CN105223187B - A kind of device that heavy metal element in gas is measured based on LIBS - Google Patents

A kind of device that heavy metal element in gas is measured based on LIBS Download PDF

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Publication number
CN105223187B
CN105223187B CN201510678985.8A CN201510678985A CN105223187B CN 105223187 B CN105223187 B CN 105223187B CN 201510678985 A CN201510678985 A CN 201510678985A CN 105223187 B CN105223187 B CN 105223187B
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China
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cylinder
gas
libs
heavy metal
metal element
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CN201510678985.8A
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CN105223187A (en
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董前民
马芳丽
金尚忠
梁培
王骏
陈华才
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China Jiliang University
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China Jiliang University
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Abstract

The invention provides a kind of device that heavy metal element in gas is measured based on LIBS, described device mainly includes laser ablation system, sample chamber system, LIBS measuring systems.Sample room is the piston type system of easily-controllable air pressure and temperature in the present invention, realize detection of the LIBS device to heavy metal element in normal temperature and pressure gas, realize the measurement of heavy metal element in gas under industrial high temperature and high pressure environment again, the device has the characteristics that quick, easy and can overcome can not HTHP the shortcomings that measuring in real time.

Description

A kind of device that heavy metal element in gas is measured based on LIBS
Technical field
The present invention relates to spectral measurement analysis technical field, heavy metal member in more particularly to a kind of measurement gas based on LIBS The device of element.
Background content
At present, in air under heavy metal particles composition and industrial high temperature hyperbaric environment heavy metals emission thing cause it is serious Environmental pollution, while the health of the mankind has also been threatened, therefore the detection to heavy metal element in gas turns into of concern Focus.
Current existing gas detection method has infrared spectrum detection technique, gas chromatographic column-ionic mobility spectral technology With atomic absorption spectroscopy etc., heavy metal element in gas is detected although above method can be realized, sample pretreatment Complexity, operating cost is high, and sensitivity is low.LIBS (Laser Induced Breakdown Spectroscopy, abbreviation LIBS) as a kind of new on-line analysis detection technique, it is to pass through the pulse laser of high-energy to gather Focus lens are irradiated to sample surfaces, sample is produced plasma, and the light that plasma emission goes out is transferred to by spectrometer detection Computer control system, by carrying out data processing to spectral information, so as to realize the qualitative differentiation of sample and quantitative detection.
The present invention proposes a kind of device that heavy metal element in gas is measured based on LIBS, both can be at normal temperatures and pressures Realize detection to heavy metal element in gas, can also under high temperature and high pressure environment to gas in heavy metal element examine Survey.
The content of the invention
The purpose of this patent is the provision of a kind of device that heavy metal element in gas is measured based on LIBS, sample room system Unite as the piston type system of temperature and air pressure can be adjusted, can in the gentle pressure of different temperature is realized to gas heavy metal The detection of element, improve accuracy and signal to noise ratio that LIBS device detects to gas.
To reach above-mentioned purpose, the technical solution adopted by the present invention is:Provide a kind of based on a LIBS measurement gas huge sum of moneys Belong to the device of element, including:Laser ablation system, sample chamber system, LIBS measuring systems;
Laser ablation system in the present invention includes femtosecond solid pulse laser (1), speculum (2), lens (4), thoroughly Mirror (4) is corresponding with the quartz glass (5) on cylinder (6) surface, and femtosecond solid pulse laser (1) sends pulse laser and passed through Speculum (2), focused on through lens (4) and sample surfaces are got to by quartz glass (5), produce plasma;
LIBS measuring systems in the present invention include lens (4), optical fiber aggregation head (3), ICCD (25), spectrometer (24), Computer control system (26) and signal delay time generator (27), ICCD (25) and spectrometer (24) assemble head (3) by optical fiber LIBS spectrum are gathered, computer control system (26) is delayed with femtosecond solid pulse laser (1), ICCD (21), signal respectively Generator (27), motor (9) and sample room connection;
Sample chamber system in the present invention includes quartz glass (5), cylinder (6), crank (7), flywheel (8), motor (9), connecting rod (10), piston rod (11), piston (12), electric heater (13), temperature sensor (14), baroceptor (15), First gas flowmeter (16), inlet valve (17), air bleeding valve (18), second gas flowmeter (20), air accumulator (22), motor (9) movement of piston rod (11) and piston (12), the gas of regulation cylinder (6) are controlled by flywheel (8), crank (7), connecting rod (10) Pressure, the temperature of computer control system (26) control electric heater (13) regulation cylinder (6).
First gas flowmeter (16) and second gas flowmeter (20) in the present invention are individually positioned in inlet valve (17) With air bleeding valve (18) place, the volume flow of inlet valve (17) and air bleeding valve (18) can be shown, is easy to quantitative analysis.Cylinder (6) temperature sensor (14) and baroceptor (15) are provided with, the temperature and air pressure in cylinder (6) can be shown respectively.
Wherein, flywheel (8) is arranged on motor (9), and cylinder (6) inwall is provided with electric heater (13).
The beneficial effects of the invention are as follows:A kind of device that heavy metal element in gas is measured based on LIBS is proposed, can The detection to heavy metal element in gas is realized at normal temperatures and pressures, and and can is at high temperature under high pressure to the heavy metal element in gas Detected, improve the precision and to-noise ratio of gas detection.
Brief description of the drawings
Fig. 1 is the schematic diagram of patent of the present invention, in figure:1- femtosecond solid pulse lasers;2- speculums;3- optical fiber is assembled Head;4- lens;5- quartz glass;6- cylinders;7- cranks;8- flywheels;9- motor;10- connecting rods;11- piston rods;12- pistons; 13- electric heaters;14- temperature sensors;15- baroceptors;16- first gas flowmeters;17- inlet valves;18- is vented Valve;19- air inlets;20- second gas flowmeters;21- gas outlets;22- air accumulators;23- air accumulator doors;24- spectrometers;25- ICCD;26- computer control systems;27- signal delay time generators.
Embodiment
The implementation steps of the present invention are illustrated below in conjunction with the accompanying drawings:
1. such as the constructional device figure that Fig. 1 is the present invention, the invention provides one kind to be based on heavy metal in LIBS measurement gases The device of element, including:Femtosecond solid pulse laser (1), speculum (2), lens (4), optical fiber aggregation head (3), spectrometer (24), ICCD (25), computer control system (26), signal delay time generator (27), quartz glass (5), cylinder (6), crank (7), flywheel (8), motor (9), connecting rod (10), piston rod (11), piston (12), electric heater (13), temperature sensor (14), baroceptor (15), first gas flowmeter (16), inlet valve (17), air bleeding valve (18), second gas flowmeter (20), air accumulator (22), lens (4) are corresponding with the quartz glass (5) on cylinder (6) surface, computer control system (26) Respectively with femtosecond solid pulse laser (1), ICCD (21), signal delay time generator (27), motor (9) and sample room circuit Connection, motor (9) is connected by crank (7), flywheel (8), connecting rod (10), piston rod (11) with piston (12), positioned at gas The right side of cylinder (6), cylinder (6) left side are provided with air inlet (19) and exhaust outlet (21), and inlet valve (17) and air bleeding valve (18) are respectively Air inlet (19) and exhaust outlet (21) place are placed on, while by the control of computer control system (26), exhaust outlet (21) connection Air accumulator (22), air accumulator (22) side are provided with air accumulator door (23), first gas flowmeter (16) and second gas flowmeter (20) inlet valve (17) and air bleeding valve (18) place are individually positioned in, the body of air inlet and exhaust ports gas can be shown respectively Product flow, is easy to quantitative analysis, and cylinder (6) is provided with temperature sensor (14) and baroceptor (15) and positioned at cylinder (6) Bottom surface.It gentle to the temperature in cylinder can press and be monitored in real time.
This patent is achieved like this, and its method and step is:
Step 1:When system does not work, piston (12) is in equilbrium position, opens computer control system (26), passes through and is System control air bleeding valve (18) is turned on, and inlet valve (17) is closed, and computer control system (26) is by controlling motor (9) Rotation drives the motion of crank (7), flywheel (8), connecting rod (10), piston rod (8), promotes piston (12) the air in sample room Air accumulator (19) is discharged to, the volume in cylinder is in relative vacuum state, avoids the air in sample room to gasmetry Influence.
Step 2:When piston (12) arrival cylinder leftmost position, inlet valve (17) is opened, under test gas is passed sequentially through Air inlet (19), gas flowmeter (16) and inlet valve (17) enter cylinder (6), and computer control system (26) is by controlling electricity The rotation of motivation (9) drives the motion of crank (7), flywheel (8), connecting rod (10), piston rod (8), promotes piston (12) to transport to the right It is dynamic, make cylinder (6) interior gassy, close inlet valve.
Step 3:Motor (9) controls piston (12) compressed gas to the left, increases the pressure in cylinder, opens electrical heating Device (13), the reading by observing temperature sensor (14) and baroceptor (15) control the air pressure and temperature required for experiment Degree.
Step 4:When reaching experiment condition, laser (1), computer control system (26) control femtosecond solid arteries and veins are opened The pulse laser that laser (1) produces a branch of horizontal direction is rushed, passes sequentially through speculum (2), lens (4) focus on and pass through quartzy glass Glass (5) gets to sample surfaces, produces plasma.The light that plasma is sent assembles head (3) by optical fiber and enters spectrometer (24), spectrometer (24) gives obtained transfer spectral information to computer control system (26), and spectrogram is analyzed and located Reason, the detection to heavy metal element in gas can be achieved.

Claims (1)

  1. A kind of 1. device that heavy metal element in gas is measured based on LIBS, it is characterised in that:Described one kind is surveyed based on LIBS The device of heavy metal element includes in amount gas:Laser ablation system, sample chamber system, LIBS measuring systems;
    Described laser ablation system includes:Femtosecond solid pulse laser (1), speculum (2), lens (4), under test gas is deposited In cylinder (6), femtosecond solid pulse laser (1), speculum (2), lens (4) are placed on cylinder (6) outside, lens for storage (4) it is corresponding with the quartz glass (5) in cylinder (6);
    Described LIBS measuring systems include:Lens (4), optical fiber aggregation head (3), spectrometer (24), ICCD (25), computer control System (26) processed, signal delay time generator (27), spectrometer (24) and optical fiber aggregation head (3) connection, computer control system Unite (26) respectively with femtosecond solid pulse laser (1), ICCD (25), signal delay time generator (27), motor (9) and sample Product room connection;
    Described sample chamber system includes:Quartz glass (5), cylinder (6), crank (7), flywheel (8), motor (9), connecting rod (10), piston rod (11), piston (12), electric heater (13), temperature sensor (14), baroceptor (15), first gas Flowmeter (16), inlet valve (17), air bleeding valve (18), second gas flowmeter (20), air accumulator (22), motor (9) pass through Flywheel (8), crank (7), connecting rod (10) control the movement of piston rod (11) and piston (12), positioned at the right side of cylinder (6), cylinder (6) left side is provided with air inlet (19) and exhaust outlet (21), and inlet valve (17) and air bleeding valve (18) are individually positioned in air inlet (19) With exhaust outlet (21) place, exhaust outlet (21) connection air accumulator (22), air accumulator (22) side is provided with air accumulator door (23);
    Described first gas flowmeter (16) and second gas flowmeter (20) is individually positioned in inlet valve (17) and air bleeding valve (18) place, cylinder (6) are provided with temperature sensor (14) and baroceptor (15) and positioned at the bottom surfaces of cylinder (6);
    The flywheel (8) is arranged on motor (9), and cylinder (6) inwall is provided with electric heater (13).
CN201510678985.8A 2015-10-16 2015-10-16 A kind of device that heavy metal element in gas is measured based on LIBS Expired - Fee Related CN105223187B (en)

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CN108088813B (en) * 2017-12-08 2021-06-18 中国科学院上海应用物理研究所 On-line detection device for metal elements in molten salt
CN107831159A (en) * 2017-12-13 2018-03-23 中国科学院上海应用物理研究所 The detection means of metallic element in a kind of aerosol
CN109342390B (en) * 2018-10-29 2021-02-12 中国科学院上海技术物理研究所 Space station astronaut urine combined spectrum detection system
CN111398251A (en) * 2020-03-17 2020-07-10 浙江大学 Multi-gas-mixed L IBS signal enhancement device and heavy metal detection method
CN111398253A (en) * 2020-03-17 2020-07-10 浙江大学 Atmosphere-adjustable L IBS signal enhancement device and heavy metal detection method

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US6762835B2 (en) * 2002-03-18 2004-07-13 Mississippi State University Fiber optic laser-induced breakdown spectroscopy sensor for molten material analysis
CN100541196C (en) * 2003-02-28 2009-09-16 莱克公司 The analyser and the analytical approach that have variable volume ballast chamber
CN202256158U (en) * 2011-10-24 2012-05-30 中南民族大学 Real-time online detection analyzer for poisonous particles in smoke
CN102841078B (en) * 2012-09-10 2014-09-24 北京宝瑞光电科技有限公司 Integrated laser-induced enhanced plasma spectrum acquisition system
CN103398987B (en) * 2013-08-06 2015-04-15 中国科学院合肥物质科学研究院 Dust haze component on-line monitoring device
WO2015138035A1 (en) * 2013-12-19 2015-09-17 Rutgers, The State University Of New Jersey Methods for excitation-intensity-dependent phase-selective laser-induced breakdown spectroscopy of nanoparticles and applications thereof
CN204989030U (en) * 2015-10-16 2016-01-20 中国计量学院 Device based on heavy metal in LIBS measurement gas

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