CN102661936A - Portable heavy metal detector - Google Patents
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- CN102661936A CN102661936A CN2012101515082A CN201210151508A CN102661936A CN 102661936 A CN102661936 A CN 102661936A CN 2012101515082 A CN2012101515082 A CN 2012101515082A CN 201210151508 A CN201210151508 A CN 201210151508A CN 102661936 A CN102661936 A CN 102661936A
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Abstract
The invention discloses a portable heavy metal detector comprising a box, and a laser, a transmitting and collecting optical circuit, a rotary sample table and a high resolution spectrograph all arranged in the box, wherein a computer installed with control software and a data processing analysis program is connected to the high resolution spectrograph; the transmitting and collecting optical circuit comprises a transmitting optical circuit element, and a collecting optical circuit element; the transmitting and collecting optical circuit is connected to the high resolution spectrograph through an optical fiber; and the rotary sample table comprises a sample table base plate, a sample table top plate, a roller, an elastic mechanism, a sample table base and a motor. The detector for detecting the heavy metal content in fruits provided by the invention is capable of quickly and simultaneously detecting the content of a plurality of heavy metals in a fruit in orchard field; the detector can be mounted on an automobile, and is convenient to move, short in detection time, and capable of satisfying field real-time detection, and also capable of simultaneously detecting various element.
Description
Technical field
The present invention relates to a heavy metal species pick-up unit, particularly, relate to a kind of portable, utilize LIBS technology for detection surface configuration complicated, irregular object, the especially device of the content of beary metal of fruits and vegetables agricultural products.
Background technology
Along with the continuous development of modern industrial technology, heavy metal is used quite extensive on the road of industrial development, but the pollutant that thereupon produces also rolls up; Undressed three industrial wastes are by a large amount of being discharged in the environment; And human indispensable agricultural product also are greatly affected, and industrial pollutants disorderly row leave about the pollution that the plantation that makes fruit receives each heavy metal species, comprise Cr, Cu, Cd, Pb etc.; These heavy metals get in the human body the most at last, influence healthy.Therefore in time detect content of beary metal in the fruit, the control heavy metal human body of entering is had great significance.
The common method of detection by quantitative heavy metal has check and analysis technology such as atomic absorption spectrography (AAS), inductively coupled plasma emission spectrography at present; Though these spectroscopic methodology accuracy of detection and stability are all better; But long to sample pre-treatments complicacy and time, can't realize the demand of real-time field quick detection.
LIBS (Laser-Induced Breakdown Spectroscopy; LIBS) technology is a kind of multielement while detection technique based on atomic emission spectrum that grew up in recent years; It can detect the sample of different shape; Comprise solid, liquid, gas, therefore can be widely used in different field such as industrial products detection, agricultural product quality detection, environmental pollution monitoring.Its ultimate principle is that a branch of intense laser pulse shines sample surfaces after lens focus; The high-energy of laser makes the atom of focal spot break away from material itself; Under the effect of local highfield and other atoms, ionization has produced high temperature, highdensity plasma.These plasma resonances go out the photon of CF, form characteristic spectrum, utilize spectrometer to collect characteristic spectrum, analyze the relation of spectral intensity and concentration of element, calculate the concentration that corresponding spectral intensity can obtain said element.
Great majority are to utilize surface and the relatively regular objects of shape such as LIBS technology for detection soil, the WS, alloy in existing document and the patent; For example: Research And Design Institute Of Metallurgical Automation; Wu Shaobo etc. are based on the basis brass full elemental analysis device and method of LIBS (one Chinese patent application number: 201110280889.X); Tsing-Hua University, horse Xiao Hong etc., the LIBS pick-up unit of detection time and position-controllable (one Chinese patent application number: 201010569401.0); Chinese Marine University, the guiding deposition strengthening method that Zheng Ronger etc., LIBS water intermediate ion detect (one Chinese patent application number: 200910210855.6).Yet, do not see and utilize LIBS to detect the patent of heavy metal isolated plant aspect in the fruits and vegetables agricultural products.
Utilize LIBS to detect heavy metal in the fruits and vegetables agricultural products, also face technical barrier.Agricultural product such as fruit, vegetables require not damaged to detect.But laser energy is very strong, and temperature is very high, and as impacting for a long time, then burning can appear in the sample surfaces same point.Though this problem can be solved through sample is placed on the platform of a rotation, impacts in different positions at every turn; But the out-of-shape of most of fruit, vegetables; Make that laser focusing point ceaselessly changes in the sample surfaces degree of depth in rotation, the spectrum signal-to-background ratio that obtains is very low; The intensity of characteristic spectrum is also very unstable, brings great difficulty for the LIBS Dynamic Non-Destruction Measurement.Draw based on above analysis, sample will accomplish also that in rotation the degree of depth of laser focusing point is consistent, and this detects extremely important to the heavy metal that the LIBS technology is used for the fruits and vegetables agricultural products.
Therefore, need a kind of consistent pick-up unit of the degree of depth that can make sample rotation and laser focusing point of exploitation, be used for the detection of the irregular fruits and vegetables agricultural products of surface configuration heavy metal.
Summary of the invention
The objective of the invention is provides a kind of portable heavy metal pick-up unit based on the LIBS technology; Said device is provided with the consistent rotary sample stage of the degree of depth that can make sample rotation and laser focusing point; Technical matterss such as detection difficulty that the sample out-of-shape causes is big have been solved; And, said device can satisfy the scene, fast, multielement demand such as detects simultaneously.
In order to achieve the above object; The invention provides portable heavy metal pick-up unit; Said device comprises: casing; And be arranged on laser instrument, the emission in the casing and collect light path, rotary sample stage, high precision spectrometer, be connected and installed with the computing machine of Control Software and Data Management Analysis program on the said high precision spectrometer;
Described emission and collect light path and comprise: the emission light path element of forming by laser mirror, catoptron with holes and first plano-convex lens; And, the collection light path element of forming by first plano-convex lens, catoptron with holes, second plano-convex lens and fibre-optical probe; The fibre-optical probe of described emission and collection light path is connected to described high precision spectrometer through optical fiber;
Described rotary sample stage comprises:
Be fixed in the sample stage base on the box bottom,
Be arranged on the elastic mechanism on the sample stage base;
Be fixed on elastic mechanism upper end, and with the vertically disposed sample stage base plate of elastic mechanism, said sample stage base plate middle part is provided with some active rollers that laterally arrange, said active roller is by the motor drives that is electrically connected; And
Be fixed in the casing; And be set in parallel in the sample stage top board directly over the sample stage base plate; Said sample stage top board middle part is provided with some return idlers that laterally arrange, said active roller and the parallel corresponding setting up and down of return idler, and specimen holder places between said active roller and the return idler.
Above-mentioned portable heavy metal pick-up unit; Wherein, Described laser instrument emitted laser bundle is 45 ° and incides on the described laser mirror, the parallel correspondence of described catoptron with holes be arranged on laser mirror under, described first plano-convex lens is set in parallel in directly over the sample stage; And be positioned at catoptron with holes under, the central point of described catoptron with holes, second plano-convex lens and fibre-optical probe is on same straight line.
Above-mentioned portable heavy metal pick-up unit, wherein, described fibre-optical probe is set in place on the horizontal guide rail of laser instrument below through the fibre-optical probe stationary installation.
Above-mentioned portable heavy metal pick-up unit wherein, also is provided with first base on the described horizontal guide rail, said first base has micro-adjusting mechanism, and described fibre-optical probe stationary installation is fixed on said first base.
Above-mentioned portable heavy metal pick-up unit, wherein, described second plano-convex lens is set in place on the horizontal guide rail of laser instrument below.
Above-mentioned portable heavy metal pick-up unit wherein, also is provided with second base on the described horizontal guide rail, said second base has micro-adjusting mechanism, and described second plano-convex lens is fixed on said second base.
Above-mentioned portable heavy metal pick-up unit wherein, has certain intervals between the described active roller.
Above-mentioned portable heavy metal pick-up unit, wherein, described elastic mechanism is made up of the some springs that laterally arrange.
Above-mentioned portable heavy metal pick-up unit, wherein, described rotary sample stage also comprises to be arranged on and horizontally rotates the displacement platform on the sample stage top board.
Another object of the present invention provides the application of said portable heavy metal pick-up unit in the content of beary metal that detects erose object.Preferably; Said erose object; Be meant the fruits and vegetables agricultural products, comprise subsphaeroidal, as can be driven rotation when being placed on said sample stage fruits and vegetables agricultural products, for example apple, pears, orange, orange, apricot, plum, grape, spherical eggplant etc. by said roller; And non-subsphaeroidal, be difficult to when being placed on the said sample stage driven the fruits and vegetables agricultural products that rotates, for example cucumber, banana, cucurbita pepo etc. by said roller.
The present invention has designed the accuracy that a kind of adjustable rotary sample mounting table is used for improving LIBS test sample content of beary metal especially; Especially; Improved the LIBS quality of irregular sample, can satisfy in the orchard, the scene, vegetable plot detects various heavy content in fruit, the vegetables fast simultaneously.Device of the present invention also can be provided with universal wheel, and can use lorry loading, conveniently moving, and detection time is short, can satisfy on-site real-time and detect, and can detect multiple element simultaneously.
Description of drawings
Fig. 1 is the structural representation of portable heavy metal pick-up unit of the present invention.
Fig. 2 is emission of the present invention and collects the light path signal.
Fig. 3 is the rotary sample stage structural representation of the present invention.
Fig. 4 is the structural representation of catoptron with holes of the present invention.
Fig. 5 is the structural representation that horizontally rotates the displacement platform of the present invention.
Embodiment
Below in conjunction with accompanying drawing technical scheme of the present invention is done explanation further.
As shown in Figure 1; The invention provides a kind of portable laser induced breakdown spectroscopy fruit heavy metal pick-up unit; Said device comprises: casing 1 and be arranged on laser instrument 2, the emission in the casing and collect light path 3, rotary sample stage 4, high precision spectrometer 5 is connected with the computing machine that Control Software and Data Management Analysis program are installed on the said high precision spectrometer 5.
Described laser instrument 2 is arranged on the top board inboard of casing 1, and the laser instrument 2 that pick-up unit of the present invention uses is for transferring Q nanosecond Nd:YAG laser instrument, and launching wavelength is 1064 nm laser; Pulse width is 8ns; The monopulse highest energy is 200mJ, and diameter is 6mm, and laser energy is adjustable.
As shown in Figure 2, be the structural representation of emission of the present invention and collection light path, described emission and collection light path 3 comprise the emission light path and collect light path, and said emission light path comprises: laser mirror 13 and catoptron with holes 14.The central point of said laser mirror 13 and the laser emission port of laser instrument are on same horizontal linear, and the top board of said laser mirror 13 and casing 1 is 45 ° of arrangements and is fixed in casing 1 top board.Described catoptron with holes 14 be set in parallel in laser mirror 13 under, be fixed in the casing 1; As shown in Figure 4, it is porose 141 that the center of said catoptron 14 with holes is provided with, and passes said hole 141 through the laser mirror laser light reflected.Described collection light path comprises: first plano-convex lens 15, second plano-convex lens 16 and fibre-optical probe 18; Said fibre-optical probe 18 is connected on the high precision spectrometer 5 through optical fiber 19.Described first plano-convex lens 15 is parallel to box bottom, be arranged on catoptron 14 with holes under, and be positioned at directly over the sample stage 4.Described second plano-convex lens 16 is fixed on the guide rail 20 that is parallel to box bottom perpendicular to box bottom; More preferably, first base 21 with fine tuning structure is set on the said guide rail 20, said second plano-convex lens 16 is installed on said first base 21; Described fibre-optical probe 18 is fixed on the horizontal guide rail 20 that is parallel to box bottom through fibre-optical probe stationary installation 17; More preferably; Also be provided with second base 22 with fine tuning structure on the said guide rail 20, said fibre-optical probe 18 is installed on said second base 22.Described catoptron with holes 14, second plano-convex lens 16 and fibre-optical probe 18 threes' central point is positioned on the same horizontal linear.Described fibre-optical probe 18 is on the central shaft of second plano-convex lens 16; During being provided with of guide rail 20 for the ease of the horizontal adjustment fibre-optical probe 18 and second plano-convex lens 16; And; The position of also fine-tuning two bases during testing (first base 21 and second base 22) and height are to gather best in quality spectrum.
When said pick-up unit is worked, the laser of the horizontal direction of laser instrument emission, the laser mirror 13 of 45 ° of directions of warp is reflected into vertical direction; Pass the hole (141) of catoptron 14 with holes then, impinge perpendicularly on first plano-convex lens 15, at this moment; Laser beam is coaxial in first plano-convex lens 15; Focus on the fruit sample that is positioned on the sample stage 4 through first plano-convex lens 15 again, the spectrum line that said fruit sample gives off through superlaser changes into directional light through first planoconvex lens 15 and incides on the catoptron 14 with holes; Reflex on second plano-convex lens 16 through catoptron 14 with holes; Focus on the fibre-optical probe 18 through the convex surface of second plano-convex lens 16, again through optical fiber 19 with information transmission to high precision spectrometer 5, accomplish the collection of spectroscopic data.It is that 100mm, diameter are the quartzy plano-convex lens of 30mm that the condenser lens of described first plano-convex lens and second plano-convex lens all adopts focal length.
Sample stage of the present invention has adjustable height and also can drive characteristics such as sample rotation according to the characteristics design of the non-regular shapes of agricultural product such as most of fruit, vegetables, is used to place sample.Rotary sample stage 4 adjustable height of the present invention also have rotation roller, and said sample stage 4 is fixed on the base plate of device box 1, be positioned at first planoconvex lens 15 under.As shown in Figure 3, said sample stage 4 mainly is made up of sample stage base plate 8, sample stage top board 7, roller, elastic mechanism 11, sample stage base 12 and motor.
Described sample stage base 12 is fixed on the base plate of casing 1.
Described elastic mechanism 11 is fixed on the sample stage base 12; Said elastic mechanism 11 comprises the root spring that some parallel interval are provided with, and is held stationary, and present embodiment is selected 4 springs.
Described sample stage base plate 8 is fixedly connected on the elastic mechanism 11, and said elastic mechanism 11 is with sample stage base plate 8 roof pressure upwards.The middle part of said sample stage base plate 8 is provided with some active rollers 10 (preferred 2 rollers), and said active roller 10 is driven by the motor (not shown) that is electrically connected with it, as driving wheel.
Described sample stage top board 7 is fixed on the device box 1, is not connected the segment distance of being separated by with sample stage base plate 8.More preferably, shown sample stage top board 7 is fixed on the casing 1 through the fixed bar (not shown) that is connected on the casing 1, makes that sample stage top board 7 can be according to different needs height up and down.The middle part of said sample stage top board 7 is provided with some return idlers 9 (preferred 2 rollers), and said return idler 9 is driven by active roller 10 and rotates.During work, press down sample stage base plate 8, guarantee that through elastic mechanism 11 sample 23 is folded between active roller and the return idler.Separated by a distance between said two active rollers, make laser can arrive sample surfaces smoothly, and the sample stage top board can satisfy laser and impact the different degree of depth of sample surfaces according to different needs adjusting height.
When laser from directly over first plano-convex lens 15 impact subglobose fruits and vegetables sample surfaces vertically downward, said sample constantly slowly rotates under the effect of said roller, along the latitude direction of sample, laser impacts at sample surfaces uniformly.The characteristic spectrum that plasma resonance goes out is after catoptron 14 reflections with holes; Impinge perpendicularly on second plano-convex lens of vertical placement; Focus on fibre-optical probe; The plano-convex lens of fibre-optical probe and vertically placement is through adjusting adjustable frames fixed in position highly accurately on a guide rail, with the function that further is up to the standard and regulates.Said fibre-optical probe connects arrival high precision spectrometer through optical fiber, and it has eight different-waveband passages and enhancement mode inductance coupled apparatus ICCD, can each width of cloth spectral signal of Accurate Analysis.Further, on of the present invention and the computing machine that spectrometer is connected LIBS collection analysis software and relevant procedures are installed, are provided with and detect required correlation parameter, comprise delay time, integral time, impact number of times.Impact completion after relevant procedures are calculated data processing at laser, can demonstrate the content of detection elements fast.
Further, said motor has CS, the scalable rotating speed; Adopt different rotating speed when satisfy detecting different sample, driving wheel rotates to two different directions on the said base plate of motor drives, and driving wheel drives sample again and slowly rotates; Laser impacts at sample surfaces uniformly, reaches the purpose of Non-Destructive Testing, and said sample stage can guarantee that the laser focusing degree of depth remains unchanged; Thereby improved the stability and the signal-to-background ratio of LIBS, make that to detect data more accurate.
For non-subglobose fruits and vegetables agricultural products, be difficult to drive its rotation through the rotation of said active roller 10.Therefore; This device can be installed one in said rotary sample stage and horizontally rotate the displacement platform; As shown in Figure 5, this horizontally rotates the displacement platform and places on the sample stage top board, through moving horizontally rotary sample stage; Laser beam can at the uniform velocity be hit at said sample surfaces, thereby realizes utilizing the heavy metal to non-subglobose fruits and vegetables agricultural products to detect.
In some embodiments of the invention, further, the front and back of the casing 1 of said device are designed with two windows; Can close and open; Be used to adjust light path element position and device maintenance, laser instrument 2 is installed on the top in the device box, guide rail 20 be installed in laser instrument 2 under; Settle two movable pedestals (first base 21 and second base 22) on the guide rail 20; High precision spectrometer 5 and sample stage 4 are fixed on the base plate of device box, and are equipped with one in the side of sample stage 4 and move up and down the formula sliding door, are used for the turnover of sample.
All parts of said device all are fixed in the device box, and 4 universal wheels 6 are equipped with in device case bottom, and conveniently moving is quick, and in the open air, the use of device can provide power supply by automobile.
With subglobose fruit is example, and the workflow that apparatus of the present invention are complete is:
(1) the device energized is successively opened laser instrument 2, spectrometer 5, computing machine;
(2) open Control Software after all starting normally, Control Software is used for control device hardware and shows the concrete spectrum that collects of gatherer process;
(3) correlation parameters such as laser energy, delay time, integral time, laser frequency of LIBS work are set;
(4) open the firing button of laser instrument 2; Launch laser beam; Whether inspection emission and collection light path be normal; Adjust the position of catoptron with holes 14, first plano-convex lens 15, second plano-convex lens 16 and fibre-optical probe stationary installation 17, make fibre-optical probe 18 can collect the laser-induced breakdown characteristic spectrum of various detection elements in correct position.
(5) after the preliminary work of above-mentioned steps (4) was accomplished, laser emitted from laser instrument 2, through passing catoptron 14 with holes vertically downward after catoptron 13 reflections; After 15 focusing of first plano-convex lens, laser arrives places the fruit surface that slowly rotates on the sample stage 4, formation plasma under the effect of superlaser; Plasma resonance goes out spectrum line; After 15 refractions of first plano-convex lens, form parallel rays, after catoptron 14 reflections with holes, glancing incidence is to second plano-convex lens 16; Focus on the fibre-optical probe 18, spectral information is delivered to high precision spectrometer 5 through optical fiber 19.
(6) be equipped with outside the Control Software on the computing machine; Also be useful on the program that Treatment Analysis high precision spectrometer 5 receives spectral information; The spectral information of routine analyzer through collecting, whether the characteristic wavelength of every kind of element that automatic search is set in program qualitatively judges detection elements and exists; And in the calibration curve that the spectral intensity of the character pair wavelength program that is input to is provided with, quantitative Analysis goes out the content of detection elements and is presented on the screen.
Although content of the present invention has been done detailed introduction through above-mentioned preferred embodiment, will be appreciated that above-mentioned description should not be considered to limitation of the present invention.After those skilled in the art have read foregoing, for multiple modification of the present invention with to substitute all will be conspicuous.Therefore, protection scope of the present invention should be limited appended claim.
Claims (9)
1. portable heavy metal pick-up unit; It is characterized in that; Said device comprises: casing (1); And be arranged on laser instrument (2), the emission in the casing (1) and collect light path (3), rotary sample stage (4), high precision spectrometer (5), be connected and installed with the computing machine of Control Software and Data Management Analysis program on the said high precision spectrometer (5);
Described emission and collect light path (3) and comprise: the emission light path element of forming by laser mirror (13), catoptron with holes (14) and first plano-convex lens (15); And, the collection light path element of forming by first plano-convex lens (15), catoptron with holes (14), second plano-convex lens (16) and fibre-optical probe (18); The fibre-optical probe (18) of described emission and collection light path (3) is connected to described high precision spectrometer (5) through optical fiber (19);
Described rotary sample stage (4) comprises:
Be fixed in the sample stage base (12) on casing (1) base plate,
Be arranged on the elastic mechanism (11) on the sample stage base (12);
Be fixed on elastic mechanism (11) upper end and with the vertically disposed sample stage base plate of elastic mechanism (11) (8); Said sample stage base plate (8) middle part is provided with some active rollers that laterally arrange (10), and said active roller (10) is by the motor drives that is electrically connected; And
Be fixed in the casing (1); And be set in parallel in the sample stage top board (7) of sample stage base plate (8) top; Said sample stage top board (7) middle part is provided with some return idlers that laterally arrange (9); Said active roller (10) and the parallel up and down corresponding setting of return idler (9), specimen holder places between said active roller (10) and the return idler (9).
2. portable heavy metal pick-up unit as claimed in claim 1; It is characterized in that; Described laser instrument (2) emitted laser bundle is 45 ° and incides on the described laser mirror (13); The parallel correspondence of described catoptron with holes (14) be arranged on laser mirror under; Described first plano-convex lens (15) is set in parallel in directly over the sample stage, and be positioned at catoptron with holes (14) under, the central point of described catoptron with holes (14), second plano-convex lens (16) and fibre-optical probe (18) is on same straight line.
3. according to claim 1 or claim 2 portable heavy metal pick-up unit is characterized in that, described fibre-optical probe (18) is set in place on the horizontal guide rail (20) of laser instrument (2) below through fibre-optical probe stationary installation (17).
4. portable heavy metal pick-up unit as claimed in claim 3; It is characterized in that; Also be provided with first base (21) on the described horizontal guide rail (20); Said first base (21) has micro-adjusting mechanism, and described fibre-optical probe stationary installation (17) is fixed on said first base (21).
5. like claim 1 or 2 or 4 described portable heavy metal pick-up units, it is characterized in that described second plano-convex lens (16) is set in place on the horizontal guide rail (20) of laser instrument (2) below.
6. portable heavy metal pick-up unit as claimed in claim 5; It is characterized in that; Also be provided with second base (22) on the described horizontal guide rail (20), said second base (22) has micro-adjusting mechanism, and described second plano-convex lens (16) is fixed on said second base (22).
7. like claim 1 or 2 or 4 or 6 described portable heavy metal pick-up units, it is characterized in that described active roller has certain intervals between (10).
8. like claim 1 or 2 or 4 or 6 described portable heavy metal pick-up units, it is characterized in that described elastic mechanism (11) is made up of the some springs that laterally arrange.
9. portable heavy metal pick-up unit as claimed in claim 8 is characterized in that, described rotary sample stage (4) also comprises to be arranged on and horizontally rotates the displacement platform on the sample stage top board (7).
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CN104458872A (en) * | 2014-12-17 | 2015-03-25 | 中国计量学院 | Device for measuring heavy metal ions in water |
CN104655606A (en) * | 2013-11-15 | 2015-05-27 | 中国农业大学 | Optical detection system for nondestructive detection of pesticide residue on surface of fruit and vegetable |
CN105548094A (en) * | 2016-01-22 | 2016-05-04 | 清华大学 | Twin-lens based LIBS system for trace heavy metal detection |
CN105572103A (en) * | 2016-03-02 | 2016-05-11 | 中华人民共和国台州出入境检验检疫局 | Method for quantitatively detecting multiple heavy metals in leather at same time based on LIBS (Laser-Induced Breakdown Spectroscopy) technology |
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