the processing and control unit 48 is a microprocessor 52. It
performs all the control functions and carries out the preprocessing of
optical density data measured. It transmits the preprocessed data via an
interface unit 71 to the bus 50 which is connected with the evaluation
unit 49. The microprocessor 52 is connected with a clock generator 53
providing timer signals continuously for logging, as well as it separately
indicates the measuring time and checks the lapse of maximum time of
measurement set. By setting the maximum time of measurement on a keyboard
69 the operator actually determines the minimum particle diameter to be
measured (e.g. for 1-2 minutes 1 .mu.m, for 2-5 minutes already less than
1 .mu.m).
There are further units attached to the microprocessor 52: a keyboard 69, a
display 68, a printer 70, a Random Access Memory or RAM memory 67, as well
as Read Only Memory or ROM memories 72, 73 and 74. This as a whole
represents substantially a data processing device. The display 70 is used
for the visualization of questions, conditions of measurement and data
measured. Its purpose is partly the use of the equipment also as a
laboratory instrument, partly to enable the operator conducting the
measurement for an industrial process to directly intervene on the spot
and check up the consequence or result of the intervention, respectively.
The keyboard 69 is required for the input of material parameters and
denomination of the standard solution and for the operation on the site,
respectively. These input values, answers, orders/instructions are also
stored in the RAM memory 67. The ROM memory 72 holds the control program
of calibrating measurement carried out before the measurement. The ROM
memory 73 holds the evaluation and preprocessing programs of the
measurement, whereas the ROM memory 74 holds the main program controlling
the measuring process.
Further units attached to the microprocessor 52 are an electronic circuit
82 of the level detectors 19, 30 and 31, electronic circuit 83 of the
liquid sensor 46, a pump control unit 84 driving the operating coil 15 and
a pump control unit 86 driving the operating coil 37. Substantially, the
pump control unit 84 is a frequency controller. The required frequency
depending on the maximum grain size is calculated by the microprocessor 52
based on the measuring main program stored in the ROM memory 74. The pump
control unit 84 controls also the valve control unit 85 driving the
operating coils 22A, 23A and 25A corresponding to the order received from
the microprocessor 52. The pump control unit 86 controls also the valve
control unit 87 driving the operating coils 24A, 40A and 41A corresponding
to the order received from the microprocessor 52. Temperature control of
the circulating tank 11 and the standard solution tank 29 is performed by
the temperature control unit 75 which is on starting from the moment of
applying power to the equipment irrespective of the operation of the
microprocessor 52. The temperature control unit 75 comprises two
independent temperature control subunits. To one of them are attached the
temperature sensor 21 through an amplifier 78 and an analogue-digital
converter 76, as well as the heating device 20 through a switching relay
80. To the other subunit the temperature sensor 32 is connected via an
amplifier 79 and an analogue-digital converter 77, as well as the heating
device 33 through a switching relay 81. The measuring heads 2, 3, 4, 5 and
6 are also connected with the microprocessor 52. The measuring head 2
comprises a photodiode 58, the pertaining optics (condenser and
diaphragm), as well as a photosensor 63, e.g. photo resistor or
photoelement. Similarly, the measuring heads 3, 4, 5, 6 comprise
photodiodes 57, 56, 55 and 54 and corresponding photosensors 62, 61, 60
and 59, respectively. The measuring heads 2, 3, 4, 5 and 6 are
successively operated by the microprocessor by the help of a measuring
point selector 64. The measuring point selector 64 applies current
successively on the photodiodes 58, 57, 56, 55 and 54 and in the meantime
it switches the outputs of photosensors 63, 62, 61, 60 and 59 to the input
terminal of a gain-controlled amplifier 65 the output terminal of which is
connected via an analogue-digital converter 66 with the microprocessor 52.
Eitehr the amplifier 65 of the analogue-digital converter forms
logarithmic values out of measured values. This way the measured
extinction values are transmitted in the digital form to the
microprocessor 52 which stores them in the RAM memory.
The system according to the invention operates as follows:
Before the measurement of optical density of the suspension, a preliminary
measurement is performed according to the control program stored in the
ROM memory. In the course of the latter reference measurement is made with
the measurement heads 2, 3, 4, 5 and 6. Therefore, by opening the valve 22
the circulating tank 11 and the settling tank 1 is filled up with standard
solution while the pump 14 is running. When filling with plain standard
solution is completed and indicated by the level detector 19 for all the
measuring heads 2, 3, 4, 5 and 6 the values D=0 and D=.infin., better to
say the optical density of the standard solution and the dark current of
the measuring head are measured.
Subsequently, to the standard solution in the circulated system samples are
given in small batches from the suspension to be analyzed by the use of
feed pump 35 as long as the optical density of the mixture of standard
solution and the suspension to be analyzed reaches D=0.7-1. During
circulation the mixture of standard solution and suspension is
homogenized. In favour of this the velocity of circulation should be such
that even the largest particle does not start settling.
In the course of circulation the starting D.sub.O1 . . . D.sub.On optical
density, where n represents the number of measuring heads, corresponding
to maximum masking of the adjusted mixture of liquor is measured for all
the measuring heads. The microprocessor 52 forms reciprocal values of the
latter and multiplies the reciprocal values with the least measured
starting D.sub.Oi optical value (D.sub.Oi /D.sub.O1 . . . D.sub.Oi
/D.sub.Oi . . . D.sub.Oi /D.sub.On). It stores the correction factors less
than unit or even the unit thus obtained and subsequently corrects the
optical density values going to be measured for every measuring head after
subtracting the stored dark current value by the foregoing factors
eliminating hereby the differences resulting from the deviating
characteristic curves of the measuring heads.
When starting measurement, the circulation is halted and settling of
particles can take place which can be carried out in the settling tank by
the measuring heads 2, 3, 4, 5, and 6 at nearly same point of time,
expediently at intervals ranging 0.002-0.2 s, expediently for a period of
90-120 s by means of photoextinction measurement. Full measuring time will
be set in the function of settling rate/velocity of the particle least in
size yet to be measured. The microprocessor 52 stores the optical density
values measured during settling in a corrected form in the RAM memory.
Based on the points of time of successive measurements, as well as the
prevailing conditions of temperature, density, viscosity, the
microprocessor 52 computes for every individual measuring head the least
and largest measurable grain size (equivalent grain diameter). The grain
size ranges thus resulted overlap each other. The microprocessor 52
selects from the optical density values corresponding to the individual
measuring times i.e. particle diameters that one which pertains to the
longest path of measurement. To this, starting from the lowermost
measuring head, it accepts only those optical density values to be valid
which relate to coarser grains than the measuring head arranged above the
one before was able to measure. In such an assembly of data thus reduced,
one grain size corresponds only to a single optical density value. On
making the product of grain size and the pertaining optical density value
the microprocessor 52 computes the relative weights, their sum and the
mass proportions by forming the quotient of relative weights and the sum.
The data pairs of grain size - mass proportion determine the cumulative
grain size distribution, thus they may be listed or the distribution may
be drawn on the printer 70 and/or the data pairs may be transmitted over
the bus 50 to the evaluation unit 49.
After having measured the optical density values, the circulating system is
drained by opening the valve 25 and is cleaned with flushing liquor by
opening the valve 23.
Then the filling-up with the subsequent suspension sample can be started
immediately by the feed pump 35.
The evaluation unit 49 shown in FIG. 4 comprises a digital data processing
device 97 which is either a microcomputer carrying out detailed processing
of measured data or an object-oriented microprocessor-furnished process
controlling small computer, morover, it comprises a display 98 for the
visualization of data and promoting the communication (in case of
microcomputer it can be a constituent of it), further a keyboard 99 for
data input and communication (this also forms a constituent of the
microcomputer), an interface unit 103 for a high capacity central process
control computer, the connection being performed by the data bus 104, a
programme store 102 which is for instance a floppy-disc store for storing
users' own specific programs, data logger 101 which is a floppy-disc unit
for the quick storage of measured data rendering possible the separation
of measurement and data processing and the shifting in time (e.g. if
checking takes place hourly at 10 points then it is about 30 minutes, so
for further processing another half an hour is at disposal) and finally
the ROM memory with read only programs forming a part of the measuring
system which the user cannot change. The program store 102, however,
renders possible that the user can extend the area of application by
programs of his own.
The subroutines of the ROM memory 100 render possible the performance of
the following tasks for the evaluation unit 49:
(1) The measuring data pretreating and reducing subroutine reads the mass
proportion and grain size data pairs by records (e.g. by tens), approaches
them by a third-degree parabolic arc, then counts down from this at
integral .mu.-meters (.mu.) with available path spacings the mass
proportions (thus again reducing the number of data to its fourth-fifth
part). In order to achieve break-free curve fitting it takes two
calculated points from the end of the previous stage with multiple weight
into consideration. It traces the distribution values thus obtained,
further on the differential and integral (cumulative) curves, too and
lists out the same. These data will be the basis of further calculations,
Of course, The corresponding heading is also constructed.
(2) Based on the data having been reduced twice in number, the measuring
system subroutine carries out the regression of the functions being known
by themselves, i.e. Rosin-Rammler (Benet), Schuman-Gaudin, Fauss and
Kolmogorov. It prints the point of time of measurements, denomination of
samples, denomination of functions, lists out the values of constants, the
remarkable distribution values, the mode, the minimum and maximum grain
size, the 20% and 80% grain size (36.8% for RR) and an optional minimum
and maximum competent grain size (e.g. on selecting .DELTA.=5%, the 5% and
95% grain size). It lists out the integral (cumulative) and differential
distribution function values which it plots by solid lines, indicating
besides also the measuring points to demonstrate the merit of approach,
moreover, it prints out scattering value or correlation coefficient valid
for the entire function. In the case of parallel measurements it also
computes the scattering in the function of grain size. It visualizes all
data on the display and also on the printer.
(3) Another subroutine computes the regression of a new multi-mode
distribution function which is a modified Cauchy distribution. Its
advantage lies in the condition that it possesses also an axial section
both for minimum and maximum grain size enabling the accurate calculation
of the specific surface and other parameters, moreover, it renders also
possible the description of asymmetrical distributions and multi-mode
distributions by means of superimposition. Its latter feature makes it
suitable for the description of processes comprising a classifier,
respectively for the solution of fine control of such kind of processes.
The machine performs the printing activity outlined with the subroutine
(2), however, it does it also by part-density functions and with the
integer function, too.
(4) A short subroutine which selects the minimum from the scattering values
and prints on basis of this the name of type function providing the best
approach, possibly those also being suitable based on the supposition that
the scattering does not exceed a certain value.
(5) Evaluation of standard sieve analysis used for checking the values
measured by the instrument or for converting the distribution from the
equivalent spherical diameters into the actual dimensions. Operation of
the subroutine is based on the condition that the progress in time of
sieving on siebes of given mesh is well known for the type of material to
be measured. This may be carried out by a previous set of tests. As a
result of tests a series of data pairs consisting of time and sieve
residue is obtained. From these data the most probable sieve residue
figures of a perfect sieving can be calculated, serving as a basis of
comparison on which the subroutines (2), (3) and (4) could be performed.
In the case of grain function considered to be most suitable it forms the
quotient of mass proportions obtained with the equipment in question and
those with a measure identic with the sieve. In the case of proper
measurement the figures will be close to each other. By plotting the
latter and carrying out the regression a straight line parallel with the
abscissa intersecting the ordinate is obt | | |