Summary of the invention
The invention provides a kind of drilling fluid analytical equipment and analytical approach thereof, can directly carry out real-time quantitative analysis to drilling fluid, detection speed is fast, and is with high accuracy, and apparatus structure is simple, stable performance, lower cost.
The present invention realizes by the following technical solutions: a kind of drilling fluid analytical equipment, and this described device comprises computing machine, is characterized in, and described drilling fluid analytical equipment also comprises: sensor, direct supply, signal processing circuit; Described direct supply and sensor are connected to it working power are provided; Described signal processing circuit is connected with sensor, computing machine respectively; Described sensor output analog electrical signal also sends to signal processing circuit, signal processing circuit is carried out analog to digital conversion with analog electrical signal to be made it to become the Raman digital signal and sends to computing machine, computing machine is processed the Raman digital signal that receives, and by signal processing circuit and sensor transmitted in both directions control signal and data.
Above-mentioned a kind of drilling fluid analytical equipment is characterized in, described sensor comprises housing and the sapphire window that is arranged on the housing, also comprises excitation source, avalanche diode detection module, right-angle prism, dichroic filter in the housing; Described avalanche diode detection module and excitation source interval arranged side by side arranges; The corresponding interval with the avalanche diode detection module of described right-angle prism arranges; Described dichroic filter interval is tilting between right-angle prism and sapphire window, and corresponding with excitation source; Described excitation source, right-angle prism and dichroic filter, avalanche diode detection module form the light path in the sensor.
Above-mentioned a kind of drilling fluid analytical equipment is characterized in that the shape of cross section of described sapphire window is made as plane or cambered surface.
Above-mentioned a kind of drilling fluid analytical equipment is characterized in that described excitation source is the pulse excitation light source; The frequency of operation of described avalanche diode detection module and the pulsed frequency of excitation source are complementary.Above-mentioned a kind of drilling fluid analytical equipment, be characterized in, also comprise a radiator valve in the described housing, described radiator valve is arranged on the periphery of excitation source and avalanche diode detection module, and this radiator valve carries out thermostatic control to excitation source and the avalanche diode detection module of its inside.Above-mentioned a kind of drilling fluid analytical equipment is characterized in, also comprises one group of Raman optical filter in the housing of described sensor, and described one group of Raman optical filter is arranged between right-angle prism and the avalanche diode detection module; Described one group of Raman optical filter comprises at least a slice narrow band pass filter.Above-mentioned a kind of drilling fluid analytical equipment is characterized in, also comprises many group optical fiber in the housing of described sensor, and each described optical fiber connects excitation source, dichroic filter, right-angle prism, Raman optical filter, avalanche diode detection module successively.
Above-mentioned a kind of drilling fluid analytical equipment is characterized in, also comprises one or more groups lens in the housing of described sensor, and each described lens is arranged in the light path of sensor, regulates and optimize the light path of raman excitation light and Raman diffused light propagation.
A kind of drilling fluid analytical approach is used for above-mentioned a kind of drilling fluid analytical equipment, is characterized in that described analytical approach comprises following steps:
Step 1 in drilling fluid canal, is connected with this drilling fluid analytical equipment the sensor setting of described a kind of drilling fluid analytical equipment and opens corresponding power switch with external power source, direct supply provides working power to sensor;
Step 2, computing machine by signal processing circuit to the sensor settings parameter;
The sample emission raman excitation light of the setup parameter that step 3, sensor receive according to step 2 in the drilling fluid canal, and receive the sample Raman diffused light that scattering returns that is excited is converted to analog electrical signal with the light signal of Raman diffused light;
Step 4, sensor outputs to signal processing circuit with analog electrical signal, signal processing circuit is carried out analog to digital conversion to analog electrical signal, makes it to change into the Raman digital signal, and with this Raman digital signal to computer export.
Step 5, computing machine comprise the concentration of standard sample and the data of Raman scattering light intensity to a kind of hydrocarbons standard sample building database in this database; Computing machine compares analysis with the size of the Raman digital signal that receives and the Raman scattering light intensity data of database Plays sample, calculates the hydrocarbons concentration in the drilling fluid sample.
Above-mentioned a kind of drilling fluid analytical approach is characterized in that described step 3 also comprises:
Step 3.1, the excitation source of sensor is outwards launched raman excitation light according to the setup parameter that step 2 receives,
Step 3.2, because dichroic filter has the characteristic of the light of optionally reflection or a certain frequency range of transmission, the raman excitation light that is transmitted on the dichroic filter is reflected, and the raman excitation light of reflection propagates on the sample in the drilling fluid canal by sapphire window;
Step 3.3, sample is by the backward outer scattering Raman diffused light of Raman excitation optical excitation;
Step 3.4, the Raman diffused light that sample scatters propagates on the dichroic filter by sapphire window, because dichroic filter has the characteristic of the light of optionally reflection or a certain frequency range of transmission, dichroic filter is crossed in the Raman diffused light transmission, and propagates to right-angle prism;
Step 3.5, the Raman diffused light of propagating to right-angle prism is transmitted in the right-angle prism perpendicular to a right angle face of right-angle prism, and the inclined-plane that propagates into right-angle prism is inboard, Raman diffused light changes the direction of propagation after through the reflection on inclined-plane to be propagated to another right angle face of right-angle prism, and is transmitted to outside the right-angle prism at this right angle face;
Step 3.6, the Raman diffused light that changes the direction of propagation through right-angle prism propagates on the avalanche diode detection module, and the avalanche diode detection module is converted to analog electrical signal with the light signal of the Raman diffused light that receives.
Compared with prior art, the present invention has following beneficial effect:
A kind of drilling fluid analytical equipment of the present invention is owing to comprise sensor, direct supply, signal processing circuit, computing machine, and device structure is simple, and is with low cost, and is convenient to maintenance and maintenance in the routine work; Apparatus of the present invention have been saved a series of supplement production equipment such as degassed separating treatment owing to being provided with sensor and sensor setting directly being measured drilling fluid in drilling fluid canal, rate of breakdown is lower, stable performance; The present invention is owing to be provided with sensor, and in sensor, be provided with the avalanche diode detection module of excitation source and reception and conversion Raman scattering light signal, utilize hydrocarbons at Raman spectrum similar Raman shift to be arranged, and the characteristic that the Raman scattering light intensity is directly proportional with sample concentration, realization is measured the real-time quantitative of hydrocarbons concentration in the drilling fluid, analysis speed is fast, accuracy is high, can satisfy petroleum prospecting and coal-seam gas, the petroleum exploration domains such as non-conventional gas exploitation such as shale gas, and geologic media monitoring, the laboratory, the needs in the fields such as chemical real-time analysis.
Embodiment
Below in conjunction with accompanying drawing, by describing a better specific embodiment in detail, the present invention is further elaborated.
Consult shown in the accompanying drawing 2, a kind of drilling fluid analytical equipment of the present invention comprises: sensor 1, direct supply 2, signal processing circuit 3, computing machine 4.Direct supply 2 is connected to it with sensor 1 working power is provided; Signal processing circuit 3 is connected with sensor 1, computing machine 4 respectively; Sensor 1 output analog electrical signal also sends to signal processing circuit 3, signal processing circuit 3 is carried out analog to digital conversion with analog electrical signal to be made it to become the Raman digital signal and sends to computing machine 4, the Raman digital signal that 4 pairs in computing machine receives is processed, and by signal processing circuit 3 and sensor 1 transmitted in both directions control signal and data.
Sensor 1 is core component of the present invention, and it is arranged in the drilling fluid canal 5, directly contacts with the drilling fluid sample, carries out the measurement of hydrocarbon content.Consult shown in the accompanying drawing 3, sensor 1 comprises housing 10 and the sapphire window 11 that is arranged on the housing 10.Sapphire window 11 is sensor 1 unique optical elements that contact with the drilling fluid sample, because sapphire has corrosion-resistant, high-intensity characteristics, so it is optical window material desirable under harsh and unforgiving environments, the complex working condition.The shape of cross section of sapphire window 13 is made as plane or cambered surface such as shapes such as sphere, semisphere, convex surfaces, its shape of cross section can be adjusted as required, be set to cambered surface and can make sapphire window 13 have the function of optical focusing, simplify the one-piece construction of sensor 1.In the present embodiment, select spherical sapphire lens as sapphire window 13 reaching the simplification optical element, optimize the purpose of the structure of sensor 1.
Comprise excitation source 12, avalanche diode (APD) detection module 13, right-angle prism 14, dichroic filter 15 in the housing 10.Avalanche diode detection module 13 arranges with excitation source 12 intervals arranged side by side; Right-angle prism 14 arranges with avalanche diode detection module 13 corresponding intervals; Dichroic filter 15 intervals are tilting between right-angle prism 14 and sapphire window 11, and corresponding with excitation source 12.The light path that excitation source 12, right-angle prism 14 and dichroic filter 15, avalanche diode detection module 13 form in the sensors 1.The raman excitation light that excitation source 12 sends is through dichroic filter 15 and by being radiated at after the sapphire window 11 on the sample 17, sample 17 is excited the Raman diffused light that scatters by being received by avalanche diode detection module 13 through dichroic filter 15 and right-angle prism 14 after the sapphire window 11, and is converted to analog electrical signal.
Excitation source 12 is for the invention provides raman excitation light.Excitation source 12 is the pulse excitation light source, and its pulsed frequency scope is 1kHz ~ 10MHz.Owing to usually in drilling fluid, there is the material that has in a large number fluorescence, the large several orders of magnitude of strength ratio Raman scattering light intensity of fluorescence, the accuracy in detection of meeting severe jamming sensor 1, principle according to photoluminescence, the generation of fluorescence has about a few microsecond to arrive several milliseconds delay, and Raman scattering is to produce moment, therefore utilize the instantaneity of Raman scattering and the hysteresis quality of fluorescence, select the long pulse excitation light source of wavelength as excitation source 12, can avoid hyperfluorescenceCeng Yongminggaoyingguang material in the drilling fluid to the interference of the faint Raman diffused light of sample scattering.The excitation source 12 preferred pulsed laser light sources that use visible light or near-infrared band can also be selected other various pulse excitation light sources.The pulse excitation light source of visible light-near-infrared band has two advantages: the one, and the laser technique comparative maturity of this wave band has very high cost performance; The 2nd, select visible light or near infrared light can reduce fluorescence to the interference of Raman scattering.In the present embodiment, select wavelength be the red visible light pulses laser instrument of 660nm as excitation source 12, power is not less than 100mW.
Avalanche diode detection module 13 is converted to analog electrical signal with the light signal that receives, and it utilizes avalanche effect can amplify fast and detect faint Raman scattering light signal.The operating frequency range of avalanche diode detection module 13 is 1kHz ~ 10MHz, and the pulsed frequency of its frequency of operation and excitation source 12 is complementary.Avalanche diode detection module 13 has very high frequency of operation, utilize the characteristics of the hysteresis quality of the instantaneity of Raman scattering and fluorescence, before fluorescence produces, Raman diffused light is detected, can avoid fluorescent material in the drilling fluid to the interference of the detection of Raman diffused light, improve the signal to noise ratio (S/N ratio) of light signal.In the present embodiment, avalanche diode detection module 13 is selected the APD detection module C5331 of shore pine.
Housing 10 is interior can also to arrange a radiator valve 18, radiator valve (18) is arranged on the periphery of excitation source (12) and avalanche diode detection module (13), is opposite to its inner excitation source 12 and avalanche diode detection module 13 carries out thermostatic control.The luminous power of excitation source 12 is relevant with its working temperature with glow frequency, experiment showed, in the present embodiment, and 5 ℃ of the every variations of temperature, the Raman excitation light wavelength that excitation source 12 sends can change 1nm, and its optical output power can change about 5mW.Therefore for the consistance of the stable of the luminous power that guarantees excitation source 12 and the Raman excitation optical wavelength sent, must carry out thermostatic control to excitation source 12.Simultaneously, in order to improve drilling fluid is detected the accuracy of analyzing, select in the present embodiment high sensitivity avalanche diode detection module 13 at a high speed, it is carried out thermostatic control, can make sensor 1 reliable and stable work in a wider ambient temperature range.In the present embodiment, usage ratio-integral-derivative controller (Proportion Integration Differentiation, the PID controller), its temperature-controlled precision can reach 0.2 ℃, the error of the Raman excitation optical wavelength that makes the luminous power of the excitation source 12 that is caused by temperature and send has improved the job stability of sensor 1 and the environmental suitability of drilling fluid analytical equipment of the present invention all less than per mille.
The raman excitation light that excitation source 12 sends is through dichroic filter 15 and by being radiated at after the sapphire window 11 on the sample 17, and the Raman diffused light that sample 17 is inspired is by being received by avalanche diode detection module 13 through dichroic filter 15 and right-angle prism 14 after the sapphire window 11.Dichroic filter 15 has the characteristic of the light of optionally reflection or a certain frequency range of transmission.Select suitable dichroic filter 16 according to user demand, can optimize structure and the inner light path of sensor 1.In the present embodiment, dichroic filter 16 can reflect raman excitation light, and the transmission Raman diffused light.Right-angle prism 14 arranges with avalanche diode detection module 13 corresponding intervals; Can also use by a plurality of right-angle prisms interval the prism group that forms is set, arrange with avalanche diode detection module 13 corresponding intervals, to optimize light path.In the present embodiment, select one with the right-angle prism 14 of optical anti-reflective film, so that maximize by the Raman diffused light of right angle lens 14.
The housing 11 of sensor 1 is interior can also to arrange one group of Raman optical filter 16, and this group of Raman optical filter 16 is arranged between right-angle prism 14 and the avalanche diode detection module 13, comprises at least a slice narrow band pass filter.This narrow band pass filter must have very high optical density (Optical Density, OD), its optical density value is greater than 4, when guaranteeing the Raman scattering light transmission rate, the light that reduces as far as possible other wave band passes through, thereby reduce elastic scattering (Ruili line) to the interference of Raman diffused light, improve the signal to noise ratio (S/N ratio) of the light signal that is sent to avalanche diode detection module 13.In the present embodiment, according to the red visible light pulses laser instrument of selecting and the feature Raman shift of the hydrocarbon key chattering of alkane, selected two optical density value to form one group of Raman optical filter 16 greater than 4 narrow band pass filter for the Raman scattering optical band of hydrocarbons.
Housing 10 interior can also the settings of sensor 1 are organized optical fiber (not marking in the accompanying drawing) more, and each optical fiber connects excitation source 12, dichroic filter 15, right-angle prism 14, Raman optical filter 16, avalanche diode detection module 13 successively.Wherein one group of optical fiber sends the moral raman excitation light with excitation source 12 and transfers to dichroic filter 15; Wherein another group optical fiber receives the Raman diffused light through right-angle prism 14 reflections, and transfers to avalanche diode detection module 13.Can make up long distance, flexible light path at the sensor 1 interior optical fiber that arranges.
The housing 10 of sensor 1 is interior can also to arrange one or more groups lens (not marking in the accompanying drawing), each is organized in the light path that lens are arranged on the sensor 1 that excitation source 12, dichroic filter 15, right-angle prism 14, Raman optical filter 16, avalanche diode detection module 13 form, in order to regulate and to optimize the light path of raman excitation light and Raman diffused light, improve the detection quality of Raman scattering light signal.
Direct supply 2 is connected to it with sensor 1 working power is provided, direct supply 2 be arranged on computing machine 4 near, with the potential safety hazard of avoiding execute-in-place to bring.In the present embodiment, this direct supply 2 uses the direct supply of 24V.
Signal processing circuit 3 is connected with sensor 1, computing machine 4 respectively, respectively to sensor 1 and computing machine 4 transmitted signals, and receives the signal that comes from sensor 1 and computing machine 4.Signal processing circuit 3 be arranged on computing machine 4 near, it can be connected with sensor 1 by wired or wireless multiple communication modes, and can arrange according to various actual conditions such as field working conditions; This signal processing circuit 3 can be used the wired connection mode and access computing machine 4 by many general interfaces such as 232 serial ports or USB interface, process thereby the signal of sensor 1 is sent to computing machine 4, the parameter information that perhaps computing machine 4 is sent sends to sensor 1 and arranges and adjust.Signal processing circuit 3 is the circuit module of prior art.
Computing machine 4 is the computing machine of prior art, inner the Raman digital signal that special-purpose software and database send signal processing circuit 3 can be set carry out analytical calculation, and send a signal to excitation source frequency, the light intensity that sensor 1 is adjusted sensor 1, the parameters such as control temperature by signal processing circuit 3.
Consult shown in the accompanying drawing 4, a kind of drilling fluid analytical approach, be used for above-mentioned a kind of drilling fluid analytical equipment, comprise following steps: step 1, the sensor 1 of a kind of drilling fluid analytical equipment of the present invention is arranged in the drilling fluid canal 5, this drilling fluid analytical equipment is connected with external power source and opens corresponding power switch, direct supply 2 provides working power to sensor 1;
Step 2, computing machine 4 is set excitation source frequency, light intensity, the parameters such as control temperature by 3 pairs of sensors of signal processing circuit 1.
The sample 17 emission raman excitation lights of the parameter that step 3, sensor 1 receive according to step 2 in the drilling fluid canal 5, and receive sample 17 Raman diffused light that scattering returns that is excited are converted to analog electrical signal with the light signal of Raman diffused light;
Consult shown in the accompanying drawing 5, step 3 also comprises:
Step 3.1, the excitation source 12 of sensor 1 is outwards launched raman excitation light according to the setup parameter that step 2 receives,
Step 3.2, because dichroic filter 15 has the characteristic of the light of optionally reflection or a certain frequency range of transmission, the raman excitation light that is transmitted on the dichroic filter 15 is reflected, and the raman excitation light of reflection shines on the sample 17 in the drilling fluid canal 5 by sapphire window 11;
Step 3.3, sample 17 is by the backward outer scattering Raman diffused light of Raman excitation optical excitation;
Step 3.4, the Raman diffused light that sample 17 scatters propagates on the dichroic filter 15 by sapphire window 11, because dichroic filter 15 has the characteristic of the light of optionally reflection or a certain frequency range of transmission, dichroic filter 15 is crossed in the Raman diffused light transmission, and propagates to right-angle prism 14;
Step 3.5, the Raman diffused light of propagating to right-angle prism 14 is transmitted in the right-angle prism perpendicular to a right angle face of right-angle prism 14, and the inclined-plane that propagates into right-angle prism 14 is inboard, Raman diffused light changes the direction of propagation after through the reflection on inclined-plane to be propagated to another right angle face of right-angle prism 14, and is transmitted to outside the right-angle prism 14 at this right angle face;
Step 3.6, the Raman diffused light that changes the directions of propagation through right-angle prism 14 shine on the avalanche diode detection module 13 after through Raman optical filter 16, and avalanche diode detection module 13 is converted to analog electrical signal with the light signal of the Raman diffused light that receives.Step 4, sensor 1 outputs to signal processing circuit 3 with analog electrical signal, and 3 pairs of analog electrical signals of signal processing circuit carry out analog to digital conversion, make it to change into the Raman digital signal, and this Raman digital signal is exported to computing machine 4.Step 5, utilize the intensity of Raman diffused light (Stockes line) and the relational expression of sample concentration:
P=kcVΩP
0 (1),
Wherein, P is the Raman scattering light intensity; K is the Raman scattering factor of sample; C is the concentration of sample; V is the volume of raman excitation light and sample generation Raman scattering; Ω is the solid angle that receives Raman diffused light; P
0It is the luminous power of raman excitation light.For a certain Raman sensor, the luminous power P of raman excitation light
0, Raman scattering factor k, the sample solid angle Ω that produces the volume V of Raman scattering and receive Raman scattering is fixed value, so the concentration c of the Raman scattering light intensity P that receives and sample is proportional.
Because the feature Raman spectrum of the hydrocarbon key C-H vibration of various hydrocarbons has similar Raman shift, therefore can use a certain hydrocarbons as standard sample various hydrocarbons to be measured, thereby realize the quantitative measurment to the hydrocarbons concentration in the drilling fluid.Take a certain hydrocarbons as standard sample, 4 pairs of these hydrocarbons standard sample building databases of computing machine comprise the concentration of standard sample and the data of Raman scattering light intensity in the database.In the present embodiment, with the standard sample of normal hexane as the hydrocarbons in the drilling fluid, accompanying drawing 6 is depicted as the testing result to the sample that contains the variable concentrations normal hexane, horizontal ordinate is the normal hexane concentration in the sample, ordinate is the Raman scattering light intensity, as can be seen from Figure 4, the normal hexane concentration in Raman scattering light intensity and the sample has good linear dependence relation, its linearly dependent coefficient R=0.9931.Computing machine 4 compares analysis with the size of the Raman digital signal that receives and the Raman scattering light intensity data of database Plays sample, calculates the hydrocarbons concentration in the drilling fluid sample.Because the present invention is arranged in the drilling fluid canal 5 and directly the drilling fluid sample is measured, and analysis speed is fast, therefore can realize the real-time quantitative of the hydrocarbons concentration in the drilling fluid is measured.
In sum, apparatus of the present invention are simple in structure, and are with low cost, are convenient to maintenance and maintenance in the routine work; And owing to being provided with sensor and sensor setting directly being measured drilling fluid in drilling fluid canal, saved a series of supplement production equipment such as degassed separating treatment, rate of breakdown is lower, stable performance; The present invention is owing to be provided with sensor, and in sensor, be provided with the avalanche diode detection module of excitation source and reception and conversion Raman scattering light signal, utilize hydrocarbons at Raman spectrum similar Raman shift to be arranged, and the characteristic that the Raman scattering light intensity is directly proportional with sample concentration, realization is measured the real-time quantitative of hydrocarbons concentration in the drilling fluid, analysis speed is fast, accuracy is high, can satisfy petroleum prospecting and coal-seam gas, the petroleum exploration domains such as non-conventional gas exploitation such as shale gas, and geologic media monitoring, the laboratory, the needs in the fields such as chemical real-time analysis.
Although content of the present invention has been done detailed introduction by above preferred embodiment, will be appreciated that above-mentioned description should not be considered to limitation of the present invention.After those skilled in the art have read foregoing, for multiple modification of the present invention with to substitute all will be apparent.Therefore, protection scope of the present invention should be limited to the appended claims.