SU1689817A1 - X-ray absorption analyzer of sulphur in oil and liquid petroleum products - Google Patents

Abstract

The invention relates to devices for measuring the concentration of elements in an organic liquid, which are based on the interaction of radioactive radiation with an analyte, and is intended to measure the sulfur content in petroleum and petroleum products. The purpose of the invention is to improve the accuracy and speed of analysis. The device contains a cadmium-109 gamma-ray source, a sample measuring cell, a detection unit with a proportional counter, an amplifier, an amplitude discriminator, a switch, a reversible counter, an computing unit, a data setting unit, a display unit, a timer, and a clock generator. The essence of the invention is that the device implements an optimal background measurement procedure for the type of measurement carried out, as well as a quick calculation of the measured value using a computing unit. The outputs of the switch are connected to the inputs of the addition and subtraction of a reversible counter, one of the outputs of which is connected to the control input of the switch. The background value is measured before each sample is analyzed, then this value, along with other initial data, is entered into the data setting block. When analyzing the sample, the background value is transferred to the reversible counter, and the detection unit pulses through the switch are fed to the subtraction input, after reversing the reversible counter switches the switch and the remaining pulses of the detection unit are fed to the addition input. 7 il. s Ј Os 00 about 00

Description

The invention relates to devices for measuring the concentration of elements in an organic liquid, which are based on the interaction of radioactive radiation with an analyte, and is intended to measure the sulfur content in petroleum and petroleum products.

The aim of the invention is to improve the accuracy and speed of the analyzer.

Figure 1 shows the structural diagram of the analyzer; figure 2 is a structural diagram of a computing device; FIG. 3 is a block diagram of an input block of the algorithm; 4 is a schematic diagram of a reversible counter and switch; Figures 5 and 6 are schematic diagrams of an algorithm input unit and a data setting unit; figure 7 - diagram of the arithmetic unit.

The x-ray absorption analyzer of sulfur contains a cadmium-109 radiation source 1, measuring cell 2, proportional X-ray counter 3, detection unit 4, amplitude discriminator 5, power supply unit b, reversible counter 7, timer 8, clock generator 9, switch 10, unit 11 data installation, computing device 12 and display unit 13.

The output of the amplitude discriminator is connected to the first input of the switch 10, the second input of the switch 10 is connected to the first output of the timer 8, the third input of the switch 10 to the first output of the reversing counter 7, the first output of the switch 10 with the first input of the reversible counter 7, the second output of the switch 10 to the second the input of the reversible counter 7, the third input of the reversible counter 7 is connected to the first output of the data setting unit 11, the second output of the reversing counter 7 to the first input of the computing device 12, the fourth reversing input counter 7 - with the first output of the computing device 12, the input of the data setting unit 11 is connected to the second output of the computing device 12, the second output of the data setting unit 11 is connected to the second input of the computing device 21, the third input of the computing device is connected to the second output of the timer 8, fourth input computing device 12 - with the output of the generator 9 clock pulses and the input of the timer 8, the third output of the computing device 12 - with the input of the display unit 13, the input of the timer 8 is connected to the output of the generator 9 clock and pulses and the fourth input 12 of the computing device.

The computing device 12 (RF, FIG. 2) contains an algorithm input block (BVA), the first input of which is connected to the second output of timer 8 and is the third input of the RF, the second input of the algorithm input block 14 is connected to the output of the 9 clock pulse generator and is The fourth RF input, the first output of the algorithm input block 14 is connected to the fourth input of the reversing counter 7 and is the first RF output, the second output of the algorithm input block 14 is connected to the input of the data setting unit 11 and is the second RF output, the third output of the input block 14 algorithm It is connected to the first output of the arithmetic unit 15, the second input of which is connected to the second output of the data setting unit 11 and is the second input of the RF, the third input of the arithmetic unit 15 is connected to the second output of the reversible counter 7, and is the first input of the RF, the output of the arithmetic unit 15, which is the third RF output, is connected to display unit 13.

The algorithm input unit (FIG. 3) contains a control trigger 16, an AND circuit 17, a command counter 18, a command distributor 19, a gate signal generator 20 and an enable signal driver 21. The first input of the control trigger 16 is the first input of the BSA, the second input of the control trigger 16 is connected to the fourth

the output of the distributor 19 commands, the first output of the control trigger 16 - with the first input of the AND 17 circuit, the second output of the control trigger 16 - with the second input of the command counter 18, the second input of the And 17 circuit

is the second input of the BSA. The output of the circuit 17 is connected to the first input of the command counter 18 and the input of the gate signal generator 20, the first output of the counter 18

commands connected to the second input of the command distributor 19, the second output of the command counter 18 to the input of the resolver 21, the output of which is connected to the third input of the distributor 19

commands, the output of the gate signal generator 20 is connected to the first input of the command distributor 19, the first and second outputs of the command distributor 19 are the first and second outputs of the CBA, respectively, the third output of the command distributor 19 is the third output of the CBA.

The analyzer works as follows

The proposed analyzer allows

quickly measure the true value of the NCJ background immediately before analyzing each sample. For this, the radiation source is isolated from the proportional counter by

a lead screen that is placed between the source and the counter. Before starting to measure the background, the Reset command will put the analyzer into a ready state. On code switch unit 11

data settings are set to zeros. Upon a Start command, timer 8 generates a measurement start signal, which from the first output goes to the second input of switch 10 and ensures the passage of pulses.

to the reversible counter 7. Simultaneously, on the Start command, a signal is written to write the contents of the switch (the first output of the data setting unit 11) to the reversing counter 7 via the third input. The zero state of the reversible counter 7 generates a signal (first output), which is fed to the third input of the switch 10 and opens the first output to pass to the first input of the reversible counter of measured background pulses for summation. After the end of the exposure time of 100 s, timer 8 generates a signal that arrives at the second input of switch 10 and blocks the passage of pulses to the first input of the reversing counter 7. The number of pulses typed in counter 7 is displayed on a digital display, after which the lead screen is removed. The obtained background value is set at the background code switch of the data setting unit 11. Rapid measurement and correction of the natural background before each analysis improves the accuracy of determining the sulfur concentration. The magnitude of the background is recorded by the data setting unit 11 in the memory of the reversible counter 7 at the third input. No pulses corresponding to the intensity of the gamma radiation source with an empty cell, or N pulses corresponding to the gamma radiation transmitted through the sample from the amplitude discriminator output go to the first input of the switch 10, which transmits these pulses from the second output to the second reversing input counter 7. This input subtracts the background impulses recorded in the reversible counter 7. After the background pulses are compensated, the reversible counter 7 goes through the zero state and generates a signal which from the first output of the reversible counter 7 goes to the third input of the switch 10. According to this signal, the switch 10 switches the signal from the subtracted second input of the reversible counter to the first addition input, and the pulses from the first output of the switch 10 are fed to the first input of the reversible counter 7. The time ti 12, during which a set of pulses is maintained by the reversing counter 7 in the background subtraction and addition mode, is determined by TC timer 8. At time ti, from the first output of timer 8, a signal is received that the switch 10 connects to the second input of the reversible counter 7. At time t2, corresponding to the end of the exposure, the signal from timer 8 blocks the passage of pulses to the reversible counter 7. After the end of the timer time analyzer goes into the processing of the received information. In the automatic information processing mode, a reversible counter 7, a data setting unit 11, an algorithm input unit 14, an arithmetic unit 15 are used. Timer 8 and clock generator 9. In this case, the block diagram of the device and its operation implement the calculation of the concentration of sulfur using the expression

-M, (1)

p N - Mt where p is the density of the hydrocarbon, g / cm °

.3.

No, N - the number of registered gamma-kzanty in the absence of the sample and passed through it during the exposure, respectively;

N f - the number of background pulses;

Ki, K-calibration coefficients.

A reversible counter records pulses proportional to the number of gamma quanta from the radioactive source cadmium -109 and the ambient background lf. The use of a reversible counter allows one to subtract the background pulses IF from the number of pulses recorded by the reversing counter in the absence of sample No and in the presence of sample N, i.e. N0-, Y-YF.

Thus, part of the expression (1) is implemented. Enter tc notation:

No - No1, (2)

N-N1 (3)

The notation used is used in expression (1), which takes the form

Ki

Ni

P m1 (4)

Expression (4) is used in the proposed analyzer for automatically calculating the concentration of sulfur. The values of KL K, p, N01 and Nф in the analyzer using the data setter. Moreover, the value of the background Yf goes directly to the information inputs of the reversible counter. The algorithm input block generates a certain sequence of commands with the help of which the values Ki, K, p, No1 and N1 are entered into the arithmetic unit and perform mathematical operations in accordance with expression (4). The computing device calculates the percentage of sulfur concentration. The result is displayed on a digital display.

The time taken by the analyzer to count N-Mf pulses and automatically calculate the concentration in the hydrocarbon sample is 120 s.

Thus, the invention improves the accuracy and speed of analysis.

due to the optimal for this type of measurement procedure, the measurement and accounting of the background, as well as the automatic processing of the measurement results and the calculated desired quantity.

Let us consider briefly the work of the analyzer according to principle diagrams.

In the initial state of the reversible counter (Fig. 4), logical O is present on the counting outputs D7-D12, on outputs D1-D3-logical 1, on output 04.1-logical 1, on output Q D6.1 - logical G, on outputs 1 -10 D13-D18 and inputs 019- D28 - logical 1, outputs 019-D28 - logical O, inputs D29-D38 - logical 1, the operation of the reversing counter starts on the Start command, From the moment of start, the Record signal is generated, which goes to the input of the low-order bits D7-D9, and the binary-decimal background code Mt set on information inputs 1-4, is entered into these counters, From the counting outputs D7-D9, the recorded code N (| is set at the inputs D1-D3. Timer 8 generates a resolution signal, which is fed to the second input D4.2 m determines the counting start. At the beginning of the counting, the reversible counter works on subtracting the number of pulses corresponding to background pulses. The state of the counters D7-D9 is monitored by the zero-state separation circuit D1-D3, D4.1-D5.1. With N f high signal potential the Resolution opens on the second input D4.2, the first input of which receives counting pulses N with amplitude discriminator 5. With output and D4.2, the counting pulses pass through D5.3 through the second input to the subtracting input 7 of the counter D7. When the reversing counter is switched to the summation mode. In this case, logical O is set at the counting outputs D7-D9, and logic level 1 is set at outputs D1-D3, which switches through D4.1 via the first input D5.1. From output D5.1, the voltage drop from high level to low switches D6.1. As a result, a low voltage level is established at the output of QD6.1, which closes D5.3, and a high voltage level from the output O opens 05.2 for playing counting pulses on the summing input 0.7. The pulses arriving at the input of the counter during the summation process carry background pulses, so they are denoted by N. During the pulse counting, information from the counting outputs of the reversing estimator is fed to the elements D13-D18, with which the binary-decimal conversion is performed.

code in decimal. After the end of the counting time of 100 s, the action of the Spread signal ends. At the second input, D4.1, a logical O is established, which blocks the passage of counting pulses. The analyzer enters the automatic calculation mode.

8, the automatic calculation mode uses an algorithm input block 14,

0 unit 11 installation data and arithmetic unit 15,

In the initial state of the algorithm input block 14 (FIG. 5), the output Q of the control trigger 06.2 contains a logical O,

5 at output 039.3 is logical 1, at the first and second outputs 041 - logical O, at output D42.1 - logical O, at output D42.3 and D42.4 - logical 1, at outputs 1-39 D43-D45 - logical one.

0 In the automatic calculation mode, the Automatic calculation (AB) command is sent to the S D6.2 input. At output Q D6.2, a logic level is established which opens circuit D39.1 via the first input for passing the second input of pulses from generator 9 with frequency f 2 Hz to input C1 of command counter 040. Each pulse arriving at 040 is the command for organizing the calculation of the algorithm of expression (4). The sequence number of the next command is converted into a binary code and from the outputs of the D40 in parallel arrives at the inputs of the elements D43-D45. At the same time, the command from output 039.1 through 5 steps to the second input D39.2 of the gate signal generator 20. With this generator, the input signal is delayed along the leading edge by the time t - 0.3 RC required for installation

0 code potentials at the inputs D43-D45, and fed to the inputs W0 for gating the input code. The selection of the command distributor element for recording the input code is determined by the presence of the signal Raz5 solution 1 (P1), P2 or P3, corresponding to logical O, on one of the inputs of the WiD43-D45, which is formed by elements 041-039.4 and D42.1-D42.4. The signal P1 at the second input element 043

0 is determined when the analyzer is installed and the initial state at the beginning of the measurements. In this case, the logic levels O from the outputs 041 after inversion to D39.4 and D42.2 go to inputs 042.1 as logical 5, and the output 042.1 supports logical O for converting binary command shoe on the first 16 outputs of the decoder 043-045. With the arrival of the 16th pulse at the input C1 040, the signal P1 is terminated and the RC signal is generated, which opens the D44 to the fourth input to convert the binary code of the commands on the second sixteen outputs. In this case, from the fourth output of D40, logical 1 switches 041 to input C1 and a high level is set at its first output, which after inversion to D39.4 switches D42.1 to the first input, and logical 1 is set to output 1. output D41 goes to the second input D42.3, and from the second output D41 logical O through inverter 042.2 as logical 1 goes to the first input D42.3 and logical 0 is set at its output, corresponding to the RC signal. With the arrival of the 32nd pulse, the D41 switches to 040 logical 1 from its fourth output. At the first output of D.41, the logical O is inverted to D39.4, and a high level is set at the first input 042.4. Logical 1 from the second output 041 switches the element 042.4 to the second input, and at its output sets the RZ signal to convert the code to D45. Each command after conversion sets a logical O to a specific output of the D43-D45. This signal determines the action of this command and the sequence of execution set by the command distributor.

The distribution of commands by the distributor 19 is carried out in accordance with the program for calculating expression (4).

From the first output of the distributor 19 commands, the command arrives at the fourth input of the reversible counter 7 for its serial polling. The polling commands are set at the outputs 8-13 of the D44 element and fed to the inputs W of the converters D13-D18, the outputs of the single digits of the converters are connected to the inputs of the corresponding circuits OR D19-D28, the outputs of the latter are connected to the inputs D29-D38, the commands polled are polled each time The decimal bit code is fed to the corresponding OR circuit and then inverted to D29-D38. From the inverter outputs, the information enters the computing device.

From the second output of the distributor, 19 command commands are sent to the data setting unit 11, in which, prior to the analysis, the values of values No1, Ki, K, p are entered. In the process of automatic calculation, the commands that come into the data installation block in a certain sequence, are IN-RUNNED 12 values N0, KL K, p.

The data installation block consists of code switches P1 P5, OR circuits D46-D85 and inverters D86-D126.

Switch P1 is designed to set the number of pulses No and has six decimal places, switches P2-P4 are intended to set KL

K, p, respectively, and have five decimal digits and a comma, switch P5 is designed to set the background of the Mt and has three decimal places. The П1-ПЧ switches are of the linear type, the П5 switch - with the binary-decimal code conversion. Switch bits are connected to the corresponding D43-D45 outputs. The logic level O at a certain output of the D43-D45 allows the potential to be at the switch. For example, when the first command arrives at element 043, a logical impulse O appears at its first output and is set at switch P1 of the sixth bit of number N01. 8 depending on the position of the switch defining the choice of contact from O to 9, corresponding to the number set on it, the level is set at the output of the discharge.

logic O and is fed to the input of the OR circuit () which combines the same type contacts of a given number of bits of the switch. Each switch has ten OR circuits.

The number of inputs to the OR circuitry is determined by the number of bits of the switch. From the output of the circuit OR logical 1 is fed to the input of one of the inverter elements D86-D126, which have a high load capacity. The same digits of decimal numbers are combined at the outputs of these elements according to the installation OR scheme. The numerical value of the bit, in our case, the sixth, as a logical Oh comes in

to the corresponding input of the computing device 12. Switch P5 converts the decimal code into the binary-decimal code 1-2-4-8, which goes directly to the potential inputs of the reversing counter 07-09.

From the third output of the distributor, 19 commands are sent to the arithmetic unit 15 to perform mathematical operations on the input

in quantities.

After selecting the last command, the command distributor 19 generates a Stop signal, which, from output 39 045, switches the trigger 16 via the second input

control performed on the element D6.2, and logical O at the output Q of this trigger blocks the passage of pulses from the generator 9 through the circuit I15, executed on D39.1, to the command counter D40. Logical G at the output of Q D6.2 sets D40 and D41 to the initial state.

The arithmetic unit 15 (Fig.7) consists of inverters D127-D146, a circuit of electronic keys D147-D162 and a computing element D163. Outputs 1-10 of the D29-D38 reversible counter and outputs 11-20 of the data setting block are combined at inputs 1-10 of the D127-D136 arithmetic unit, forming the wiring circuit OR, From the output of one of the elements of D127-D136, the decimal number code in the form of a logical 1 enters the input of an electronic key, which by means of mounting AND (bus1 -9) closes the corresponding inputs of D163 m provides input of a number into the computing element. Commands of mathematical operations from outputs 21-30 (figure 5) are fed to inputs 11-20 of elements D137-D146 and from their outputs using electronic keys and mounting In D163, C computational element outputs information outputted on the display unit 13, reading the digital indm- locator corresponds to the content of sulfur in the sample and is expressed in percentage with an accuracy of 1.

In this way, the concentration of sulfur in the sample is determined,

Claims (1)

Invention Formula A x-ray absorption analyzer of sulfur in petroleum and liquid petroleum products, including a radiation source cadmium109, a measuring cell, subsequently connected by a proportional x-ray counter, a detection unit, an amplitude discriminator, and power supply, characterized in that, in order to improve the accuracy and speed of the analyzer, a switch, a reversible counter, a data setting unit, a computing device, a display unit, a timer, a clock generator, are added to it, the output of the amplitude discriminator is connected to the first input of the switch, the second input of the switch is connected to the first output timer, the third input of the switch is connected to the first output of the reversible counter, the first output of the switch is connected to the first input of the reversible counter, the second output of the switch is connected to the second input of the reversible counter, the input of the data setting unit is connected to the second output of the computing device, the first output of the data installation unit is connected to third input reversing the counter, the second output of the data setting unit is connected to the second input of the computing device, the second output of the reversible counter is connected to the first input of the computing device, the third input the computing device is connected to the second timer output, the fourth input of the computing device is connected to the output of the clock generator and the timer input, the first output of the computing device is connected to the fourth input of the reversing counter, the third output of the computing device is connected to the display unit. Have Fig, 1 FIG. 2 Fig.Z T VyhoZ on bychisligplenny mustache / proc / l $ o-yykh.2 Shchi g. 4 iInput 2 FIG. five Sh, 6P R W) is $ b. P1 No byyyyyyyyy:  2 Outputs of the commands “POLL to S13-DI8 Teams S mathematically to action P2 .one tg / 73 nit I A5 and Pisa i5sh // : t  22 b№ I Bi & //. / VyhGZO P ) 55 /ten- I 3B-B «1 J B at § § I I "about Isyo D / 25 No. U №7 FIG. 6