CN102636580B - Measuring method of multifold organic constituent desorption efficiency in an active carbon pipe - Google Patents
Measuring method of multifold organic constituent desorption efficiency in an active carbon pipe Download PDFInfo
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- CN102636580B CN102636580B CN 201210118189 CN201210118189A CN102636580B CN 102636580 B CN102636580 B CN 102636580B CN 201210118189 CN201210118189 CN 201210118189 CN 201210118189 A CN201210118189 A CN 201210118189A CN 102636580 B CN102636580 B CN 102636580B
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- desorption
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- activated carbon
- desorb
- stripping liquid
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 142
- 238000003795 desorption Methods 0.000 title claims abstract description 68
- 238000000034 method Methods 0.000 title claims abstract description 23
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 18
- 239000000470 constituent Substances 0.000 title abstract 3
- 239000007788 liquid Substances 0.000 claims abstract description 34
- 239000012086 standard solution Substances 0.000 claims abstract description 27
- 238000003556 assay Methods 0.000 claims description 11
- 238000005070 sampling Methods 0.000 claims description 5
- 238000004458 analytical method Methods 0.000 claims description 3
- 239000012467 final product Substances 0.000 claims description 3
- 230000000149 penetrating effect Effects 0.000 claims description 3
- 238000002360 preparation method Methods 0.000 claims description 3
- 125000001997 phenyl group Chemical class [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 claims 5
- 239000000203 mixture Substances 0.000 claims 2
- 238000005259 measurement Methods 0.000 abstract description 5
- 239000000463 material Substances 0.000 description 10
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 9
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 9
- YNQLUTRBYVCPMQ-UHFFFAOYSA-N Ethylbenzene Chemical compound CCC1=CC=CC=C1 YNQLUTRBYVCPMQ-UHFFFAOYSA-N 0.000 description 6
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 6
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical group CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 5
- IVSZLXZYQVIEFR-UHFFFAOYSA-N m-xylene Chemical group CC1=CC=CC(C)=C1 IVSZLXZYQVIEFR-UHFFFAOYSA-N 0.000 description 5
- 239000002904 solvent Substances 0.000 description 5
- URLKBWYHVLBVBO-UHFFFAOYSA-N Para-Xylene Chemical group CC1=CC=C(C)C=C1 URLKBWYHVLBVBO-UHFFFAOYSA-N 0.000 description 3
- 239000003463 adsorbent Substances 0.000 description 3
- 229940078552 o-xylene Drugs 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 150000001555 benzenes Chemical class 0.000 description 1
- 239000003610 charcoal Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
Abstract
The invention discloses a measuring method of a multifold organic constituent desorption efficiency in an active carbon pipe. The measurement result is exact, and the multifold organic constituent desorption efficiency in the active carbon pipe can be detected. The measuring method comprises the specific steps of: A, measuring each component content in a stripping liquid generated by desorption of active carbon to be measured; B, preparing a standard solution according to each component content; C, taking out the section of a blank active carbon pipe to be measured, and adding a standard solution to carry out equilibrium and D, desorbing and measuring each component content, and calculating a desorbing efficiency. The method provided by the invention solves the problem of the components which differ greatly in concentration have mutual interference caused by desorption competing in a desorption to the stripping liquid process, and real process of the sample desorption is reflected furthest.
Description
Technical field:
The present invention relates to a kind of assay method of desorption efficiency, specifically the assay method of multiple organic component desorption efficiency in a kind of activated carbon tube.
Background technology:
At present, the volatile organic matter concentration determination adopts the method for activated carbon tube sampling to be widely used in the air.
Behind the intact air sample of activated carbon tube collection, sample is carried out desorb, desorption method has two kinds of thermal desorption and solvent desorptions, but most unit adopts the method for solvent desorption mostly because still there not being thermal desorption device.The concentration of the stripping liquid that sample forms behind solvent desorption is analyzed by chromatographic apparatus, then in conjunction with the desorption efficiency of sampling volume and activated charcoal, thereby finally obtains the actual concentrations of each component in the air.Therefore the whether accurate accuracy that directly influences net result of desorption efficiency must accurately be measured the analyzing efficiency of every batch of each component of activated carbon tube.
At present, still do not have relevant criterion at the mensuration of activated carbon tube desorption efficiency, the common method of measuring polycomponent organism desorption efficiency is:
Be the mixed standard solution that solvent is prepared high, medium and low three dosage with the stripping liquid with the polycomponent organism, wherein every kind of component concentrations of high dose representative is all higher, and every kind of component concentrations of low dosage representative is all lower.Get a certain amount of mixed standard solution then and inject blank activated carbon tube, shut, after the placement certain hour balance, use the stripping liquid desorb, measure the amount of each component in the stripping liquid then, compare with the amount of injecting activated charcoal, draw desorption efficiency.
The shortcoming that present method exists is:
When (1) carrying out sample determination, clearly stipulate in the standard, earlier the leading portion of solvent desorption type activated carbon tube is poured into desorb and mensuration in the desorb bottle, if measurement result show do not exceed adsorbent penetrate capacity the time, back segment can not desorb and mensuration, when measurement result show exceed adsorbent penetrate capacity the time, again with the desorb of back segment adsorbent and measure.
Present method is directly mixed standard solution to be injected activated carbon tube.It exists shortcoming to be: standard solution in activated carbon tube by after the charcoal absorption balance, if only the activated charcoal of leading portion is poured out and is carried out the efficiency test of leading portion active carbon desorption, then may be absorbed by back segment owing to standard solution, thereby can not be clearly by the adsorbed sample size of leading portion activated charcoal, thereby cause leading portion active carbon desorption efficient accurately to measure;
If simultaneously the activated charcoal of leading portion and back segment is poured out mixing simultaneously, measure desorption efficiency then, then the desorption efficiency of Ce Dinging is measured for the desorption efficiency that carries out at the total amount of front and back section activated charcoal, can not represent the desorption efficiency of leading portion activated charcoal, can not represent the desorption efficiency of back segment activated charcoal, and require the adsorbed sample size of section activated charcoal before and after the independent measurement in the present standard, so the desorption efficiency that this method records can't be used.
When (2) carrying out polycomponent mensuration, the concentration of each material in most cases can differ bigger in the air, and the concentration of possible certain material is higher, and the concentration of certain material is lower.
The activated carbon tube that collects this kind air sample competition can occur and separate suction phenomenon when carrying out desorb, the desorption efficiency of the material that concentration is high may be higher, and the desorption efficiency of the low material of concentration since be subjected to the influence of the high material of concentration may be lower.
And this moment if adopt the desorption efficiency of the immediate standard solution of each material concentration in the sample to represent the desorption efficiency of certain material, then can not reflect really the actual conditions of each component desorb in the sample can not take into full account the desorb influence between each material of sample.That is to say that the desorption efficiency of each material that measures by high, normal, basic standard solution can not reflect the desorption efficiency of each component when each concentration of component of sample differs big really.
Summary of the invention:
The present invention provides the assay method of multiple organic component desorption efficiency in a kind of activated carbon tube for overcoming above-mentioned the deficiencies in the prior art, and its measurement result is accurate, can measure multiple organic component desorption efficiency in the activated carbon tube.
The objective of the invention is to adopt following technical proposals to realize:
The assay method of multiple organic component desorption efficiency in a kind of activated carbon tube, concrete steps are:
Each components contents in the stripping liquid that A, to be measured section active carbon desorption of mensuration produce;
B, according to each component concentration preparing standard solution;
To be measured section of C, the blank activated carbon tube of taking-up, and the adding standard solution carries out balance;
Each component concentration is measured in D, desorb, calculates desorption efficiency.
The amount of each component of sample that described steps A calculates is compared with the capacity of penetrating of leading portion activated charcoal, when the leading portion that relatively shows activated carbon tube is not penetrated, adopts above-mentioned steps to measure leading portion active carbon desorption efficient and gets final product; When the leading portion that relatively shows activated carbon tube is penetrated, when measuring leading portion active carbon desorption efficient, again by the method identical with above-mentioned steps, change into and measure back segment active carbon desorption efficient.
The detailed process of described steps A is:
A1. get the activated carbon tube after the sampling, the leading portion activated charcoal is poured in the desorb bottle, add the 1ml stripping liquid, desorb 30min;
A2. stripping liquid measures the mass concentration of each component to be measured in the stripping liquid by the chromatograph analysis, multiply by then amount A1, A2 that the stripping liquid volume calculates each component ... An.
Among the described step B, preparation is when comprising the standard solution of each component, and the mass concentration of each component satisfies following condition: in the 10ul standard solution each components contents in the scope of " (A ÷ 95%)-(A ÷ 85%) ", A represent A1, A2 ... or An.
Among the described step c,
C1. get and sample with activated carbon tube with many of a collection of blank activated carbon tubes, the leading portion of each activated carbon tube is poured into respectively in the 1ml desorb bottle, the desorb bottle is sealed;
C2. respectively get the standard solution 10ul for preparing and be added in each desorb bottle, the desorb bottle is sealed;
C3. place and spend the night, carry out balance.
Among the described step D,
D1. in each desorb bottle, respectively add the 1ml stripping liquid, desorb 30min;
The D2 stripping liquid is analyzed by chromatograph, measures the mass concentration of each component to be measured in the stripping liquid, multiply by amount A1 ', A2 ' that the stripping liquid volume calculates each component ... An ';
D3 averages the desorption efficiency data of respectively organizing that each component records, and calculates the desorption efficiency of each component.
The method of multiple organic component desorption efficiency is compared and is mainly had following characteristics in the mensuration activated carbon tube of the present invention and present employing:
This method is measured the desorption efficiency of activated carbon tube front and back section activated charcoal respectively, front and back section activated charcoal is positioned over respectively in the desorb bottle, inject standard solution, measure its desorption efficiency then, avoided directly standard solution being injected the error of bringing when activated carbon tube is measured.
The component that this method has taken into full account variant concentration is drawn to mutual interference problem in the process of stripping liquid in solution, has farthest embodied the true desorption process of sample.
Embodiment:
The present invention is further described below in conjunction with embodiment.
The assay method of benzene series thing desorption efficiency is as follows in a kind of activated carbon tube:
1. get the activated carbon tube after the sampling, the leading portion activated charcoal is poured in the desorb bottle, add the 1ml stripping liquid, desorb 30min;
2. stripping liquid is by the chromatograph analysis, measure the concentration of benzene in the stripping liquid, toluene, ethylbenzene, styrene, o-xylene, m-xylene, P-xylene, multiply by stripping liquid volume (1ml), calculate the amount of each component in the stripping liquid, be assumed to be benzene 12.5ug, toluene 34.2ug, ethylbenzene 17.9ug, styrene 101ug, o-xylene 204ug, m-xylene 157ug, P-xylene 169ug.
3. preparation comprises the standard solution of each component, and each component concentrations satisfies following condition: in the 10ul standard solution in the scope of the amount of each component for " (A ÷ 95%)-(A ÷ 85%) " (namely use each component amount A1, A2 ... An is divided by 95%-85%) obtain;
The amount of each component is as follows in the 10ul standard solution:
Benzene 14.0ug satisfies the 13.2-14.7ug scope;
Toluene 38.0ug satisfies the 36.0-40.2ug scope;
Ethylbenzene 20ug satisfies the 18.8-21.1ug scope;
Styrene 110ug satisfies the 106-119ug scope;
O-xylene 230ug satisfies the 215-240ug scope;
M-xylene 175ug satisfies the 185-165ug scope;
P-xylene 190ug satisfies the 199-178ug scope.
4. get and sample with activated carbon tube with 6 of a collection of activated carbon tubes, the leading portion of each activated carbon tube is poured into respectively in the 1ml desorb bottle, the desorb bottle is sealed;
5. respectively get the standard solution 10ul for preparing be added to 6 desorb bottles in, the desorb bottle is sealed;
6. place and spend the night, carry out balance;
7. in 6 desorb bottles, respectively add the 1ml stripping liquid, desorb 30min;
8. stripping liquid is analyzed by chromatograph, measures each component concentrations to be measured in the stripping liquid, multiply by the amount that the stripping liquid volume calculates each component (A1 ', A2 ' ... An ');
9. 6 groups of desorption efficiency data that each component is recorded are averaged, and calculate the desorption efficiency of each component.
The amount of each component of sample that described step B calculates is compared with the capacity of penetrating of leading portion activated charcoal, when the leading portion that relatively shows activated carbon tube is not penetrated, adopts above-mentioned steps to measure leading portion active carbon desorption efficient and gets final product; When the leading portion that relatively shows activated carbon tube is penetrated, when measuring leading portion active carbon desorption efficient, again by the method identical with above-mentioned steps, change into and measure back segment active carbon desorption efficient.
Claims (5)
1. the assay method of benzene series thing desorption efficiency in the activated carbon tube is characterized in that concrete steps are:
Each components contents in the stripping liquid that A, to be measured section active carbon desorption of mensuration produce;
B, according to each component concentration preparing standard solution, preparation is when comprising the standard solution of each component, the mass concentration of each component satisfies following condition: each components contents is in the scope of " (A ÷ 95%)-(A ÷ 85%) " in the 10ul standard solution;
C, take out to be measured section of blank activated carbon tube, and add standard solution and carry out balance, each composition in the standard solution is fully absorbed by activated charcoal;
Each component concentration is measured in D, desorb, calculates desorption efficiency.
2. the assay method of benzene series thing desorption efficiency in the activated carbon tube as claimed in claim 1, it is characterized in that, the amount of each component of sample that described steps A calculates is compared with the capacity of penetrating of leading portion activated charcoal, when the leading portion that relatively shows activated carbon tube is not penetrated, adopt above-mentioned steps to measure leading portion active carbon desorption efficient and get final product; When the leading portion that relatively shows activated carbon tube is penetrated, when measuring leading portion active carbon desorption efficient, again by the method identical with above-mentioned steps, change into and measure back segment active carbon desorption efficient.
3. the assay method of benzene series thing desorption efficiency in the activated carbon tube as claimed in claim 1 or 2 is characterized in that the detailed process of described steps A is:
A1. get the activated carbon tube after the sampling, the leading portion activated charcoal is poured in the desorb bottle, add the 1ml stripping liquid, desorb 30min;
A2. stripping liquid measures the mass concentration of each component to be measured in the stripping liquid by the chromatograph analysis, multiply by then amount A1, A2 that the stripping liquid volume calculates each component ... .An.
4. the assay method of benzene series thing desorption efficiency in the activated carbon tube as claimed in claim 3 is characterized in that, among the described step c,
C1. get and sample with activated carbon tube with many of a collection of blank activated carbon tubes, the leading portion of each activated carbon tube is poured into respectively in the 1ml desorb bottle, the desorb bottle is sealed;
C2. respectively get the standard solution 10ul for preparing and be added in each desorb bottle, the desorb bottle is sealed;
C3. place and spend the night, carry out balance, each composition in the standard solution is fully absorbed by activated charcoal.
5. the assay method of benzene series thing desorption efficiency in the activated carbon tube as claimed in claim 1 or 2 is characterized in that, among the described step D,
D1. in each desorb bottle, respectively add the 1ml stripping liquid, desorb 30min;
The D2 stripping liquid is analyzed by chromatograph, measures the mass concentration of each component to be measured in the stripping liquid, multiply by amount A1 ', A2 ' that the stripping liquid volume calculates each component ... .An ';
D3 averages the desorption efficiency data of respectively organizing that each component records, and calculates the desorption efficiency of each component.
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