CN101655458B - Liquid phase sample laser-induced spectroscopic analysis device - Google Patents
Liquid phase sample laser-induced spectroscopic analysis device Download PDFInfo
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- CN101655458B CN101655458B CN2009100755778A CN200910075577A CN101655458B CN 101655458 B CN101655458 B CN 101655458B CN 2009100755778 A CN2009100755778 A CN 2009100755778A CN 200910075577 A CN200910075577 A CN 200910075577A CN 101655458 B CN101655458 B CN 101655458B
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Abstract
The invention relates to laser measurement technology, in particular to a liquid phase sample laser-induced spectroscopic analysis device which applies laser-induced spectroscopic technique to measure elemental composition in liquid phase sample, aiming at solving a plurality of problems caused by the self characteristics of liquid when the existing laser-induced spectroscopic technique is used for analyzing the elemental composition of the liquid. The liquid phase sample laser-induced spectroscopic analysis device comprises a laser measuring component and a liquid containing device which includes a refrigerating chamber, a measuring pond, a refrigerating machine, a fan and a circulating pump, wherein the refrigerating chamber adopts double-shell structure provided with an internal and an external shells, a door cover on the top of the chamber is provided with a measuring hole, and a refrigeration agent circulation evaporating pipe connected with the refrigerating machine is stuck outside the internal shell; heat insulating material is filled between the refrigeration agent circulation evaporating pipe and the external shell; and the upper part of the internal shell is provided with an induced draught hole which is connected with the fan by an induced draught pipeline, and the lower part thereof is provided with two circulation pipelines connected with the circulating pump. The device has simple and reasonable structure and high accuracy of the measuring results, can realize automatic detection, needs no human intervention, and is applicable to analyzing the elemental composition of the noxious liquid, thus being convenient for measurement and little in maintenance.
Description
Technical field
The present invention relates to laser measuring technique, specifically is a kind of liquid phase sample laser-induced spectroscopic analysis device that the laser-induced spectrum technology is measured elemental composition in the liquid phase sample of using.
Background technology
In industrial and agricultural production, environment monitoring, food safety detection, often need carry out constituent analysis to liquid.More common liquid component analytical approach mainly contains at present: x-ray fluorescence analysis (X-Ray), atomic absorption spectroscopy (AAS) and inductively coupled plasma atomic emission spectrum technology (ICP-AES).Wherein, the x-ray fluorescence analysis method can realize fast detecting, but sensitivity is lower; Atomic absorption spectroscopy and inductively coupled plasma atomic emission spectrum technology for detection precision height, good stability, but because the application apparatus costliness, sample pre-treatments is time-consuming, is difficult to be adopted by manufacturing enterprise.
Laser-induced spectrum (Laser Induced Breakdown Spectroscopy, LIBS) be a kind of novel spectral analysis technique, utilize the intense pulse laser that focuses on to excite material to produce plasma, obtain material element component content information by atom or the ionoluminescence spectrum of analyzing in the plasma, realize ultimate analysis sample.Advantages such as the LIBS technology has that specimen preparation is simple, multielement Synchronization Analysis, analysis speed are fast, so this technology is widely used in the qualitative or quantitative test of various materials, and great practical value is arranged.At present, the LIBS technology has been applied to fields such as environmental pollution monitoring, industrial products detection and archaeology analysis, also has some scholars to be applied to Analytical Chemistry of Heavy Metals in the water body.
But when utilizing the LIBS technology that the elemental composition of liquid is analyzed, because the self character of liquid, and bring many adverse influences: 1, when laser action arrives liquid surface, easily produce the liquid sputter, pollute optical measuring system; 2, the ripple that produces after liquid self instability and the laser excitation influences the accuracy of laser focusing focal length, has reduced the repeatability of test; 3, the sputter liquid that produces after the laser excitation can absorb or block the light that plasma emission goes out, the accuracy that influence is surveyed; 4, laser pulse can produce bubble at liquid internal, and these bubbles can change the characteristic of the plasma that laser excitation produces at liquid surface; 5, laser pulse meeting high temperature heating liquid, make liquid evaporation, the steam that liquid evaporation causes can influence the power of laser pulse, or causes it to shift to an earlier date ionization and do not affact liquid surface, and steam also can influence the detection accuracy of optical system article on plasma body spectrum simultaneously.In addition, there are many liquid to have high volatility, inflammable and poisonous and harmful characteristics in industry and the environmental monitoring field, adopt conventional measurement means to be difficult to satisfy security requirement.
In order to address the above problem, there is the researcher to propose in liquid, to add hardening agent (for example calcium oxide) and makes its curing, but because the hardening agent that is added also produces plasma spectrometry under the effect of laser, therefore it is complicated to cause spectroscopic data to be handled, and has reduced automation degree of equipment to a certain extent; The researcher who also has inserts liquid in the container that optical glass makes, allowing laser pulse pass the optical glass chamber wall excites the liquid of inside, though this method can prevent the liquid sputter, but it is still powerless for the problem that bubble causes, the most disadvantageously when the inwall of optical glass container has dust with liquid deposit or outer wall, can cause that laser excites the problem of ionization in advance, can cause spot if excite at the optical glass inside and outside wall, can influence the optical glass characteristic, the light that conduction pulsed laser energy that it no longer can be good and plasma are sent, so there are big problem in the reliability of this method and long-time stability.
Summary of the invention
The problems that cause because of the liquid self character when the present invention carries out the elemental composition analysis with the laser-induced spectrum technology to liquid at present in order to overcome provide a kind of liquid phase sample laser-induced spectroscopic analysis device.
The present invention adopts following technical scheme to realize: liquid phase sample laser-induced spectroscopic analysis device, comprise laser measuring assembly, hold the Sheng liquid device of liquid phase sample when being used to measure, laser measuring assembly comprises pulsed laser, spectrometer, through conducting the fibre-optical probe that optical fiber links to each other with spectrometer, contain liquid device place pulsed laser under, the optical window of pulsed laser and Sheng liquid device are over against setting, and be provided with condenser lens before the optical window of pulsed laser, described Sheng liquid device comprises refrigerating chamber, and place measuring cell in the refrigerating chamber, and dispose cold machine, blower fan, low temperature conduction oil ebullator, refrigerating chamber adopts inside and outside duplex shell structure, the top, chamber is furnished with door closure, have on the door closure with the pulsed laser optical window over against measured hole, the refrigerant cycle evaporation tube that the refrigerating chamber inner casing is sticked outward and links to each other with cold machine, and be filled with thermal insulation material between refrigerant cycle evaporation tube and shell, inner casing top offers the air inducing hole that links to each other with blower fan through induced pipe, and the inner casing bottom is provided with the circulation line that two-way links to each other with low temperature conduction oil ebullator.
Liquid phase sample laser-induced spectroscopic analysis device also is provided with the precooling thawing apparatus, comprise the thawing chamber, reach around melting the outdoor precooling chamber of putting that encloses, melt between chamber and the precooling chamber and be provided with the several semiconductor Cooling and Heat Source, the hot junction in semiconductor cold-hot source contacts with melting chamber outer wall, and cold junction contacts with chamber, precooling chamber wall, and is filled with thermal insulation material between the semiconductor cold-hot source, melt the top, chamber and be furnished with door closure, the bottom is provided with discharging tube, and top, precooling chamber is provided with feed tube, and feed tube is provided with the feed liquor valve; Bottom, precooling chamber is provided with the two-way discharging tube, and is respectively equipped with fixed displacement pump and liquid valve on the two-way discharging tube.
The discharging tube below that the precooling thawing apparatus melts the chamber is provided with the waste liquid temporary storage mechanism that comprises exhausted bath box, the exhausted bath box bottom is provided with sewer pipe, and sewer pipe is provided with valve, the level gauging nanubrium that the lower end is communicated with exhausted bath box suspends in the exhausted bath box, level gauging nanubrium top is fixed with the level switch of valve opening and closing on the control sewer pipe, is provided with the ball float that triggers level switch in the level gauging nanubrium.
Contain between liquid device and the precooling thawing apparatus and be provided with measuring cell transposition mechanism, comprising column, be arranged at the column top can be the transverse arm that axle rotates with the column, and transverse arm is vertical with column; Column bottom is provided with by motor-driven elevating mechanism, and it is the first automatically controlled rotating mechanism that axle rotates with the column that transverse arm is provided with the control transverse arm that is positioned at directly over the column; The free end of the transverse arm suspension rod that has been hung, transverse arm are provided with and are positioned at the second automatically controlled rotating mechanism that the control suspension rod directly over the suspension rod rotates, and measuring cell and suspension rod bottom are fixed with bearing pin; Described measuring cell central authorities are provided with and are used for and fixture that suspension rod bottom bearing pin is fixing, and measuring cell pool wall top has leakage hole, and the leakage hole center line is vertical with suspension rod bottom bearing pin; The door closure of containing liquid device refrigerating chamber and precooling thawing apparatus thawing chamber configuration all adopts two-door fan structure, and the two door leaf places of being harmonious have the through hole that passes for suspension rod.The first automatically controlled rotating mechanism, the second automatically controlled rotating mechanism and elevating mechanism in the described measuring cell transposition mechanism is existing known technology, and those skilled in the art are easy to realize.
Be fixed with backguy on the pool wall of measuring cell leakage hole opposite side, transverse arm is provided with the motor that the traction backguy has a down dip measuring cell drainage oral-lateral.
The operating process of measuring equipment of the present invention is as follows:
1, preparation process: the feed tube of precooling thawing apparatus fixedly is communicated with the container that holds fluid sample to be analyzed, and the sewer pipe of waste liquid temporary storage mechanism is communicated with blow-off line in the laboratory, adds an amount of low temperature conduction oil in refrigerating chamber; Wherein, the low temperature conduction oil can quicken the freezing quick-frozen of fluid sample to be analyzed in the measuring cell, avoids measuring cell and refrigerating chamber locular wall to freeze simultaneously.
2, precooling step: start the cold machine of Sheng liquid device outfit and the semiconductor cold-hot source in the precooling thawing apparatus, open the feed liquor valve on the precooling thawing apparatus feed tube then, make fluid sample to be analyzed flow into precooling in the precooling chamber;
3, get the liquid step: the elevating mechanism action of first automatically controlled rotating mechanism on the control transverse arm and column bottom, make transverse arm drive measuring cell and move to the discharging tube mouth of pipe place (promptly getting liquid level puts) that bottom, precooling thawing apparatus precooling chamber is provided with fixed displacement pump, start fixed displacement pump, in measuring cell, quantitatively inject fluid sample to be analyzed;
4, freezing step: open the door closure of containing the liquid device refrigerating chamber, the elevating mechanism action of first automatically controlled rotating mechanism on the control transverse arm and column bottom, making transverse arm drive measuring cell moves in the refrigerating chamber, closed door closure, simultaneously, start and contain the low temperature conduction oil ebullator that liquid device is equipped with, begin freezing fluid sample to be analyzed;
5, set-up procedure: after treating that sample is freezing, the elevating mechanism action of control column bottom makes ice face position in the measuring cell be positioned at the focus point that excites of laser pulse, i.e. the focus place of pulsed laser optical window condenser lens;
6, measuring process: start the spectrometer of laser measuring assembly and contain the blower fan that liquid device is equipped with, spectrometer starting impulse laser instrument carries out single measurement, after single measurement is finished, the second automatically controlled rotating mechanism action on the control transverse arm, the suspension rod drive measuring cell of cross arm free end is rotated to an angle, measure once more,, stop cold machine, blower fan and low temperature conduction oil ebullator up to finishing predetermined measurement number of times;
7, ending step: open the door closure of containing the liquid device refrigerating chamber, the elevating mechanism action of first automatically controlled rotating mechanism on the control transverse arm and column bottom, making transverse arm drive measuring cell, to move to the thawing of precooling thawing apparatus indoor, the closed chamber door closure that melts, after the sample in the measuring cell melts, start the motor that is used to draw backguy on the transverse arm, measuring cell is tilted, fluid sample in the measuring cell flows into from leakage hole and melts the chamber, discharging tube through melting the bottom, chamber flows in the exhausted bath box, rising along with waste liquid liquid level in the exhausted bath box, ball float come-up in the level gauging nanubrium, touch the level switch at level gauging nanubrium top until the ball float come-up, make valve open on the sewer pipe, waste liquid flows into the blow-off line in the laboratory in the exhausted bath box.
In addition, in order to realize automatic measurement of the present invention, liquid phase sample laser-induced spectroscopic analysis device also is provided with and is used to control laser measuring assembly, contain liquid device, the precooling thawing apparatus, measuring cell transposition mechanism, the self-con-tained unit of waste liquid temporary storage mechanism work, described self-con-tained unit comprises signal gathering unit, with the control module that the signal gathering unit output terminal links to each other, signal gathering unit comprises the distance measuring sensor that is arranged at pulsed laser optical window position in the laser measuring assembly, be arranged at respectively and contain liquid device cooling chamber and the indoor temperature sensor of precooling thawing apparatus thawing, and be arranged to be respectively applied on the transverse arm in the measuring cell transposition mechanism and realize the transverse arm rotational positioning, suspension rod rotates the alignment sensor that resets; The output terminal of control module is connected (all controlled unit controls of action that is following electric component) with following electric component: the spectrometer of laser measuring assembly, contain cold machine, blower fan, the low temperature conduction oil ebullator of liquid device, semiconductor cold-hot source in the precooling thawing apparatus, feed liquor valve, liquid valve, fixed displacement pump, the motor of the motor of the first automatically controlled rotating mechanism, the second automatically controlled rotating mechanism, elevating mechanism and traction backguy in the measuring cell transposition mechanism, the valve in the waste liquid temporary storage mechanism on the sewer pipe; Wherein, the valve in the feed liquor valve in the precooling thawing apparatus, liquid valve and the waste liquid temporary storage mechanism on the sewer pipe is all solenoid valve, and the level switch in the waste liquid temporary storage mechanism links to each other with the input end of control module.The status information that described control module will collect according to signal gathering unit, automatically realize the operating process of device of the present invention, finish constituent analysis, need not human intervention, make measurement mechanism of the present invention be particularly useful for poisonous and hazardous liquid component analysis the liquid sample.And for those skilled in the art, the control module that each electric component in the device is controlled is easy to realize.
Compared with prior art, measurement mechanism of the present invention is at first realized the curing of fluid sample to be analyzed with reasonable succinct structure, be about to fluid sample snap frozen to be analyzed and become solid ice, and then adopt the laser-induced spectrum technology that fluid sample is carried out constituent analysis.Like this, not only the elemental composition of fluid sample does not change, and has avoided adopting the laser-induced spectrum technology to carry out the problems that exist when liquid component is measured, and has improved the accuracy of measuring.Can realize the robotization of liquid phase sample is detected, can be widely used in need not human intervention in production run, the environmental protection field, be particularly useful for poisonous and hazardous liquid component analysis, have and measure advantages such as convenient, that maintenance is little.
Description of drawings
Fig. 1 is a structural representation of the present invention;
Fig. 2 is for containing the structural representation of liquid device;
Fig. 3 is for containing the vertical view of liquid device refrigerating chamber door closure;
Fig. 4 is the structural representation of precooling thawing apparatus;
Fig. 5 melts the vertical view of chamber door closure for the precooling thawing apparatus;
Fig. 6 is the structural representation of laser measuring assembly;
Fig. 7 is the structural representation of measuring cell transposition mechanism;
Fig. 8 is the vertical view of measuring cell;
Fig. 9 is the structural representation of waste liquid temporary storage mechanism;
Among the figure: the 1-pulsed laser; The 2-spectrometer; 3-conducts optical fiber; The 4-fibre-optical probe; The 5-condenser lens; The 6-refrigerating chamber; The 7-measuring cell; The cold machine of 8-; The 9-blower fan; 10-low temperature conduction oil ebullator; The 11-door closure; The 12-measured hole; The 13-inner casing; 14-refrigerant cycle evaporation tube; 15 shells; The 16-thermal insulation material; 17-air inducing hole; 18,19-circulation line; 20-melts the chamber; 21-precooling chamber; 22-semiconductor cold-hot source; The 23-thermal insulation material; The 24-door closure; The 25-discharging tube; The 26-feed tube; 27-feed liquor valve; 28,29-discharging tube; The 30-fixed displacement pump; The 31-liquid valve; The 32-exhausted bath box; The 33-sewer pipe; The 34-valve; 35-level gauging nanubrium; The 36-level switch; The 37-ball float; The 38-column; The 39-transverse arm; The 40-motor; The 41-elevating mechanism; The 42-first automatically controlled rotating mechanism; The 43-suspension rod; The 44-second automatically controlled rotating mechanism; The 45-bearing pin; The 46-fixture; The 47-leakage hole; The 48-through hole; The 49-backguy; The 50-motor; The 51-distance measuring sensor; 52,53-temperature sensor; 54,55-alignment sensor; The 56-induced pipe; The 57-port lid; The 58-balancing weight; The 59-through hole; The 60-control module.
Embodiment
Liquid phase sample laser-induced spectroscopic analysis device, comprise laser measuring assembly, hold the Sheng liquid device of liquid phase sample when being used to measure, as shown in Figure 6, laser measuring assembly comprises pulsed laser 1, spectrometer 2, through conducting the fibre-optical probe 4 that optical fiber 3 links to each other with spectrometer 2, contain liquid device place pulsed laser 1 under, the optical window of pulsed laser 1 and Sheng liquid device are over against setting, and be provided with condenser lens 5 before the optical window of pulsed laser 1, as Fig. 2, shown in 3, described Sheng liquid device comprises refrigerating chamber 6, and place measuring cell 7 in the refrigerating chamber 6, and dispose cold machine 8, blower fan 9, low temperature conduction oil ebullator 10, refrigerating chamber 6 adopts inside and outside duplex shell structure, the top, chamber is furnished with door closure 11, have on the door closure 11 with pulsed laser 1 optical window over against measured hole 12, the refrigerating chamber 6 inner casings 13 outer refrigerant cycle evaporation tubes 14 that are sticked and link to each other with cold machine 8, and 15 on refrigerant cycle evaporation tube 14 and shell are filled with thermal insulation material 16, inner casing 13 tops offer the air inducing hole 17 that links to each other with blower fan 9 through induced pipe 56, and inner casing 13 bottoms are provided with the circulation line 18 that two-way links to each other with low temperature conduction oil ebullator 10,19.
Liquid phase sample laser-induced spectroscopic analysis device also is provided with the precooling thawing apparatus, as Fig. 4, shown in 5, comprise and melt chamber 20, and around melting the 20 peripheral precooling chambeies 21 that are provided with, chamber, melt between chamber 20 and the precooling chamber 21 and be provided with several semiconductor Cooling and Heat Source 22, the hot junction in semiconductor cold-hot source 22 contacts with thawing chamber 20 outer walls, cold junction contacts with precooling chamber 21 chamber walls, and be filled with thermal insulation material 23 between the semiconductor cold-hot source 22, melt 20 tops, chamber and be furnished with door closure 24, the bottom is provided with discharging tube 25,21 tops, precooling chamber are provided with feed tube 26, and feed tube 26 is provided with feed liquor valve 27; 21 bottoms, precooling chamber are provided with two- way discharging tube 28,29, and are respectively equipped with fixed displacement pump 30 and liquid valve 31 on the two- way discharging tube 28,29.
Discharging tube 25 belows that the precooling thawing apparatus melts the chamber are provided with the waste liquid temporary storage mechanism that comprises exhausted bath box 32, as shown in Figure 8, exhausted bath box 32 bottoms are provided with sewer pipe 33, and sewer pipe 33 is provided with valve 34, the level gauging nanubrium 35 that the lower end is communicated with exhausted bath box 32 suspends in the exhausted bath box 32, level gauging nanubrium 35 tops are fixed with the level switch 36 that valve 34 opens and closes on the control sewer pipe 33, are provided with the ball float 37 that triggers level switch 36 in the level gauging nanubrium 35.
Contain between liquid device and the precooling thawing apparatus and be provided with measuring cell transposition mechanism, as shown in Figure 7, comprising column 38, being arranged at column 38 tops to serve as the transverse arm 39 that axle rotates with column 38, and transverse arm 39 is vertical with column 38; Column 38 bottoms are provided with the elevating mechanism 41 that is driven by motor 40, and it serve as first an automatically controlled rotating mechanism 42 of axle rotation with column 38 that transverse arm 39 is provided with the control transverse arm 39 that is positioned at directly over the column 38; The free end of transverse arm 38 suspension rod 43 that has been hung, transverse arm 39 are provided with and are positioned at the second automatically controlled rotating mechanism 44 that the control suspension rod 43 directly over the suspension rod 43 rotates, and measuring cell 7 is fixing with bearing pin 45 with suspension rod 43 bottoms; Described measuring cell 7 central authorities are provided with and are used for and fixture 46 that suspension rod 43 bottom bearing pins are fixing, and measuring cell 7 pool wall tops have leakage hole 47, and leakage hole 47 center lines are vertical with suspension rod 43 bottom bearing pins 45; The door closure 11,24 of containing liquid device refrigerating chamber 6 and precooling thawing apparatus thawing chamber 20 configurations all adopts two-door fan structure, and 11,24 liang of door leaf places of being harmonious of door closure have the through hole 48,59 that passes for suspension rod 43 respectively.Be fixed with backguy 49 on the pool wall of measuring cell 7 leakage holes 47 opposite sides, transverse arm 39 is provided with the motor 50 that traction backguy 49 has a down dip measuring cell 7 leakage holes 47 sides.
The course of work of measuring equipment of the present invention is as follows:
1, preparation process: the feed tube 26 of precooling thawing apparatus fixedly is communicated with the container that holds fluid sample to be analyzed, and the sewer pipe 33 of waste liquid temporary storage mechanism is communicated with the blow-off line in the laboratory, adds an amount of low temperature conduction oil in refrigerating chamber 6;
2, precooling step: start the cold machine 8 of Sheng liquid device outfit and the semiconductor cold-hot source 22 in the precooling thawing apparatus, open the feed liquor valve 27 on the precooling thawing apparatus feed tube 26 then, make fluid sample to be analyzed flow into precooling in the precooling chamber 21;
3, get the liquid step: first automatically controlled rotating mechanism 42 on the control transverse arm 39 and 41 actions of the elevating mechanism of column 38 bottoms, make transverse arm 39 drive discharging tube 28 mouth of pipe places (promptly getting liquid level puts) that measuring cell 7 moves to 21 bottoms, precooling thawing apparatus precooling chamber, is provided with fixed displacement pump 30, start fixed displacement pump 30, in measuring cell 7, quantitatively inject fluid sample to be analyzed;
4, freezing step: open the door closure 11 of containing liquid device refrigerating chamber 6, first automatically controlled rotating mechanism 42 on the control transverse arm 39 and 41 actions of the elevating mechanism of column 38 bottoms, making transverse arm 39 drive measuring cell 7 moves in the refrigerating chamber 6, closed door closure 11, simultaneously, start and contain the low temperature conduction oil ebullator 10 that liquid device is equipped with, begin freezing fluid sample to be analyzed;
5, set-up procedure: after treating that sample is freezing, elevating mechanism 41 actions of control column 38 bottoms make ice face positions in the measuring cell 7 be positioned at the focus point that excites of laser pulse, i.e. the focus place of pulsed laser 1 optical window condenser lens 5;
6, measuring process: start the spectrometer 2 of laser measuring assembly and contain the blower fan 9 that liquid device is equipped with, spectrometer 2 starting impulse laser instruments 1 carry out single measurement, after single measurement is finished, second automatically controlled rotating mechanism 44 actions on the control transverse arm 39, making transverse arm 39 free-ended suspension rods 43 drive measuring cell 7 rotates to an angle, measure once more,, stop cold machine 8, blower fan 9 and low temperature conduction oil ebullator 10 up to finishing predetermined measurement number of times;
7, ending step: open the door closure 11 of containing liquid device refrigerating chamber 6, first automatically controlled rotating mechanism 42 on the control transverse arm 39 and 41 actions of the elevating mechanism of column 38 bottoms, making transverse arm 39 drive measuring cell 7 moves in the thawing chamber 20 of precooling thawing apparatus, closed chamber 20 door closures 24 that melt, after the sample in the measuring cell 7 melts, start the motor 50 that is used to draw backguy 49 on the transverse arm 39, measuring cell 7 is tilted, fluid sample in the measuring cell 7 flows into from leakage hole 47 and melts chamber 20, discharging tube 25 through melting 20 bottoms, chamber flows in the exhausted bath box 32, rising along with waste liquid liquid level in the exhausted bath box 32, ball float 37 come-ups in the level gauging nanubrium 35, touch the level switch 36 at level gauging nanubriums 35 tops until ball float 37 come-up, valve 34 is opened, waste liquids flow into the blow-off line in the laboratories in the exhausted bath box 32.
In addition, in order to realize automatic measurement of the present invention, liquid phase sample laser-induced spectroscopic analysis device also is provided with and is used to allocate laser measuring assembly, contain liquid device, the precooling thawing apparatus, measuring cell transposition mechanism, the self-con-tained unit of waste liquid temporary storage mechanism work, described self-con-tained unit comprises signal gathering unit, the control module 60 that links to each other with the signal gathering unit output terminal, signal gathering unit comprise the distance measuring sensor 51 that is arranged at pulsed laser 1 optical window position in the laser measuring assembly, be arranged at the temperature sensor of containing in liquid device cooling chamber 6 and the precooling thawing apparatus thawing chamber 20 52 respectively, 53, and be arranged to be respectively applied on the transverse arm 39 in the measuring cell transposition mechanism and realize transverse arm 39 rotational positioning, suspension rod 43 rotates the alignment sensor 54 that resets, 55; The output terminal of control module 60 is connected (action all controlled unit 60 controls that are following electric component) with following electric component: the spectrometer 2 of laser measuring assembly, contain cold machine 8, blower fan 9, the low temperature conduction oil ebullator 10 of liquid device, semiconductor cold-hot source 22 in the precooling thawing apparatus, feed liquor valve 27, liquid valve 31, fixed displacement pump 30, the motor 50 of the motor 40 of first automatically controlled rotating mechanism 42, the second automatically controlled rotating mechanism 44, elevating mechanism 41 and traction backguy in the measuring cell transposition mechanism, the valve 34 in the waste liquid temporary storage mechanism on the sewer pipe 33; Wherein, the valve 34 in the feed liquor valve 27 in the precooling thawing apparatus, liquid valve 31 and the waste liquid temporary storage mechanism on the sewer pipe 33 is all solenoid valve, and the level switch 36 in the waste liquid temporary storage mechanism links to each other with the input end of control module 60.
During concrete enforcement, measuring cell 7 bottoms, contain that the ends are all inverted cone shape in the thawing chamber 20 of the ends, precooling thawing apparatus in the refrigerating chamber 6 of liquid device, and tapering is identical, is convenient to measuring cell 7 and topples over the liquid sample, melt chamber 20 and drain the liquid sample; The measured hole of containing on liquid device refrigerating chamber 6 door closures 11 12 is furnished with port lid 57, when carrying out laser measurement, takes off and gets final product; The xsect of described measuring cell 7 central fixtures 46 is a C shape, and in the measuring cell 7 with fixture 46 gap over against a side be provided with the balancing weight 58 that makes measuring cell 7 balances, leakage hole 47 offer position and balancing weight 58 positions over against.
Claims (6)
1. liquid phase sample laser-induced spectroscopic analysis device, comprise laser measuring assembly, hold the Sheng liquid device of liquid phase sample when being used to measure, laser measuring assembly comprises pulsed laser (1), spectrometer (2), through conducting the fibre-optical probe (4) that optical fiber (3) links to each other with spectrometer (2), contain liquid device place pulsed laser (1) under, the optical window of pulsed laser (1) and Sheng liquid device are over against setting, and be provided with condenser lens (5) before the optical window of pulsed laser (1), it is characterized in that: described Sheng liquid device comprises refrigerating chamber (6), and place measuring cell (7) in the refrigerating chamber (6), and dispose cold machine (8), blower fan (9), low temperature conduction oil ebullator (10), refrigerating chamber (6) adopts inside and outside duplex shell structure, the top, chamber is furnished with door closure (11), have on the door closure (11) with pulsed laser (1) optical window over against measured hole (12), the outer refrigerant cycle evaporation tube (14) that is sticked and links to each other of refrigerating chamber (6) inner casing (13) with cold machine (8), and be filled with thermal insulation material (16) between refrigerant cycle evaporation tube (14) and shell (15), inner casing (13) top offers the air inducing hole (17) that links to each other with blower fan (9) through induced pipe (56), and inner casing (13) bottom is provided with the circulation line (18 that two-way links to each other with low temperature conduction oil ebullator (10), 19).
2. liquid phase sample laser-induced spectroscopic analysis device according to claim 1, it is characterized in that: also be provided with the precooling thawing apparatus, comprise and melt chamber (20), and around melting the peripheral precooling chamber (21) that is provided with, chamber (20), melt between chamber (20) and precooling chamber (21) and be provided with several semiconductor Cooling and Heat Source (22), the hot junction in semiconductor cold-hot source (22) contacts with thawing chamber (20) outer wall, cold junction contacts with chamber, precooling chamber (21) wall, and be filled with thermal insulation material (23) between semiconductor cold-hot source (22), melt top, chamber (20) and be furnished with door closure (24), the bottom is provided with discharging tube (25), top, precooling chamber (21) is provided with feed tube (26), and feed tube (26) is provided with feed liquor valve (27); Bottom, precooling chamber (21) is provided with two-way discharging tube (28,29), and is respectively equipped with fixed displacement pump (30) and liquid valve (31) on the two-way discharging tube (28,29).
3. liquid phase sample laser-induced spectroscopic analysis device according to claim 2, it is characterized in that: discharging tube (25) below that the precooling thawing apparatus melts the chamber is provided with the waste liquid temporary storage mechanism that comprises exhausted bath box (32), exhausted bath box (32) bottom is provided with sewer pipe (33), and sewer pipe (33) is provided with valve (34), the level gauging nanubrium (35) that the lower end is communicated with exhausted bath box (32) suspends in the exhausted bath box (32), level gauging nanubrium (35) top is fixed with control sewer pipe (33) and goes up the level switch (36) that valve (34) opens and closes, and is provided with the ball float (37) that triggers level switch (36) in the level gauging nanubrium (35).
4. liquid phase sample laser-induced spectroscopic analysis device according to claim 3, it is characterized in that: contain between liquid device and the precooling thawing apparatus and be provided with measuring cell transposition mechanism, comprising column (38), being arranged at column (38) top to serve as the transverse arm (39) that axle rotates with column (38), and transverse arm (39) is vertical with column (38); Column (38) bottom is provided with the elevating mechanism (41) that is driven by motor (40), and it serve as first an automatically controlled rotating mechanism (42) of axle rotation with column (38) that transverse arm (39) is provided with the control transverse arm (39) that is positioned at directly over the column (38); The free end of transverse arm (38) suspension rod (43) that has been hung, transverse arm (39) are provided with and are positioned at the second automatically controlled rotating mechanism (44) that the control suspension rod (43) directly over the suspension rod (43) rotates, and measuring cell (7) is fixing with bearing pin (45) with suspension rod (43) bottom; Described measuring cell (7) central authorities are provided with and are used for and the fixing fixture (46) of suspension rod (43) bottom bearing pin, and measuring cell (7) pool wall top has leakage hole (47), and leakage hole (47) center line is vertical with suspension rod (43) bottom bearing pin (45); The door closure (11,24) of containing liquid device refrigerating chamber (6) and precooling thawing apparatus thawing chamber (20) configuration all adopts two-door fan structure, and door closure (11,24) the two door leaf places of being harmonious have the through hole (48,59) that passes for suspension rod (43) respectively.
5. liquid phase sample laser-induced spectroscopic analysis device according to claim 4, it is characterized in that: be fixed with backguy (49) on the pool wall of measuring cell (7) leakage hole (47) opposite side, transverse arm (39) is provided with the motor (50) that traction backguy (49) has a down dip measuring cell (7) leakage hole (47) side.
6. liquid phase sample laser-induced spectroscopic analysis device according to claim 5, it is characterized in that: also be provided with and be used to allocate laser measuring assembly, contain liquid device, the precooling thawing apparatus, measuring cell transposition mechanism, the self-con-tained unit of waste liquid temporary storage mechanism work, described self-con-tained unit comprises signal gathering unit, the control module (60) that links to each other with the signal gathering unit output terminal, signal gathering unit comprise the distance measuring sensor (51) that is arranged at pulsed laser in the laser measuring assembly (1) optical window position, be arranged at the temperature sensor of containing in liquid device cooling chamber (6) and the precooling thawing apparatus thawing chamber (20) (52 respectively, 53), and be arranged to be respectively applied on the transverse arm (39) in the measuring cell transposition mechanism and realize transverse arm (39) rotational positioning, suspension rod (43) rotates the alignment sensor (54 that resets, 55); The output terminal of control module (60) is connected with following electric component: the spectrometer of laser measuring assembly (2), contain cold machine (8), blower fan (9), the low temperature conduction oil ebullator (10) of liquid device, semiconductor cold-hot source (22) in the precooling thawing apparatus, feed liquor valve (27), liquid valve (31), fixed displacement pump (30), the motor (50) of the motor (40) of the first automatically controlled rotating mechanism (42), the second automatically controlled rotating mechanism (44), elevating mechanism (41) and traction backguy in the measuring cell transposition mechanism, the valve (34) on the sewer pipe in the waste liquid temporary storage mechanism (33); Wherein, the valve (34) in the feed liquor valve (27) in the precooling thawing apparatus, liquid valve (31) and the waste liquid temporary storage mechanism on the sewer pipe (33) is all solenoid valve, and the level switch in the waste liquid temporary storage mechanism (36) links to each other with the input end of control module (60).
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| Application Number | Priority Date | Filing Date | Title |
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| CN2009100755778A CN101655458B (en) | 2009-09-30 | 2009-09-30 | Liquid phase sample laser-induced spectroscopic analysis device |
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| Application Number | Priority Date | Filing Date | Title |
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| CN2009100755778A CN101655458B (en) | 2009-09-30 | 2009-09-30 | Liquid phase sample laser-induced spectroscopic analysis device |
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| CN101655458B true CN101655458B (en) | 2010-12-01 |
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| CN102735657B (en) * | 2012-07-10 | 2014-07-23 | 广东电网公司电力科学研究院 | Laser induced breakdown spectrometer and spectral signal collection method of same |
| CN103543065B (en) * | 2013-10-14 | 2016-01-20 | 北京工业大学 | A kind of ice body nano impress sample bench and related experimental methods |
| EP3912255A4 (en) * | 2019-01-17 | 2022-11-09 | Wi-Charge Ltd. | Safe enclosures for wireless power supply |
| CN114910986A (en) * | 2022-04-22 | 2022-08-16 | 上海酷聚科技有限公司 | Liquid lens |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101441175A (en) * | 2007-11-19 | 2009-05-27 | 中国科学院理化技术研究所 | Surface plasma resonance detection device based on laser scanning surface confocal microscopic system |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101441175A (en) * | 2007-11-19 | 2009-05-27 | 中国科学院理化技术研究所 | Surface plasma resonance detection device based on laser scanning surface confocal microscopic system |
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| Title |
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| D.M. Diaz Pace et al.,.Analysis of Heavy metals in liquids using Laser Induced Breakdown Spectroscopy by liquid-to-solid matrix conversion.《Spectrochimica Acta Part B》.2006,第61卷(第8期),929-933. * |
| JP昭61-222287A 1986.10.02 |
| 冯晓霞 等.激光诱导击穿光谱测量土壤重金属污染研究.《测试技术学报》.2009,第23卷(第3期),275-278. |
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