JPS62187240A - Component analyzing instrument for sample to be measured - Google Patents

Abstract

PURPOSE:To make quantitative determination of the components in a sample to be measured with good accuracy by radiation measuring systems of the same number as the number of the components in said sample. CONSTITUTION:The radiation of photon energy corresponding to water is irradiated from a radiation source 1 to the sample 2 to be measured and the radiation transmitted through the sample 2 is detected 4 if the component in the component analysis of the sample to be measured contg. a hydrocarbon compd. is water. The signal from the detector 4 is subjected to pulse height discrimination 7 through amplifiers 5, 6. The signal propertional to the logarithm of the intensity of the transmitted radiation is outputted from a signal processing circuit 11. The mass of the water is calculated from the signal of the circuit 11 and the preliminarily measured absorption coefft. of the radiation mass of the water in an arithmetic processor 8 and the result thereof is displayed on a display unit 9. The analysis is made by the respective measurement systems of the radiation source 1A or 1B which radiates the photon energy corresponding to hydrogen or carbon in the case of hydrogen and carbon as well. The respective components in the sample to be measured contg. the water and hydrocarbon compd. are thus quantitatively determined with good accuracy.

Description

[Detailed Description of the Invention] [Industrial Application Field] The present invention provides a solid,
The present invention relates to an apparatus for analyzing the component ratio of a sample to be measured in a liquid or gas state.

[Conventional technology]

Conventionally, test oil-water separators have been used to measure the amount of water contained in hydrocarbon compounds. This device separates water contained in a hydrocarbon compound and then determines the amount of separated water as the water content.

[Problem that the invention seeks to solve]

With the conventional oil-water separator for the first test, as mentioned above, the amount of water could only be measured using the Sochi method, and it was not possible to measure it online. Also, specialized hydrogen compounds become emulsified due to the water they contain. In many cases, the hydrocarbon compound and water are not completely separated, resulting in problems such as errors in the measurement of water and hydrogen and carbon in the hydrocarbon compound.

This invention was made to solve this problem, and it is possible to measure the component proportions of water, hydrogen and carbon in hydrocarbons in a sample to be measured that contains water and is in a solid, liquid, or gas state online. Even when the temperature, pressure, etc. fluctuate, or when the type or composition ratio of the hydrocarbon compound changes, f The purpose is to obtain an analytical device.

[Means for solving problems]

A component analysis device for a sample to be measured according to the present invention is composed of a radiation source that irradiates the sample to be measured, a radiation detector that detects the irradiated radiation, and a signal processing circuit thereof, and is capable of detecting the number of components in the sample to be measured. The apparatus is equipped with at least the same number of radiation measurement systems as the number of radiation measurement systems, and an arithmetic processing device that calculates the mass proportion of the component to be measured from the transmitted radiation intensity and a predetermined mass absorption coefficient.

[For production]

In this invention, since the amount of components in the sample to be measured is determined by the radiation measurement system, component analysis can be performed online. In addition, the radiation sources of each radiation measurement system are selected and discussed in such a way that the equations including the radiation mass absorption coefficients corresponding to the components to be measured are linearly independent of each other. The mass of the measured component can be determined.

〔Example〕

A case where the components in the sample to be measured are water, hydrogen, and carbon will be described below.

FIG. 1 is a block diagram showing an embodiment of the present invention, in which 11 is a radiation source that emits radiation of photon energy corresponding to water pressure, such as γ rays or Xi, and (2) is a radiation source containing water and hydrocarbon compounds. The sample to be measured is, for example, crude oil, (Jl is the sample container (sampler) containing the sample to be measured (21), such as piping, +tIl is the sample to be measured (K)? A radiation detector that detects the transmitted radiation set, (5) is the radiation Detector (g
A preamplifier that amplifies the output signal of l.

(6) is the main amplifier that further amplifies the signal from the preamplifier (!r), (7) is the pulse height discriminator that sets the window level according to the photon energy, (gl is the pulse height (9) is an arithmetic processing unit that processes the output from the discriminator (7) and calculates the mass of each component in the sample to be measured by four arithmetic operations on a signal proportional to the logarithm of the transmitted radiation intensity; The display unit (tO) is a DC high-voltage power supply that supplies the operating voltage to the radiation detector (RI1), the preamplifier (ff+), the main amplifier (6), and the The discriminator (71) constitutes a signal processing circuit (ti) for water. Also, the radiation measurement system (l) corresponding to water includes a radiation source (ll), a radiation detector (
q), signal processing circuit (11), and DC high voltage electric TA (t
O). As mentioned above, the radiation measurement system (not shown) corresponding to water, that is, hydrogen, is a “radiation source (
/A), radiation detector (gA), signal processing circuit (preamplifier (jA), main amplifier (4A).

and a wave height discriminator (7A)), and a DC high voltage power supply (toA), and the radiation measuring thread corresponding to carbon is a radiation source (/B), a radiation detector (4'
B), signal processing circuit (preamplifier 5 (sB), main amplifier (
6B), a pulse height discriminator (7B)), and a DC high voltage power supply (10B).

Component analysis of a sample to be measured using the component analyzer configured as described above is carried out as follows. First, when the component is water, radiation with photon energy corresponding to water is irradiated from the radiation source (C) to the sample to be measured (U), and the radiation that has passed through the sample to be measured (Y1) is detected by radiation detection 5 (Q). The signal from the radiation detector (ul) is amplified by a preamplifier (y+) and a main amplifier (6), and is further subjected to pulse height discrimination by a pulse height discriminator (71).Signal processing circuit (
ll) outputs a signal proportional to the logarithm of the transmitted radiation intensity. Alternatively, the signal processing circuit (11) outputs a signal based on the transmitted radiation intensity.

Based on this signal, a signal proportional to the logarithm of the intensity may be generated using arithmetic processing bag #(t). The arithmetic processing unit (fl) uses the signal from the signal processing circuit (, /) and the radiation mass absorption coefficient of water measured in advance to determine the water quality t by performing four arithmetic operations.
Compute ff. This calculation result is displayed on the display unit (9).

Hydrogen and carbon were analyzed in the same way as above,
Arithmetic processing is performed simultaneously.

FIG. 2 is a block diagram showing another embodiment of the present invention, where (IC) represents three different photon energies corresponding to water, hydrogen, and carbon! 7) A radiation source emitting at least one of radiation, e.g. r-rays and X#, (uc)Tt
A pulse counting type radiation detector that outputs i-pulse signals! ? +, (7A), and (7B) are wave height discriminators whose window levels are set corresponding to the photon energies of the three plants, respectively. A single signal processing circuit (//C) corresponding to water, hydrogen, and carbon includes a preamplifier (S), a main amplifier (6), and a wave height P separater (7),
Similarly, the radiation measurement system (1C) includes a radiation source (IC), a radiation detector (HiroC), and a signal processing circuit (//C).

and a DC high voltage power supply (IOC).

The component analysis apparatus for a sample to be measured thus constructed operates in the same manner as the embodiment shown in FIG. That is, three types of radiation emitted from the radiation source (IC) pass through the sample to be measured (21) and are detected by the radiation set detector (gc) K. Pulses from the radiation detector ('tc) The signal is amplified by a preamplifier (s) and a main amplifier (61), and is subjected to pulse height discrimination by a pulse height discrimination a (71, (RIA), (RIC). Signal processing circuit (/ /C) counts only the Xll-valved pulses individually and outputs a signal based on the transmitted radiation intensity of each radiation measurement system (consisting of a single device except for the pulse height discriminator).Hereinafter, It operates in the same way as in FIG.

In this way, by using a pulse counting type radiation detector and a pulse height discriminator, it is possible to use a single radiation measurement system except for the pulse height discriminator, which is very advantageous in terms of device design. In addition, since this method can be applied to four or more types of components in the Ka: sample to be measured, it is possible to respond to a wide range of component analyzes Z).

In addition, the radiation detector (1, (daA), (gl3),
As (αC), a gas-filled proportional counter tube can be used.

Pre-amplifier (s'), (rk), (sB), main amplifier (
6).

You can use what is available, and there is no difficulty in obtaining it.

In addition, an arithmetic processing unit (ffl is a microcomputer)
Alternatively, the arithmetic processing unit tf can be easily constructed using an analog circuit.

Now, in general, radiation attenuation in materials.

It is described in Here, ko is the intensity of the incident radiation.

is the intensity of the transmitted radiation, μ is the radiation mass absorption coefficient of the material, ρ is the density of the material, and d is the transmission thickness in the material. C
is the weight of material per unit area.

C of each component is expressed as CW + CH + CC, and s
/'W+μH9μC? Assuming the radiation mass absorption coefficients of water, hydrogen, and carbon, respectively.

μW/”CW 0μH/”CH+μCl0CC:tn(I
O7/engine]) (haμWλ”0w+4., e−1μ.

U・C(H= 1.n(1,ko/I,) [ko)μW
J@CW+IIHJ・CH+μ. 3"Co"'An(1
6JA3) (Three equations of Jl are obtained. Engineering g
Since i can be determined in advance, the strength of the transmitted radiation is
By measuring , the right side of equation (z) is determined. this? G/
Similarly, equations (21 and (3) are tno, )t15) = al -tn(5) = a
l (a) An(10 pieces/I 2')”
” a2 7n (I,) ” GJ (51An
(10J/r = aJ An(I, 7) = G3
fil. Here -a/ * aJ laJ
is a constant.

(μwl, μH/Iμc/) and Cμ7, μHJIμC
The photon energy of the radiation is selected so that J) and (μW, 71μ, 1.μ.,) are linearly independent of each other. Therefore, [1), (al.

Equation (3) can be solved for Cw HCH* Cc as shown in the following equation.

Cw = Nw / M (7
1c,, = NH7M (g
ICC=NG 7M ffl
however.

NW =G, 1H-0μc, y+o”μcl@μH
j+Gj''μH70μCt2-a, aμCJ'μHJ
GJ"μH/"μc, -(), lc, #μHJIn a given sample, μW/1μm2. μ711μm2
9μm.

μ) II μC1) μC co-μCj is constant a Gt
+Gx*GJ/fi can be known from the transmitted radiation intensity, and CW * CHr Cc can be found from the above equation. cW r CFi * CC is, by its definition,
μH1) μHJIμI(
j-μc, + TμCJIμcJVc is given a fixed value in advance, and while measuring the transmitted radiation intensity, Gt + G
If J I Ga is determined by (tll, (yl,

The mass percentage of carbon is determined.

In this way, the transmitted Gur line intensity can be measured online, so water and hydrogen can be measured as components to be measured.

The mass fraction of carbon can be determined online without using any other information. This means that even if the temperature and pressure of the sample to be measured changes, and the content and composition ratio of multiple types of liquid or gaseous hydrocarbon compounds (e.g. oil, natural gas) change, there will be no effect. I don't accept it.

Next, specific numerical examples of the component analyzer according to the present invention will be shown.

Am (americium)-cog/ is selected as one of the radiation sources. This is s9. j ke'v, λ&, Jkev
gamma ray, t, 7.9 key, t 73 ke
v, 20. ! : Emit kev X-rays. So 26. All the low energy below J kev is t
g kev x-ray, and this x-ray and 2 b kev.

When measuring 60 keV gamma rays using a proportional counter as a pulse-counting radiation detector, the energy resolution is about tO%, so these three energies are easily separated by a pulse height discriminator, and a single detector is used. It is possible to simultaneously measure the intensity of at least one of the three types of gamma rays and X-rays transmitted by the sensor. The radiation mass absorption coefficient of each component is given by the seventh order.

μW/ μmko μwJl'H/ μHu μH3
μC/ μC μC, 7 Therefore, (μW1) μH
/1μ. ) and (μ71.μl(J +μ.,) and (μ
m51μm2. μ. j) are linearly independent of each other, and Cw
.

It can be seen that CH*CC is uniquely determined. In other words, if the intensity of the transmitted radiation is known, -CW+CH+CC can be determined in a -m manner, and the mass of hydrogen and carbon in the water content and hydrocarbon compound of the tentative measurement sample can be determined. The mass absorption coefficient is a material constant that does not depend on temperature or pressure.

Regardless of the temperature and pressure of the sample to be measured, or even if the content or type of hydrocarbon compound changes, the mass of moisture in the sample to be measured and hydrogen and carbon in the hydrocarbon compound can be determined.

In the above embodiment, Am-λQ/ was used as the radiation source, but an X-ray tube? Alternatively, both may be used. Furthermore, although the pulse counting method was used to measure the residual radiation, it is also possible to measure the radiation intensity as a direct current using a direct current type detector.

Further, in the above embodiment, a signal proportional to the logarithm of the transmitted radiation intensity was created by the arithmetic processing unit (ffl), but a logarithmic count rate meter was provided after the pulse height discriminators (7), (7A), and (7B), and It is also possible to consider the part up to the part as a radiation measurement system, and configure this measurement system to output a signal proportional to the logarithm of the transmitted radiation intensity.

It is possible to achieve the intended purpose. Furthermore, by increasing the number of radiation measurement systems to q or more types, it is possible to correct measurement errors due to fluctuations of at least tg or more in elemental components such as sulfur, nitrogen, nickel, and sodium chloride in the sample to be measured.

〔Effect of the invention〕

As explained above, the present invention includes a radiation source for irradiating and transmitting at least one of X-rays and γ-rays to a sample to be measured containing moisture and hydrocarbon compounds, and a radiation source for detecting the radiation transmitted through the sample to be measured. It is composed of a radiation detector for detecting the components in the sample to be measured and a signal processing circuit for processing the output signal of the radiation detector and outputting a signal based on the intensity of the radiation that has passed through the sample to be measured. and at least the same number of radiation measurement systems.

an arithmetic processing device for calculating a mass ratio of a component by four arithmetic operations from the intensity of transmitted radiation corresponding to each component obtained by the signal processing circuit and a predetermined radiation mass absorption coefficient of each component;

ntty even when the temperature and pressure of the constant sample fluctuates, or the type and composition ratio of hydrocarbon compounds in the sample change.
This has the effect of allowing better component analysis. Also,
By increasing the number of radiation measurement systems to, for example, q or more types,
Sulfur and nitrogen in the sample to be measured.

At least one of elemental components such as nickel and vanadium
This has the effect of being able to correct measurement errors due to variations of more than one species.

[Brief explanation of drawings]

FIG. 1 is a block diagram showing one embodiment of the invention, and FIG. 2 is a block diagram showing another embodiment of the invention. In the figure, (1), (/A), (/B), (/C) are radiation sources, (21 is the sample to be measured, (3) is the sample container, (
≠1° (taA), (daB), ('IC) are radiation detectors, (s), (yA). (SB) is a preamplifier, (6), (6A), (AB) are main amplifiers, (7), (7A), (7B) are pulse height discriminators,
(rl is an arithmetic processing unit, (91 is a display unit. (io), (tOk), (ioB>, (IOC>) are DC high-voltage power supplies, (//'), (//C) are signal processing circuits,
(/, 2)1(t2C) is a radiation measurement system. In each figure, the same reference numerals indicate the same or corresponding parts.

Claims (7)

[Claims] (1) A radiation source for irradiating and transmitting at least one of X-rays and γ-rays to a sample to be measured containing moisture and hydrocarbon compounds, and a radiation detector for detecting the radiation that has passed through the sample to be measured. and a signal processing circuit that processes the output signal of this radiation detector and outputs a signal based on the intensity of radiation transmitted through the sample to be measured, and measures at least the same number of radiation as the components in the sample to be measured. and an arithmetic processing device for determining the mass proportion of the component by four arithmetic operations from the intensity of the transmitted radiation obtained by the signal processing circuit and corresponding to the component, and the radiation mass absorption coefficient of each component determined in advance. A component analysis device for a sample to be measured, comprising: and. (2) The component analysis device for a sample to be measured according to claim 1, wherein the signal outputted by the signal processing circuit is a signal proportional to the logarithm of the intensity of radiation transmitted through the sample to be measured. (3) The signal output by the signal processing circuit is a signal based on the intensity of the radiation that has passed through the sample to be measured, and based on this signal, an arithmetic processing device calculates a signal proportional to the logarithm of the intensity. Component analysis device for a sample to be measured according to item 1. (4) The radiation detector is a pulse counting type radiation detector common to two or more radiation measurement systems, and the signal processing circuit discriminates the pulse height of the pulse signal from the pulse counting type radiation detector. The component of the sample to be measured according to claim 1, wherein only the pulses corresponding to the photon energy of the radiation in each radiation measurement system are individually counted, and a signal based on the transmitted radiation intensity of each radiation measurement system is output. Analysis equipment. (5) The radiation measurement system is a three-type measurement system corresponding to water, hydrogen, and carbon as components, and the four arithmetic operations are performed using the following equations. Analysis equipment. Equation: μ_W_1・C_W+μ_H_1・C_H+μ_C_1
・C_C=a_1-lnI_1μ_W_2・C_W+μ
_H_2・C_H+μ_C_2・C_C=a_1-ln
I_2μ_W_3・C_W+μ_H_3・C_H+μ_
C_3・C_C=a_3-lnI_3 (here, C_W
, C_H, C_C are the total weights of water, hydrogen, and carbon per unit area, respectively, along the radiation transmission path in the sample to be measured, μ_W_1, μ_H_1, μ_C_1, μ_W_2
, μ_H_2, μ_C_2, μ_W_3, μ_H_3,
μ_C_3 is the mass absorption coefficient for water, hydrogen, and carbon of the first, second, and third radiation measurement systems, respectively, and I_
1, I_2, and I_3 are the intensities of transmitted radiation in the first, second, and third radiation measurement systems, a_1, a_2, respectively.
, a_3 are constants. ) (6) The radiation source is Am-241, γ-rays near 60kev are sent to the first radiation measurement system, X-rays near 26kev are sent to the second radiation measurement system, and X-rays near 17kev are sent to the third radiation measurement system.
An apparatus for analyzing components of a sample to be measured according to claim 5, which is used in a radiation measurement system. (7) The sample to be measured further contains one selected from sulfur, nitrogen, nickel, and vanadium, and the radiation measurement system has four
An apparatus for analyzing components of a sample to be measured according to claim 1, which is a type of test sample.