CN105259014B - A kind of measurement method of VOCs solution and the preparation method of calibrating gas - Google Patents
A kind of measurement method of VOCs solution and the preparation method of calibrating gas Download PDFInfo
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- CN105259014B CN105259014B CN201510742198.5A CN201510742198A CN105259014B CN 105259014 B CN105259014 B CN 105259014B CN 201510742198 A CN201510742198 A CN 201510742198A CN 105259014 B CN105259014 B CN 105259014B
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Abstract
The present invention provides a kind of measurement methods of VOCs solution, and the measurement method is accurate and reliable, and error is small；The present invention also provides a kind of preparation methods of calibrating gas, equipment required for this method is simple, formulation operations are easy, based on quality base, it only needs to weigh the first total quality and filter paper of filter paper and centrifuge tube, the second total quality of centrifuge tube and the VOCs solution being added, then subtracts each other the two, just the exact mass of VOCs solution being added has been obtained, the use of filter paper can guarantee the quick abundant transfer of VOCs solution and avoid the unnecessary flowing of VOCs solution；In step S5, when VOCs solution is stood after a certain period of time under predetermined temperature in flexible container, gross mass of the VOCs by the standard gas concentration in the carrier gas for sufficiently volatilizing and being dispersed in the predetermined volume, obtained equal to VOCs solution is multiplied by the mass concentration of contained VOCs again divided by the predetermined volume of carrier gas.
Description
Technical field
The invention belongs to the preparation technique fields of the measurement of VOCs gas and calibrating gas, more particularly, to a kind of VOCs gas
The measurement method of body and the preparation method of calibrating gas.
Background technique
Standard substance is a kind of substance or material for having determined that and having one or more sufficiently uniform characteristic values, is
" measurer " in analysis measurement industry, that is, standard substance is a kind of measurement criteria of measurement of species ingredient or characteristic, be can be used in
Calibration or identification measuring instrument, evaluation measurement process and quality control, to guarantee the one of different time or space measurement result
Cause property.Wherein, volatile organic compounds (volatile organic compounds, VOCs) calibrating gas is commonly to mark
One of quasi- substance, to guarantee the analysis instruments detected values such as the quick detection device of VOCs, gas chromatograph-mass spectrometer, high performance liquid chromatograph
Accuracy, validity.
Currently, the air distributing method of gas reference material (i.e. calibrating gas) is generally divided into Devince By Dynamic Gas Ration Method and static volumetric method
Two kinds.
Devince By Dynamic Gas Ration Method is that the unstripped gas of known concentration and carrier gas is made by constant ratio continuously to enter mixer
Mixing, so as to continuously prepare and supply certain density calibrating gas, can count according to the flow-rate ratio of two strands of air-flows
Extension rate is calculated, the concentration of calibrating gas is calculated according to extension rate.It is larger that this method is suitable for calibrating gas dosage
Or the longer experimental work of duration of ventilation, it is particularly suitable for preparing the calibrating gas of low concentration, but its instrument equipment is matched
It makes cumbersome, air distribution system volume is big, operating process is complicated, needs a large amount of manpower and material resources, and be not suitable for the mark of compounding high concentration
Quasi- gas.
Static volumetric method is a certain amount of unstripped gas to be added in the container of known volume, is re-filled with carrier gas and mixes system
?.The concentration of calibrating gas is calculated according to amount and vessel volume that unstripped gas and carrier gas is added.Static volumetric method it is excellent
Point is that device therefor is simple, operation is easy, but chamber wall has certain suction-operated, will cause prepare gas concentration inaccuracy or its
Concentration changes with standing time, especially preparation low concentration calibrating gas, often causes biggish error.For common high pressure
Steel cylinder static volumetric method matches gas cylinder static volumetric method, and there is also calibrating gas transport inconvenience, is unfavorable for carrying out different experiments room
Between comparison the problems such as.It, can be in the occasion for preparing a small amount of calibrating gas in order to solve the transportation problem of calibrating gas
Using syringe static volumetric method, a certain amount of unstripped gas first is drawn with syringe, then can be obtained through repeatedly dilution certain dense
The calibrating gas of degree.
For VOCs calibrating gas, it is frequently used for the less occasion of disposable dosage, as examined between different experiments room
The links such as comparison, sampling efficiency evaluation, Specification Curve of Increasing, analysis instrument calibration and the quality control of survey method, therefore
It is suitble to prepare using syringe static volumetric method.However, due to benzene, toluene, ethylbenzene, dimethylbenzene, styrene, acetaldehyde, propylene
The common VOCs such as aldehyde is the liquid of highly volatile at room temperature, can be due to when being drawn with syringe or released a small amount of above-mentioned substance
Uncontrollable volatilization loss or adsorption and generate large error, concentration consistency is poor.
Summary of the invention
In view of this, the present invention is directed to propose a kind of measurement method of VOCs solution and the preparation method of calibrating gas, with
Error is big, consistency is poor when solving the problems, such as to measure VOCs solution, can it is easy, quick, accurately prepare certain concentration
VOCs calibrating gas.
In order to achieve the above objectives, the technical scheme of the present invention is realized as follows:
A kind of measurement method of VOCs solution, this method use filter paper as the carrier for absorbing and releasing VOCs, measured
Filter paper is placed in closed transfer vessel the first total quality for weighing filter paper and transfer vessel by Cheng Zhongxian, is absorbed to filter paper pre-
Determine the second total quality for weighing filter paper and transfer vessel after the VOCs solution of quality again, the second total quality and the first whole matter
The difference of amount is the quality of the VOCs solution measured.
The measurement method of VOCs solution provided by the invention only needs to weigh the first total quality of filter paper and transfer vessel,
And the second total quality of filter paper, transfer vessel and the VOCs solution being added, then the two is subtracted each other, has just been obtained added
The use of the exact mass of the VOCs solution entered, filter paper can guarantee the quick abundant transfer of VOCs solution, and be avoided that VOCs
The unnecessary flowing of solution；When this measurement method can also avoid drawing in traditional syringe static volumetric method or releasing VOCs
The large error generated due to uncontrollable volatilization loss or adsorption.
The present invention also provides a kind of preparation methods of calibrating gas, include the following steps:
S1: preparing the VOCs solution of predetermined concentration or gets out the VOCs solution of predetermined concentration；
S2: filter paper is placed in transfer vessel, is weighed and is recorded the first total quality；
S3: the VOCs solution of predetermined amount is injected into the transfer vessel, will be predetermined amount of to the filter paper
VOCs solution covers tightly rapidly after sufficiently adsorbing and seals the transfer vessel, weighs and records the second total quality；
S4: the transfer vessel being sealed is put into flexible container, evacuates the air in the flexible container, and with dilution
Gas cleans several times；
S5: after injecting the carrier gas of predetermined volume in the flexible container, the sealing cover of the transfer vessel being opened,
And the predetermined time is stood at a predetermined temperature together with the flexible container, to obtain required calibrating gas；
Wherein step S1, S2 sequence interchangeable.
Flexible container is for convenience of in the container for opening the sealing cover of the transfer vessel in it across flexible container.
Preferably, flexible container is plastics sampler bag.
Further, the storage container for the VOCs solution for filling predetermined concentration is placed in ice-water bath in step S1.
Transfer vessel is for convenience of in the container for opening the sealing cover of transfer vessel in flexible container across flexible container.
Preferably, the transfer vessel is centrifuge tube.
Further, in step S1 in the VOCs solution of predetermined concentration, containing one or more VOC components, and every kind of group
The predetermined concentration divided is known.
Further, filter paper described in step S2 is the filter paper that adsorption capacity is relatively strong and VOC free s itself is distributed.
Preferably, the predetermined amount of VOCs solution described in step S3 is 0.01mL-1mL.
Preferably, the carrier gas is one of nitrogen, helium or air of cleaning or a variety of.
Further, it in step S4, is cleaned with carrier gas and is specifically included several times:
A certain amount of carrier gas is injected into the flexible container, is then vacuumized, such repeated several times, with sufficiently clear
Wash the flexible container.
Preferably, the predetermined volume of the carrier gas is 1.5L-3000L.
Preferably, the predetermined temperature is 23 DEG C -65 DEG C.
Preferably, the predetermined time that the flexible container is stood at a predetermined temperature is 5min-16h.
The present invention also provides a kind of verification method of calibrating gas, this method uses gas chromatograph-mass spectrometer and high performance liquid chromatography
Method verifies the calibrating gas.
Compared with the existing technology, the preparation method of calibrating gas of the present invention has the advantage that
(1) it is based on quality base, it is only necessary to weigh filter paper and the first total quality and filter paper of transfer vessel, transfer
Second total quality of container and the VOCs solution being added, then subtracts each other the two, has just obtained the VOCs solution being added
Exact mass, filter paper use can guarantee VOCs solution it is quick it is abundant transfer and avoid its unnecessary flowing；Step
In S5, the volume of the carrier gas injected into flexible container be it is known, when VOCs solution stands pre- timing at a predetermined temperature
Between after, thus VOCs has just obtained required calibrating gas in the carrier gas for sufficiently volatilizing and being dispersed in the predetermined volume,
Concentration be equal to VOCs solution gross mass multiplied by the mass concentration of contained VOCs again divided by the predetermined volume of carrier gas；
(2) compared with the existing technology in calibrating gas preparation method, set required for preparation method provided by the invention
Standby simple, formulation operations are easy, the transfer vessel convenient transportation by taking centrifuge tube as an example, and centrifuge tube internal surface area is smaller, can subtract
The absorption of few chamber wall, standard gas concentration are obtained by the quality of VOCs divided by the predetermined volume of carrier gas, thus accurate and can
Arbitrarily to regulate and control, the preparation steps for solving traditional air distributing method are cumbersome, air distribution system volume is big, operating process is longer, not really
Surely the problems such as assessment process spent is complicated, great practical value.
Detailed description of the invention
The attached drawing for constituting a part of the invention is used to provide further understanding of the present invention, schematic reality of the invention
It applies example and its explanation is used to explain the present invention, do not constitute improper limitations of the present invention, for those of ordinary skill in the art
For, without creative efforts, it is also possible to obtain other drawings based on these drawings.In the accompanying drawings:
Fig. 1 is the operating process schematic diagram of the preparation method of calibrating gas described in the embodiment of the present invention.
Description of symbols:
1- ice-water bath, 2- storage container, 3- transfer vessel, 4- filter paper, the first valve of 5-, the second valve of 6-, 7- flexibility are held
Device, 8- temperature adjusting cabin.
Specific embodiment
It should be noted that in the absence of conflict, the feature in embodiment and embodiment in the present invention can phase
Mutually combination.
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation description.Obviously, described embodiment is only a part of the embodiments of the present invention, instead of all the embodiments.Base
Embodiment in the present invention, those of ordinary skill in the art are obtained all without making creative work
Other embodiments shall fall within the protection scope of the present invention.
The embodiment of the present invention provides a kind of measurement method of VOCs solution, and this method uses filter paper as absorbing and releasing
Filter paper is first placed in closed transfer vessel during measuring and weighs the first entirety of filter paper and transfer vessel by the carrier of VOCs
Quality m0, weigh the second total quality m of filter paper and transfer vessel again after filter paper absorbs the VOCs solution of predetermined quality1, measure
VOCs solution quality be the second total quality m1Subtract the first total quality m0That is (m1-m0), by the gross mass of VOCs solution
And the mass concentration C of every kind of VOC componentiIt can be obtained the quality (m of every kind of VOC component of measurement1-m0)Ci。
The embodiment of the invention provides a kind of preparation methods of calibrating gas, as shown in Figure 1, comprising steps of
S1, the VOCs solution for preparing predetermined concentration or the VOCs solution for getting out predetermined concentration；
S2, filter paper is placed in transfer vessel 3, weighs and records the first total quality；
S3, the VOCs solution of predetermined amount is injected into transfer vessel 3, sufficiently inhales the VOCs solution of predetermined amount to filter paper
Attached cover tightly rapidly seals transfer vessel 3, weighs and records the second total quality；
S4, the transfer vessel 3 being sealed is put into flexible container 7, evacuate flexible container 7 in air, and with dilute
Gas cleans several times；
S5, after injecting the carrier gas of predetermined volume in flexible container 7, the sealing cover of transfer vessel 3 is opened, and with soft
Property container 7, which is placed in together in temperature adjusting cabin 8, stands the predetermined time, to obtain required calibrating gas；Wherein step S1, S2 is suitable
Sequence interchangeable.
Transfer vessel 3 is centrifuge tube in the present embodiment, and the storage that the VOCs solution of predetermined concentration will be filled in step S1 is held
Device 2 is placed in ice-water bath 1, and flexible container 7 is plastics sampler bag, and the solvent in the present embodiment in step S1 in VOCs solution is first
Alcohol or acetonitrile or other, filter paper select Whatman filter paper.
Specifically, in above-mentioned steps S1, in the VOCs solution of the predetermined concentration, containing one or more VOC components, and
The predetermined quality concentration C of every kind of componentiIt is known.
In step sl, as shown in Figure 1, the container 2 for filling VOCs solution is placed in ice-water bath 1, to reduce the step
The volatilization loss of middle VOCs solution, to guarantee the accuracy of institute's preparing calibrating gas concentration as far as possible.
In step S2, filter paper 4 is placed in transfer vessel 3 i.e. centrifuge tube, weigh and records the first total quality m0, i.e.,
The gross mass of (filter paper 4+ transfer vessel 3).
In step S2, used filter paper should be the filter paper that adsorption capacity is relatively strong and VOC free s itself is distributed, to guarantee
Quick, the abundant absorption of VOCs solution, to reduce the solution loss in transfer process and avoid VOCs solution in use process
Unnecessary flowing.
In step S3, the predetermined amount (volume of the VOCs solution injected into transfer vessel 3) can be 0.01mL-
1mL, preferably 0.01mL, 0.02mL, 0.05mL, 0.1mL, 0.5mL, 1mL, the volume usually can be adjusted arbitrarily, so as to
The concentration of calibrating gas needed for any regulation.
It should be noted that in step S3, when pipettors such as syringe, microsyringe, pipette or adjustable pipettes
After VOCs solution in tool (being not shown) contacts about 2s with the filter paper 4 in transfer vessel 3, filter paper 4 can be by pipettor
VOCs solution in tool all adsorbs, at this point, should take away liquid relief utensil rapidly and seal transfer vessel 3.It weighs and records second
Total quality m1, i.e. the gross mass of (the VOCs solution of filter paper 4+ transfer vessel 3+ predetermined amount).
In step S4, described cleaned with carrier gas such as nitrogen, helium or pure airs specifically includes several times:
A certain amount of carrier gas is injected into flexible container 7, is then vacuumized, such repeated several times, sufficiently to clean
Flexible container 7.The step focuses on, and cleans original air in discharge flexible container 7, sufficiently using carrier gas to avoid system
Contain impurity air in standby calibrating gas, to guarantee the high-purity of prepared calibrating gas.
Specifically, in the present embodiment step S4:
The transfer vessel 3 being sealed is put into the flexible container 7 i.e. plastics sampler bag of 50L, flexible container 7 is carried out clearly
It washes, flexible container 7 is equipped with the first valve 5 and the second valve 6, as shown in Figure 1.By the first valve 5 to soft in the present embodiment
Property container 7 in inject and 25L nitrogen and close the first valve 5 immediately.Flexible container 7 is vacuumized by the second valve 6 again,
In triplicate, to sufficiently clean flexible container 7.
In step S5, the predetermined volume V of the carrier gas injected into flexible container 7 can be 1.5L-3000L, preferably
For 25L, 100L, 500L, 1000L.The volume usually can arbitrarily be adjusted according to the size and experiment demand of flexible container 7, with
Just any concentration for adjusting required calibrating gas.
In step S5, the temperature in temperature adjusting cabin 8 is usually 23 DEG C -65 DEG C, and the predetermined time is usually 5min-16h,
To guarantee that VOC solution is sufficiently volatilized and is dispersed in the carrier gas of predetermined volume, to obtain the VOC calibrating gas of high quality.
Specifically, the temperature in temperature adjusting cabin 8 can be 60 DEG C, and the predetermined time of standing can be 1h.
In this way, in temperature adjusting cabin 8, VOCs solution volatilize completely after to get the VOCs calibrating gas for arriving certain concentration,
Wherein the mass concentration of every kind of VOC isTransfer process and volatilization process after weighing quality due to VOCs solution
It all carries out in a sealed container, thus the volatilization loss in operating process can be effectively reduced and prepare error.
It should be noted that used equipment, container, solution are conventional laboratory apparatus in the embodiment of the present invention
Or consumptive material, it can be obtained by commercially available mode, can also be made by oneself and be obtained by those skilled in the art, the present invention sets these
Standby, container, the design parameter of solution or other situations are not described in detail.
Equipment required for preparation method provided by the invention is simple, and formulation operations are easy, the flexibility by taking centrifuge tube as an example
Container traffic is convenient, and centrifuge tube internal surface area is smaller, can reduce the absorption of chamber wall, standard gas concentration is by VOCs solution
Then gross mass is obtained divided by the predetermined volume of carrier gas multiplied by the mass concentration of contained VOCs, thus accurate and can arbitrarily adjust
Control, the preparation steps for solving traditional air distributing method are cumbersome, air distribution system volume is big, operating process is longer, uncertainty comment
The problems such as valence program is complicated, great practical value.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, any to be familiar with this technology
In the technical scope disclosed by the present invention, any changes or substitutions that can be easily thought of by the technical staff in field, should all cover in this hair
Within bright protection scope.All within the spirits and principles of the present invention, any modification, equivalent replacement, improvement and so on,
It should be included within protection scope of the present invention.
Claims (11)
1. a kind of preparation method of calibrating gas, characterized by the following steps:
S1: preparing the VOCs solution of predetermined concentration or gets out the VOCs solution of predetermined concentration；
S2: filter paper is placed in transfer vessel, is weighed and is recorded the first total quality；
S3: the VOCs solution of predetermined amount is injected into the transfer vessel, to the filter paper that predetermined amount of VOCs is molten
Liquid covers tightly rapidly after sufficiently adsorbing and seals the transfer vessel, weighs and records the second total quality；
S4: the transfer vessel being sealed is put into flexible container, evacuates the air in the flexible container, and clear with carrier gas
It washes several times, the transfer vessel is for convenience of in the appearance for opening the sealing cover of transfer vessel in flexible container across flexible container
Device；
S5: after injecting the carrier gas of predetermined volume in the flexible container, the sealing cover of the transfer vessel is opened, and same
The flexible container stands the predetermined time together at a predetermined temperature, to obtain required calibrating gas；
Wherein step S1, S2 sequence interchangeable.
2. the preparation method of calibrating gas according to claim 1, it is characterised in that: predetermined concentration will be filled in step S1
The storage container of VOCs solution be placed in ice-water bath.
3. the preparation method of calibrating gas according to claim 1, it is characterised in that: the transfer vessel is centrifuge tube.
4. the preparation method of calibrating gas according to claim 1, it is characterised in that: the flexible container for convenience of in every
The flexible container container of opening the sealing cover of the transfer vessel in it.
5. the preparation method of calibrating gas according to claim 4, it is characterised in that: the flexible container is plastics sampling
Bag.
6. the preparation method of calibrating gas according to claim 1, it is characterised in that: the VOCs of predetermined concentration in step S1
In solution, containing one or more VOC components, and the predetermined concentration of every kind of VOC component is known.
7. the preparation method of calibrating gas according to claim 1, it is characterised in that: filter paper described in step S2 is absorption
The filter paper that ability is relatively strong and VOC free s itself is distributed.
8. the preparation method of calibrating gas according to claim 1, it is characterised in that: VOCs solution described in step S3
Predetermined amount is 0.01mL-1mL.
9. the preparation method of calibrating gas according to claim 1, it is characterised in that: the predetermined volume of the carrier gas is
1.5L-3000L。
10. the preparation method of calibrating gas according to claim 1, it is characterised in that: the predetermined temperature is 23 DEG C -65
℃。
11. the preparation method of calibrating gas according to claim 1, it is characterised in that: the flexible container is in predetermined temperature
The degree lower predetermined time stood is 5min-16h.
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| CN106955617B (en) * | 2017-04-07 | 2022-09-13 | 长沙湘智离心机仪器有限公司 | RC-12 automatic counterweight liquid adding instrument |
| CN107843473A (en) * | 2017-12-07 | 2018-03-27 | 中国计量科学研究院 | Multicomponent volatile organic matter gravimetric method gas distribution device and air distributing method |
| CN108333077A (en) * | 2018-02-08 | 2018-07-27 | 北京市临床检验中心 | A method of measuring fluid density |
| CN108889149B (en) * | 2018-07-04 | 2020-04-21 | 中国汽车技术研究中心有限公司 | Standard gas configuration method for training odor evaluation personnel |
| CN114264535A (en) * | 2021-11-29 | 2022-04-01 | 曼哈格检测技术股份有限公司 | Method for preparing solution of volatile solute |
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| CN102539202A (en) * | 2010-12-30 | 2012-07-04 | 深圳光启高等理工研究院 | Preparation method for ethyl nitrite standard gas |
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| CN102553468A (en) * | 2010-12-30 | 2012-07-11 | 深圳光启高等理工研究院 | Preparation method for ethyl nitrite standard air |
| JP2013205298A (en) * | 2012-03-29 | 2013-10-07 | Sumitomo Seika Chem Co Ltd | Device and method for filling raw material for standard gas |
| KR101341762B1 (en) * | 2012-05-17 | 2013-12-16 | 한국표준과학연구원 | The apparatus and method for elemental analysis of the sample gas using liquids reference gas |
| KR20130017079A (en) * | 2012-12-26 | 2013-02-19 | 주식회사 케이엔알 | Dilution system for standard gas |
| CN103675134B (en) * | 2013-12-05 | 2015-05-13 | 上海金玺实验室有限公司 | Method for detecting benzene series pollutants in gas by using internal standard method |
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| CN102539202A (en) * | 2010-12-30 | 2012-07-04 | 深圳光启高等理工研究院 | Preparation method for ethyl nitrite standard gas |
| CN103134875A (en) * | 2011-12-01 | 2013-06-05 | 中国科学院大连化学物理研究所 | On-line pretreatment device of aquatic volatile organic compounds |
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