CN108693261A - A kind of detection method and sampling apparatus of Indoor Air Benzene and total volatile organic compounds - Google Patents
A kind of detection method and sampling apparatus of Indoor Air Benzene and total volatile organic compounds Download PDFInfo
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Abstract
The invention discloses the detection methods and sampling apparatus of a kind of Indoor Air Benzene and total volatile organic compounds.It is described that detection method includes the following steps:1) adsorption tube is used to carry out gas sampling, the temperature that the adsorption tube is controlled by temperature-adjusting device is 28 DEG C or less, wherein the adsorbent filled in the adsorption tube includes the Tenax-TA adsorbents of 60~80 mesh;2) by the adsorption tube in solution analyzer parsing, parsing gas is sent directly into chromatograph and is analyzed;3) with peak area quantification, the content that retention time is qualitative, area external standard method calculates separately benzene and total volatile organic compounds.The detection method of the present invention can simultaneously be detected benzene and total volatile organic compounds, and overcome the influence of environment temperature, avoid penetration phenomenon, the rate of recovery is high, and easy to operate, effectively saves workload and cost.
Description
Technical field
The present invention relates to a kind of gas detection method and sampling apparatus more particularly to a kind of Indoor Air Benzenes and total volatilization
The detection method of property organic compound, belongs to environmental monitoring technology field.
Background technology
Existing national standards"Code for indoor environmental pollution control of civil building engineering"(GB50325-2010 (2013
Version)) (hereinafter referred to as < specification >) middle regulation, different sides is respectively adopted in benzene in air and total volatile organic compounds (TVOC)
Method carries out sample detecting.Wherein, benzene applied activated carbon pipe is acquired, sampling volume about 10L, thermal desorption direct injected gas phase
Chromatography, peak area quantification;TVOC then applies the gaseous sample of Tenax-TA adsorption tubes acquisition volume about 10L, Thermal desorption straight
Tap into sample gas chromatographic analysis.
But during using Activated charcoal tube to surveying benzene, some problems are encountered, if activated carbon is to the adsorption energy of water
Power is very strong, when with Thermal desorption/gas chromatography analysis, is damaged to instrument larger;Activated carbon thermal desorption temperature is high, at high temperature
The problems such as incomplete desorption or generation Irreversible Adsorption can often occur, decompose.Therefore, a small amount of report proposes to be inhaled with Tenax-TA
Attached dose is detected the benzene concentration in air.The factor for influencing Tenax-TA adsorbent detection accuracies may have the adsorption tube of filling
Quality, sampling flow velocity, sampling volume, environment temperature, the concentration etc. of benzene to be collected.
It is Tenax-TA and the adsorption tube simulation collection in worksite indoor environment of activated carbon that adsorbent, which is respectively adopted, in citation 1
Air understands the absorption property of Tenax-TA and activated carbon to benzene in air.When Tenax-TA adsorbents are with the stream of 0.5L/min
When amount acquisition 10L air, there are penetration phenomenons for benzene.Illustrate that the acquisition of benzene in air should not use Tenax-TA adsorbents to substitute activity
Carbon adsorbent.
Citation 2 discloses under 35 DEG C of environment temperature, under same traffic, with the increase of sampling volume,
Tenax-TA is gradually reduced the rate of recovery of benzene, at such a temperature, when with the traffic sampling 1.5L of 0.1-0.4L/min, the rate of recovery
Less than 95%, benzene has penetrated.Therefore, citation 2 is proposed when summer temperature is higher, when detection scene temperature reaches 35
DEG C, when sampling, should reduce sampling quantity, control within 0.7L.
It is most weak to the reserve capability of benzene when citation 3 is proposed with Tenax-TA adsorbents to TVOC acquisition testings, with
The raising of sample temperature, the sampling volume that benzene penetrates in sample are also smaller.It is accurate in order to ensure qualitatively or quantitatively to detect
Property, 20-30 DEG C is more suitable sample temperature.But it is concerned with the temperature for adjusting sampling laboratory, and is actually adopted
The environment of sample operation, it may be possible to field or the place etc. for lacking large-scale temperature controlling instruments, it is impossible in order to detect the benzene in air
Environment temperature is adjusted to laboratory condition.Moreover, because adsorbent own temperature in sampling can also increase, lead to adsorption tube
There are certain difference, the temperature of adjusting ambient also differs surely and Tenax-TA sampling pipes is made to adopt safely for temperature and environment temperature
Sample.
Citation 4 discloses a kind of thermostatic type two-way atmospheric sampling device, including two-way atmospheric sampling device ontology, Yi Jishe
Bottle holder and two sets of inlet ducts are absorbed in two on two-way atmospheric sampling device ontology, is set in the two-way atmospheric sampling device ontology
There is thermostat corresponding with described two absorption bottle holder, and flowmeter is respectively equipped in described often cover on inlet duct.The perseverance
Warm type two-way atmospheric sampling device can be achieved at the same time temperature incubation function and sampling flow control function.But the thermostatic type two-way air is adopted
Sample device is the device suitable for liquid absorption bottle adsorbed gas, is not particularly suited for the temperature control to adsorption tube, and it does not have yet
The open temperature controlling range that can be realized.
Document referenced above shows that the detection of benzene cannot use the benzene data in TVOC analysis results, the reason is that:
Tenax-TA adsorbents detect in the analysis of Indoor Air Benzene concentration, and the variation of environment temperature influences to show on Tenax-TA samplings
It writes, when sample temperature is more than 30 DEG C, Tenax-TA is easy to happen when adsorbing benzene and penetrates, and therefore, presses (< specification > annex G (2013
Version)) method using Tenax-TA adsorbents acquisition TVOC when, benzene concentration by < specification > annex F than being detected in analysis result
Benzene concentration wants low.
However, in actual environment, the hot weather of summer may be frequently encountered, or need the regional work in long-term high temperature
Make, indoor hot environment greatly limits the sample detecting to benzene using Tenax-TA adsorption tubes.
As can be seen that in the prior art, although detecting air for the sampling pipe for using Tenax-TA adsorbents to fill
Middle benzene has carried out certain research, but can not say it is sufficient for the control of adsorption tube temperature.
Citation 1:Zhu little Hong, Pan Hong etc.,;J], the adsorptivity of adsorbent Tenax-TA and activated carbon to benzene in air
It can compare, chemical building material, 05 phase in 2006;
Citation 2:He little Jun, Yang Yuhua etc.,;J], Tenax-TA adsorbents grinding to the absorption property of benzene at 35 DEG C
Study carefully, Guangdong building materials, the 8th phase in 2008;
Citation 3:He little Jun, Yang Yuhua etc.,;J], the benzene and TVOC in air are detected with Tenax-TA adsorbents
Technique study;
Citation 4:Patent application CN203101133U.
Invention content
Problems to be solved by the invention
For above the problems of in the prior art, the present invention provide it is a kind of can be under any environment temperature to air
The method that middle benzene and TVOC concentration are detected realizes primary sampling, once accurately obtains two analysis results of benzene and TVOC, carries
High working efficiency
In addition, the present invention also provides a kind of sampling apparatus suitable for the detection method, the sampling apparatus can
The temperature for sensitively controlling the adsorption tube makes it be held at 28 DEG C or less during the entire process of adsorption sampling.
The solution to the problem
The present invention solves above-mentioned technical problem using following technical scheme:
Present invention firstly provides the detection method of a kind of Indoor Air Benzene and total volatile organic compounds, including it is as follows
Step:
1) use adsorption tube carry out gas sampling, by temperature-adjusting device control the adsorption tube temperature be 28 DEG C with
Under, wherein the adsorbent filled in the adsorption tube includes the Tenax-TA adsorbents of 60~80 mesh;
2) by the adsorption tube in solution analyzer parsing, parsing gas is sent directly into chromatograph and is analyzed;
3) with peak area quantification, retention time is qualitative, area external standard method calculates separately benzene and total volatile organic compounds
Content.
According to above-described detection method, the temperature that the adsorption tube is controlled by the temperature-adjusting device is 20-
25℃。
According to above-described detection method, the temperature-adjusting device controls the range of temperature wave of the adsorption tube
It is dynamic to be no more than ± 2 DEG C, preferably more than ± 1 DEG C.
According to above-described detection method, the temperature-adjusting device includes insulating box, is installed in the insulating box
Surface temperature sensor, be installed on the insulating box lateral ends refrigerating plant and the other end heating device, the suction
Attached pipe is placed in the insulating box, and the surface temperature sensor is in contact with the outer wall of the adsorption tube.
Further include following steps according to above-described detection method:
Before sampling, first the adsorption tube is deposited in the insulating box, controlled at 28 DEG C or less;
After sampling, the adsorption tube is deposited in the insulating box, controlled at 28 DEG C or less.
According to above-described detection method, in step 1), the adsorbent mass filled in the adsorption tube is 200-
300mg, sampling volume 1-3L.
In addition, the present invention also provides a kind of sampling apparatus for above-described detection method, the sampling apparatus packet
It includes:
Adsorption tube, flowmeter, aspiration pump, control system, power supply, and
Temperature-adjusting device, the temperature-adjusting device includes insulating box, the surface temperature that is installed in the insulating box
Sensor, be installed on the insulating box lateral ends refrigerating plant and the other end heating device, the adsorption tube is placed in institute
It states in insulating box, the surface temperature sensor is in contact with the outer wall of the adsorption tube.
According to above-described sampling apparatus, the refrigerating plant includes cooling piece, cooling fin and fan, the cooling piece
Cold end be bonded with the insulating box lateral ends, the hot junction of the cooling piece is bonded with the cooling fin, and the fan is set to
The outer end of the cooling fin.
According to above-described sampling apparatus, the heating device includes heater, the heater and the insulating box
The other end in outside is bonded.
According to above-described sampling apparatus, holder is provided in the insulating box, the adsorption tube is fixed on the branch
On frame.
The effect of invention
The detection method and sampling apparatus of Indoor Air Benzene and TVOC provided by the present invention have following excellent effect
Fruit:
(1) detection method provided by the present invention, can control the adsorption tube by the temperature-adjusting device makes
Ambient temperature is overcome hereinafter, effectively prevent the generation of penetration phenomenon at 28 DEG C with tube body temperature whole in the process
Limitation to detection method;
(2) detection method can be realized simultaneously the sampling to benzene in air and TVOC, and to the rate of recovery of the two
All higher, testing result is accurate;
(3) sampling apparatus provided by the present invention can make adsorption tube in the whole process of sampling by temperature-adjusting device
Middle temperature all at 28 DEG C hereinafter, avoid ambient temperature short-time fluctuations or sorbing material it is short caused by exotherm
When temperature anomaly increase, temperature automatically controlled, intelligence degree is high;
(4) temperature-adjusting device of the sampling apparatus has insulating box and built-in surface temperature sensor, relatively close
It is sensitiveer that the isoperibol of envelope and the surface temperature sensor being in contact with absorption pipe outer wall so that temperature is adjusted.
Description of the drawings
Fig. 1 is the thermostatic structure chart of the sampling apparatus in the 2nd embodiment;
Fig. 2 is the overall schematic of the sampling apparatus in the 2nd embodiment;
1:Adsorption tube;2:Temperature-adjusting device;
21:Insulating box;22:Surface temperature sensor;
23:Refrigerating plant;231:Cooling piece;232:Cooling fin;233:Fan;
24:Heating device.
Specific implementation mode
Hereinafter, mode for carrying out the present invention will be described in detail.
<1st Shi Shifangshi >
Embodiments, provides the detections of a kind of Indoor Air Benzene and total volatile organic compounds the 1st by the present invention
Method, described method includes following steps:
1) adsorption tube 1 is used to carry out gas sampling, the temperature that the adsorption tube 1 is controlled by temperature-adjusting device 2 is 28
DEG C or less, wherein the adsorbent filled in the adsorption tube 1 includes the Tenax-TA adsorbents of 60~80 mesh;
2) by the adsorption tube 1 in solution analyzer parsing, parsing gas is sent directly into chromatograph and is analyzed;
3) with peak area quantification, retention time is qualitative, area external standard method calculates separately benzene and total volatile organic compounds
Content.
Detection method described above can be realized simultaneously the detection to benzene and TVOC, and the benzene content in being measured with TVOC replaces
The detection of benzene, i.e., only do the detection of benzene and TVOC the detection of TVOC, the result of benzene during the data of benzene are just directly detected by TVOC
It quotes.
Sampling
Solid absorbent sampling principle:Solid absorbent is belonged to the sampling of benzene and TVOC in existing national standards < specifications >
Concentration Sampling, sampling process are analyzed similar to the sample pre-treatments in chromatography.Air passes through absorption as a mixing sample
Column, oxygen, nitrogen and carbon dioxide flow out first since their adsorptivity is weak and content is high in air, a little group of some strong adsorptions
Fractionation is on the sorbent.When sampling starts, most components are all trapped in adsorbent inlet end in air, with being pumped through volume of air
Increase, each component adsorbed pushes ahead, since the absorption property of each component has differences, spaces out between each component,
The small component of some adsorptivities 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 1 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 1.
Safe sampling volume=(penetration volume (L/g)/1.5) × adsorbent weight (mg)." 1.5 " in formula are can
A safety coefficient of safe sampling volume is calculated under the environmental condition of variation.If environment temperature increases, this coefficient should increase
Greatly.That is, the variation of environment temperature influences significantly the adsorptivity of a certain substance in adsorbent.Moreover, adsorption tube 1
In adsorption sampling, since adsorbent has adsorbed the pernicious gases such as benzene and TVOC, the heating of itself is also resulted in, adsorbent is caused
The reduction of adsorption efficiency, the influence of the variation of 1 own temperature of adsorption tube to adsorbent absorption property also be can not ignore.
In detection method in present embodiment, the adsorption tube 1 sampling when can keep always temperature be 28 DEG C with
Under, by reducing the temperature of adsorption process, the absorption property of Tenax-TA is improved, penetrator when Tenax-TA absorption benzene is reduced
Product.It was found by the inventors of the present invention that the rate of recovery is increased with the reduction of 1 temperature of adsorption tube, but temperature reduces to a certain extent
Afterwards, the raised amplitude of the rate of recovery is not obvious, and is not further continued for reducing necessity of temperature, therefore, in order to further increase recycling
Rate, in some preferred embodiments of present embodiment, the temperature that the adsorption tube 1 is controlled by the temperature-adjusting device 2 is
20-25℃.Since the air inlet of the adsorption tube 1 needs sudden and violent leakage in air, environment temperature is inevitably to described
The temperature of adsorption tube 1 generates some adverse effects, simultaneously as in adsorption process, adsorption tube itself can discharge heat of adsorption, and
It may lead to the temporary unusual fluctuations of adsorption tube temperature in adsorption process, but due to temperature-adjusting device of the present invention
2 high sensitivities, therefore, the range of temperature fluctuation of adsorption tube 1 is no more than ± 2 DEG C in above-mentioned sampling process, preferably more than
± 1.5 DEG C, more preferably no more than ± 1.2 DEG C are further preferably no more than ± 1 DEG C, and such control is to adsorbing and detecting
Accuracy etc. be advantageous.That is, scheme according to the present invention, can not only control temperature when adsorbing efficient
In the operation interval of rate, and can ensure the adsorption tube 1 work when during the entire process of temperature be not in excessive wave
It is dynamic.
The detection method provided according to the present embodiment, before sampling after, can also include the following steps:Before sampling,
First the adsorption tube 1 is deposited in refrigerating box, controlled at 28 DEG C or less;After sampling, the adsorption tube 1 is deposited in cold
It hides in case, controlled at 28 DEG C or less.The purpose of above-mentioned steps is so that the control of 1 temperature of adsorption tube is at 28 DEG C hereinafter, can
To be timely applied in sample collection, and without being cooled down in advance to adsorption tube 1 by temperature-adjusting device 2, when avoiding waste
Between;It may need to wait for a period of time to adsorption tube 1 analyze after being acquired sample under sampling environment, will adsorb
Pipe 1 is stored in refrigerating box and is generated to collected sample hereinafter, avoiding because environment temperature changes controlled at 28 DEG C
Harmful effect ensure that the accuracy of subsequent analysis result.
For the adsorbent filled in adsorption tube 1, if adsorbent is too many, when parsing partial adsorbates agent cannot put pyrolysis into
In the heating zone of analyzer, parsing is incomplete;If adsorbent is very little, adsorption efficiency is too poor, and the rate of recovery is very low, therefore, this hair
In bright, the quality of the adsorbent loaded in adsorption tube 1 is 200-300mg.The rate of recovery of how many pairs of benzene of Tenax-TA adsorbents
It influences very big.If other conditions are the same, the rate of recovery of increasing with Tenax-TA adsorbents, benzene significantly increases.
This is because acquiring the process of benzene in air using Tenax-TA adsorbents, exactly benzene is in Tenax-TA fixed bed of sorbent
Adsorption-desorption process repeatedly.The benzene for being introduced into and being adsorbed in the Tenax-TA fixed bed of sorbent of 1 arrival end of adsorption tube, rear
Desorption is generated under the air driven of entrance, and absorption, suction repeatedly are then generated in next section of Tenax-TA fixed bed of sorbent
After echoing desorption, the benzene being introduced into is possible to be transferred to the gas outlet of adsorption tube 1 and be desorbed again, thus from adsorption tube
It is leaked out in 1, at this moment the rate of recovery of benzene is just not achieved 100%.When the benzene of leakage reaches 5%, just generation penetrates.Therefore, it is using
Tenax-TA adsorbents detect air in benzene when, can it is appropriate increase Tenax-TA adsorbents quality, to increase fixation
The length of bed extends and generates the time that benzene penetrates, to ensure the benzene concentration in accurate quantitative analysis air.
Identical in other sampling conditions for sampling volume, sampling volume is more than 3L, and the rate of recovery of benzene is apparent
Decline, sampling volume is less than 1L, then testing result accuracy is not high, and therefore, the sampling volume in the present invention is 1-3L.
For sampling flow velocity, when sampling volume is identical, sampling flow velocity increases, and the rate of recovery of benzene is declined slightly, but influences
Unobvious.In the benzene in using the 1 accurate quantitative analysis air of adsorption tube, can not consider, therefore, in present embodiment
Sampling flow velocity general control is 0.1-1.5L/min, preferably 0.2L/min.
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 1 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.
<2nd Shi Shifangshi >
Embodiments, provides a kind of sampling apparatus for the detection method being used for the 1st embodiment, institutes the 2nd by the present invention
Stating sampling apparatus includes:
Adsorption tube 1, flowmeter, aspiration pump, control system, power supply, and
Temperature-adjusting device 2, the temperature-adjusting device 2 include insulating box 21, the table being installed in the insulating box 21
The heating device 24 of face temperature sensor 22, the refrigerating plant 23 for being installed on 21 lateral ends of the insulating box and the other end, institute
It states adsorption tube 1 to be placed in the insulating box 21, the surface temperature sensor 22 is in contact with the outer wall of the adsorption tube 1.
It is appreciated that the detection device of present embodiment, wherein the control system and flowmeter, steam extraction pump, power supply,
The equal components connection of temperature-adjusting device 2, controls the size of flow by control system, steam extraction pump, surface temperature sensor 22,
The unlatching of refrigerating plant 23 and heating device 24 is closed, to realize the sampling apparatus constant-temperature constant-current function.
Tenax-TA adsorbents are showed to the adsorption effect function well of total volatile organism, but to the suction-operated of benzene
To increase with the temperature from low temperature to high temperature, suction-operated reduces rapidly, such as, it is generally the case that when use contains
The adsorption tube 1 of Tenax-TA adsorbents when general room temperature samples, can there are the following problems, summer using or temperature compared with
High area is in use, easy higher than the 28 DEG C temperature high in this way of indoor temperature cause benzene to penetrate readily through adsorption tube 1 and largely flow
It loses so that test result is relatively low.In addition, the adsorbent containing Tenax-TA is in use, adsorbent is due to having adsorbed benzene
Or other pernicious gases and lead to the heating of itself, in use but also itself temperature increase and lead to absorption property
Decline, to cause the distortion of test result.It therefore, can be to inhaling after using preceding or use although in certain tests
Attached pipe 1 carries out cooling processing, but these measures are it is difficult to ensure that adsorption tube 1 can keep efficient suction in the overall process used
Authenticity that is attached, ensureing test result.Therefore, based on the considerations of further increasing testing result accuracy, in present embodiment
It is preferred that during the use of adsorption tube 1, temperature that the adsorption tube 1 is controlled by the temperature-adjusting device 2 be 28 DEG C with
Down, it is preferable to use the temperature of adsorption tube 1 is controlled in 20-25 DEG C by temperature-adjusting device 2 always.
Temperature-adjusting device 2
The present invention controls temperature of the adsorption tube 1 in sampling process using temperature-adjusting device 2.When sampling, the suction
Attached pipe 1 is placed in the insulating box 21 of the temperature-adjusting device 2, and the refrigerating plant 23 and the heating device 24 are according to environment
Temperature and the detection temperature of setting judge whether work, and the uniform constant temperature of temperature is formed in the insulating box 21 of relative closure
Area is suitble to sampling operation steady in a long-term.
Difference lies in the present invention uses surface temperature sensor to the present invention with sensor installation position in citation 3
22, so that the surface temperature sensor 22 and the outer wall of the adsorption tube 1 is in direct contact, can more accurately obtain adsorption tube in this way
The temperature change of adsorbent in 1, sensitivity higher instruct refrigerating plant 23 or heating device 24 to work in time so that adsorption tube 1
Range of temperature fluctuate smaller, range of temperature fluctuation is no more than ± 2 DEG C, preferably more than ± 1.5 DEG C, more excellent
Choosing is no more than ± 1.2 DEG C, is further preferably no more than ± 1 DEG C.And the sensor in citation 3 is then arranged in absorption bottle branch
On frame, for monitoring the environment inside constant temperature unit, if the temperature sensor in the present invention is also disposed at 21 inner wall of insulating box
On the upper or holder of adsorption tube 1, the accuracy and sensitivity of temperature monitoring may be influenced.
Specifically, Fig. 1 is a kind of structure chart of sampling apparatus in present embodiment, the refrigerating plant 23 includes refrigeration
Piece 231, cooling fin 232 and fan 233, the cold end of the cooling piece 231 are bonded with 21 lateral ends of the insulating box, the system
Cold 231 hot junction is bonded with the cooling fin 232, and the fan 233 is set to the outer end of the cooling fin 232.The heating
Device 24 includes heater, and the heater is bonded with the other end in 21 outside of the insulating box.Fig. 2 is in present embodiment
A kind of overall schematic of sampling apparatus.The sampling apparatus has control panel, selects the sampling configuration on control panel, then
Start to sample according to parameters, starting switches such as required test condition setting sample temperature, flow, sampling times.
After setting sample temperature by control system, control system can be according to the judgement of the environment temperature of current detection
It is no to need to heat or freeze to insulating box 21, when the temperature for the adsorption tube 1 that surface temperature sensor 22 detects is higher than setting temperature
When spending, refrigerating plant 23 can start work, and the cold junction temperature of cooling piece 231 reduces at this time, can be with by the transmission of insulating box 21
The temperature of adsorption tube 1 is set to reduce, 231 hot junction of cooling piece then transfers heat to cooling fin 232 at this time, passes through the work of fan 233
Make, the heat that cooling fin 232 sheds is discharged to the outside of sampling apparatus;When the adsorption tube that surface temperature sensor 22 detects
When 1 temperature is less than set temperature, control system can control heater work, and heater transfers heat to insulating box 21, from
And adsorption tube 1 is heated, when the temperature for the adsorption tube 1 that surface temperature sensor 22 detects is higher than set temperature, control system
System can control heater and be stopped.
The insulating box 21 can also be used as refrigerating box.Before sampling, the adsorption tube 1 is first deposited in into the constant temperature
In case 21, controlled at 28 DEG C or less;After sampling, the adsorption tube 1 is deposited in the insulating box 21, controlled at
28 DEG C or less.Further, the temperature range that temperature-adjusting device 2 of the invention can regulate and control be not limited to 28 DEG C hereinafter, than
The range to 100-150 DEG C can also such as be regulated and controled, in the case where lacking the professional activation equipment of adsorption tube 1, this embodiment party
Sampling apparatus in formula, which is connected on nitrogen cylinder, can serve as easily activating device use.
Holder is also provided in insulating box 21, the adsorption tube 1 is fixed on the bracket, and multiple adsorption tubes are avoided
It is in contact between 1.
Adsorption tube 1
The tube body of adsorption tube 1 in present embodiment is stainless steel tube or glass tube, in view of the heat conductivility of stainless steel tube
It is better, be conducive to fast cooling, it is therefore preferable that using stainless steel tube.
The adsorption tube 1 has the mark of airintake direction, attachment device when facilitating acquisition gas, such as in adsorption tube 1
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.Set gradually stainless steel mesh screen, Tenax-TA adsorbents inside adsorption tube 1, in pipe, stainless steel mesh screen is in order to avoid adopting
Air-flow drives the nozzle of adsorbent blocking adsorption tube 1 when collecting sample.
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) length is 150mm, and outer diameter 6.35mm, thickness is the stainless steel adsorption tube 1 of 1.0mm, is filled with 200mg 60
The Tenax-TA adsorbents of~80 mesh are clean to no miscellaneous peak by adsorption tube activation;
(2) it is 1m in volume3Environmental testing storehouse in discharge known concentration stupid and total volatile organism gas, environment
Air pressure in survey formula storehouse is 101.50kPa, and relative humidity 70.5%, environment temperature is 35 DEG C,
The sampling apparatus provided using the 2nd embodiment is sampled, and following sampling parameter is arranged:Sample temperature is 28
DEG C, sampling flow velocity is 0.2L/min, sampling time 10min;
(3) after sampling, adsorption tube 1 is parsed in 300 DEG C of pyrolysis analyzer, parsing gas is sent directly into gas phase
Chromatograph carries out chromatography;
(4) with peak area quantification, retention time is qualitative, area external standard method calculates separately benzene and total volatile organic compounds
Content, calculate the rate of recovery.
Embodiment 2
In addition to sample temperature is 25 DEG C, other conditions are same as Example 1.
Embodiment 3
In addition to sample temperature is 20 DEG C, other conditions are same as Example 1.
Embodiment 4
In addition to sample temperature is 10 DEG C, other conditions are same as Example 1.
Comparative example 1
Environment temperature in environmental testing storehouse is 35 DEG C, and adsorption tube 1 is controlled without using the function of temperature control of sampling apparatus
Temperature makes adsorption tube 1 carry out the process of adsorption sampling naturally under the environment temperature in environmental testing storehouse, other conditions with implementation
Example 1 is identical.
Comparative example 2
Environment temperature in environmental testing storehouse is 30 DEG C, and adsorption tube 1 is controlled without using the function of temperature control of sampling apparatus
Temperature makes adsorption tube 1 carry out the process of adsorption sampling naturally under the environment temperature in environmental testing storehouse, other conditions with implementation
Example 1 is identical.
Comparative example 3
Environment temperature in environmental testing storehouse is 25 DEG C, and adsorption tube 1 is controlled without using the function of temperature control of sampling apparatus
Temperature makes adsorption tube 1 carry out the process of adsorption sampling naturally under the environment temperature in environmental testing storehouse, other conditions with implementation
Example 1 is identical.
Rate of recovery test method
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).
The data of embodiment 1-4 and comparative example the 1-3 rate of recovery measured are listed in table 1-7 respectively.
The rate of recovery of adsorption tube 1 in 1 embodiment 1 of table
The rate of recovery that the rate of recovery for the benzene being calculated is 95.2%, TVOC is 96.3%.
The rate of recovery of adsorption tube 1 in 2 embodiment 2 of table
The rate of recovery that the rate of recovery for the benzene being calculated is 98.6%, TVOC is 99.5%.
The rate of recovery of adsorption tube 1 in 3 embodiment 3 of table
The rate of recovery that the rate of recovery for the benzene being calculated is 99.8%, TVOC is 100.0%.
The rate of recovery of adsorption tube 1 in 4 embodiment 4 of table
The rate of recovery that the rate of recovery for the benzene being calculated is 99.9%, TVOC is 100.2%.
The rate of recovery of adsorption tube 1 in 5 comparative example 1 of table
The rate of recovery that the rate of recovery for the benzene being calculated is 81.3%, TVOC is 89.6%.
The rate of recovery of adsorption tube 1 in 6 comparative example 2 of table
The rate of recovery that the rate of recovery for the benzene being calculated is 86.8%, TVOC is 92.6%.
The rate of recovery of adsorption tube 1 in 7 comparative example 3 of table
The rate of recovery that the rate of recovery for the benzene being calculated is 97.7%, TVOC is 98.4%.
The temperature for controlling the adsorption tube 1 by temperature-adjusting device 2 it can be seen from the test result of table 1-4 is 28
DEG C hereinafter, adsorption tube 1 is higher to the rate of recovery of benzene and TVOC.With the reduction of temperature, the rate of recovery of benzene and TVOC are gradual
Rise.Therefore, detection method of the invention is suitable for when summer temperature is high or high temperature area is to benzene in air and TVOC concentration
Accurate measurement.
In table 5 and table 6, comparative example 1 and 2 carries out adsorption sampling under the environment temperature in environmental testing storehouse, does not use temperature
Degree regulating device 2 controls the temperature of adsorption tube 1, and test result indicates, adsorption tube 1 is equal to the rate of recovery of benzene and TVOC
Less than 95%, illustrates that adsorption tube 1 has occurred and that at this time and penetrate.
In table 7, comparative example 3 also carries out adsorption sampling under the environment temperature in environmental testing storehouse, is adjusted without temperature in use
Device 2 controls the temperature of adsorption tube 1, and adsorption tube 1 is also higher to the adsorption rate of benzene and TVOC, and there is no penetrate.
But compare comparative example 3 with embodiment 2, the rate of recovery of comparative example 3 is still less than the rate of recovery of embodiment 2, and explanation does not use
The result accuracy that the mode that temperature-adjusting device 2 controls the temperature of adsorption tube 1 measures is relatively low.
Industrial availability
Since the adsorption tube and its detection method of the present invention can simultaneously be detected benzene and TVOC, reduce workload
And cost, easy to operate, the rate of recovery is high.
Claims (10)
1. the detection method of a kind of Indoor Air Benzene and total volatile organic compounds, which is characterized in that include the following steps:
1) use adsorption tube carry out gas sampling, by temperature-adjusting device control the adsorption tube temperature be 28 DEG C hereinafter,
Wherein, the adsorbent filled in the adsorption tube includes the Tenax-TA adsorbents of 60~80 mesh;
2) by the adsorption tube in solution analyzer parsing, parsing gas is sent directly into chromatograph and is analyzed;
3) with peak area quantification, retention time is qualitative, area external standard method calculates separately benzene and total volatile organic compounds contains
Amount.
2. detection method according to claim 1, which is characterized in that control the absorption by the temperature-adjusting device
The temperature of pipe is 20-25 DEG C.
3. detection method according to claim 1 or 2, which is characterized in that the temperature-adjusting device controls the absorption
The range of temperature fluctuation of pipe is no more than ± 2 DEG C, preferably more than ± 1 DEG C.
4. according to claim 1-3 any one of them detection methods, which is characterized in that the temperature-adjusting device includes constant temperature
Case, the surface temperature sensor being installed in the insulating box, the refrigerating plant for being installed on the insulating box lateral ends and another
The heating device of one end, the adsorption tube are placed in the insulating box, and the surface temperature sensor is outer with the adsorption tube
Wall is in contact.
5. detection method according to claim 4, which is characterized in that further include following steps:
Before sampling, first the adsorption tube is deposited in the insulating box, controlled at 28 DEG C or less;
After sampling, the adsorption tube is deposited in the insulating box, controlled at 28 DEG C or less.
6. according to claim 1-5 any one of them detection methods, which is characterized in that in step 1), filled out in the adsorption tube
The adsorbent mass filled is 200-300mg, sampling volume 1-3L.
7. a kind of sampling apparatus for claim 1-6 any one of them detection methods, which is characterized in that the sampling cartridge
Set including:
Adsorption tube, flowmeter, aspiration pump, control system, power supply, and
Temperature-adjusting device, the temperature-adjusting device includes insulating box, the surface temperature sensing that is installed in the insulating box
Device, be installed on the insulating box lateral ends refrigerating plant and the other end heating device, the adsorption tube is placed in the perseverance
In incubator, the surface temperature sensor is in contact with the outer wall of the adsorption tube.
8. sampling apparatus according to claim 7, which is characterized in that the refrigerating plant include cooling piece, cooling fin and
Fan, the cold end of the cooling piece are bonded with the insulating box lateral ends, and the hot junction of the cooling piece is pasted with the cooling fin
It closes, the fan is set to the outer end of the cooling fin.
9. sampling apparatus according to claim 7 or 8, which is characterized in that the heating device includes heater, described to add
Hot device is bonded with the other end on the outside of the insulating box.
10. according to claim 7-9 any one of them sampling apparatuses, which is characterized in that it is provided with holder in the insulating box,
The adsorption tube is fixed on the bracket.
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