CN108692993A - Total volatile organic compounds adsorption tube and preparation method thereof and detection method in a kind of room air - Google Patents
Total volatile organic compounds adsorption tube and preparation method thereof and detection method in a kind of room air Download PDFInfo
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- CN108692993A CN108692993A CN201810326824.6A CN201810326824A CN108692993A CN 108692993 A CN108692993 A CN 108692993A CN 201810326824 A CN201810326824 A CN 201810326824A CN 108692993 A CN108692993 A CN 108692993A
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/02—Devices for withdrawing samples
- G01N1/22—Devices for withdrawing samples in the gaseous state
- G01N1/2202—Devices for withdrawing samples in the gaseous state involving separation of sample components during sampling
- G01N1/2214—Devices for withdrawing samples in the gaseous state involving separation of sample components during sampling by sorption
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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- G01N30/02—Column chromatography
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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Abstract
The invention discloses total volatile organic compounds adsorption tube in a kind of room air and preparation method thereof and detection methods.The adsorption tube includes:Adsorb tube body, and the adsorbent filled in the adsorption tube body, the adsorbent includes Tenax-TA adsorbents, wherein, when progress adsorbent is packed into adsorption tube, loaded using automatic vibration device, the automatic vibration device generates continuous vibration, adsorbent is set to be homogeneously added into the adsorption tube by the continuous vibration, Tenax-TA adsorbent loading densities are 0.36~0.43mg/L in the adsorption tube.The sampling resistance that still keeps relative stability after being used for multiple times of adsorption tube of the present invention, is not susceptible to penetration phenomenon, and can simultaneously in TVOC high boiling component and low boiling component be detected.
Description
Technical field
The present invention relates in a kind of gas sampler and preparation method thereof and detection method more particularly to a kind of room air
Total volatile organic compounds adsorption tube and preparation method thereof and detection method belong to environmental monitoring technology field.
Background technology
Tenax-TA is a kind of porous polymer polymer, and chemical name is poly- 2,6- diphenyl p-phenylene, is had good
Temperature tolerance (extremely low leachability), there is good adsorptivity and pyrolysis absorption to the hydro carbons of C6 or more, be widely used in having
The absorption of machine volatile matter and half volatile matter, and it is poisonous and harmful in air to adsorb by domestic and international multiple standards to be chosen to be adsorbent
Substance is to be detected.
"Code for indoor environmental pollution control of civil building engineering"(GB50325-2010 (version in 2013)) (hereinafter referred to as
< specification >) limitation regulation has been carried out to total volatile organic compounds (TVOC), and in annex G " general volatiles in room air
The sample detecting method of TVOC is defined in the measurement of organic compound (TVOC) ", wherein G.0.3 having to reagent and material following
Regulation:Tenax-TA adsorption tubes can be the stainless steel tube of glass tube or inner wall smooth, in pipe equipped with 200mg grain sizes be 0.18mm~
The Tenax-TA adsorbents of 0.25mm (60-80 mesh).Nitrogen heat-activated should be led to before use, activation temperature should be higher than that desorption temperature
Degree, soak time should not be less than 30min, activate until no miscellaneous peak, and when flow is 0.5L/min, sampling resistance should be in 5-
Between 10kPa.
And in the prior art, commercially available Tenax-TA adsorption tubes often have the following problems:(1) filler filling pine in adsorption tube
It dissipates, adsorbent is easy leakage, causes the sampling resistance of adsorption tube to become smaller, adsorption tube easy tos produce penetration phenomenon;(2) new pipe enables
When sampling resistance meet < specifications > requirement, but after being used for multiple times, Tenax-TA solid particles easily lump, so that adsorbent bed is adopted
Sample resistance becomes larger so that the sample size of acquisition is insufficient, does not meet the > requirements of < specifications, and influence Tenax-TA adsorption tubes uses the longevity
Life;(3) due to the influence of the factors such as environment temperature, sampling volume, Tenax-TA adsorption tubes to benzene,toluene,xylene and
The adsorption efficiency of the low boiling points volatile organic matter such as butyl acetate is not high, and testing result is relatively low.
Citation 1 discloses molecular sieve vibration loading density experiment research, and experimental study particle size distribution range exists
Molecular sieve between 1.3mm~3.0mm during vibration loading, various vibration parameters include vibration frequency, Oscillation Amplitude and
The influence to molecular sieve loading density such as time of vibration, and obtain best vibration loading technological parameter.These can be used as true
The basis of molecular sieve vibration loading technological parameter in the fixed particle size range.But its obtained parameter may be not particularly suited for Tenax-
The filling of TA adsorbents, and it is not related to the research to loading homogeneity yet.
Citation 2 discloses a kind of electric eccentric wheel type absorbent filling vibration device, passes through several bullets on pedestal
Spring connects shaking platform, and shaking platform center bottom is connected with motor, motor connecting eccentric wheel.The utility model works as motor
When rotation, the eccentric wheel rotation on axis generates eccentric force and generates vibration.In order to avoid starting-impact and adjusting vibration intensity are set
Set frequency device smoothly adjustable-speed.Tamp the separation of compact air and cleaning equipment adsorbent and drier, so as not to strain air-flow crushing and
It reduces the service life.But it is not related to the research to the packed density and packed density uniformity of adsorbent.
Citation 3 discloses a kind of packing method of adsorbent in II types iodine adsorber, uses two vibration performances
Different shake tables is filling equipment, and No.1 shake table provides exciting force by vibrating motor, and direction of vibration is horizontal X-direction
With vertical Z-direction, No. two shake tables generate exciting force by collision rigid support after working plate and absorber freely falling body,
Direction of vibration is vertical Z-direction.Adsorbent is multiple batches of to be loaded into II type iodine adsorber shells.But its be first load it is a certain amount of
Adsorbent, be then turned on shake table vibration certain time, the uniformity of adsorbent filling may be a bit weaker.
Therefore, it is necessary to design a kind of adsorption tube for loading consistent in density, being not easy loosely or to lump, the sampling resistance of adsorption tube
It can keep stable in a long time;And the high boiling component that adsorption tube can be acquired well in TVOC can take into account low boiling point again
Component.
Citation 1:Liu Yingshu, Ge Mingxia, Chen Qidong etc.,;J], molecular sieve vibration loading density experiment research,"Experiment
Mechanics", 03 phase in 2010;
Citation 2:Patent application CN201291109;
Citation 3:Patent application CN104772001A.
Invention content
Problems to be solved by the invention
It easily leaks, easily lump, to the low boiling points volatile organic matter such as benzene for the filler in the presence of the above prior art
The not high problem of adsorption efficiency, the present invention provide total volatile organic compounds adsorption tube and its preparation side in a kind of room air
Method.
In addition, the present invention also provides a kind of detection methods of total volatile organic compounds in room air.
The solution to the problem
The present invention solves above-mentioned technical problem using following technical scheme:
Present invention firstly provides total volatile organic compounds adsorption tubes in a kind of room air comprising absorption tube body,
And the adsorbent filled in the adsorption tube body, the adsorbent include Tenax-TA adsorbents,
Wherein, it when progress adsorbent is packed into adsorption tube, is loaded using automatic vibration device, the automatic vibration
Device generates continuous vibration, and adsorbent is made to be homogeneously added into the adsorption tube by the continuous vibration,
Tenax-TA adsorbent loading densities are 0.36~0.43mg/L in the adsorption tube.
The electromagnet of electric current after being passed through halfwave rectifier is applied according to above-described adsorption tube, in the automatic vibration device
The energy for generating electric and magnetic oscillation makes vibrating device generate continuous vibration.
According to above-described adsorption tube, when loading the Tenax-TA adsorbents, the vibration of the automatic vibration device
Frequency is 15-35Hz, amplitude 0.5-3.5mm.
According to above-described adsorption tube, the adsorbent further includes carbon system adsorbent, preferably Graphon, the carbon
The loading density for being adsorbent is 0.50~0.59mg/L.
According to above-described adsorption tube, when loading the carbon system adsorbent, the vibration frequency of the automatic vibration device
25-40Hz, amplitude 0.5-4mm.
In addition, the present invention also provides a kind of preparation method of total volatile organic compounds adsorption tube in room air,
Wherein, the adsorption tube includes:
Tube body is adsorbed,
And the adsorbent filled in the adsorption tube body, the adsorbent include Tenax-TA adsorbents,
Wherein, it when progress adsorbent is packed into adsorption tube, is loaded using automatic vibration device, the automatic vibration
Device generates continuous vibration, and adsorbent is made to be homogeneously added into the adsorption tube by the continuous vibration,
Tenax-TA adsorbent loading densities are 0.36~0.43mg/L in the adsorption tube.
The electromagnetism of electric current after being passed through halfwave rectifier is applied according to above-described preparation method, in the automatic vibration device
Iron generates the energy of electric and magnetic oscillation, and vibrating device is made to generate continuous vibration.
According to above-described preparation method, when loading the Tenax-TA adsorbents, the automatic vibration device shakes
Dynamic frequency is 15-35Hz, amplitude 0.5-3.5mm.
According to above-described preparation method, the adsorbent further includes carbon system adsorbent.In addition, also being provided in the present invention
The detection method of total volatile organic compounds in a kind of room air, described method includes following steps:
Gas sampling is carried out using the adsorption tube;
By the adsorption tube in solution analyzer parsing, parsing gas is sent directly into chromatograph and is analyzed;
With peak area quantification, retention time is qualitative, area external standard method calculates separately benzene and total volatile organic compounds
Content;
The wherein described adsorption tube be according to above-described adsorption tube, or for according to above-described preparation method obtain
Adsorption tube.
The effect of invention
Total volatile organic compounds adsorption tube and preparation method thereof and detection side in room air provided by the present invention
Method has following excellent technique effect:
(1) the adsorbent filling in the adsorption tube is uniform, and loading density is suitable, and adsorbent is not easy loose or caking,
In certain access times, adsorbent sampling resistance can keep relative stability, and be conducive to extend the service life of adsorption tube;
(2) when containing carbon system adsorbent in the adsorption tube, adsorption tube can be realized simultaneously to low boiling component in air
And all higher to the rate of recovery of the two with the sampling of high boiling component, testing result is accurate;
(3) adsorbent in the adsorption tube can take out at any time, and reloading after processing uses, and is conducive to economize on resources
And cost;
(4) preparation method of the adsorption tube is conducive to the homogeneity of adsorbent filling, compactness, does not stay dead angle, and
The method is simple and convenient, and full-automatic production may be implemented;
(5) detection method provided by the present invention is relatively simple, and can analyze the benzene in air and total volatilization simultaneously
Property organic compound, reduces workload and testing cost, easy to operate.
Specific implementation mode
Hereinafter, mode for carrying out the present invention will be described in detail.
<1st Shi Shifangshi >
The present invention the 1st embodiments, provides a kind of room air in total volatile organic compounds adsorption tube, institute
Stating adsorption tube includes:Tube body is adsorbed, and the adsorbent filled in the adsorption tube body, the adsorbent includes Tenax-TA
Adsorbent, wherein when progress adsorbent is packed into adsorption tube, loaded using automatic vibration device, the automatic vibration
Device generates continuous vibration, so that adsorbent is homogeneously added into the adsorption tube by the continuous vibration, in the adsorption tube
Tenax-TA adsorbent loading densities are 0.36~0.43mg/L.
Adsorbent
The adsorbent filled in the adsorption tube body includes Tenax-TA adsorbents, in present embodiment, the adsorption tube
Interior Tenax-TA adsorbent loading densities are 0.36~0.43mg/L, can ensure that the sampling resistance of adsorption tube meets < specifications >'s
It is required that is, when sampling flow is 0.5L/min, adsorbent samples resistance between 5-10kpa, moreover, by repeatedly inhaling
After attached-resolving, both it had been not easy loosely, to be not easy to lump, and had effectively maintained the stability of adsorption tube sampling resistance, extend suction
The service life of attached pipe.
Tenax-TA adsorbents are to the adsorption effect function well of total volatile organism, but to benzene therein, toluene, two
The adsorption efficiency of the low boiling points object such as toluene, butyl acetate is not high, and suction-operated is shown as with the temperature from low temperature to high temperature
Degree increases, and suction-operated reduces rapidly, such as, it is generally the case that when adsorption tube of the use containing Tenax-TA adsorbents is one
As room temperature sampling when, can there are the following problems, summer using or temperature it is higher area in use, there is indoor temperature appearance
Easily more than 30 DEG C temperature high in this way cause the low boiling components such as benzene to penetrate readily through adsorption tube and are largely lost so that test result
It is relatively low.In addition, containing Tenax-TA adsorbents in use, adsorbent due to adsorbed the low boiling components such as benzene or other
Pernicious gas and the heating for leading to itself, in use but also the temperature of itself increases and causes under absorption property
Drop, to cause the distortion of test result.
Detection accuracy of the adsorption tube to high boiling component in TVOC and low boiling component in order to balance, it is preferred that this reality
It further includes carbon system adsorbent to apply the adsorption tube in mode.Compared to the adsorption tube for only having loaded Tenax-TA adsorbents, filling
The adsorption tube of Tenax-TA adsorbents and carbon system adsorbent can acquire high boiling component in TVOC well can take into account low boiling again
The component of point so that we can be obtained in analyzing TVOC closer to true data.
As long as not destroying the technique effect of the present invention in present embodiment, used carbon system adsorbent is in principle without spy
Other restriction, such as can be activated carbon commonly used in the art, Graphon, carbon molecular sieve, preferably graphitized charcoal
It is black.
In present embodiment, the loading density of carbon system adsorbent is 0.36~0.43mg/L, Neng Goubao in the adsorption tube
The sampling resistance of card adsorption tube meets the requirement of < specifications >, i.e., when sampling flow is 0.5L/min, adsorbent sampling resistance exists
Between 5-10kpa, moreover, by repeatedly adsorb-resolving after, be both not easy loose, and be not easy to lump, effectively maintain suction
The stability of attached pipe sampling resistance, extends the service life of adsorption tube.
Adsorb tube body
Absorption tube body in present embodiment is stainless steel tube or glass tube.
According to stainless steel tube, the outer wall at stainless steel tube both ends is processed into threaded end (TE), can be used after sampling
STAINLESS STEEL NUTS is closed, and filler can be effectively prevent to reveal, and STAINLESS STEEL NUTS is lined with silicagel pad so that sealing is tighter
It is close.According to glass tube, glass tube both ends are handled through frosted, it is close by silica gel sheath or grournd glass cap after sampling
Envelope.
The adsorption tube has the mark of airintake direction, attachment device when facilitating acquisition gas, such as in absorption tube body
Label with the arrow is done on outer wall, can also mark air inlet or the printed words of gas outlet, or marked with different colors, etc.
Deng.
It is managed in absorption tubular body in order to avoid when acquiring sample, air-flow drives adsorbent to block the nozzle of adsorption tube
Inside set gradually stainless steel mesh screen, Tenax-TA adsorbents, stainless steel mesh screen.If adsorption tube is also filled with carbon system adsorbent,
Then set gradually stainless steel mesh screen in pipe, Tenax-TA adsorbents, stainless steel mesh screen, Graphon, stainless steel mesh screen is stainless
Steel mesh sieve also acts as the effect for separating Tenax-TA adsorbents and carbon system adsorbent, when needing replacing filler, facilitates taking-up.
Further, the mesh screen is equipped with lead, when needing replacing the filler in adsorption tube, pulls lead that can drive
Mesh screen takes out adsorbent.Preferably, the other end of the lead is equipped with draw ring, facilitates pulling mesh screen.Adsorption tube through a long time
After use, high temperature parsing and the influence of ambient humidity repeatedly is easy that filling adsorption agent therein is made to lump, and present embodiment is carried
The adsorption tube of confession can conveniently take out filler, then filler is backfilling into suction by handling such as crushing, dry etc. again
It is reused in attached pipe, or adds new adsorbent into adsorption tube.
<2nd Shi Shifangshi >
The present invention the 2nd embodiments, provides a kind of room air in total volatile organic compounds adsorption tube system
Preparation Method comprising:When progress adsorbent is packed into adsorption tube, adsorbent is loaded using automatic vibration device, institute
It states automatic vibration device and generates continuous vibration, adsorbent is made to be homogeneously added into the adsorption tube by the continuous vibration.With
The upper automatic Loading mode is conducive to improve uniformity of the adsorbent in pipe, it is ensured that Tenax-TA adsorbents filling in pipe
Density is 0.36~0.43mg/L, and the loading density of optional carbon system adsorbent is 0.50~0.59mg/L.
For the detection of total volatile organic compounds, the filling of adsorbent is a critically important link, filling
Quality is the important leverage of subsequent detection work.The leading indicator for weighing filling quality is loading density, further needs exist for making dress
The adsorbent uniform throughout filled out, it is close, do not stay dead angle (or cavity), that is, there is uniformity.Above-described type of feed makes
Adsorption tube in the present invention has good filling quality, and after being used for multiple times, the sampling resistance of the adsorption tube still meets
The > requirements of < specifications, and the higher rate of recovery is all had to benzene and volatile organic matter.
In existing adsorbent filling process, although the considerations of for production efficiency, it is also possible to use mechanical equipment
Various adsorbents are filled into adsorption tube by (automatically or semi-automatically pad device) simultaneously or in a certain order, but in this way
Filling process, belong to disposable filling, there is no well solve filling homogeneity question.For example, can be by inhaling
The processing of attached dose of overall flow it is expected that filler is smoothly filled into absorption tube body, but may lead to packed density at this time
Or the stability of packed density is affected.In addition, after carrying out mechanical filling, in order to ensure the uniform and phase of filler
The packed density of prestige is needed to carry out concussion processing to tube body in the filling process or after filling, is frequently necessary at this time to inhaling
Occur excessively filling in the filling process of attached pipe, and is removed the part overcharged by subsequent processing.Such process is not only led
Cause the cumbersome of production technology, it is also possible to lead to the waste of unnecessary filler or cause to bear to environment, increase is produced into
This.
And the type of feed of adsorbent provided by the present invention, on the one hand, since automatic vibration device generation is utilized
Continuous vibration so that adsorbent has stable discharging speed in the discharge port of automatic vibration device, so that adsorbent
The speed that grain falls into absorption tube body is consistent, i.e., the power of generation is mutually collided between the adsorbent newly loaded and the adsorbent loaded
It is almost the same, be conducive to the closely knit and uniformity of adsorbent filling;On the other hand, the continuous vibration that automatic vibration device generates makes
Absorbent particles just have good dispersibility during the decline, but also absorbent particles disperse in adsorption tube
It is even.Preferably, the automatic vibration device also drives absorption tube body to be vibrated simultaneously so that is packed into adsorption tube body
It further interacts between absorbent particles, reduces the gap between particle, increase the tight ness rating of adsorbent filling.Cause
This, type of feed of the present invention is not only provided with higher production efficiency, also ensures the uniformity and stabilization of filler
Packed density, adsorbent sampling resistance can also keep relative stability, that is to say, that the preparation side of adsorption tube of the present invention
The continuous filling of mechanization may be implemented in method, convenient and efficient, need not interrupt filling process and carry out compacting operation, also not need
Carry out additional compacting operation again after automatic Loading.
The continuous vibration is carried out by controlling vibration frequency and amplitude, the adsorbent species that can be loaded as needed
Vibration frequency and amplitude are set with the needs of loading density.By taking Tenax-TA adsorbents as an example, filling in the present invention
Density is 0.36~0.43mg/L, is 15-35Hz, amplitude 0.5-3.5mm therefore, it is necessary to control vibration frequency.It is inhaled with carbon system
For attached dose, loading density in the present invention is 0.50~0.59mg/L, is 25- therefore, it is necessary to control vibration frequency
40Hz, amplitude 0.5-4mm.
Specifically, the method for the invention includes the following steps:When progress adsorbent is packed into adsorption tube, using automatic
Vibrating device loads adsorbent, and the electromagnet of electric current after being passed through halfwave rectifier is applied to generate in the automatic vibration device
The energy of electric and magnetic oscillation, so that vibrating device is generated continuous vibration makes adsorbent be homogeneously added into the suction by the continuous vibration
In attached pipe.
The control principle of electric and magnetic oscillation is halfwave rectifier.Electromagnetic coil is powered by alternating current through diode rectification.Work as circuit
After connection, positive half cycle pulsating dc voltage is added on electromagnetic coil, by the effect of electromagnet, is generated between vibrating body and engine base
Pulse-electromagnetic force, vibrating body are attracted, and elastic system stores potential energy at this time, is not turned in negative half period diode, and electromagnetic force disappears,
By the potential energy that elastic system is stored, vibrating body is made to vibrate in the opposite direction.So in cycles, vibrating body is just with alternating current
Frequency it is of reciprocating vibration.The periodic dither of vibrating body passes to bin wall by impact block.The periodicity of bulkhead is shaken
It is dynamic, on the one hand material is made to be disengaged with bulkhead, material is on the other hand made to be influenced by alternation speed and acceleration, in shakiness
State is determined, to the internal friction and focusing force efficiently against material.Material is set to be smoothly discharged out from material outlet.
There is no particular limitation in principle for automatic vibration device in present embodiment, as long as continuous vibration can be generated, makes
Adsorbent is homogeneously added by the continuous vibration in the adsorption tube, for example filling machine, Material sucking machine, true may be used
Empty filling machine, suction feeder etc..But inventor be further discovered that when in automatic vibration device using be passed through halfwave rectifier after electricity
The electromagnet of stream generates the energy of electric and magnetic oscillation, when vibrating device being made to generate continuous vibration, and vibrating device in this way into
When row charging, more preferably effect can be obtained in terms of the uniformity of filling and stability, it is therefore preferable that electromagnetic oscillation device.
It is weighed in addition, the method further includes the steps that adsorbent.The weighing of the adsorbent uses automatic weighing device
It carries out, it is only necessary to which setting needs type, quality and the filling sequence of the various adsorbents loaded, the automatic weighing device
Start to weigh, and load weighted various adsorbents are transmitted in the automatic vibration device, in case filling.The above weighs
Process and filling process can realize automation mechanized operation, be conducive to large-scale industrial production, save time and manpower.
<3rd Shi Shifangshi >
The present invention the 3rd embodiments, provides a kind of room air in total volatile organic compounds detection side
Method comprising following steps:
It is obtained using the preparation method that the adsorption tube or the 2nd embodiment that are provided according to the 1st embodiment are provided
Adsorption tube carries out gas sampling;
By the adsorption tube in solution analyzer parsing, parsing gas is sent directly into chromatograph and is analyzed;
With peak area quantification, retention time is qualitative, area external standard method calculates separately benzene and total volatile organic compounds
Content.
The detection to TVOC may be implemented in detection method described above, further, the higher boiling group in accurately detection TVOC
While dividing, moreover it is possible to take into account the accurate detection to the low boiling components such as benzene,toluene,xylene, butyl acetate in TVOC.
Sampling
Solid absorbent sampling principle:Solid absorbent enrichment is belonged to the sampling of TVOC in existing national standards < specifications >
Sampling, sampling process are analyzed similar to the sample pre-treatments in chromatography.Air passes through adsorption column as a mixing sample, empty
Oxygen, nitrogen and carbon dioxide flow out first since their adsorptivity is weak and content is high in gas, a little group fractionation of some strong adsorptions
On the sorbent.When sampling starts, most components are all trapped in adsorbent inlet end in air, with the increasing for being pumped through volume of air
Adding, each component adsorbed is pushed ahead, and since the absorption property of each component has differences, is spaced out between each component, some
The small component of adsorptivity first flows out.
When being sampled with adsorbent it is noted that the amount adsorbed is more than the penetration phenomenon caused by adsorbent adsorption capacity, by
In the generation of penetration phenomenon, the inaccuracy of quantitative result may be caused.Enter after adsorption tube until just from this organic gas
When having gas to reach outlet, it is exactly penetration volume to preserve the volume of this organic matter in adsorption tube.
Acquisition finishes, and adsorption tube both ends are sealed, to be analyzed.
Parsing and chromatography
Thermal desorption is used to the parsing of TVOC in present embodiment.Thermal desorption is carried out using pyrolysis analyzer, by the absorption
Pipe is put into the heating zone of pyrolysis analyzer, and parsing is complete.
After parsing, will parsing gas be sent directly into chromatograph carry out chromatography, the chromatograph be gas chromatograph or
Gas chromatograph-mass spectrometer.
Embodiment
More specific description is carried out to the present invention below by embodiment, but the present invention is not limited to these embodiments.
Embodiment 1
(1) it is 150mm by length, outer diameter 6.35mm, thickness is that the stainless steel adsorption tube of 1.0mm is fixed on electric and magnetic oscillation
On the shake table of batcher, face discharge port carries out layering filling according to following provisions:Tenax-TA adsorbents are 150mg (60
~80 mesh), loading density 0.36mg/L, vibration frequency 20Hz, amplitude 1.0mm vibrate 5min;Graphon is
100mg (60~80 mesh), loading density 0.50mg/L, vibration frequency 30Hz, amplitude 2.5mm vibrate 5min,
Adsorption tube obtained is activated totally to free from admixture peak;
(2) it is 1m in volume3Environmental testing storehouse in discharge known concentration stupid and styrene, carried out according to the following conditions
Gas sampling:Temperature is 25 DEG C, sampling volume 10L, sampling flow 0.5L/min;
(3) after sampling, adsorption tube is parsed in 350 DEG C of solution analyzer, parsing gas is sent directly into gas phase color
Spectrometer carries out chromatography;
(4) it with peak area quantification, the content that retention time is qualitative, area external standard method calculates separately benzene and styrene, calculates
The rate of recovery.
(5) adsorption tube 101 times made from step (1) are reused, the rate of recovery is calculated.
Embodiment 2
Tenax-TA adsorbent loading densities are 0.40mg/L, vibration frequency 25Hz, amplitude 1.5mm, vibrate 3min;
The loading density of Graphon is 0.59mg/L, vibration frequency 35Hz, amplitude 3.0mm, vibrates 3min, in addition to this,
Other conditions are same as Example 1.
Embodiment 3
Tenax-TA adsorbent loading densities are 0.43mg/L, quality 250mg, vibration frequency 35Hz, and amplitude is
2.5mm vibrates 3min, and in addition to this, other conditions are same as Example 1.
Comparative example 1
Tenax-TA adsorbent loading densities are 0.3mg/L, vibration frequency 15Hz, amplitude 0.5mm, vibrate 8min;
The loading density of Graphon is 0.45mg/L, vibration frequency 25Hz, amplitude 0.5mm, vibrates 8min, in addition to this,
Other conditions are same as Example 1.
Comparative example 2
Tenax-TA adsorbent loading densities are 0.45mg/L, vibration frequency 35Hz, amplitude 0.5mm, vibrate 5min;
The loading density of Graphon is 0.63mg/L, vibration frequency 40Hz, amplitude 0.5mm, vibrates 5min, in addition to this,
Other conditions are same as Example 1.
Comparative example 3
Stainless steel absorption tube body is fixed on common shake table (direction of vibration is vertical direction, amplitude 1.5mm,
Vibration frequency is 30Hz), it is more than adsorbent tube body to prevent adsorbent filling height, a filling in absorption tube body upper lid
Tenax-TA adsorbents are packed into absorption tube body by sleeve, are then turned on shake table, vibrate 5min, then carbon system adsorbent is filled
Filling absorption tube body, is then turned on shake table, vibrates 5min, in addition to this, other conditions are identical with embodiment 1.
Test method
1. loading density
The quality for the adsorbent that loading density is loaded by unit volume.Prepare a glass adsorption tube with a scale, claims
Measure the quality m of glass adsorption tube0, according to packing method as defined in above example or comparative example, filled in the glass adsorption tube
The adsorbent of certain volume V is filled out, weighs the quality m for the glass adsorption tube for having loaded adsorbent again1, loading density is (m1-
m0)/V。
2. sampling resistance
The ABP-SLL type air drag test devices test adsorption tube produced using Ji Kong finite instruments company of Jiangsu Province is existed
Drag size when flow is 0.5L/min.
3. the rate of recovery
Mass concentration × 100% of benzene/(matter of known benzene in environmental testing storehouse is detected in the rate of recovery=adsorption tube of benzene
Measure concentration).
Mass concentration × 100% of TVOC/(known in environmental testing storehouse is detected in the rate of recovery=adsorption tube of TVOC
The mass concentration of TVOC).
By adsorption tube made from embodiment 1-3 at the 1st time and the 101st time in use, the sampling resistance measured, the rate of recovery
Data are listed in Table 1 below, by adsorption tube made from comparative example 1-3 at the 1st time and the 101st time in use, the sampling resistance measured, return
The data of yield are listed in Table 2 below.
The performance parameter of the adsorption tube of 1 embodiment 1-3 of table
The performance parameter of the adsorption tube of 2 comparative example 1-3 of table
The adsorption tube of the present invention when enabling for the first time it can be seen from the test result of Tables 1 and 2, to benzene and styrene
The rate of recovery it is all higher, after 101 uses, the rate of recovery slightly reduces, but all penetrating, the suction with comparative example 1-3
Attached pipe is compared, and adsorption tube of the invention loads quality higher, and testing result is more acurrate.
From table 2 it can be seen that in comparative example 1, the loading density of Tenax-TA adsorbents and Graphon adsorbent is low
In the framework of the present definition, although adsorption tube resistance and rate of recovery when enabling for the first time all meet the requirements, by for a long time
After use, the rate of recovery of adsorption tube significantly reduces, no matter still being adsorbed for styrene to absorption benzene, the rate of recovery is below
95%, penetration phenomenon occurs for adsorption tube.
In comparative example 2, the loading density of Tenax-TA adsorbents and Graphon adsorbent is higher than what the present invention limited
Range, although adsorption tube resistance and rate of recovery when enabling for the first time all meet the requirements, after long-time use, although absorption
The rate of recovery reduction amplitude of pipe is less, but its resistance has exceeded critical field.
In comparative example 3, using the type of feed different from embodiment 1-3, the adsorption tube of comparative example 3 is hindered when enabling for the first time
Power and the rate of recovery all meet the requirements, but after long-time use, and the rate of recovery of adsorption tube significantly reduces, no matter also to absorption benzene
It is for absorption styrene, the rate of recovery is below 95%, and penetration phenomenon occurs for adsorption tube, illustrates the type of feed of comparative example 3
Not as good as the type of feed of the present invention, probably due to comparative example 3 is taken load in batches after, the mode of jolt ramming is easy to cause filling again
Adsorbent is unevenly distributed, and is easy to leave a void, therefore adsorption efficiency is not high.
Industrial availability
In the room air of the present invention total volatile organic compounds adsorption tube and preparation method thereof can industrially into
Row production, also, in the room air of the present invention total volatile organic compounds detection method accuracy it is high.
Claims (10)
1. total volatile organic compounds adsorption tube in a kind of room air, which is characterized in that the adsorption tube includes:
Tube body is adsorbed,
And the adsorbent filled in the adsorption tube body, the adsorbent include Tenax-TA adsorbents,
Wherein, it when progress adsorbent is packed into adsorption tube, is loaded using automatic vibration device, the automatic vibration device
Continuous vibration is generated, adsorbent is made to be homogeneously added into the adsorption tube by the continuous vibration,
Tenax-TA adsorbent loading densities are 0.36~0.43mg/L in the adsorption tube.
2. adsorption tube according to claim 1, which is characterized in that applied in the automatic vibration device and be passed through halfwave rectifier
The electromagnet of electric current generates the energy of electric and magnetic oscillation afterwards, and vibrating device is made to generate continuous vibration.
3. adsorption tube according to claim 1 or 2, which is characterized in that when loading the Tenax-TA adsorbents, it is described from
The vibration frequency of dynamic vibrating device is 15-35Hz, amplitude 0.5-3.5mm.
4. according to claim 1-3 any one of them adsorption tubes, which is characterized in that the adsorbent further includes the absorption of carbon system
The loading density of agent, preferably Graphon, carbon system adsorbent is 0.50~0.59mg/L.
5. adsorption tube according to claim 4, which is characterized in that when loading the carbon system adsorbent, the automatic vibration
The vibration frequency of device is 25-40Hz, amplitude 0.5-4mm.
6. the preparation method of total volatile organic compounds adsorption tube in a kind of room air, which is characterized in that the adsorption tube
Including:
Tube body is adsorbed,
And the adsorbent filled in the adsorption tube body, the adsorbent include Tenax-TA adsorbents,
Wherein, it when progress adsorbent is packed into adsorption tube, is loaded using automatic vibration device, the automatic vibration device
Continuous vibration is generated, adsorbent is made to be homogeneously added into the adsorption tube by the continuous vibration,
Tenax-TA adsorbent loading densities are 0.36~0.43mg/L in the adsorption tube.
7. preparation method according to claim 6, which is characterized in that whole using half-wave is passed through in the automatic vibration device
The electromagnet of electric current generates the energy of electric and magnetic oscillation after stream, and vibrating device is made to generate continuous vibration.
8. the preparation method described according to claim 6 or 7, which is characterized in that described when loading the Tenax-TA adsorbents
The vibration frequency of automatic vibration device is 15-35Hz, amplitude 0.5-3.5mm.
9. according to claim 6-8 any one of them preparation methods, which is characterized in that the adsorbent further includes the absorption of carbon system
Agent.
10. the detection method of total volatile organic compounds in a kind of room air, which is characterized in that include the following steps:
Gas sampling is carried out using the adsorption tube;
By the adsorption tube in solution analyzer parsing, parsing gas is sent directly into chromatograph and is analyzed;
With peak area quantification, the content that retention time is qualitative, area external standard method calculates separately benzene and total volatile organic compounds;
The wherein described adsorption tube be according to claim 1-5 any one of them adsorption tubes, or for according to claim 6-9 appoint
The adsorption tube that preparation method described in one obtains.
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