CN104345104A - Standard sample for headspace analysis of trace benzene in water, preparation method thereof and method for determining trace benzene in water by using standard sample - Google Patents
Standard sample for headspace analysis of trace benzene in water, preparation method thereof and method for determining trace benzene in water by using standard sample Download PDFInfo
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Abstract
The invention provides a standard sample for analyzing trace benzene in water in headspace, a preparation method thereof and a method for determining trace benzene in water by using the standard sample, wherein the preparation method comprises the steps of dissolving a benzene solution in a polar sulfone organic solvent which has a high boiling point and is mutually soluble with water and benzene to obtain a standard sample, and diluting the standard sample to a required concentration by using water; the mass ratio of the benzene to the polar sulfone organic solvent is 1: 100-1: 1000. The method improves the concentration of benzene in the standard sample, and the validity period of the standard sample is prolonged to more than 1 year; increasing the sample weighing amount of benzene, and reducing the weighing error to reduce the relative weighing error from 10% to 1%; the invention also provides a method for measuring trace benzene in water by using the standard sample, and the standard sample does not interfere with the measurement of benzene in headspace analysis.
Description
Technical field
The invention belongs to detection technique field, be specifically related to a kind of method that standard model for headspace analysis underwater trace benzene and compound method and this standard model headspace analysis of application thereof measure underwater trace benzene.
Background technology
Headspace analysis and head space gas chromatography, be a kind of analytical model of vapor-phase chromatography, it sample is placed in a closed container, after uniform temperature, pressure are issued to balance, the gas phase portion getting top carries out stratographic analysis, is widely used in the volatile constituent in Analysis of Complex sample.
In water quality monitoring field, as when measuring Trace Benzene in potable water, surface water, waste water, the standard model of benzene in water must be prepared.
In preparation water, the existing common method of the standard model of benzene has two kinds, and one is that benzene is directly soluble in water.In " the mensuration vapor-phase chromatography of GB11890-1989 To Determine Benzene Using ", take 10mg benzene and be dissolved in 1000mL water, prepare benzene concentration in the standard specimen obtained like this and be only 10mg/L, the term of validity shorter (only a week).And, because the sample weighting amount of benzene is less, weigh relative error comparatively large (if be 0.1mg with scale division value, franchise is ± the analytical balance weighing of 1mg, and weighing error can reach 10%).
Another kind method is first dissolved in methyl alcohol by benzene, is mixed with the standard model that concentration is 100 ~ 1000mg/L.As " in methyl alcohol the benzene Standard Reference Materials for Determination " of State Standard Matter Research Centre's development, concentration: 1000mg/L, production code member: GBW08703, the term of validity 15 months, is diluted with water to desired concn during use.Because the boiling point of methyl alcohol is lower, be only 64.5 DEG C, be evaporated together with benzene when headspace analysis, the mensuration of interference benzene.
Summary of the invention
In order to solve the problem, the object of the present invention is to provide a kind of standard model for headspace analysis underwater trace benzene and compound method thereof, improve the concentration of benzene in standard model, extend the term of validity of standard model; Increase the sample weighting amount of benzene, reduce weighing error; The present invention also provides the described standard model of application to measure the method for underwater trace benzene, and this standard model does not cause interference to the mensuration of benzene in headspace analysis.
Technical solution of the present invention is as follows:
The invention provides a kind of standard model for headspace analysis underwater trace benzene, it is characterized in that, described standard model is benzene solvent and higher boiling and the mixed solution of the polarity sulfone class organic solvent all dissolved each other with water and benzene; The mass ratio of described benzene solvent and polarity sulfone class organic solvent is 1: 100 ~ 1: 1000.
According to the standard model for headspace analysis underwater trace benzene provided by the invention, preferably, described polarity sulfone class organic solvent be selected from dimethyl sulfone, dimethyl sulfoxide (DMSO), sulfolane one or more.
According to the standard model for headspace analysis underwater trace benzene provided by the invention, further preferably, described polarity sulfone class organic solvent be selected from dimethyl sulfoxide (DMSO), sulfolane one or more.
According to the standard model for headspace analysis underwater trace benzene provided by the invention, preferably, described higher boiling is for being greater than 150 DEG C.
The invention provides the compound method of also a kind of standard model for headspace analysis underwater trace benzene, benzene solvent is dissolved in higher boiling and in the polarity sulfone class organic solvent all dissolved each other with water and benzene, gets standard samples, during use, be diluted with water to desired concn; It is 1: 100 ~ 1: 1000 that described benzene and polarity sulfone class organic solvent add mass ratio.
According to the compound method of the standard model for headspace analysis underwater trace benzene provided by the invention, preferably, described benzene solvent and polarity sulfone class organic solvent add mass ratio is 1: 500 ~ 1: 1000
According to the compound method of the standard model for headspace analysis underwater trace benzene provided by the invention, preferably, taking 0.1g benzene, to be dissolved in 100g boiling point higher and dissolve each other in polarity sulfone class organic solvent with water and benzene simultaneously, the concentration obtaining benzene is the standard model solution of 1000mg/kg, is diluted with water to desired concn during use.
According to the compound method of the standard model for headspace analysis underwater trace benzene provided by the invention, preferably, one or more in described polarity sulfone class organic solvent dimethyl sulfone, dimethyl sulfoxide (DMSO), sulfolane.
According to the compound method of the standard model for headspace analysis underwater trace benzene provided by the invention, further preferably, one or more in described polarity sulfone class organic solvent dimethyl sulfoxide (DMSO), sulfolane.
According to the compound method of the standard model for headspace analysis underwater trace benzene provided by the invention, preferably, described higher boiling is for being greater than 150 DEG C.
The present invention also provides a kind of and applies the method that the described standard model for headspace analysis underwater trace benzene measures underwater trace benzene, comprises the steps:
(1) preparation of the standard model of benzene: by the compound method of the described standard model for headspace analysis underwater trace benzene, obtain the standard model of described benzene;
(2) preparation of benzene intermediate liquid: the standard model taking the benzene that 1g step (1) obtains, in 1000mL volumetric flask, is diluted with water to scale, obtains the benzene intermediate liquid that concentration is 1mg/L;
(3) preparation of benzene working fluid: removing step (2) gained benzene intermediate liquid is in 100mL volumetric flask respectively, is diluted with water to scale, obtains the benzene working fluid of variable concentrations;
(4) drawing curve: the benzene working fluid of step (3) variable concentrations is done HS GC analysis, the peak area of record benzene, determines the working curve that the concentration of benzene is corresponding with peak area;
(5) pipette 10mL aqueous solution to be measured in ml headspace bottle, be placed in head-space sampler, do HS GC analysis, record the peak area of benzene in aqueous solution to be measured, obtain the concentration of benzene in aqueous solution to be measured according to the working curve of step (4) gained.
Measure the method for underwater trace benzene for the standard model of headspace analysis underwater trace benzene according to application provided by the invention, preferably, the preparation of described step (3) benzene working fluid: pipette benzene intermediate liquid described in 0.5mL, 2.5mL, 5mL, 7.5mL, 10mL respectively in 100mL volumetric flask, be diluted with water to scale, obtain the benzene working fluid that concentration is 0.005mg/L, 0.025mg/L, 0.05mg/L, 0.075mg/L, 0.1mg/L.
According to application provided by the invention, measure the method for underwater trace benzene for the standard model of headspace analysis underwater trace benzene, preferably, the GC conditions of described HS GC analysis is:
Chromatographic column: DB-Wax capillary column;
Temperature of vaporization chamber: 200 ~ 300 DEG C;
Detector temperature: 200 ~ 300 DEG C;
Input mode: shunting, split ratio: 1: 1 ~ 1: 10;
Carrier gas line speed: 20 ~ 40cm/s;
Hydrogen flowing quantity: 20 ~ 40mL/min;
Air mass flow: 200 ~ 400mL/min;
Tail wind drift amount: 20 ~ 40mL/min;
Post case temperature: initial 40 ~ 50 DEG C, keeps 5 ~ 10min, is warming up to 150 ~ 200 DEG C with the rate program of 20 ~ 30 DEG C/min, keeps 10 ~ 20min.
According to application provided by the invention, measure the method for underwater trace benzene for the standard model of headspace analysis underwater trace benzene, preferably, the head space condition of described HS GC analysis is:
Equilibrium temperature: 50 ~ 80 DEG C, equilibration time: 10 ~ 20min;
Quantitative loop temperature: 80 ~ 100 DEG C; GC cycling time: 30 ~ 40min;
Transfer tube temperature: 100 ~ 120 DEG C; Ml headspace bottle pressing time: 0.2 ~ 0.3min;
Quantitative loop fills the sample time: 0.1 ~ 0.2min; Quantitative loop equilibration time: 0.05 ~ 0.1min;
Sample injection time: 0.5 ~ 1min; Headspace sample bottle volume: 10 ~ 20mL;
Sample volume: 5 ~ 10mL; Sodium chloride: 3.95 ~ 4.05g.
Measure the method for underwater trace benzene for the standard model of headspace analysis underwater trace benzene according to application provided by the invention, preferably, the scope that described method measures benzene content in water is 0.005 μ g/mL ~ 0.1 μ g/mL, can suitably dilute when benzene content is higher.
Measure the method for underwater trace benzene for the standard model of headspace analysis underwater trace benzene according to application provided by the invention, preferably, described standard model is benzene solvent and higher boiling and the mixed solution of the polarity sulfone class organic solvent all dissolved each other with water and benzene; The mass ratio of described benzene solvent and polarity sulfone class organic solvent is 1: 100 ~ 1: 1000.
Measure the method for underwater trace benzene for the standard model of headspace analysis underwater trace benzene according to application provided by the invention, preferably, described polarity sulfone class organic solvent be selected from dimethyl sulfone, dimethyl sulfoxide (DMSO), sulfolane one or more.
For the method for the standard model mensuration underwater trace benzene of headspace analysis underwater trace benzene according to application provided by the invention, further preferably, described polarity sulfone class organic solvent is selected from one or more in dimethyl sulfoxide (DMSO), sulfolane.
According to application provided by the invention, measure the method for underwater trace benzene for the standard model of headspace analysis underwater trace benzene, preferably, described higher boiling is for being greater than 150 DEG C.
The present invention is with a kind of polarity sulfone class organic solvent (sulfone class, code name F), and this solvent both had good mutual solubility with benzene and water, also had higher boiling point (being greater than 150 DEG C), non-volatile in headspace analysis, did not disturb the mensuration of benzene.
The key step that the described standard model of application provided by the invention measures the method for underwater trace benzene is:
(1) standard solution preparation
The preparation of the standard model (1000 μ g/g) of a benzene
The preparation of b benzene intermediate liquid (1 μ g/mL)
The preparation of c benzene working fluid (0.005 μ g/mL ~ 0.1 μ g/mL)
(2) drafting of working curve
Pipette 10mL benzene working fluid respectively in ml headspace bottle, add about 4g(3.95g ~ 4.05g) sodium chloride, cover bottle cap, compress, vibration 1min, makes sodium chloride fully dissolve.Be placed in head-space sampler, measure under certain chromatographic condition and head space condition, the peak area of record benzene.
With benzene working fluid concentration for horizontal ordinate, with the peak area of benzene for ordinate drawing curve.
(3) mensuration of sample
Pipette 10mL test solution in ml headspace bottle, add about 4g(3.95g ~ 4.05g) sodium chloride, cover bottle cap, compress, vibration 1min, makes sodium chloride fully dissolve.Be placed in head-space sampler, measure under certain chromatographic condition and head space condition, the peak area of record benzene.The concentration of benzene in the sample asked by working curve.
Polar organic solvent of the present invention can may not be sulfone class for sulfone class, and be preferably polarity sulfone class organic solvent, described polar organic solvent meets the following conditions simultaneously: 1) dissolve each other with water; 2) dissolve each other with benzene; 3) boiling point is enough high, non-volatile when sample headspace balances; 4) higher purity is had, the not disturbed specimen analysis of its impurity; 5) toxicity is less.Part sulfone class reagent meets the demands.
" trace " of the present invention is the definition according to GB/T 14666-2003 " analytical chemistry term ", and trace analysis refers to the analysis that the massfraction of component to be measured is less than 0.01%.
Useful technique effect:
A kind of standard model for headspace analysis underwater trace benzene provided by the invention and compound method thereof, improve the concentration of benzene in standard model, more than the extension of validity to 1 of standard model year; Increase the sample weighting amount of benzene, reduce weighing error, make weighing relative error be decreased to 1% by 10%; The present invention also provides the described standard model of application to measure the method for underwater trace benzene, and this standard model does not disturb the mensuration of benzene in headspace analysis.
Accompanying drawing explanation
Fig. 1 is the compound method process flow diagram for headspace analysis underwater trace benzene standard model provided by the invention;
Fig. 2 is the working curve that the described standard model of application provided by the invention measures underwater trace benzene;
Fig. 3 is the standard gas figure for headspace analysis underwater trace benzene standard model provided by the invention.
Embodiment
In order to understand the present invention better, illustrate content of the present invention further below in conjunction with embodiment, but the content of invention is not only confined to the following examples.
The key instrument that the present embodiment adopts and reagent:
Automatic headspace sample injector: 7694E, Agilent company;
Gas chromatograph: 7890A, Agilent company;
Sulfolane: analyze pure;
Dimethyl sulfoxide (DMSO): analyze pure;
Benzene: chromatographically pure;
Sodium chloride: analyze pure;
The explanation of standard specimen blank: during preparation standard specimen, organic solvent F is pure for analyzing, and water is ultrapure water, through blank test, does not detect benzene.
Embodiment 1
Compound method for headspace analysis underwater trace benzene standard model provided by the invention:
(1) preparation of benzene standard model: take 0.1g benzene in 100g sulfolane, shake up.Benzene standard model concentration is 1000mg/kg.
(2) preparation of benzene intermediate liquid: take 1g benzene standard model in 1000mL volumetric flask, be diluted with water to scale.Benzene intermediate liquid concentration is 1mg/L.
(3) preparation of benzene working fluid: pipette 0.5mL, 2.5mL, 5mL, 7.5mL, 10mL benzene intermediate liquid respectively in 100mL volumetric flask, be diluted with water to scale.Benzene working fluid concentration is 0.005mg/L, 0.025mg/L, 0.05mg/L, 0.075mg/L, 0.1mg/L.
(4) drawing curve: pipette 10mL benzene working fluid respectively in ml headspace bottle, add about 4g(3.95g ~ 4.05g) sodium chloride, cover bottle cap, compress, vibration 1min, makes sodium chloride fully dissolve.Be placed in head-space sampler, under certain chromatographic condition and head space condition, do HS GC analysis, the peak area of record benzene.With benzene working fluid concentration for horizontal ordinate, with the peak area of benzene for ordinate drawing curve, working curve is shown in Fig. 2.
Show that the related data of working curve is as follows:
Linear equation: y=1401.5x-0.7042, R
2=0.9991.
Table 1 benzene working fluid standard model peak area
| Standard specimen sequence number | 1# | 2# | 3# | 4# | 5# |
| Standard specimen concentration, mg/L | 0.005 | 0.025 | 0.05 | 0.075 | 0.1 |
| Benzene peak area, pA.S | 6.05 | 35.5 | 69.3 | 102 | 141 |
(5) mensuration of sample: pipette 10mL test solution to be measured in ml headspace bottle, adds about 4g(3.95g ~ 4.05 g) sodium chloride, covers bottle cap, compresses, and vibration 1min, makes sodium chloride fully dissolve.Be placed in head-space sampler, measure under certain chromatographic condition and head space condition, the peak area of record benzene.The concentration of benzene in the sample asked by working curve.
Head space condition in the present embodiment: can suitably adjust in real work, in table 2
Table 2 head space operating conditions
| Equilibrium temperature: 80 DEG C | Quantitative loop temperature: 100 DEG C | Transfer tube temperature: 120 DEG C |
| Equilibration time: 20min | GC cycling time: 40min | Ml headspace bottle pressing time: 0.2min |
| Quantitative loop fills the sample time: 0.1min | Quantitative loop equilibration time: 0.05min | Sample injection time: 1min |
| Headspace sample bottle volume: 20mL | Sample volume: 10mL | Sodium chloride: 4.0g |
GC conditions in the present embodiment: can suitably adjust in real work, in table 3
Table 3 operation condition of chromatogram
(5) apply the inventive method, at different date-time, the measured data of benzene is contained in table 4 to certain chemical plant wastewater
Table 4 measured data
| Sequence number | Not same date sample | Measured value |
| 1 | North row's mouth | 0.02mg/L |
| 2 | Regulating reservoir | 0.005mg/L |
| 3 | Ammonia still process import | 567mg/L |
| 4 | Ammonia still process exports | 0.04mg/L |
| 5 | Regulating reservoir | 0.07mg/L |
| 6 | North row's mouth | 0.01mg/L |
| 7 | Extraction column import | 145mg/L |
| 8 | North row's mouth | 0.03mg/L |
[0094]
| 9 | Whole cold water | 50mg/L |
| 10 | North row's mouth | 0.01mg/L |
| 11 | Outer draining | 0.02mg/L |
| 12 | North row's mouth | 0.01mg/L |
The standard gas figure of the standard model of benzene is shown in Fig. 3, and in figure, the organic solvent F of visible higher than the concentration of benzene 1000 times does not go out peak completely, does not disturb the mensuration of benzene.
Embodiment 2
Compound method for headspace analysis underwater trace benzene standard model provided by the invention:
(1) preparation of benzene standard model: take 0.1g benzene in 100g dimethyl sulfoxide (DMSO), shake up.Benzene standard model concentration is 1000mg/kg.
(2) preparation of benzene intermediate liquid: take 1g benzene standard model in 1000mL volumetric flask, be diluted with water to scale.Benzene intermediate liquid concentration is 1mg/L.
(3) preparation of benzene working fluid: pipette 0.5mL, 2.5mL, 5mL, 7.5mL, 10mL benzene intermediate liquid respectively in 100mL volumetric flask, be diluted with water to scale.Benzene working fluid concentration is 0.005mg/L, 0.025mg/L, 0.05mg/L, 0.075mg/L, 0.1mg/L.
(4) drawing curve: pipette 10mL benzene working fluid respectively in ml headspace bottle, add about 4g(3.95g ~ 4.05g) sodium chloride, cover bottle cap, compress, vibration 1min, makes sodium chloride fully dissolve.Be placed in head-space sampler, under certain chromatographic condition and head space condition, do HS GC analysis, the peak area of record benzene.With benzene working fluid concentration for horizontal ordinate, with the peak area of benzene for ordinate drawing curve.
Show that the related data of working curve is as follows:
Linear equation: y=1353.6x-0.7230, R
2=0.9991.
Table 5 benzene working fluid standard model peak area
| Standard specimen sequence number | 1# | 2# | 3# | 4# | 5# |
| Standard specimen concentration, mg/L | 0.005 | 0.025 | 0.05 | 0.075 | 0.1 |
| Benzene peak area, pA.S | 5.85 | 33.6 | 67.9 | 98.2 | 136 |
[0106](5) mensuration of sample: pipette 10mL test solution to be measured in ml headspace bottle, add about 4g(3.95g ~ 4.05g) sodium chloride, cover bottle cap, compress, vibration 1min, makes sodium chloride fully dissolve.Be placed in head-space sampler, measure under certain chromatographic condition and head space condition, the peak area of record benzene.The concentration of benzene in the sample asked by working curve.
Head space condition in the present embodiment: can suitably adjust in real work, in table 6
Table 6 head space operating conditions
| Equilibrium temperature: 60 DEG C | Quantitative loop temperature: 80 DEG C | Transfer tube temperature: 100 DEG C |
| Equilibration time: 10min | GC cycling time: 30min | Ml headspace bottle pressing time: 0.3min |
| Quantitative loop fills the sample time: 0.2min | Quantitative loop equilibration time: 01min | Sample injection time: 0.5min |
| Headspace sample bottle volume: 10mL | Sample volume: 5mL | Sodium chloride: 3.95g |
GC conditions in the present embodiment: can suitably adjust in real work, in table 7
Table 7 operation condition of chromatogram
(5) apply the inventive method, on the different dates, the measured data of benzene is contained in table 8 to certain chemical plant wastewater
Table 8 measured data
| Sequence number | Not same date sample | Measured value |
| 1 | North row's mouth | 0.05mg/L |
| 2 | Regulating reservoir | 0.05mg/L |
| 3 | Outer draining | 0.01mg/L |
| 4 | Ammonia still process exports | 0.01mg/L |
| 5 | Regulating reservoir | 0.03mg/L |
[0116]
| 6 | North row's mouth | 0.02mg/L |
| 7 | North row's mouth | 0.02mg/L |
| 8 | North row's mouth | 0.01mg/L |
| 9 | Whole cold water | 45mg/L |
| 10 | North row's mouth | 0.02mg/L |
The standard gas figure of benzene standard model is shown in Fig. 3, and in figure, the organic solvent F of visible higher than the concentration of benzene 1000 times does not go out peak completely, does not disturb the mensuration of benzene.
The stability of standard model provided by the invention: the concentration of the 1# benzene standard model of certain research institute preparation is 1020 ± 20mg/kg, after 1 year, again the concentration preparing 2# benzene standard model is 995 ± 20mg/kg, by 2# benzene standard model stepwise dilution, drawing curve, be 1010mg/kg by the concentration of this curve anti-1# of survey benzene standard model, show that the concentration of benzene standard model is stable within 1 year.
One provided by the invention is used for headspace analysis underwater trace benzene standard model and compound method thereof, improves the concentration of benzene in standard model, more than the extension of validity to 1 of standard model year; Increase the sample weighting amount of benzene, reduce weighing error, make weighing relative error be decreased to 1% by 10%; The present invention also provides the described standard model of application to measure the method for underwater trace benzene, and this standard model does not disturb the mensuration of benzene in headspace analysis.
The foregoing is only the schematic embodiment of the present invention; and be not used to limit scope of the present invention; any those skilled in the art, the equivalent variations done under the prerequisite not departing from design of the present invention and principle, amendment and combination all should belong to the scope of protection of the invention.
Claims (10)
1. for a standard model for headspace analysis underwater trace benzene, it is characterized in that, described standard model is benzene solvent and higher boiling and the mixed solution of the polarity sulfone class organic solvent all dissolved each other with water and benzene; The mass ratio of described benzene solvent and polarity sulfone class organic solvent is 1: 100 ~ 1: 1000.
2., according to claim 1 for the standard model of headspace analysis underwater trace benzene, it is characterized in that, described polarity sulfone class organic solvent be selected from dimethyl sulfone, dimethyl sulfoxide (DMSO), sulfolane one or more.
3. according to claim 1 for the standard model of headspace analysis underwater trace benzene, it is characterized in that, described higher boiling is for being greater than 150 DEG C.
4. described in a claim 1 for the compound method of the standard model of headspace analysis underwater trace benzene, it is characterized in that, benzene solvent is dissolved in higher boiling and in the polarity sulfone class organic solvent all dissolved each other with water and benzene, gets standard samples, during use, be diluted with water to desired concn; It is 1: 100 ~ 1: 1000 that described benzene solvent and polarity sulfone class organic solvent add mass ratio.
5. according to claim 4 for the compound method of the standard model of headspace analysis underwater trace benzene, it is characterized in that, taking 0.1g benzene, to be dissolved in 100g boiling point higher and in the polarity sulfone class organic solvent simultaneously dissolved each other with water and benzene, the concentration obtaining benzene is the standard model solution of 1000mg/kg, is diluted with water to desired concn during use.
6. according to claim 4 or 5 for the compound method of the standard model of headspace analysis underwater trace benzene, it is characterized in that, described polarity sulfone class organic solvent be selected from dimethyl sulfone, dimethyl sulfoxide (DMSO), sulfolane one or more.
7. according to claim 4 or 5 for the compound method of the standard model of headspace analysis underwater trace benzene, it is characterized in that, described higher boiling is for being greater than 150 DEG C.
8. application rights requires the method measuring underwater trace benzene described in 1 for the standard model of headspace analysis underwater trace benzene, it is characterized in that, comprises the steps:
(1) preparation of benzene standard model: by preparation method according to claim 4, obtains benzene standard model;
(2) preparation of benzene intermediate liquid: take benzene standard model that 1g step (1) obtains in 1000mL volumetric flask, be diluted with water to scale, obtain the benzene intermediate liquid that concentration is 1mg/L;
(3) preparation of benzene working fluid: removing step (2) gained benzene intermediate liquid is in 100mL volumetric flask respectively, is diluted with water to scale, obtains the benzene working fluid of variable concentrations;
(4) drawing curve: the benzene working fluid of step (3) variable concentrations is done HS GC analysis, the peak area of record benzene, determines the working curve that the concentration of benzene is corresponding with peak area;
(5) pipette 10mL aqueous solution to be measured in ml headspace bottle, be placed in head-space sampler, do HS GC analysis, record the benzene peak area in aqueous solution to be measured, obtain the benzene concentration in aqueous solution to be measured according to the working curve of step (4) gained.
9. the method for mensuration underwater trace benzene according to claim 8, it is characterized in that, the preparation of described step (3) benzene working fluid: pipette benzene intermediate liquid described in 0.5mL, 2.5mL, 5mL, 7.5mL, 10mL respectively in 100mL volumetric flask, be diluted with water to scale, obtain the benzene working fluid that concentration is 0.005mg/L, 0.025mg/L, 0.05mg/L, 0.075mg/L, 0.1mg/L.
10. the method for mensuration underwater trace benzene according to claim 8, is characterized in that, the GC conditions of described HS GC analysis is:
Chromatographic column: DB-Wax capillary column;
Temperature of vaporization chamber: 200 ~ 300 DEG C;
Detector temperature: 200 ~ 300 DEG C;
Input mode: shunting, split ratio: 1: 1 ~ 1: 10;
Carrier gas line speed: 20 ~ 40cm/s;
Hydrogen flowing quantity: 20 ~ 40mL/min;
Air mass flow: 200 ~ 400mL/min;
Tail wind drift amount: 20 ~ 40mL/min;
Post case temperature: initial 40 ~ 50 DEG C, keeps 5 ~ 10min, is warming up to 150 ~ 200 DEG C with the rate program of 20 ~ 30 DEG C/min, keeps 10 ~ 20min;
The head space condition of described HS GC analysis is:
Equilibrium temperature: 50 ~ 80 DEG C, equilibration time: 10 ~ 20min;
Quantitative loop temperature: 80 ~ 100 DEG C; GC cycling time: 30 ~ 40min;
Transfer tube temperature: 100 ~ 120 DEG C; Ml headspace bottle pressing time: 0.2 ~ 0.3min;
Quantitative loop fills the sample time: 0.1 ~ 0.2min; Quantitative loop equilibration time: 0.05 ~ 0.1min;
Sample injection time: 0.5 ~ 1min; Headspace sample bottle volume: 10 ~ 20mL;
Sample volume: 5 ~ 10mL; Sodium chloride: 3.95 ~ 4.05g.
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| CN105527353A (en) * | 2016-01-07 | 2016-04-27 | 华南理工大学 | Method for determining solvent solubility by tracer agent headspace gas chromatography |
| CN106959228A (en) * | 2017-02-27 | 2017-07-18 | 广东风华高新科技股份有限公司 | The processing method of spectrofluorimetry sample |
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