CN103364483A - System and method for realizing linkage of independent instruments in mass spectrometry analysis system - Google Patents

System and method for realizing linkage of independent instruments in mass spectrometry analysis system Download PDF

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CN103364483A
CN103364483A CN2013102991080A CN201310299108A CN103364483A CN 103364483 A CN103364483 A CN 103364483A CN 2013102991080 A CN2013102991080 A CN 2013102991080A CN 201310299108 A CN201310299108 A CN 201310299108A CN 103364483 A CN103364483 A CN 103364483A
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laser ablation
instrument
quality
interlock
trigger pip
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CN103364483B (en
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黄超
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Institute of Geology and Geophysics of CAS
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Institute of Geology and Geophysics of CAS
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Abstract

The invention discloses a system and a method for realizing linkage of independent instruments in a mass spectrometry analysis system. The system comprises the independent instruments and a digital input/output interface card, wherein the independent instruments comprise a mass analysis instrument and a laser ablation instrument; the linkage of the independent instruments in the mass spectrometry analysis system comprises a linkage trigger mode and a linkage interruption mode. Through the mode, the laser ablation process and the mass analysis process can be linked to realize automatic analysis of a sample, so that the mass spectrometry analysis system integrally has higher efficiency and better reliability, and each independent instrument in the mass spectrometry analysis system can also automatically, efficiently and stably operate.

Description

A kind of system and method for realizing independent instrument interlock in the mass spectrometry system
Technical field
The present invention relates to mass spectrometry system, particularly a kind of system and method for realizing independent instrument interlock in the mass spectrometry system.
Background technology
" a workman wants to do his work well, must first sharpen his tools ".Advanced scientific instruments equipment is the prerequisite of technological innovation and knowledge innovation, also is one of body matter of innovation research.Mass spectrometer is as one of the instrument of most significant end in the scientific instrument, in many hot fields such as geology, biological chemistry, materia medica, medical science, petrochemical complex, the energy, environmental protection and food processing, have more and more significant effect, the development level of mass-spectrometric technique and mass spectrometer has determined the development of related discipline to a certain extent.Learn the field on ground, mass spectrometer is being played the part of important role equally.Take isotope mass spectrometer as example, at the beginning of setting up, its technology just is used in the middle of the earth science research, and through the development of many decades, this technology is widely applied in ground is learned, has promoted foundation and the development of isotope geology, isotope geochemistry.Current isotope mass spectrometer is mainly used in the mensuration of nature natural element isotopics, geologic chronology, and rock, the mineral origin cause of formation and Material Source thereof, the earth's crust, earth mantle develop, and Tectonic Evolution, is looked for the field such as ore deposit at geologic prospecting.
At present, study a plurality of Disciplinary Frontiers at the earth and planetary science, as the earth and planet develop in early days, collision orogenic belts formation and evolution, Lithospheric Structure process, ultra-large type origin of ore deposit, Paleoclimatic Changes etc., the competition of its research level has entered micro-nano scale, by the research microprocess, disclose the micromanagement mechanism of Macroscopic Process, such as trace element and isotope partition and again equilibrium process and the mechanism research etc. of micro-nano scale.Therefore, the isotope of in-situ micro area trace and geochemistry of trace element analysis have become the important fulcrum of modern Solid Earth Sciences development.Different from conventional Isotope Analysis Method, the microcell isotope analysis has disclosed a large amount of microscopic geological information of covering in the total analysis effectively, make us can directly observe element or isotopic variation in the geological process, in other words, these isotope record geological process starting, the overall process that develops, finish.These elements or the isotope original position distribution record in mineral the development of these geological processes, mensuration to them can make our these geological processes of inverting, thereby understand their cause, mechanism, controlling factor, developing direction, be our final purpose service, as becoming ore deposit mechanism, the changing of physiognomy, the evolution of shell curtain, hazard prediction etc.
The mass spectrometry system that is usually used in the analysis of geology in-situ micro area for example can be laser ablation-accept inductivity coupled plasma mass spectrometry system (Laser Ablation – Multi-Collector Inductively Coupled Plasma Mass Spectrometry is called for short LA-MC ICP MS) more.This system is comprised of the two large divisions, also is analytical instrument of quality and laser ablation configuration of instrument.Solid sample is sent into analytical instrument of quality by carrier gas after by laser ablation and is carried out ionization in the laser ablation instrument, thereby finishes the analysis of solid sample.Analytical instrument of quality and laser ablation instrument in the LA-MC ICP MS system, have separately and independently control software, when testing, need the experimenter according to two independent instrument of certain sequential operation (also being analytical instrument of quality and laser ablation instrument).Take Inst of Geology and Geophysics, Chinese Academy of Sciences accept the inductivity coupled plasma mass spectrometry laboratory as example more, be to guarantee the utilization ratio of instrument, the laser ablation in laboratory-accept inductivity coupled plasma mass spectrometry system running 24 hours long-term every days more.And in the middle of testing for a long time, rely on the method for degrading a little of manually choosing the laser ablation instrument to exist obvious drawback: at first to be the conventional efficient problem, because manually choose and degrade a little consuming timely and efficient is lower, so the automaticity that how to improve experiment is to need the technical barrier that solves always; Next is integrity problem, because geological sample is relatively precious often, and for a long time in the experiment, owing to the reasons such as fatigue cause the reconnaissance mistake of degrading a little possibly, thereby cause the waste of sample, so the reliability of manual type is relatively poor.
Therefore need that a kind of efficient is higher, the system and method for independent instrument interlock in the realization mass spectrometry system of better reliability, thereby realize the automatical and efficient stable operation of each independent instrument in the mass spectrometry system.
Summary of the invention
Fundamental purpose of the present invention provides the system and method for independent instrument interlock in the higher realization mass spectrometry system of a kind of efficient.
Another object of the present invention provides the system and method for independent instrument interlock in a kind of realization mass spectrometry system of better reliability.
In order to achieve the above object, the present invention proposes a kind of system that realizes independent instrument interlock in the mass spectrometry system, it is characterized in that, the system of described interlock comprises independent instrument and numeral input/digital output interface card, described independent instrument comprises analytical instrument of quality and laser ablation instrument, wherein
Described analytical instrument of quality comprises sampling system, ion gun, analyzer, detecting device and computing machine; Described sampling system is sent into sample and is made its ionization in the described ion gun; The sample ions of described analyzer after to ionization separated by the mass/charge ratio; The sample ions of described detecting device after to the separation of described analyzer output detects; Described computing machine receives the sample signal of described detecting device output and it is carried out Storage and Processing;
Described laser ablation instrument comprises laser instrument, lens, object lens and degrades the pond; The laser that described laser instrument sends is focused to the described sample surfaces that degrades in the pond through after the described lens shaping by described object lens, and the sample particle that sample surfaces is degraded is out transferred in the described sampling system of described analytical instrument of quality by carrier gas;
Described numeral input/digital output interface card is connected with described laser ablation instrument with described analytical instrument of quality respectively by USB interface, and described numeral input/digital output interface card is used for transmitting trigger pip and look-at-me; Described trigger pip comprises quality analysis trigger pip and laser ablation trigger pip, and described look-at-me comprises quality analysis look-at-me and laser ablation look-at-me;
The system of independent instrument interlock comprises interlock trigger mode and interlock interrupt mode in the described realization mass spectrometry system, wherein:
Described interlock trigger mode comprises: described analytical instrument of quality confirms to receive the quality analysis trigger pip that described laser ablation instrument sends, and after described laser ablation instrument confirms to receive the laser ablation trigger pip that described analytical instrument of quality sends, described laser ablation instrument begins sample surfaces is degraded, and described analytical instrument of quality begins the sample that imports into is analyzed;
Described interlock interrupt mode comprises: described laser ablation instrument then sends the quality analysis look-at-me to described analytical instrument of quality if break down in the process of degrading, make it stop analytic process; Described analytical instrument of quality then sends the laser ablation look-at-me to described laser ablation instrument if break down in the process of analyzing, make it stop denudation.
Further, described analytical instrument of quality also comprises the quality analysis module, and described laser ablation instrument also comprises the laser ablation module, wherein,
In described interlock trigger mode, described quality analysis module and laser ablation module are respectively applied to confirm to receive described quality analysis trigger pip and laser ablation trigger pip;
In described interlock interrupt mode, described quality analysis module and laser ablation module are respectively applied to the quality of reception and analyze look-at-me and laser ablation look-at-me.
Further, described independent instrument is based in described interlock interrupt mode that operation to the control of the control software on the described independent instrument realizes, described independent instrument is based on the MFC of Windows, and the operation of described control is the action that realizes this control by the handle that obtains this control; Described numeral input/digital output interface jig has the input of 16 railway digitals and the output of 16 railway digitals, compatible 5VTTL level.
Further, the trigger pip of transmitting in the described numeral input/digital output interface card is transistor-transistor logic level (TTL) signal; Described analyzer comprises magnetic field or electric field; Described carrier gas comprises He gas; Described computing machine also is used for the system of described interlock is controlled, and stores standard diagram on it, and the described sample signal and the described standard diagram that are used for obtaining are retrieved contrast, to provide corresponding structural formula.
Further, described mass spectrometry system comprises laser ablation-accept inductivity coupled plasma mass spectrometry system or laser ablation-quadrupole rod inductivity coupled plasma mass spectrometry system more; Described analytical instrument of quality also comprises vacuum system, electrical system and data handling system, wherein said vacuum system is used to the ion of generation that vacuum environment is provided, described electrical system is used for providing power supply, and described data handling system is used for inputting described computing machine after the processing that sample signal to described detecting device output comprises denoising and integration again.
The present invention also provides a kind of method that realizes independent instrument interlock in the mass spectrometry system, the system of described interlock comprises independent instrument and numeral input/digital output interface card, described independent instrument comprises analytical instrument of quality and laser ablation instrument, it is characterized in that, said method comprising the steps of:
Step 1: choose N laser ablation point in the laser ablation module in the laser ablation instrument, N is more than or equal to 3, these x, y and z three-dimensional coordinates that degrade a little are recorded in the array, simultaneously default following at least parameter: a) each frequency of degrading of degrading a little is a1, and unit is Hz; B) each number of times that degrades that degrades a little is a2 time; C) the laser ablation energy is a3 in the laser ablation instrument, and unit is that milli is burnt; D) the laser ablation instrument arrives each to degrade the needed time of a position is a4 second; E) be a5 second lock in time;
Step 2: the laser ablation module of laser ablation instrument confirms that the laser ablation instrument is ready, and sends the quality analysis trigger pip by numeral input/digital output interface card to analytical instrument of quality;
Step 3: in analytical instrument of quality, open the sample sequence analytical model, set respectively N analysis mode and instrument tuner parameters that degrades a little;
Step 4: the quality analysis module in the analytical instrument of quality confirms that analytical instrument of quality is ready, and sends the laser ablation trigger pip by numeral input/digital output interface card to the laser ablation instrument;
Step 5: the quality analysis module in the analytical instrument of quality confirms to receive the quality analysis trigger pip;
Step 6: the laser ablation module in the laser ablation instrument confirms to receive the laser ablation trigger pip;
Step 7: mass spectrometer begins first is degraded under the sample sequence analytical model and a little carries out quality analysis, this moment, the laser ablation module of laser ablation instrument moved to the three-dimensional platform of laser ablation instrument that selected first degrades a little x, y and z three-dimensional coordinate position in the step 1, and began sample is carried out laser ablation according to the parameter of presetting;
Step 8: in the process of laser ablation and quality analysis, if analytical instrument of quality or laser ablation instrument break down, then quality analysis module and laser ablation module send laser ablation look-at-me and quality analysis look-at-me to the other side respectively, so that the process of laser ablation and quality analysis interrupts protecting sample, and enter step 9; If analytical instrument of quality and laser ablation instrument do not break down, then after having carried out a laser ablation and quality analysis of degrading a little, enter step 9;
Step 9: analytical instrument of quality and laser ablation instrument quality analysis module and laser ablation module separately begins to carry out separately whether ready inspection of state;
Step 10: after analytical instrument of quality and laser ablation instrument standby condition are ready, send respectively laser ablation trigger pip and quality analysis trigger pip by numeral input/digital output interface card to the other side; Quality analysis module in the analytical instrument of quality confirms to receive the quality analysis trigger pip; Laser ablation module in the laser ablation instrument confirms to receive the laser ablation trigger pip;
Step 11: mass spectrometer begins the next one degraded under the sample sequence analytical model and a little carries out quality analysis, this moment the laser ablation instrument the laser ablation module with the three-dimensional platform of laser ablation instrument move in the step 1 selected degrade a little in next x, y and z three-dimensional coordinate position of degrading a little, and begin sample is carried out laser ablation according to the parameter of presetting;
Step 12: repeating step 8-step 11, until individual the degrading of N a little is disposed, whole flow process finishes.
Further, described numeral input/digital output interface card is connected with described laser ablation instrument with described analytical instrument of quality respectively by USB interface, and described numeral input/digital output interface card is used for transmitting trigger pip and look-at-me; Described trigger pip comprises quality analysis trigger pip and laser ablation trigger pip, and described look-at-me comprises quality analysis look-at-me and laser ablation look-at-me; The interlock of independent instrument comprises interlock trigger mode and interlock interrupt mode in the described mass spectrometry system, wherein: described interlock trigger mode comprises: described analytical instrument of quality confirms to receive the quality analysis trigger pip that described laser ablation instrument sends, and after described laser ablation instrument confirms to receive the laser ablation trigger pip that described analytical instrument of quality sends, described laser ablation instrument begins sample surfaces is degraded, and described analytical instrument of quality begins the sample that imports into is analyzed; Described interlock interrupt mode comprises: described laser ablation instrument then sends the quality analysis look-at-me to described analytical instrument of quality if break down in the process of degrading, make it stop analytic process; Described analytical instrument of quality then sends the laser ablation look-at-me to described laser ablation instrument if break down in the process of analyzing, make it stop denudation.
Further, mass spectrometer can be realized startup to the quality analysis process by controlling startup control on its software interface when receiving the quality analysis trigger pip; Mass spectrometer is when receiving the quality analysis look-at-me, can realize termination to the quality analysis process by controlling termination control on its software interface, the corresponding handle that wherein starts control and stop control is obtained in advance by the mass spectrometer based on the MFC of Windows.
Further, the laser ablation instrument when receiving the laser ablation trigger pip, can by control beginning control, the D coordinates value control on its software interface and move to the target control realize respectively to the laser ablation process startup, degrade the selection of a position coordinates and will degrade a little to move to and degrade the position; The laser ablation instrument is when receiving the laser ablation look-at-me, can realize termination to the laser ablation process by controlling end control on its software interface, the corresponding handle that wherein begins control, D coordinates value control, moves to the target control and finish control is obtained in advance by the laser ablation instrument based on the MFC of Windows.
Further, N is 100 in N the laser ablation point, and degrading frequency a1 is 8Hz, and degrading number of times is for a2 time 216 times, and laser ablation energy a3 is that 80 millis are burnt, and time a4 second is 30 seconds, and time a5 second is 3 seconds; N analysis mode of degrading a little comprises that setting each degrades 200 detections of collection data, and each detects data acquisition time is 0.131 second; Fault in the described analytical instrument of quality comprises: ion gun died, lens combination voltage failure and vacuum failure; Fault in the described laser ablation instrument comprises: laser energy decay, laser three-D platform fault and laser optical path blanket gas fault.
Compared with prior art; the present invention has the following advantages: the present invention forms the interlock network by numeral input/digital output interface card with the independent instrument that comprises analytical instrument of quality and laser ablation instrument in the mass spectrometry system; and by this numeral input/digital output interface card transmission trigger pip and look-at-me; and make realize the cooperatively interacting triggering work or interrupt protection of each independent instrument in the mass spectrometry system by interlock trigger mode and interlock interrupt mode; for artificial (for example manually choose degrade a little and analyze) mode; owing to can realize interlock between the independent instrument; therefore can be so that the process of laser ablation and quality analysis links; realize the automatic analysis of sample; thereby so that mass spectrometry system efficient is higher on the whole; better reliability is also so that each independent instrument can automatical and efficient stable operation in the mass spectrometry system.
Description of drawings
For clearer explanation technical scheme of the present invention, the accompanying drawing of required use was done simple the introduction during the below will describe embodiment, apparent, accompanying drawing in the following describes only is some embodiments of the present invention, for those of ordinary skills, under the prerequisite of not paying creative work, can also obtain according to these accompanying drawings other accompanying drawing.
Fig. 1 is the structural representation of analytical instrument of quality in the mass spectrometry system of the present invention;
Fig. 2 is the structural representation of laser ablation instrument in the mass spectrometry system of the present invention;
Fig. 3 is the structural representation of the system of independent instrument interlock in the realization mass spectrometry system of the embodiment of the invention 1;
Fig. 4 is the schematic flow sheet of the method for independent instrument interlock in the realization mass spectrometry system of the embodiment of the invention 2.
Fig. 5 is the synoptic diagram of software interface on the analytical instrument of quality of the present invention;
Fig. 6 is the synoptic diagram of software interface on the laser ablation instrument of the present invention.
Fig. 7 is the software interface synoptic diagram that the present invention realizes independent instrument interlock in the mass spectrometry system.
Embodiment
Below in conjunction with the accompanying drawing in the embodiment of the invention; technical scheme in the embodiment of the invention is carried out clear, complete description; obvious described embodiment only is a part of embodiment of the present invention; not whole embodiment; based on the embodiment among the present invention; those of ordinary skills belong to the scope of protection of the invention not paying the every other embodiment that obtains under the creative work prerequisite.
Shown in Fig. 1-2, mass spectrometry system for example can adopt laser ablation-accept inductivity coupled plasma mass spectrometry system more among the present invention, wherein analytical instrument of quality for example adopts " many receiving inductances coupled plasma mass spectrometer ", the laser ablation instrument for example adopts " 193nm quasi-molecule gas laser degrades system ", and these two corresponding introduction about the constructions of instrument are as follows:
1, analytical instrument of quality is the quality analysis (being also referred to as mass spectrometer) of carrying out sample.Its principle is to convert sample molecule to ion, and the mass/charge of pressing ion is than (m/z) isolating ions, and carries out a kind of instrument of qualitative and quantitative analysis.The analytical instrument of quality here is based on magnetic fields and realizes quality analysis, particularly, when the ion of different quality number moves in magnetic field, its moving radius is different, we place detecting device in different positions, just can detect the ionic strength of different quality number, thereby realize the quality analysis of ion.Analytical instrument of quality generally is comprised of sampling system, ion gun, analyzer, detecting device and computing machine, also comprises the utility appliance such as vacuum system, electrical system and data handling system.As shown in Figure 1, be specifically described as follows:
(1) sampling system: minute storage tank sample introduction, probe sample introduction, chromatogram sample introduction.Mass spectral:mass spectrographic sample generally will be vaporized, again ionization.The available direct inlet probe of the fluid sample that solid and boiling point are higher (sterling) (sample introduction of for example popping one's head in) is sent into sample in the ion gun.Low boiling sample (sterling) can pass through storage tank system (for example storage tank sample introduction) and import.Impure sample will be used chromatogram and GC-MS, is by the chromatogram sample introduction;
(2) ion gun: make sample produce the device of ion ion gun;
(3) analyzer (also being mass analyzer): the ion that ion gun produces is separated than (m/z) by mass/charge by it.Mass analyzer has: magnetic field and electric field etc.;
(4) detecting device: ion detector is comprised of gatherer and amplifier.The signal that is directly proportional with the ion current abundance is given birth in the positive ion miscarriage of beating on gatherer;
(5) computing machine: the effect of computing machine has two aspects.The one, for the control of instrument, the 2nd, as reception, the Storage and Processing of data.Can also there be standard diagram in the computing machine, be used for sample data and does automatically retrieval, and provide suitable structural formula.
(6) utility appliance such as vacuum system, electrical system and data handling system, wherein vacuum system can be the ion that sample produces vacuum environment is provided, electrical system can be analytical instrument of quality power supply is provided, and described data handling system is used for inputting described computing machine after the processing that sample signal to described detecting device output comprises denoising and integration again.
2, the laser ablation instrument is with laser (bundle spot size is micron order) bundle spot bombardment solid sample surface, because the effect of laser energy, the solid sample ablated surface is become molten condition, sample can become aerosol particle, then by carrier gas (for example helium) these aerosol particles are transmitted, the ionisation region that transfers to analytical instrument of quality by transmission pipeline is carried out ionization with aerosol sample, so that quality analysis is realized in the back.Specifically, after the shaping of the laser that laser instrument (laser) sends through lens (Lens), focused to sample (Sample) surface of degrading in the pond (Cell) by object lens (Objective).The sample particle that is degraded is out transferred to mass spectrometric ion gun place by carrier gas (Carrier Gas) and is ionized, so the laser ablation instrument also can be regarded as the injector of analytical instrument of quality, is applicable to solid sample.As shown in Figure 2.
Embodiment 1
As Figure 1-3, the embodiment of the invention 1 provides a kind of system that realizes independent instrument interlock in the mass spectrometry system.The system of this interlock adopts DI/DO(Data Input/Data Output, also i.e. numeral input/numeral output) interface (for example DI/DO interface card) is linked together independent instrument (for example analytical instrument of quality, laser ablation instrument).The DI/DO interface for generation of with transmit trigger pip and look-at-me (here for example analytical instrument of quality or laser ablation instrument ready or when interrupting, can make it produce the Transistor-Transistor Logic level of 5V to DI/DO interface card transmitted signal, laser ablation instrument or analytical instrument of quality can receive this level subsequently, thereby carry out triggering work or interruption of work), it is an interface card, on 16 road DI and 16 road DO are arranged, compatible 5VTTL level, be connected with analytical instrument of quality and laser ablation instrument by USB, its signal produces and transmits the software control of being installed at mass spectrometer and laser ablation instrument by the present invention.Concrete coordinated operation mode is such: adopt the DI/DO interface, be connected respectively to analytical instrument of quality and laser ablation instrument, write respectively two software kits in analytical instrument of quality and laser ablation instrument.Thus, the present invention realizes that the hardware components of the system of independent instrument interlock in the mass spectrometry system comprises three parts: two independent instrument (also being analytical instrument of quality and laser ablation instrument) and a DI/DO interface (for example adopt a DI/DO interface card, the DI/DO interface card is for generation of triggering and look-at-me with receiving, 16 passages are arranged on it, can satisfy fully two between the independent instrument triggering and generation and the transmission of look-at-me).
A kind of system that realizes independent instrument interlock in the mass spectrometry system in the embodiment of the invention 1, the system of described interlock comprises independent instrument and numeral input/digital output interface card, described independent instrument comprises analytical instrument of quality and laser ablation instrument, wherein, described analytical instrument of quality comprises sampling system, ion gun, analyzer, detecting device and computing machine; Described sampling system is sent into sample and is made its ionization in the described ion gun; The sample ions of described analyzer after to ionization separated by the mass/charge ratio; The sample ions of described detecting device after to the separation of described analyzer output detects; Described computing machine receives the sample signal of described detecting device output and it is carried out Storage and Processing; Described laser ablation instrument comprises laser instrument, lens, object lens and degrades the pond; The laser that described laser instrument sends is focused to the described sample surfaces that degrades in the pond through after the described lens shaping by described object lens, and the sample particle that sample surfaces is degraded is out transferred in the described sampling system of described analytical instrument of quality by carrier gas; Described numeral input/digital output interface card is connected with described laser ablation instrument with described analytical instrument of quality respectively by USB interface, and described numeral input/digital output interface card is used for transmitting trigger pip and look-at-me; Described trigger pip comprises quality analysis trigger pip and laser ablation trigger pip, and described look-at-me comprises quality analysis look-at-me and laser ablation look-at-me; The system of independent instrument interlock comprises interlock trigger mode and interlock interrupt mode in the described realization mass spectrometry system, wherein: described interlock trigger mode comprises: described analytical instrument of quality confirms to receive the quality analysis trigger pip that described laser ablation instrument sends, and after described laser ablation instrument confirms to receive the laser ablation trigger pip that described analytical instrument of quality sends, described laser ablation instrument begins sample surfaces is degraded, and described analytical instrument of quality begins the sample that imports into is analyzed; Described interlock interrupt mode comprises: described laser ablation instrument then sends the quality analysis look-at-me to described analytical instrument of quality if break down in the process of degrading, make it stop analytic process; Described analytical instrument of quality then sends the laser ablation look-at-me to described laser ablation instrument if break down in the process of analyzing, make it stop denudation.
Here; by numeral input/digital output interface card the independent instrument that comprises analytical instrument of quality and laser ablation instrument in the mass spectrometry system is formed the interlock network; and by this numeral input/digital output interface card transmission trigger pip and look-at-me; and make realize the cooperatively interacting triggering work or interrupt protection of each independent instrument in the mass spectrometry system by interlock trigger mode and interlock interrupt mode; (for example manually choose the mode of degrading a little and analyzing one by one with respect to manual type; the flow process of artificial experiment was in the past; select what a point; then operate two independent instrument; analyze according to flow process; analysis process essence after each reconnaissance is identical; this manual type is being degraded in a little more situation; expend time in very much and energy; because the analysis time of each point is basically about 30 seconds; so an experiment often need to be carried out all night; time has been grown unavoidably and has made mistakes; also can waste sample); owing to can realize interlock between the independent instrument; therefore can be so that the process of laser ablation and quality analysis links; realize the automatic analysis of sample; thereby so that mass spectrometry system efficient is higher on the whole; better reliability; also (for example the present invention only need spend the less time to choose to degrade a little so that each independent instrument can automatical and efficient stable operation in the mass spectrometry system; then allow two independent instrument automatically carry out sample analysis; the experimenter does not need to stare at instrument again like this; can do simultaneously other things; saved time and efforts; the waste of experiment mistake and sample can not appear causing owing to experimenter's fatigue factor in addition yet; the analysis efficiency of instrument is also fast than artificial, and efficient improves greatly).
Described analytical instrument of quality also comprises the quality analysis module, described laser ablation instrument also comprises the laser ablation module, wherein, in described interlock trigger mode, described quality analysis module and laser ablation module are respectively applied to confirm to receive described quality analysis trigger pip and laser ablation trigger pip; In described interlock interrupt mode, described quality analysis module and laser ablation module are respectively applied to the quality of reception and analyze look-at-me and laser ablation look-at-me.
Described independent instrument is based in described interlock interrupt mode that operation to the control of the control software on the described independent instrument realizes, described independent instrument is based on the MFC of Windows, and the operation of described control is the action that realizes this control by the handle that obtains this control; Described numeral input/digital output interface jig has the input of 16 railway digitals and the output of 16 railway digitals, compatible 5VTTL level (n is 16 among Fig. 3).
The trigger pip of transmitting in the described numeral input/digital output interface card is transistor-transistor logic level (TTL) signal; Described sampling system comprises at least a in storage tank sample introduction, probe sample introduction and the chromatogram sample introduction; Described analyzer comprises magnetic field or electric field; Described carrier gas comprises He gas; Described computing machine also is used for the system of described interlock is controlled, and stores standard diagram on it, and the described sample signal and the described standard diagram that are used for obtaining are retrieved contrast, to provide corresponding structural formula.
For example, the present invention realizes that the software section of the system of independent instrument interlock in the mass spectrometry system can be installed on respectively in analytical instrument of quality and the laser ablation instrument.This system judges at first whether analytical instrument of quality and laser ablation instrument running status separately are ready to, and then wait for respectively the trigger pip after two independent instrument running statuses are ready to, and the transmission of trigger pip is by the DI/DO interface.Two independent instrument are started working after the trigger pip that receives separately.The mode of two independent instrument of this system triggers is based on the MFC(Microsoft Foundation Classes of Windows, also be the microsoft foundation class storehouse), the relevant control handle of the control software by obtaining two independent instrument is realized the action of this control, for example the pressing and decontroling of button, the input of content and the error message etc. of obtaining each instrument operation in the text box.In the process of two platform independent instruments interlock; the software of this linked system is monitored fault (the also namely wrong) information whether this two platform independent instrument is arranged always and is occurred; in case a certain in the two platform independent instruments error message occurred; this linked system will be interrupted two instruments immediately simultaneously, thereby realize effective protection of sample.
Linked system proposed by the invention is by to the operation of control on the control software of two independent instrument and interlock and the interruption of obtaining to realize two platform independent instruments of relevant information, (mouse of namely controlling computer is realized the operation of system controlling software with adopting the analog mouse control mode, if have the people to run into mouse this moment in the process of mouse movement, will disturb the motion of mouse, make mistakes easily) compare, have the advantage of stability and better reliability, and can prevent artificial mouse maloperation.This is because adopt the behavior of analog mouse keyboard to realize that there are some risks in the mode of two instrument interlocks, if just might cause the overdue of mouse such as in experimentation, there being the people to run into mouse, and the present invention is owing to be directly to control button control and the Input of respectively controlling software in the mass spectrometry system, no matter whether there have been artificial run into because of carelessness mouse or keyboard like this, can not cause control the overdue of software hit or erroneous input.
Described mass spectrometry system comprises laser ablation-accept inductivity coupled plasma mass spectrometry system or laser ablation-quadrupole rod inductivity coupled plasma mass spectrometry system more; Described analytical instrument of quality also comprises vacuum system, electrical system and data handling system, wherein said vacuum system is used to the ion of generation that vacuum environment is provided, described electrical system is used for providing power supply, and described data handling system is used for the sample data of detecting device output is carried out inputting computing machine after filtering is processed again.The present invention realizes the system and method for the interlock of independent instrument in the mass spectrometry system, is not only applicable to laser ablation-accept inductivity coupled plasma mass spectrometry system (also being LA-MC ICP MS) more; Also be applicable to LA(Laser Ablation, laser ablation) with the system of other analytical instrument of quality combination, LA-ICP-QMS(Laser Ablation Qudrupole Inductively Coupled Plasma Mass Spectrometry for example, be called for short LA-Q ICP MS, laser ablation-quadrupole rod inductivity coupled plasma mass spectrometry system).
Embodiment 2
The invention provides a kind of method that realizes independent instrument in the mass spectrometry system (comprising many platform independent instrument) interlock.The method relates to the interlock of each independent instrument in the mass spectrometry system, can substitute manually-operated, thereby realizes the automatic operation of mass spectrometry system efficient stable.Mass spectrometry system comprises many platform independent instrument usually, such as analytical instrument of quality, laser ablation instrument etc.The method forms the interlock network with the instrument of the many platform independent in the mass spectrometry system by numeral input/numeral output (DI/DO) mode, according to the work schedule of mass spectrometry system, adopts Signal trigger mode to coordinate the interlock of each independent instrument.The method is based on the MFC(Microsoft Foundation Classes of Windows operating system), the function software interface phase that at first obtains each independent instrument is answered control, and (" control " here is a kind of graphical user-interface element in the Windows operating system, form for example, button or text box) handle (" handle " here be used for indicating in the Windows operating system in the different objects and homogeneous object unique round values of different instances), according to the mass spectrometry system work schedule, behind the signal (for example trigger pip/look-at-me) that obtains the DI/DO transmission, utilize the corresponding control handle that obtains to carry out the orderly interlock that software operation is realized many platform independent instrument in the mass spectrometry system subsequently.
The method is applicable to the interlock based on independent instrument in the mass spectrometry system of Windows operating system, mainly comprises: 1) independent instrument in the mass spectrometry system is formed the interlock network; 2) adopt Signal trigger mode to coordinate the interlock of each independent instrument; 3) based on the MFC of Windows operating system, the corresponding control handle at the function software interface by obtaining each independent instrument carries out software operation, realizes the automatic operation of mass spectrometry system efficient stable; Wherein, adopt numeral input/numeral output (DI/DO) mode with many platform independent configuration of instrument interlock network in the mass spectrometry system; Signal in the described Signal trigger mode is transistor-transistor logic level (TTL) signal.
Specifically, a kind of method that realizes independent instrument interlock in the mass spectrometry system of the present invention, the system of described interlock comprises independent instrument and numeral input/digital output interface card, and described independent instrument comprises analytical instrument of quality and laser ablation instrument, said method comprising the steps of:
Step 1: choose N laser ablation point in the laser ablation module in the laser ablation instrument, N is more than or equal to 3, these x, y and z three-dimensional coordinates that degrade a little are recorded in the array, simultaneously default following at least parameter: a) each frequency of degrading of degrading a little is a1, and unit is Hz; B) each number of times that degrades that degrades a little is a2 time; C) the laser ablation energy is a3 in the laser ablation instrument, and unit is that milli is burnt; D) the laser ablation instrument arrives each to degrade the needed time of a position is a4 second; E) be a5 second lock in time;
Step 2: the laser ablation module of laser ablation instrument confirms that the laser ablation instrument is ready, and sends the quality analysis trigger pip by numeral input/digital output interface card to analytical instrument of quality;
Step 3: in analytical instrument of quality, open sample sequence analytical model (also being the Sequence analytical model, sample sequence of N sample composition under this pattern), set respectively N analysis mode and instrument tuner parameters that degrades a little; Here " analysis mode " refers to the mode of collection signal, for example comprise that setting integral time is 0.131 second, totally 200 circle(also namely gather circulation), the 200circle here refers to one and degrades 200 detections of collection data, and each detects data acquisition time is 0.131 second (also being integral time); Here " instrument is tuning " for example comprises that the focusing of instrument is tuning, this is because the ion in the analytical instrument of quality needs a series of ion lens to carry out shaping to avoid as much as possible ion to disperse, mutually pin down between the voltage that applies on these ion lenss, therefore need to carry out voltage optimization, it is tuning that the voltage optimization process here just is called instrument, these magnitudes of voltage are exactly the instrument tuner parameters, the in addition tuning adjustment that also comprises instrumental resolution of instrument is to obtain maximum instrumental resolution;
Step 4: the quality analysis module in the analytical instrument of quality confirms that analytical instrument of quality is ready, and sends the laser ablation trigger pip by numeral input/digital output interface card to the laser ablation instrument;
Step 5: the quality analysis module in the analytical instrument of quality confirms to receive the quality analysis trigger pip, and (for example quality analysis module has a thread detecting the USB mouth always, in case receive a Transistor-Transistor Logic level, will trigger the startup control " Start " of sample sequence analytical model);
Step 6: the laser ablation module in the laser ablation instrument confirms to receive the laser ablation trigger pip;
Step 7: mass spectrometer begins first is degraded under the sample sequence analytical model and a little carries out quality analysis, this moment, the laser ablation module of laser ablation instrument moved to the three-dimensional platform of laser ablation instrument that selected first degrades a little x, y and z three-dimensional coordinate position in the step 1, and began sample is carried out laser ablation according to the parameter of presetting;
Step 8: in the process of laser ablation and quality analysis, if analytical instrument of quality or laser ablation instrument break down, then quality analysis module and laser ablation module send laser ablation look-at-me and quality analysis look-at-me to the other side respectively, so that the process of laser ablation and quality analysis interrupts protecting sample, and enter step 9; If analytical instrument of quality and laser ablation instrument do not break down, then after having carried out a laser ablation and quality analysis of degrading a little, enter step 9;
Step 9: analytical instrument of quality and laser ablation instrument quality analysis module and laser ablation module separately begins to carry out separately whether ready inspection of state;
Step 10: after analytical instrument of quality and laser ablation instrument standby condition are ready, send respectively laser ablation trigger pip and quality analysis trigger pip by numeral input/digital output interface card to the other side; Quality analysis module in the analytical instrument of quality confirms to receive the quality analysis trigger pip; Laser ablation module in the laser ablation instrument confirms to receive the laser ablation trigger pip;
Step 11: mass spectrometer begins the next one degraded under the sample sequence analytical model and a little carries out quality analysis, this moment the laser ablation instrument the laser ablation module with the three-dimensional platform of laser ablation instrument move in the step 1 selected degrade a little in next x, y and z three-dimensional coordinate position of degrading a little, and begin sample is carried out laser ablation according to the parameter of presetting;
Step 12: repeating step 8-step 11, until that N degrades point analysis is complete, whole flow process finishes.
Described numeral input/digital output interface card is connected with described laser ablation instrument with described analytical instrument of quality respectively by USB interface, and described numeral input/digital output interface card is used for transmitting trigger pip and look-at-me; Described trigger pip comprises quality analysis trigger pip and laser ablation trigger pip, and described look-at-me comprises quality analysis look-at-me and laser ablation look-at-me; The interlock of independent instrument comprises interlock trigger mode and interlock interrupt mode in the described mass spectrometry system, wherein: described interlock trigger mode comprises: described analytical instrument of quality confirms to receive the quality analysis trigger pip that described laser ablation instrument sends, and after described laser ablation instrument confirms to receive the laser ablation trigger pip that described analytical instrument of quality sends, described laser ablation instrument begins sample surfaces is degraded, and described analytical instrument of quality begins the sample that imports into is analyzed; Described interlock interrupt mode comprises: described laser ablation instrument then sends the quality analysis look-at-me to described analytical instrument of quality if break down in the process of degrading, make it stop analytic process; Described analytical instrument of quality then sends the laser ablation look-at-me to described laser ablation instrument if break down in the process of analyzing, make it stop denudation.
Mass spectrometer can be realized the startup to the quality analysis process by the startup control (" Start ") on its software interface of control when receiving the quality analysis trigger pip; Mass spectrometer is when receiving the quality analysis look-at-me, can realize the termination to the quality analysis process by the termination control (" End " button) of control on its software interface, the corresponding handle that wherein starts control and termination control is obtained in advance by the mass spectrometer based on the MFC of Windows.
The laser ablation instrument when receiving the laser ablation trigger pip, can by control on its software interface beginning control (the Start Button), D coordinates value control (three text boxes) and move to target control (goto target ") realize respectively to the laser ablation process startup, degrade the selection of a position coordinates and will degrade a little to move to and degrade the position; The laser ablation instrument is when receiving the laser ablation look-at-me, can realize the termination to the laser ablation process by the end control (" abort ") of control on its software interface, the corresponding handle that wherein begin control, D coordinates value control, moves to target control and end control is obtained in advance by the laser ablation instrument based on the MFC of Windows.
N is 100 in N the laser ablation point, and degrading frequency a1 is 8Hz, and degrading number of times is for a2 time 216 times, and laser ablation energy a3 is that 80 millis are burnt, and time a4 second is 30 seconds, and be 3 seconds a5 second lock in time; N analysis mode of degrading a little comprises that setting each degrades 200 detections of collection data, each detects data acquisition time is that (also namely setting integral time was 0.131 second in 0.131 second, totally 200 circle, 200 circle here refer to one degrade gather 200 and detect data); Fault in the described analytical instrument of quality comprises: ion gun died, lens combination voltage failure and vacuum failure; Fault in the described laser ablation instrument comprises: laser energy decay, laser three-D platform fault and laser optical path blanket gas fault.
Embodiment 3
The control software of two independent instrument for example all is based on the windows system among the present invention, is described in detail as follows.The analysis process of MC-ICP-MS is divided into two types: the analysis of (1) single sample; (2) analysis of Multi-example.When adopting Multi-example to analyze, can use Sequence analysis process (also being the sample sequence analytical model), that is to say that a series of sample will analyze.To analyze 10 samples as example, as shown in Figure 5.This figure signal be the software interface (Sequence Editor) that MC-ICP-MS carries out the Multi-example analysis and is; In this software interface, be provided with " External Trigger " pattern (circle 1 sign), also namely before beginning to analyze each sample, can wait for external trigger, only (for example receiving analysis that trigger pip just begins later on each sample, after finishing first sample analysis, before second sample of beginning begins, system is waiting for outer triggering signal always, just begins the analysis of second sample after receiving outer triggering signal).The order of 10 sample analysis is carried out according to black arrow indicated direction among the figure, begins until the 10th sample analysis finishes from first sample.What circle 4 identified is the analysis Data Filename (can see the data of sample analysis in this document) that can input 10 samples in this zone.Circle 3 signs be when carrying out each sample analysis, the tuning file of the parameter of instrument (this document has comprised mass spectrometric each running parameter, ion lens voltage for example, the power in ICP source and carrier gas air-flow etc.).What circle 2 identified is " End " button, in the present invention, if the LA system breaks down, then utilize should " End " button handle stop all analyses (for example the software installed of the present invention can allow this button actions, thereby stops all analyses) in analytical instrument of quality.
1, the software interface of the Sequence Editor software that adopts of mass spectrometer as shown in Figure 5, for example " Start " (startup control) and " End " button (stop control, circle 2 signs) etc., these buttons are the buttons that begin or finish analysis process, are the derivation classifications among the MFC in the windows system.These buttons have unique identification code name in the windows system, also be window handle.
Software of the present invention can at first obtain the Start of Sequence Editor software and the handle of two buttons of End in operational process, after obtaining two button handles, just can utilize the action of two buttons of handle control of acquisition.Such as, for the Start button, the corresponding handle that utilize to obtain, the software that the present invention adopts will be controlled the Start button and carry out that button " is pressed " and " relieving " these two actions, thereby realize the purpose of artificial mouse click after obtaining trigger pip.Employing is obtained method that the button handle realizes button control with respect to utilizing mouse beacon click method to compare, and is safer reliable.In the analytic process of system and method for the present invention, no matter Sequence Editor software interface is maximization or minimizes, or mouse can not affected the used software of the present invention to the control of Sequence Editor software by artificial movement.
2, the software interface of the software that adopts of laser ablation instrument as shown in Figure 6, shown in the circle 1 is beginning and the conclusion button of laser ablation.That each degrades coordinate a little shown in the circle 2, during manually-operated, manually coordinate is a little degraded in input, then click shown in the goto target(circle 3), selected degrading will move to a little that (this circle is exactly the size of laser facula in the circle of circle shown in 4, the position of laser beam namely, this position is motionless, mobile is the position of sample).
Software of the present invention at first obtains the handle of following button and text box in operational process: the handle of the Start Button shown in the circle 1 (beginning control, this button is used for starting or stoping laser ablation); The handle (the D coordinates value control is respectively the D coordinates value of degrading a little in three text boxes, can select degrading a little of diverse location by the change of this D coordinates value) of three text boxes shown in the circle 2; The handle of " goto target " button shown in the circle 3 (move to the target control, be used for a little moving in the circle shown in the circle 4 degrading); The handle (this button is used for making the laser ablation instrument to move after receiving look-at-me, also namely stops the operation of laser ablation system) of " abort " button (end control) shown in the circle 5.
3, analysis process
(1) in software of the present invention, chooses the required point (for example 100 degrade a little) that degrades.Particularly, as shown in Figure 7, utilize in the software that the laser ablation instrument adopts xyz platform movement button to select first to degrade a little, then click the Take button (enclosing 1 signal) in the software of the present invention, selected x, y and the z coordinate that degrades a little will be stored in the middle of the forms of circle 3 expressions.Next select second to degrade a little, after choosing, click Take, second coordinate that degrades a little is stored in the middle of the form.Remaining 98 degrade and a little also adopt identical method to choose.After all degrading a little all chosen, click the Confirm key of circle 2 signs, confirm the coordinate of selected 100 points.
Then set other parameter, for example:
Analysis time (shown in the circle 4), take the test of laser hafnium as example, be 50 seconds each analysis time of degrading a little.
Shown in the Goto Time(circle 5) be that sample degrades a little to move to and degrades the interior required time of circle, generally be made as 30 seconds, also be that sample moves the needed time.
Syn time for MS(and MS(Mass Spectrometry, mass spectrometer) lock in time, shown in the circle 5), this time is to consider that each has a setup time (3 seconds) before degrading point analysis to analytical instrument of quality in beginning, so within this setup time, analytical instrument of quality can not be started working, after this setup time, analytical instrument of quality is just started working, and the Syn time for MS here is exactly this delay time, is made as 3 seconds.
(2) set 100 analytical approach, tuner parameters, filename and other parameters of degrading a little in the Sequence Editor software in analytical instrument of quality, as shown in Figure 5.Notice that must select external trigger mode (External Trigger) this moment.After parameter sets, click the start key on End button next door.Analytical instrument of quality begins to enter ready state, waits for the trigger pip of laser ablation instrument.
(3) after wait analytical instrument of quality parameter sets, click " Start Auto-control " button (circle 6 signs) of the present invention's software of compiling in the laser ablation instrument.The laser ablation instrument is ready, sends trigger pip to analytical instrument of quality, waits for that analytical instrument of quality provides trigger pip.
(4) analytical instrument of quality receives the trigger pip of laser ablation instrument, begins first and degrades a little analysis, before analyzing beginning 3 seconds time-delay is arranged, and sends trigger pip for simultaneously the laser ablation instrument.
(5) after the laser ablation instrument receives analytical instrument of quality and sends trigger pip, delayed time 3 seconds, begin first and degrade degrading a little, analytical instrument of quality also began first and degraded a little quality analysis this moment.
(6) through after 50 seconds the quality analysis, analytical instrument of quality enters waiting status, the laser ablation instrument begins second degraded and a little moves to (30 seconds consuming time of this process) in the laser ablation circle, then enters and waits for ready state, sends trigger pip to analytical instrument of quality.
(7) analytical instrument of quality receives the trigger pip of laser ablation instrument, begins second analysis of degrading a little, before analyzing beginning 3 seconds time-delay is arranged, and sends trigger pip for simultaneously the laser ablation instrument.
(8) after the laser ablation instrument receives analytical instrument of quality and sends trigger pip, delayed time 3 seconds, begin second and degrade degrading a little, this moment, analytical instrument of quality also began second quality analysis of degrading a little.
(9) afterwards the analysis process that degrades a little namely repeats the process of (4)-(8), and to the last one degrades point analysis and finishes.
Annotate: if in the middle of analytic process, analytical instrument of quality breaks down, software that the present invention compiles can catch this failure message, and send look-at-me to the laser ablation instrument, software that the present invention compiles will allow the abort key of circle 5 signs shown in Figure 6 move in the laser ablation instrument, thereby stops laser ablation.
Annotate: if in the middle of analytic process, the laser ablation instrument breaks down, software that the present invention compiles can catch this failure message, and send look-at-me to analytical instrument of quality, software that the present invention in the analytical instrument of quality compiles will allow the stop key of circle 2 signs shown in Figure 5 move, thereby stops quality analysis.
Embodiment 4
Here the laser Hf isotopic ratio with zircon sample is determined as example, and the idiographic flow of institute of the present invention extracting method may further comprise the steps:
(1) utilizes and choose 100 laser ablation points in the laser ablation module 8 of the inventive method in laser ablation instrument 2, also be that laser ablation module 8 is recorded in these 100 x, y and the z three-dimensional coordinates that degrade a little in the array, established simultaneously following three parameters: a) each frequency of degrading of degrading a little is 8Hz; B) each number of times that degrades that degrades a little is 216 times; C) laser ablation instrument 2 arrives each to degrade the needed time of a position is 30 seconds;
(2) the laser ablation module 8 of laser ablation instrument 2 confirms that the laser ablation instrument is ready, and sends quality analysis trigger pip 6 by DI/DO interface 3 to analytical instrument of quality;
(3) open the sample sequence analytical model in the control software of analytical instrument of quality 1, set respectively 100 analytical approach and instrument tuner parameters that degrade a little, wherein for example setting integral time in analytical approach is 0.131 second, totally 200 circle;
(4) the quality analysis module in the analytical instrument of quality 19 confirms that analytical instrument of quality is ready, and sends laser ablation trigger pip 4 for the laser ablation instrument by DI/DO interface 3;
(5) the quality analysis module in the analytical instrument of quality 19 confirms to receive quality analysis trigger pip 6;
(6) the laser ablation module in the laser ablation instrument 28 confirms to receive laser ablation trigger pip 4;
(7) the sample sequence analytical model of mass spectrometer 1 (also being Sequence analytical model or Sequence flow process or Sequence analysis process) begins first and degrades point measurement, at this moment, the laser ablation module 8 of laser ablation instrument 2 moves to the three-dimensional platform of laser ablation instrument that selected first degrades a little x, y and z position in the step (1), and begins sample according to default parameter and degrade;
(8) in the laser ablation analytic process, if mistake (for example, the normal fault that occurs (also namely wrong) in the analytical instrument of quality: ICP source died, lens combination voltage failure and vacuum failure etc. appears in analytical instrument of quality or laser ablation instrument; The normal fault that occurs in the laser ablation instrument (also namely wrong): laser energy decay, laser three-D platform fault and laser optical path blanket gas fault etc.), it (also is that quality analysis module 9 sends laser ablation look-at-mes 5 to laser ablation module 8 that the quality analysis module 9 that has separately in two independent instrument and laser ablation module 8 will send respectively laser ablation look-at-me 5 and quality analysis look-at-me 7 to the other side's module, laser ablation module 8 sends quality analysis look-at-me 7 to quality analysis module 9), so that the laser ablation analytic process is interrupted, analytic process enters " StandBy " state, analysis process no longer goes on, thereby has effectively protected sample;
(9) after having carried out a quality analysis of degrading a little, analytical instrument of quality 1 and laser ablation instrument 2 separately quality analysis module 9 and laser ablation module 8 begin to carry out separately whether ready inspection of state (several parameters of the ready Sequence of the referring to analytical model of analytical instrument of quality for example, whether parameters such as tuning file, filename, method file sets; The laser ablation instrument is ready refer to each degrade a little degrade frequency, each degrades degrading the parameters such as number of times, laser energy and whether set a little, these all are self-verifyings);
(10) after two instrument standby condition are ready, to send respectively the first trigger pip 4 and the second trigger pip 6 to the other side (also be that analytical instrument of quality 1 sends laser ablation trigger pip 4 to laser ablation instrument 2, laser ablation instrument 2 sends quality analysis trigger pips 6 to analytical instrument of quality 1) by the DI/DO interface;
(11) the sample sequence analytical model of mass spectrometer 1 begins the next one and degrades point measurement, at this moment, the laser ablation module 8 of laser ablation instrument 2 with the three-dimensional platform of laser ablation instrument move in the step (1) selected degrade a little in next x, y and z position of degrading a little, and begin sample according to the parameter of presetting and degrade;
(12) repeating step (8), (9) and (10), until the 100th to degrade point measurement complete, whole flow process finishes.
Through the above description of the embodiments, those skilled in the art can be well understood to the present invention can also realize that by other structures feature of the present invention is not limited to above-mentioned preferred embodiment.Any personnel that are familiar with this technology are in technical field of the present invention, and the variation that can expect easily or modification all should be encompassed within the scope of patent protection of the present invention.

Claims (10)

1. a system that realizes independent instrument interlock in the mass spectrometry system is characterized in that, the system of described interlock comprises independent instrument and numeral input/digital output interface card, and described independent instrument comprises analytical instrument of quality and laser ablation instrument, wherein,
Described analytical instrument of quality comprises sampling system, ion gun, analyzer, detecting device and computing machine; Described sampling system is sent into sample and is made its ionization in the described ion gun; The sample ions of described analyzer after to ionization separated by the mass/charge ratio; The sample ions of described detecting device after to the separation of described analyzer output detects; Described computing machine receives the sample signal of described detecting device output and it is carried out Storage and Processing;
Described laser ablation instrument comprises laser instrument, lens, object lens and degrades the pond; The laser that described laser instrument sends is focused to the described sample surfaces that degrades in the pond through after the described lens shaping by described object lens, and the sample particle that sample surfaces is degraded is out transferred in the described sampling system of described analytical instrument of quality by carrier gas;
Described numeral input/digital output interface card is connected with described laser ablation instrument with described analytical instrument of quality respectively by USB interface, and described numeral input/digital output interface card is used for transmitting trigger pip and look-at-me; Described trigger pip comprises quality analysis trigger pip and laser ablation trigger pip, and described look-at-me comprises quality analysis look-at-me and laser ablation look-at-me;
The system of independent instrument interlock comprises interlock trigger mode and interlock interrupt mode in the described realization mass spectrometry system, wherein:
Described interlock trigger mode comprises: described analytical instrument of quality confirms to receive the quality analysis trigger pip that described laser ablation instrument sends, and after described laser ablation instrument confirms to receive the laser ablation trigger pip that described analytical instrument of quality sends, described laser ablation instrument begins sample surfaces is degraded, and described analytical instrument of quality begins the sample that imports into is analyzed;
Described interlock interrupt mode comprises: described laser ablation instrument then sends the quality analysis look-at-me to described analytical instrument of quality if break down in the process of degrading, make it stop analytic process; Described analytical instrument of quality then sends the laser ablation look-at-me to described laser ablation instrument if break down in the process of analyzing, make it stop denudation.
2. the system of interlock as claimed in claim 1 is characterized in that, described analytical instrument of quality also comprises the quality analysis module, and described laser ablation instrument also comprises the laser ablation module, wherein,
In described interlock trigger mode, described quality analysis module and laser ablation module are respectively applied to confirm to receive described quality analysis trigger pip and laser ablation trigger pip;
In described interlock interrupt mode, described quality analysis module and laser ablation module are respectively applied to the quality of reception and analyze look-at-me and laser ablation look-at-me.
3. the system of interlock as claimed in claim 1 or 2, it is characterized in that, described independent instrument is based in described interlock interrupt mode that operation to the control of the control software on the described independent instrument realizes, described independent instrument is based on the MFC of Windows, and the operation of described control is the action that realizes this control by the handle that obtains this control; Described numeral input/digital output interface jig has the input of 16 railway digitals and the output of 16 railway digitals, compatible 5VTTL level.
4. the system of interlock as claimed in claim 1 or 2 is characterized in that, the trigger pip of transmitting in the described numeral input/digital output interface card is transistor-transistor logic level (TTL) signal; Described analyzer comprises magnetic field or electric field; Described carrier gas comprises He gas; Described computing machine also is used for the system of described interlock is controlled, and stores standard diagram on it, and the described sample signal and the described standard diagram that are used for obtaining are retrieved contrast, to provide corresponding structural formula.
5. the system of interlock as claimed in claim 1 or 2 is characterized in that, described mass spectrometry system comprises laser ablation-accept inductivity coupled plasma mass spectrometry system or laser ablation-quadrupole rod inductivity coupled plasma mass spectrometry system more; Described analytical instrument of quality also comprises vacuum system, electrical system and data handling system, wherein said vacuum system is used to the ion of generation that vacuum environment is provided, described electrical system is used for providing power supply, and described data handling system is used for inputting described computing machine after the processing that sample signal to described detecting device output comprises denoising and integration again.
6. method that realizes the interlock of independent instrument in the mass spectrometry system, the system of described interlock comprises independent instrument and numeral input/digital output interface card, described independent instrument comprises analytical instrument of quality and laser ablation instrument, it is characterized in that, said method comprising the steps of:
Step 1: choose N laser ablation point in the laser ablation module in the laser ablation instrument, N is more than or equal to 3, these x, y and z three-dimensional coordinates that degrade a little are recorded in the array, simultaneously default following at least parameter: a) each frequency of degrading of degrading a little is a1, and unit is Hz; B) each number of times that degrades that degrades a little is a2 time; C) the laser ablation energy is a3 in the laser ablation instrument, and unit is that milli is burnt; D) the laser ablation instrument arrives each to degrade the needed time of a position is a4 second; E) be a5 second lock in time;
Step 2: the laser ablation module of laser ablation instrument confirms that the laser ablation instrument is ready, and sends the quality analysis trigger pip by numeral input/digital output interface card to analytical instrument of quality;
Step 3: in analytical instrument of quality, open the sample sequence analytical model, set respectively N analysis mode and instrument tuner parameters that degrades a little;
Step 4: the quality analysis module in the analytical instrument of quality confirms that analytical instrument of quality is ready, and sends the laser ablation trigger pip by numeral input/digital output interface card to the laser ablation instrument;
Step 5: the quality analysis module in the analytical instrument of quality confirms to receive the quality analysis trigger pip;
Step 6: the laser ablation module in the laser ablation instrument confirms to receive the laser ablation trigger pip;
Step 7: mass spectrometer begins first is degraded under the sample sequence analytical model and a little carries out quality analysis, this moment, the laser ablation module of laser ablation instrument moved to the three-dimensional platform of laser ablation instrument that selected first degrades a little x, y and z three-dimensional coordinate position in the step 1, and began sample is carried out laser ablation according to the parameter of presetting;
Step 8: in the process of laser ablation and quality analysis, if analytical instrument of quality or laser ablation instrument break down, then quality analysis module and laser ablation module send laser ablation look-at-me and quality analysis look-at-me to the other side respectively, so that the process of laser ablation and quality analysis interrupts protecting sample, and enter step 9; If analytical instrument of quality and laser ablation instrument do not break down, then after having carried out a laser ablation and quality analysis of degrading a little, enter step 9;
Step 9: analytical instrument of quality and laser ablation instrument quality analysis module and laser ablation module separately begins to carry out separately whether ready inspection of state;
Step 10: after analytical instrument of quality and laser ablation instrument standby condition are ready, send respectively laser ablation trigger pip and quality analysis trigger pip by numeral input/digital output interface card to the other side; Quality analysis module in the analytical instrument of quality confirms to receive the quality analysis trigger pip; Laser ablation module in the laser ablation instrument confirms to receive the laser ablation trigger pip;
Step 11: mass spectrometer begins the next one degraded under the sample sequence analytical model and a little carries out quality analysis, this moment the laser ablation instrument the laser ablation module with the three-dimensional platform of laser ablation instrument move in the step 1 selected degrade a little in next x, y and z three-dimensional coordinate position of degrading a little, and begin sample is carried out laser ablation according to the parameter of presetting;
Step 12: repeating step 8-step 11, until individual the degrading of N a little is disposed, whole flow process finishes.
7. method as claimed in claim 6, it is characterized in that, described numeral input/digital output interface card is connected with described laser ablation instrument with described analytical instrument of quality respectively by USB interface, and described numeral input/digital output interface card is used for transmitting trigger pip and look-at-me; Described trigger pip comprises quality analysis trigger pip and laser ablation trigger pip, and described look-at-me comprises quality analysis look-at-me and laser ablation look-at-me; The interlock of independent instrument comprises interlock trigger mode and interlock interrupt mode in the described mass spectrometry system, wherein: described interlock trigger mode comprises: described analytical instrument of quality confirms to receive the quality analysis trigger pip that described laser ablation instrument sends, and after described laser ablation instrument confirms to receive the laser ablation trigger pip that described analytical instrument of quality sends, described laser ablation instrument begins sample surfaces is degraded, and described analytical instrument of quality begins the sample that imports into is analyzed; Described interlock interrupt mode comprises: described laser ablation instrument then sends the quality analysis look-at-me to described analytical instrument of quality if break down in the process of degrading, make it stop analytic process; Described analytical instrument of quality then sends the laser ablation look-at-me to described laser ablation instrument if break down in the process of analyzing, make it stop denudation.
8. such as claim 6 or 7 described methods, it is characterized in that mass spectrometer can be realized startup to the quality analysis process by controlling startup control on its software interface when receiving the quality analysis trigger pip; Mass spectrometer is when receiving the quality analysis look-at-me, can realize termination to the quality analysis process by controlling termination control on its software interface, the corresponding handle that wherein starts control and stop control is obtained in advance by the mass spectrometer based on the MFC of Windows.
9. such as claim 6 or 7 described methods, it is characterized in that, the laser ablation instrument when receiving the laser ablation trigger pip, can by control beginning control, the D coordinates value control on its software interface and move to the target control realize respectively to the laser ablation process startup, degrade the selection of a position coordinates and will degrade a little to move to and degrade the position; The laser ablation instrument is when receiving the laser ablation look-at-me, can realize termination to the laser ablation process by controlling end control on its software interface, the corresponding handle that wherein begins control, D coordinates value control, moves to the target control and finish control is obtained in advance by the laser ablation instrument based on the MFC of Windows.
10. such as claim 6 or 7 described methods, it is characterized in that N is 100 in N the laser ablation point, degrading frequency a1 is 8Hz, and degrading number of times is for a2 time 216 times, and laser ablation energy a3 is that 80 millis are burnt, and time a4 second is 30 seconds, and time a5 second is 3 seconds; N analysis mode of degrading a little comprises that setting each degrades 200 detections of collection data, and each detects data acquisition time is 0.131 second; Fault in the described analytical instrument of quality comprises: ion gun died, lens combination voltage failure and vacuum failure; Fault in the described laser ablation instrument comprises: laser energy decay, laser three-D platform fault and laser optical path blanket gas fault.
CN201310299108.0A 2013-07-17 2013-07-17 System and method for realizing linkage of independent instruments in mass spectrometry analysis system Expired - Fee Related CN103364483B (en)

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CN114994217A (en) * 2022-08-05 2022-09-02 常州磐诺仪器有限公司 Gas chromatography-mass spectrometer with real-time online gas detection function
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