CN204330674U - For detecting the equipment of Volatile Organic Compounds in Soil - Google Patents
For detecting the equipment of Volatile Organic Compounds in Soil Download PDFInfo
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- CN204330674U CN204330674U CN201520012795.8U CN201520012795U CN204330674U CN 204330674 U CN204330674 U CN 204330674U CN 201520012795 U CN201520012795 U CN 201520012795U CN 204330674 U CN204330674 U CN 204330674U
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Abstract
The utility model relates to a kind of pick-up unit, is specifically related to a kind of equipment for detecting Volatile Organic Compounds in Soil.The utility model sample cell adopts stainless steel screw thread and pad crush seal, scavenging duct directly with sample cell by thread seal, impermeability is good, changes pedotheque convenient disassembly, and soon, use safety, stirs heating rate; Adopt three different filler enrichment method device series connection adsorption and enrichments, desorb in parallel and after gas and vapor permeation tank mixes pump take out quantitative loop sample introduction, have that arresting efficiency is high, adsorption and enrichment speed is fast, desorption rate fast, desorption gas sample mix evenly, sample size advantage accurately; Adopt time of-flight mass spectrometer to analyze composition and the concentration thereof of the volatile organic matter in soil, analyze that speed is fast, the volatile organic matter kind that detects and number is many, without the need to carrier gas, resolution is high, result is accurate; Utilize Aqua pure extract, without the need for the organic solvent that poison is harmful, environmental protection.
Description
Technical field
The utility model relates to a kind of pick-up unit, is specifically related to a kind of equipment for detecting Volatile Organic Compounds in Soil.
Background technology
Domestic soil pollution place is increased, and for grasping the volatile organic matter pollution situation of soil, needs to detect volatile organic contaminant concentration in soil.Current Volatile Organic Compounds in Soil to be detected as complete equipment little.Laboratory is sent back to after the detection of Volatile Organic Compounds in Soil mainly adopts artificial sample, organic pre-treatment is carried out to pedotheque, with artificial treatment for after the volatile organic matter in main extraction pedotheque, recycling chromatographic volatile organic matter concentration, lacks the set of equipments that can be directly used in and detect Volatile Organic Compounds in Soil.
Main employing organic solvent soak extraction method is extracted in the pre-treatment of Volatile Organic Compounds in Soil, minority adopts Puffing and trapping.Organic solvent soak extraction method boils off organic solvent again after soaking soil extract volatile organic matter wherein with organic solvent to complete concentrated, finally enters chromatographic.Organic solvent soak extraction method exists that volatile organic matter extraction ratio is low, soil and extract need isolated by filtration and carry out the organic solvent washing of filter cake, volatile organic matter volatilization loss seriously makes that measurement result is on the low side, soil soaks the shortcoming needing to consume a large amount of poisonous and hazardous organic solvent, human contact's harmful organic solvent exists potential hazard.Puffing and trapping adds water and carry out the head space vial filling soil and water to heat the then acupuncture treatment pad punctured in ml headspace bottle to utilize the volatile organic matter in inert gas purge solid-liquid mixture to trap the laggard gas chromatographic analysis of last thermal desorption through cold-trap or adsorption tube again in soil.Utilize the pre-treatment of Puffing and trapping machine to extract at present and to measure the relevant device of Volatile Organic Compounds in Soil little, and existing relevant device extract, trap and still have the following disadvantages in analysis determining technology in the pre-treatment of volatile organic matter: when 1, acupuncture treatment punctures on glass roof empty bottle pad, often occur purging that leakproofness is bad when causing purging that volatile organic matter is lost by acupuncture treatment place of ml headspace bottle pad and then causes the situation of volatile organic matter concentration determination Lower result.2, current most equipment only adopts an adsorption tube to carry out Adsorption Concentration enriched sample, volatile organic content Gao Shiyi to be measured penetrates adsorption tube, in addition enrichment method device structure is single causes not high even seizure of arresting efficiency not live the volatile organic matter that some has special nature with adsorption stuffing is single, such as lower boiling volatile organic matter, finally causes some volatile organic matter concentration determination result to be forbidden even to can't detect volatile organic matter thus.3, adopt gas Chromatographic Determination volatile organic matter, volatile organic matter to be measured needs after gas chromatographic column post is separated, to enter detecting device again with carrier gas and detects, and sample analysis speed is slow, and carrier gas consumption is large, and resolution is low; The polarity according to volatile organic matter, molecular structure, boiling point is needed to select different types of gas chromatographic column and dissimilar detecting device to measure in addition, poor universality, the volatile organic matter kind detected and Limited Number, also cannot carry out quantitative and qualitative analysis to unknown volatile organic matter.
Utility model content
According to above deficiency of the prior art, the technical problems to be solved in the utility model is: provide a kind of equipment for detecting Volatile Organic Compounds in Soil, impermeability is good, change pedotheque convenient disassembly, heating rate is fast, use safety, stir, enrichment method speed is fast, arresting efficiency is high, desorption rate is fast, desorption gas sample mix is even, analyze and measure that speed is fast, the volatile organic matter kind that detects and number is many, resolution is high, result is accurate, in pedotheque, volatile organic matter leaching process is without the need for machine solvent, health environment-friendly.
The utility model solves the technical scheme that its technical matters adopts:
Equipment for detecting Volatile Organic Compounds in Soil described in the utility model, comprise sample cell, sample cell inside is provided with scavenging duct and thermopair, sample cell top is provided with safety valve, electric furnace jacket is coated with outside sample cell, sample cell is provided with electric stirring oar, one end of electric stirring oar extend into sample cell inside, scavenging duct, needle-valve, first mass-flow gas meter, second tensimeter is connected successively with the second reduction valve, the second reduction valve by threeway respectively with the first tensimeter, 3rd reduction valve is connected, the first tensimeter, first reduction valve is connected successively with helium tank, the 3rd reduction valve, 3rd tensimeter is connected successively with the second mass-flow gas meter, and thermopair is arranged on thermopair sleeve inner, temperature controller respectively with thermopair, electric furnace jacket is connected, sample cell, first ball valve is connected successively with quantitative pot, quantitative pot respectively with the 3rd ball valve, second ball valve is connected, the 3rd ball valve, water pump is connected successively with water-storing bottle, and the second ball valve is connected with waste liquid bottle, and sample cell is connected with drying buffer pipe, drying buffer pipe by the first tee ball valve respectively with the first four-way, first enrichment method device be connected, the second mass-flow gas meter by the first four-way respectively with the first tee ball valve, 3rd tee ball valve, 5th tee ball valve be connected, the first enrichment method device by the second tee ball valve respectively with the second four-way, 3rd tee ball valve be connected, the 3rd tee ball valve is connected with the second enrichment method device, the second enrichment method device pass through the 4th tee ball valve respectively with the 5th tee ball valve, second four-way is connected, the 5th tee ball valve, 3rd enrichment method device is connected successively with the 6th tee ball valve, the 6th tee ball valve by the second four-way respectively with the second tee ball valve, 4th tee ball valve, gas and vapor permeation tank is connected, the first enrichment method device, it is inner that second enrichment method device and the 3rd enrichment method device are arranged on electrical heating case, gas and vapor permeation tank, six-way valve, gas dosing pump, injection port, time of-flight mass spectrometer is connected successively with computer, and six-way valve is provided with quantitative loop, and time of-flight mass spectrometer is connected with molecular pump, six-way valve respectively with the second tee ball valve, 4th tee ball valve, pipe insulating layer is coated with, six-way valve outside pipeline between 6th tee ball valve, Soviet Union's agate tank is connected successively with gas dilution instrument, gas dilution instrument respectively with volatile organic matter gas bottle, nitrogen cylinder is connected.
Described sample cell comprises stainless steel cover, teflon gasket and stainless steel base, and stainless steel cover, teflon gasket are connected successively with stainless steel base.
The utility model measures the volatile organic matter in soil in the following way: pedotheque mixes with quantitative pure water and utilizes temperature controller and electric furnace jacket are heated to 40 DEG C and keep constant temperature in sample cell, and the volatile organic matter purged by means of the helium constant current that the first mass-flow gas meter controls in soil and water solid-liquid mixture, electric stirring oar stirring soil and water material are beneficial to volatile organic matter and shift in gas phase, the enrichment method device adsorption and enrichment in a series arrangement that three are full of three kinds of different fillers is entered after the drying of volatile organic matter drying separator tube dewaters, enter with the helium that the second mass-flow gas meter controls the stripping gas sample extracted in quantitative loop by gas dosing pump after gas and vapor permeation tank mixes with parallel way 190 DEG C of desorption under high temperatures and enter composition and the concentration thereof that the volatile organic matter in soil analyzed by time of-flight mass spectrometer.
Helium tank is used for the source of the gas of the solid-liquid mixture that helium purge soil and water are formed in sampling pond, and the vaporization desorb that is rapidly heated simultaneously promote the volatile organic matter high-temperature sample heating of Adsorption Concentration enrichment in the first enrichment method device, the second enrichment method device, the 3rd enrichment method device as carrier gas under enters gas and vapor permeation tank and mixes.
First reduction valve, the first tensimeter are for regulating and helium pressure before showing threeway.
Second reduction valve, the second tensimeter are used for helium second depressurized makes the second tensimeter registration and the first mass-flow gas meter operating pressure adapt, thus makes the first mass-flow gas meter accurately control the helium purge flow of scavenging duct.
The helium purge source of the gas of cut-out scavenging duct after needle-valve completes for helium purge.
3rd reduction valve, the 3rd tensimeter are used for helium second depressurized makes the 3rd tensimeter registration and the second mass-flow gas meter operating pressure adapt, thus helium gas flow and volume when making the second mass-flow gas meter accurately control desorb.
First mass-flow gas meter is used for accurately controlling helium purge flow, the gas flow of the helium played a driving role as carrier gas when the second mass-flow gas meter is used for the volatile organic matter high-temperature sample desorb accurately controlling absorption in the first enrichment method device, the second enrichment method device, the 3rd enrichment method device and volume.
Scavenging duct and sample cell are by thread seal, and connect impermeability good, scavenging duct is inserted into bottom sample cell, is beneficial to helium purge water and soil mixture material.
Sample cell is made up of stainless steel cover, stainless steel base and teflon gasket.Utilize the screw thread on stainless steel chassis outer side face and stainless steel cover medial surface, and teflon gasket sealed sample pond is added in the middle of stainless steel base and stainless steel cover, air tight when guaranteeing helium purge sample, scavenging duct directly directly starts helium purge by thread seal without the need to step of having an acupuncture treatment with sample cell, avoids occurring purging volatile organic matter when leakproofness is bad to be caused purging and is made the situation of volatile organic matter concentration determination Lower result by ml headspace bottle pad acupuncture treatment place loss.Sample cell top is provided with safety valve, use safety.In sample cell, use pure water by heating, the mode that combines of helium purge and do not utilize organic solvent to extract volatile organic matter in soil, environmental protection.
Electric stirring oar is used for the liquid-solid mixture material of the water and soil sample composition in abundant stirred sample pond, is beneficial to the extraction of volatile organic matter in pedotheque and enters in ullage gas phase with helium fast transfer.
Thermopair sleeve is used for holding thermopair, and bottom is immersed in soil and aqueous mixtures material.Thermopair to insert in thermopair sleeve and is connected with temperature controller, and temperature controller panel shows soil and aqueous mixtures material temperature degree in real time.
Electric furnace jacket is used for heated sample pond, and electric furnace jacket heating power is controlled by temperature controller, remains soil and aqueous mixtures material temperature constant.Electric furnace jacket heating rate is fast, and temperature controller temperature control accurate temperature is constant.
Quantitative pot is for measuring the pure water of fixed volume, and unnecessary pure water flows into waste liquid bottle.After being full of pure water in quantitative pot, closing the 3rd ball valve and stop water pump, opening the first ball valve, utilize Action of Gravity Field to be transferred in sample cell by the pure water in quantitative pot and mix with pedotheque, water gaging and soil add water equipment price cheaply, precisely durable.
Water pump is used for the pure water in water-storing bottle to be delivered to quantitative pot.
Water-storing bottle is for storing pure water.Utilize Aqua pure extract Volatile Organic Compounds in Soil to have advantage that human body does not contact poisonous and hazardous organic solvent, environment protection health.
Drying buffer pipe is used for the gaseous sample formed after dry helium gas purges soil and water, and buffer gas flow.Drying buffer pipe adopts permeable membrane drying to dewater, and compares traditional material filling type exsiccator and has the advantage that rate of drying soon, does not lose water-soluble volatile organic matter in sample.
First tee ball valve, the second tee ball valve, the 3rd tee ball valve, the 4th tee ball valve, the 5th tee ball valve, the 6th tee ball valve, for regulating the order of connection of the first enrichment method device, the second enrichment method device and the 3rd enrichment method device, realize: helium purge series connection adsorb volatile organism, helium promote three enrichment method devices and enter gas and vapor permeation tank with parallel way fast desorption volatile organic matter.
First enrichment method device is activated charcoal enrichment method device, and active carbon filler is used for the most of volatile organic matter of enrichment method.Second enrichment method device is Tenax enrichment method device, and Tenax filler is used for the volatile organic matter of enrichment method higher.3rd enrichment method device is silica gel enrichment method device, and silica filler is used for the larger volatile organic matter of enrichment method polarity.
Three kinds of filler series connection adsorption and enrichment modes are adopted to solve: volatile organic content Gao Shiyi to be measured penetrates adsorption tube problem and enrichment method device structure is single and adsorption stuffing is single causes not high even seizure of arresting efficiency not live the problem that some has special nature volatile organic matter (such as lower boiling volatile organic matter), thus has the advantage that arresting efficiency is high, adsorption and enrichment speed is fast.Adopt desorb in parallel to solve the slow problem of the desorption rate that causes of series connection absorption series connection desorb, the gas after desorb mixes at gas and vapor permeation tank, has that desorption rate is fast, the uniform advantage of desorption gas sample mix.
Electrical heating case is used for Fast Heating first enrichment method device, the second enrichment method device, the 3rd enrichment method device, makes the volatile organic matter high-temperature sample fast desorption of absorption in three enrichment method devices.
Gas and vapor permeation tank is used for the gaseous sample of desorb in parallel for three enrichment method devices to mix.
Six-way valve is connected with quantitative loop, is switched make quantitative loop be full of the sample stripping gas of fixed volume or the volatile organic matter gas sample of concentration known by six-way valve internal duct.
Quantitative loop is for the volatile organic matter gas sample feeding of the sample stripping gas sample introduction or concentration known that measure Stationary liquid same volume, and sample size is accurate.
Gas dilution instrument is used for high pure nitrogen in the gas nitrogen cylinder in volatile organic matter gas bottle to dilute, and is made into the volatile organic matter gas sample of concentration known and is stored in Soviet Union's agate tank.Gas dilution instrument inside is furnished with pressure transducer and standard gas volume measuring apparatus, realizes the volatile organic matter gas sample of preparation concentration known smoothly.
Gas dosing pump is used for the gaseous sample in quantitative loop to be delivered to injection port.
Injection port is used for the sample introduction of the volatile organic matter gas sample of sample stripping gas sample introduction or time of-flight mass spectrometer timing signal concentration known.Injection port is the condition of high temperature, ensures that gaseous sample is gasified totally at injection port.
Time of-flight mass spectrometer measures the concentration of Volatile Organic Compounds in Soil for analyzing.Molecular pump is for maintaining the high vacuum state of time of-flight mass spectrometer.Time of-flight mass spectrometer is made up of Proton-Transfer Reactions ion gun, time of flight mass analyzer, ion detector, photomultiplier cell.In Proton-Transfer Reactions ion gun, make the hydroxonium ion H as reaction reagent ion by cathode glow discharging
3o
+with the volatile organic matter molecule generation Proton-Transfer Reactions in sample stripping gas sample, generate the specific molecular ion of a band proton.Different molions is separated according to causing drift time discrepant principle because mass-to-charge ratio is different successively by time of flight mass analyzer, and mass-to-charge ratio is less, and drift time is shorter, more early arrives ion detector.The signal of the molion that the continuous acquisition testing of ion detector arrives, then carry out after signal amplification process through photomultiplier cell, analysis result transmission arrives computer.Adopt time of-flight mass spectrometer to analyze composition and the concentration thereof of the volatile organic matter in soil, analyze that speed is fast, the volatile organic matter kind that detects and number is many, without the need to carrier gas, resolution is high, result is accurate.Pedotheque carries out detection analysis without the need to being separated through traditional gas chromatography but directly entering flight time mass spectrum after heating and blowing-enrichment method-desorption under high temperature also mixing, the chromatographic column kind avoiding gas chromatography selects the impact brought, eliminate chromatographic column be separated required for time thus greatly reduced the analysis time of each pedotheque, the volatile organic matter kind thus detected and number is many, analyze speed fast, without the need to carrier gas.Compare other type mass spectrum, flight time mass spectrum resolution is high, and mass number can be accurate to 2 significant digits, and volatile organic matter testing result is more accurate.
Principle of work and process:
Before using the equipment for detecting Volatile Organic Compounds in Soil, first utilize the volatile organic matter standard mixture of concentration known to demarcate time of-flight mass spectrometer, establish each volatile organic matter concentration and the calibration relation between the peak area detecting molecular ion peak corresponding in spectrogram.Open volatile organic matter gas bottle and nitrogen cylinder switch and gas dilution instrument power supply, utilize the accurate measurement of the built-in pressure transducer piezometry of gas dilution instrument and standard gas volume, nitrogen in gas nitrogen cylinder in volatile organic matter gas bottle is diluted, is made into the volatile organic matter gas sample of concentration known and is stored in Soviet Union's agate tank.Open time of-flight mass spectrometer and molecular pump power supply, the instrument parameter of injector temperature and time of-flight mass spectrometer is set, utilize molecular pump to maintain the high vacuum state of time of-flight mass spectrometer.Open gas dosing pumping source, switched by six-way valve internal duct, quantitative loop inside is full of the volatile organic matter gas of the concentration known in Soviet Union's agate tank.Switch six-way valve internal duct, the gas of concentration known by quantitative loop through gas dosing transport pump to injection port, and after injection port is gasified totally, enters time of-flight mass spectrometer analytical test obtains molecular ion peak mass spectrogram corresponding to the volatile organic matter gas sample of concentration known, the peak area information face display on computers of the molecular ion peak of molecular ion peak mass spectrogram and each volatile organic matter, the software of computer is utilized to carry out linear equation recurrence to the sample introduction concentration of volatile organic matter each in gas and the peak area of molecular ion peak, obtain the equation of linear regression of each volatile organic matter, and be stored in computer, ready for detecting volatile organic matter concentration in soil actual sample.
Pedotheque after freeze drying being weighed is placed in the stainless steel base of sample cell, utilize the screw thread on stainless steel chassis outer side face and stainless steel cover medial surface, and teflon gasket sealed sample pond is added in the middle of stainless steel base and stainless steel cover, guarantee air tight.Close the first ball valve and open the second ball valve, open water pump and to be delivered to by the pure water in water-storing bottle in quantitative pot and to be full of tank body thus to measure the pure water of fixed volume, unnecessary pure water flows into waste liquid bottle.After being full of pure water in quantitative pot, closing the 3rd ball valve and stop water pump, opening the first ball valve, utilize Action of Gravity Field to be transferred in sample cell by the pure water in quantitative pot and mix with pedotheque, and utilize electric stirring oar to stir.Close the first ball valve and needle-valve, electric furnace jacket is enclosed within sample cell, opening temp. control instrument power supply, with electric furnace jacket, sample cell is quickly heated up to suitable temperature 40 DEG C, and utilize temperature controller and thermopair accurate temperature controlling and keep temperature constant, thermopair is positioned at the thermopair sleeve be connected with stainless steel cover, and temperature controller utilizes the temperature of the water and soil mixture in the accurate show sample pond of thermopair.
Open helium tank switch, helium tentatively reduces pressure through the first reduction valve successively, the first tensimeter display high pressure pressure, the second reduction valve reduce pressure again, after the second tensimeter shows suitable low pressure pressure, arrive the first mass-flow gas meter.Open needle-valve, utilize the first mass-flow gas meter accurately to control helium purge flow, utilize the solid-liquid mixture 5min that scavenging duct is formed with the water and soil in firm discharge 100ml/min helium purge sample cell.Volatile organic matter in soil is diffused in the gas phase of ullage by purging in heating-stirring-helium purge process from soil and aqueous mixtures material, and the volatile organic matter in pedotheque carries out drying along with helium enters drying buffer pipe to gas.
Rotate the first tee ball valve, the second tee ball valve, the 3rd tee ball valve, the 4th tee ball valve, the 5th tee ball valve, the 6th tee ball valve, the first enrichment method device, the second enrichment method device and the 3rd enrichment method device are communicated in a series arrangement.The dried gas of drying buffer pipe passes through successively: the first tee ball valve, first enrichment method device adopts the most of volatile organic matter of active carbon filler enrichment method, second tee ball valve, 3rd tee ball valve, second enrichment method device adopts the volatile organic matter of Tenax filler enrichment method higher, 4th tee ball valve, 5th tee ball valve, 3rd enrichment method device adopts the volatile organic matter that silica filler enrichment method polarity is larger, direct emptying end gas after 6th tee ball valve and no longer by the second four-way.After purging completes, the complete adsorption and enrichment of the volatile organic matter in soil, in three enrichment method devices, stops helium purge, closes the first mass-flow gas meter and needle-valve for this reason, then stops electric furnace jacket heating and electric stirring oar to stir.
Regulate the 3rd reduction valve to make the 3rd tensimeter show suitable pressure registration, rotate the first tee ball valve, the 3rd tee ball valve, the 5th tee ball valve, the second tee ball valve, the 4th tee ball valve, the 6th tee ball valve make the first enrichment method device, the second enrichment method device is connected with parallel way pipeline with the 3rd enrichment method device.Utilize electrical heating case by the first enrichment method device, the second enrichment method device, the 3rd enrichment method device rapid temperature increases to 190 DEG C high temperature, open the second mass-flow gas meter simultaneously and accurately control helium gas flow, make helium by after the first four-way with parallel pipeline connected mode simultaneously through the first tee ball valve, the 3rd tee ball valve and the 5th tee ball valve, and arrive the first enrichment method device, the second enrichment method device and the 3rd enrichment method device simultaneously.The volatile organic matter of Adsorption Concentration enrichment in three enrichment method devices is rapidly heated vaporization under electrical heating case high-temperature heating, under helium under the second mass-flow gas meter flow control promotes, desorb is simultaneously by the second tee ball valve, the 4th tee ball valve, the 6th tee ball valve enter gas and vapor permeation tank through the second four-way, and three road sample stripping gass fully mix in gas and vapor permeation tank.Being switched by six-way valve internal duct makes quantitative loop be full of the sample stripping gas of fixed volume, rotates six-way valve and quantitative loop is communicated with gas dosing pump, utilize gas dosing pump that the sample stripping gas in quantitative loop is delivered to injection port.
Injection port keeps the condition of high temperature, and sample stripping gas enters the concentration that time of-flight mass spectrometer analysis measures Volatile Organic Compounds in Soil after injection port is gasified totally.Time of-flight mass spectrometer is made up of Proton-Transfer Reactions ion gun, time of flight mass analyzer, ion detector, photomultiplier cell.In Proton-Transfer Reactions ion gun, make the hydroxonium ion H as reaction reagent ion by cathode glow discharging
3o
+with the volatile organic matter molecule generation Proton-Transfer Reactions in sample stripping gas sample, generate the specific molecular ion of a band proton.Different molions is separated according to causing drift time discrepant principle because mass-to-charge ratio is different successively by time of flight mass analyzer, and mass-to-charge ratio is less, and drift time is shorter, more early arrives ion detector.The signal of the molion that the continuous acquisition testing of ion detector arrives, then carry out after signal amplification process through photomultiplier cell, analysis result transmission arrives computer.Adopt time of-flight mass spectrometer to analyze composition and the concentration thereof of the volatile organic matter in soil, analyze that speed is fast, the volatile organic matter kind that detects and number is many, without the need to carrier gas, resolution is high, result is accurate.
Volatile Organic Compounds in Soil Concentration Testing data show at computer.Utilize computer to control and revise the instrument parameter such as Proton-Transfer Reactions ion gun, time of flight mass analyzer, ion detector, photomultiplier cell comprising injector temperature, time of-flight mass spectrometer.In addition computer also shows the peak area of the molecular ion peak of the chromatogram of each volatile organic matter in pedotheque, mass spectrogram and correspondence thereof, and according to the equation of linear regression of each volatile organic matter calibration curve, computing machine calculates each volatile organic matter concentration in pedotheque automatically.
The beneficial effect that the utility model has is:
1. the utility model sample cell adopts stainless steel screw thread and pad crush seal, scavenging duct directly with sample cell by thread seal, impermeability is good, changes pedotheque convenient disassembly, and soon, use safety, stirs heating rate.The stainless steel base of sample cell and stainless steel cover adopt stainless steel screw thread airtight in conjunction with teflon gasket crush seal, device impermeability is good, scavenging duct directly directly starts helium purge by thread seal without the need to step of having an acupuncture treatment with sample cell, avoids occurring purging that leakproofness is bad when causing purging that volatile organic matter makes the inaccurate situation of volatile organic matter concentration determination result by ml headspace bottle pad acupuncture treatment place loss.Electric furnace jacket heating rate is fast, and temperature controller temperature control accurate temperature is constant.Be provided with safety valve, use safety.The solid-liquid mixture that electric stirring oar stirs soil and water formation is even, is beneficial to volatile organic matter to the fast transfer in gaseous state.
2. the utility model adopts three different filler enrichment method device series connection adsorption and enrichments, desorb in parallel and after gas and vapor permeation tank mixes pump take out quantitative loop sample introduction, have that arresting efficiency is high, adsorption and enrichment speed is fast, desorption rate fast, desorption gas sample mix evenly, sample size advantage accurately.Three kinds of filler series connection adsorption and enrichment modes are adopted to solve: volatile organic content Gao Shiyi to be measured penetrates adsorption tube problem and enrichment method device structure is single and adsorption stuffing is single causes not high even seizure of arresting efficiency not live the problem that some has special nature volatile organic matter (such as lower boiling volatile organic matter), has the advantage that arresting efficiency is high, adsorption and enrichment speed is fast.Adopt desorb in parallel to solve the slow problem of the desorption rate that causes of series connection absorption series connection desorb, the gas after desorb mixes at gas and vapor permeation tank, has that desorption rate is fast, the uniform advantage of desorption gas sample mix.Switched the stripping gas sample introduction being measured same volume by quantitative loop by six-way valve internal duct, sample size is accurate.
3. the utility model adopts time of-flight mass spectrometer to analyze composition and the concentration thereof of the volatile organic matter in soil, analyzes that speed is fast, the volatile organic matter kind that detects and number is many, without the need to carrier gas, resolution is high, result is accurate.Pedotheque carries out detections analysis without the need to being separated through traditional gas chromatography but directly entering Proton-Transfer Reactions flight time mass spectrum through heating and blowing-enrichment method-desorption under high temperature and after mixing, the chromatographic column kind avoiding gas chromatography selects the impact brought, eliminate chromatographic column be separated required for time thus greatly reduced the analysis time of each pedotheque, the volatile organic matter kind thus detected and number is many, analyze speed fast, without the need to carrier gas.Compare other type mass spectrum, Proton-Transfer Reactions flight time mass spectrum resolution is high, and mass number can be accurate to 2 significant digits, and volatile organic matter testing result is more accurate.
4. the mode that the utility model is combined by heating, helium purge utilizes Aqua pure extract Volatile Organic Compounds in Soil, and leaching process is without the need to poisonous and hazardous organic solvent, and environmental friendliness, is beneficial to protection analyst healthy.
Accompanying drawing explanation
Fig. 1 is the utility model structural representation;
In figure: 1, sample cell; 2, scavenging duct; 3, thermopair; 4, safety valve; 5, electric furnace jacket; 6, electric stirring oar; 7, needle-valve; 8, the first mass-flow gas meter; 9, the second tensimeter; 10, the second reduction valve; 11, threeway; 12, the first tensimeter; 13, the first reduction valve; 14, helium tank; 15, the 3rd reduction valve; 16, the 3rd tensimeter; 17, the second mass-flow gas meter; 18, thermopair sleeve; 19, temperature controller; 20, the first ball valve; 21, quantitative pot; 22, the 3rd ball valve; 23, water pump; 24, water-storing bottle; 25, the second ball valve; 26, waste liquid bottle; 27, drying buffer pipe; 28, the first tee ball valve; 29, the first four-way; 30, the first enrichment method device; 31, the 3rd tee ball valve; 32, the 5th tee ball valve; 33, the second tee ball valve; 34, the second four-way; 35, the second enrichment method device; 36, the 4th tee ball valve; 37, the 3rd enrichment method device; 38, the 6th tee ball valve; 39, gas and vapor permeation tank; 40, electrical heating case; 41, six-way valve; 42, gas dosing pump; 43, injection port; 44, time of-flight mass spectrometer; 45, computer; 46, quantitative loop; 47, molecular pump; 48, pipe insulating layer; 49, Soviet Union's agate tank; 50, gas dilution instrument; 51, volatile organic matter gas bottle; 52, nitrogen cylinder; 53, stainless steel cover; 54, teflon gasket; 55, stainless steel base.
Embodiment
Below in conjunction with accompanying drawing, embodiment of the present utility model is described further:
As shown in Figure 1, the utility model comprises sample cell 1, sample cell 1 inside is provided with scavenging duct 2 and thermopair 3, sample cell 1 top is provided with safety valve 4, electric furnace jacket 5 is coated with outside sample cell 1, sample cell 1 is provided with electric stirring oar 6, one end of electric stirring oar 6 extend into sample cell 1 inside, scavenging duct 2, needle-valve 7, first mass-flow gas meter 8, second tensimeter 9 is connected successively with the second reduction valve 10, the second reduction valve 10 by threeway 11 respectively with the first tensimeter 12, 3rd reduction valve 15 is connected, the first tensimeter 12, first reduction valve 13 is connected successively with helium tank 14, the 3rd reduction valve 15, 3rd tensimeter 16 is connected successively with the second mass-flow gas meter 17, and it is inner that thermopair 3 is arranged on thermopair sleeve 18, temperature controller 19 respectively with thermopair 3, electric furnace jacket 5 is connected, sample cell 1, first ball valve 20 is connected successively with quantitative pot 21, quantitative pot 21 respectively with the 3rd ball valve 22, second ball valve 25 is connected, the 3rd ball valve 22, water pump 23 is connected successively with water-storing bottle 24, and the second ball valve 25 is connected with waste liquid bottle 26, and sample cell 1 is connected with drying buffer pipe 27, drying buffer pipe 27 by the first tee ball valve 28 respectively with the first four-way 29, first enrichment method device 30 is connected, the second mass-flow gas meter 17 by the first four-way 29 respectively with the first tee ball valve 28, 3rd tee ball valve 31, 5th tee ball valve 32 is connected, the first enrichment method device 30 by the second tee ball valve 33 respectively with the second four-way 34, 3rd tee ball valve 31 is connected, and the 3rd tee ball valve 31 is connected with the second enrichment method device 35, the second enrichment method device 35 pass through the 4th tee ball valve 36 respectively with the 5th tee ball valve 32, second four-way 34 is connected, the 5th tee ball valve 32, 3rd enrichment method device 37 is connected successively with the 6th tee ball valve 38, the 6th tee ball valve 38 by the second four-way 34 respectively with the second tee ball valve 33, 4th tee ball valve 36, gas and vapor permeation tank 39 is connected, the first enrichment method device 30, it is inner that second enrichment method device 35 and the 3rd enrichment method device 37 are arranged on electrical heating case 40, gas and vapor permeation tank 39, six-way valve 41, gas dosing pump 42, injection port 43, time of-flight mass spectrometer 44 is connected successively with computer 45, six-way valve 41 is provided with quantitative loop 46, and time of-flight mass spectrometer 44 is connected with molecular pump 47, six-way valve 41 respectively with the second tee ball valve 33, 4th tee ball valve 36, pipe insulating layer 48 is coated with, six-way valve 41 outside pipeline between 6th tee ball valve 38, Soviet Union's agate tank 49 is connected successively with gas dilution instrument 50, gas dilution instrument 50 respectively with volatile organic matter gas bottle 51, nitrogen cylinder 52 is connected.
Sample cell 1 comprises stainless steel cover 53, teflon gasket 54 and stainless steel base 55, and stainless steel cover 53, teflon gasket 54 are connected successively with stainless steel base 55.
Before using the equipment for detecting Volatile Organic Compounds in Soil, first utilize the volatile organic matter standard mixture of concentration known to demarcate time of-flight mass spectrometer 44, establish each volatile organic matter concentration and the calibration relation between the peak area detecting molecular ion peak corresponding in spectrogram.Open volatile organic matter gas bottle 51 and nitrogen cylinder 52 switch and gas dilution instrument 50 power supply, utilize the accurate measurement of the built-in pressure transducer piezometry of gas dilution instrument 50 and standard gas volume, nitrogen in gas nitrogen cylinder 52 in volatile organic matter gas bottle 51 is diluted, is made into the volatile organic matter gas sample of concentration known and is stored in Soviet Union's agate tank 49.Open time of-flight mass spectrometer 44 and molecular pump 47 power supply, the instrument parameter of injection port 43 temperature and time of-flight mass spectrometer 44 is set, utilizes molecular pump 47 to maintain the high vacuum state of time of-flight mass spectrometer 44.Open gas dosing pump 42 power supply, switched by six-way valve 41 internal duct, quantitative loop 46 inside is full of the volatile organic matter gas of the concentration known in Soviet Union's agate tank 49.Switch six-way valve 41 internal duct, the gas of concentration known is delivered to injection port 43 by quantitative loop 46 through gas dosing pump 42, and after injection port 43 is gasified totally, enters time of-flight mass spectrometer 44 analytical test obtains molecular ion peak mass spectrogram corresponding to the volatile organic matter gas sample of concentration known, the peak area information of the molecular ion peak of molecular ion peak mass spectrogram and each volatile organic matter shows on computer 45, the software of computer 45 is utilized to carry out linear equation recurrence to the sample introduction concentration of volatile organic matter each in gas and the peak area of molecular ion peak, obtain the equation of linear regression of each volatile organic matter, and be stored in computer 45, ready for detecting volatile organic matter concentration in soil actual sample.
Pedotheque after freeze drying being weighed is placed in the stainless steel base 55 of sample cell 1, utilize the screw thread on stainless steel base 55 lateral surface and stainless steel cover 53 medial surface, and teflon gasket 54 sealed sample pond 1 is added in the middle of stainless steel base 55 and stainless steel cover 53, guarantee air tight.Close the first ball valve 20 and open the second ball valve 25, open water pump 23 and to be delivered to by the pure water in water-storing bottle 24 in quantitative pot 21 and to be full of tank body thus to measure the pure water of fixed volume, unnecessary pure water flows into waste liquid bottle 26.After being full of pure water in quantitative pot 21, closing the 3rd ball valve 22 and stop water pump 23, opening the first ball valve 20, utilize Action of Gravity Field to be transferred in sample cell 1 by the pure water in quantitative pot 21 and mix with pedotheque, and utilize electric stirring oar 6 to stir.Close the first ball valve 20 and needle-valve 7, electric furnace jacket 5 is enclosed within sample cell 1, opening temp. control instrument 19 power supply, with electric furnace jacket 5, sample cell 1 is quickly heated up to suitable temperature 40 DEG C, and utilize temperature controller 19 and thermopair 3 accurate temperature controlling and keep temperature constant, thermopair 3 is positioned at the thermopair sleeve 18 be connected with stainless steel cover 53, and temperature controller 19 utilizes the temperature of the water and soil mixture in the accurate show sample pond 1 of thermopair 3.
Open helium tank 14 switch, helium tentatively reduces pressure through the first reduction valve 13 successively, the first tensimeter 12 shows high pressure pressure, the second reduction valve 10 reduces pressure again, after the second tensimeter 9 shows suitable low pressure pressure, arrive the first mass-flow gas meter 8.Open needle-valve 7, utilize the first mass-flow gas meter 8 accurately to control helium purge flow, utilize the solid-liquid mixture 5min that scavenging duct 2 is formed with the water and soil in firm discharge 100ml/min helium purge sample cell 1.Volatile organic matter in soil is diffused in the gas phase of ullage by purging in heating-stirring-helium purge process from soil and aqueous mixtures material, and the volatile organic matter in pedotheque carries out drying along with helium enters drying buffer pipe 27 pairs of gases.
Rotate the first tee ball valve 28, second tee ball valve 33, the 3rd tee ball valve 31, the 4th tee ball valve 36, the 5th tee ball valve 32, the 6th tee ball valve 38, the first enrichment method device 30, second enrichment method device 35 and the 3rd enrichment method device 37 are communicated in a series arrangement.The dried gas of drying buffer pipe 27 passes through successively: the first tee ball valve 28, first enrichment method device 30 adopts the most of volatile organic matter of active carbon filler enrichment method, second tee ball valve 33, 3rd tee ball valve 31, second enrichment method device 35 adopts the volatile organic matter of Tenax filler enrichment method higher, 4th tee ball valve 36, 5th tee ball valve 32, 3rd enrichment method device 37 adopts the volatile organic matter that silica filler enrichment method polarity is larger, direct emptying end gas and no longer by the second four-way 34 after 6th tee ball valve 38.After purging completes, the complete adsorption and enrichment of the volatile organic matter in soil, in three enrichment method devices, stops helium purge, closes the first mass-flow gas meter 8 and needle-valve 7 for this reason, then stops electric furnace jacket 5 heating and electric stirring oar 6 to stir.
Regulate the 3rd reduction valve 15 to make the 3rd tensimeter 16 show suitable pressure registration, rotate the first tee ball valve 28, the 3rd tee ball valve 31, the 5th tee ball valve 32, second tee ball valve 33, the 4th tee ball valve 36, the 6th tee ball valve 38 make the first enrichment method device 30, second enrichment method device 35 be connected with parallel way pipeline with the 3rd enrichment method device 37.Utilize electrical heating case 40 by the first enrichment method device 30, second enrichment method device 35, the 3rd enrichment method device 37 rapid temperature increases to 190 DEG C high temperature, open the second mass-flow gas meter 17 simultaneously and accurately control helium gas flow, make helium by after the first four-way 29 with parallel pipeline connected mode simultaneously through the first tee ball valve 28, the 3rd tee ball valve 31 and the 5th tee ball valve 32, and arrive the first enrichment method device 30, second enrichment method device 35 and the 3rd enrichment method device 37 simultaneously.The volatile organic matter of Adsorption Concentration enrichment in three enrichment method devices is rapidly heated vaporization under electrical heating case 40 high-temperature heating, under helium under the second mass-flow gas meter 17 flow control promotes, desorb is simultaneously by the second tee ball valve 33, the 4th tee ball valve 36, the 6th tee ball valve 38 enter gas and vapor permeation tank 39, three road sample stripping gas through the second four-way 34 and fully mix in gas and vapor permeation tank 39.Being switched by six-way valve 41 internal duct makes quantitative loop 46 be full of the sample stripping gas of fixed volume, rotates six-way valve 41 and quantitative loop 46 is communicated with gas dosing pump 42, utilize gas dosing pump 42 that the sample stripping gas in quantitative loop 46 is delivered to injection port 43.
Injection port 43 keeps the condition of high temperature, and sample stripping gas enters the concentration that time of-flight mass spectrometer 44 analysis measures Volatile Organic Compounds in Soil after injection port 43 is gasified totally.Time of-flight mass spectrometer 44 is made up of Proton-Transfer Reactions ion gun, time of flight mass analyzer, ion detector, photomultiplier cell.In Proton-Transfer Reactions ion gun, make the hydroxonium ion H as reaction reagent ion by cathode glow discharging
3o
+with the volatile organic matter molecule generation Proton-Transfer Reactions in sample stripping gas sample, generate the specific molecular ion of a band proton.Different molions is separated according to causing drift time discrepant principle because mass-to-charge ratio is different successively by time of flight mass analyzer, and mass-to-charge ratio is less, and drift time is shorter, more early arrives ion detector.The signal of the molion that the continuous acquisition testing of ion detector arrives, then carry out after signal amplification process through photomultiplier cell, analysis result transmission arrives computer.Adopt time of-flight mass spectrometer 44 to analyze composition and the concentration thereof of the volatile organic matter in soil, analyze that speed is fast, the volatile organic matter kind that detects and number is many, without the need to carrier gas, resolution is high, result is accurate.
Volatile Organic Compounds in Soil Concentration Testing data show at computer 45.Utilize computer 45 to control and revise the instrument parameter such as Proton-Transfer Reactions ion gun, time of flight mass analyzer, ion detector, photomultiplier cell comprising injection port 43 temperature, time of-flight mass spectrometer 44.In addition computer 45 also shows the peak area of the molecular ion peak of the chromatogram of each volatile organic matter in pedotheque, mass spectrogram and correspondence thereof, and according to the equation of linear regression of each volatile organic matter calibration curve, computing machine calculates each volatile organic matter concentration in pedotheque automatically.
Claims (2)
1. one kind for detecting the equipment of Volatile Organic Compounds in Soil, comprise sample cell (1), it is characterized in that sample cell (1) inside is provided with scavenging duct (2) and thermopair (3), sample cell (1) top is provided with safety valve (4), sample cell (1) outside is coated with electric furnace jacket (5), sample cell (1) is provided with electric stirring oar (6), one end of electric stirring oar (6) extend into sample cell (1) inside, scavenging duct (2), needle-valve (7), first mass-flow gas meter (8), second tensimeter (9) is connected successively with the second reduction valve (10), second reduction valve (10) by threeway (11) respectively with the first tensimeter (12), 3rd reduction valve (15) is connected, first tensimeter (12), first reduction valve (13) is connected successively with helium tank (14), 3rd reduction valve (15), 3rd tensimeter (16) is connected successively with the second mass-flow gas meter (17), it is inner that thermopair (3) is arranged on thermopair sleeve (18), temperature controller (19) respectively with thermopair (3), electric furnace jacket (5) is connected, sample cell (1), first ball valve (20) is connected successively with quantitative pot (21), quantitative pot (21) respectively with the 3rd ball valve (22), second ball valve (25) is connected, 3rd ball valve (22), water pump (23) is connected successively with water-storing bottle (24), second ball valve (25) is connected with waste liquid bottle (26), sample cell (1) is connected with drying buffer pipe (27), drying buffer pipe (27) by the first tee ball valve (28) respectively with the first four-way (29), first enrichment method device (30) is connected, second mass-flow gas meter (17) by the first four-way (29) respectively with the first tee ball valve (28), 3rd tee ball valve (31), 5th tee ball valve (32) is connected, first enrichment method device (30) by the second tee ball valve (33) respectively with the second four-way (34), 3rd tee ball valve (31) is connected, 3rd tee ball valve (31) is connected with the second enrichment method device (35), second enrichment method device (35) by the 4th tee ball valve (36) respectively with the 5th tee ball valve (32), second four-way (34) is connected, 5th tee ball valve (32), 3rd enrichment method device (37) is connected successively with the 6th tee ball valve (38), 6th tee ball valve (38) by the second four-way (34) respectively with the second tee ball valve (33), 4th tee ball valve (36), gas and vapor permeation tank (39) is connected, first enrichment method device (30), it is inner that second enrichment method device (35) and the 3rd enrichment method device (37) are arranged on electrical heating case (40), gas and vapor permeation tank (39), six-way valve (41), gas dosing pump (42), injection port (43), time of-flight mass spectrometer (44) is connected successively with computer (45), six-way valve (41) is provided with quantitative loop (46), time of-flight mass spectrometer (44) is connected with molecular pump (47), six-way valve (41) respectively with the second tee ball valve (33), 4th tee ball valve (36), pipe insulating layer (48) is coated with outside pipeline between 6th tee ball valve (38), six-way valve (41), Soviet Union's agate tank (49) is connected successively with gas dilution instrument (50), gas dilution instrument (50) respectively with volatile organic matter gas bottle (51), nitrogen cylinder (52) is connected.
2. the equipment for detecting Volatile Organic Compounds in Soil according to claim 1, it is characterized in that described sample cell (1) comprises stainless steel cover (53), teflon gasket (54) and stainless steel base (55), stainless steel cover (53), teflon gasket (54) are connected successively with stainless steel base (55).
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| CN108226269A (en) * | 2017-11-21 | 2018-06-29 | 上海裕达实业有限公司 | For the original position of Volatile Organic Compounds in Soil, rapid detection method and device |
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| CN112782324B (en) * | 2021-03-02 | 2023-08-22 | 云南中烟工业有限责任公司 | Volatile organic compound acquisition device and application method thereof |
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| CN114199985A (en) * | 2021-11-09 | 2022-03-18 | 河北省产品质量监督检验研究院 | Portable organic waste gas adsorbs detection device |
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