CN103163237A - Method of obtaining preserved thermodynamic parameter and the adsorption isotherm of organic compound on carbon nano tube - Google Patents
Method of obtaining preserved thermodynamic parameter and the adsorption isotherm of organic compound on carbon nano tube Download PDFInfo
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- CN103163237A CN103163237A CN2013100435314A CN201310043531A CN103163237A CN 103163237 A CN103163237 A CN 103163237A CN 2013100435314 A CN2013100435314 A CN 2013100435314A CN 201310043531 A CN201310043531 A CN 201310043531A CN 103163237 A CN103163237 A CN 103163237A
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Abstract
The invention discloses a method of obtaining the preserved thermodynamic parameter and the adsorption isotherm of an organic compound on a carbon nano tube. The method of obtaining the preserved thermodynamic parameter and the adsorption isotherm of the organic compound on the carbon nano tube includes the following steps of preparing a carbon nano tube homogenate with dimethylformamide as a dispersing agent, and preparing 4.6*50mm carbon nano tube chromatographic column through a pneumatic constant pressure pump, wherein the filling quantity is 250mg; calculating the preserved chromatographic column of the organic compound on the carbon nano tube by measuring retention time of the organic compound on the carbon nano tube at different temperatures; and measuring the breakthrough curves of the organic compound at different concentrations on the carbon nano tube, fitting the Linear adsorption isotherm and the Freundlich adsorption isotherm, and calculating the adsorption equilibrium constant of the Linear and the Freundlich. The thermodynamic parameter and the adsorption isotherm on the carbon nano tube are obtained based on a chromatographic method, and therefore operation is simple, solid-liquid separation is easy, frequent replacements of the chromatographic column is not needed, and consumption of materials and medicine is reduced. The method of obtaining the preserved thermodynamic parameter and the adsorption isotherm of the organic compound on the carbon nano tube has important value on evaluation of utilization potentiality of the carbon nano tube as adsorbing material in fields of water pollution regulation, sample pretreatment, analytical tests and the like.
Description
Technical field
The present invention relates to a kind of method that obtains to keep thermodynamic parameter and adsorption isothermal by measuring the retention time of organic compound on the carbon nano-tube chromatographic column under different temperatures, belong to the environmental pollution control technique field.
Background technology
Carbon nano-tube is since 1991 find first, because the characteristic of the aspects such as its unique mechanics, electricity, optics and thermodynamics is paid close attention to widely.The basic structure of carbon nano-tube is to be rolled into seamless tubular and to be formed flawless tubulose material by graphene film (graphite galvanized hexagonal wire mesh plane).Carbon nano-tube has good absorption property, as sorbing material, can be applied at environmental area original position reparation and the sample analysis that environmental pollution is controlled, polluted, carbon nano-tube can rapidly and efficiently be removed underwater gold as adsorbent and belong to ion, organic contaminant and biological impurities etc., and carbon nano-tube is widely used in solid-phase extraction column, gas phase and liquid phase chromatographic column as the Novel adsorption filler.Therefore, the Fast Measurement of carbon nano-tube to organic compound absorption helps carbon nano-tube as the application of adsorbent in wastewater treatment and chemical analysis field.
Keeping thermodynamic parameter, saturated extent of adsorption and adsorption equilibrium costant is to estimate the important parameter (Journal ofcolloid and interface science.2011,360:760 ~ 767) of absorption property.Pollute to control and these parameters of chemical analysis technology field can be estimated the information (Journal of chromatographyA.2007,1145:133 ~ 140) such as the absorption property of adsorbent and range of application.Document " Journal of colloid and interface science.2009; 330:1 ~ 8 ", adopt By Batch Equilibrium Method to measure adsorpting data, match 1,3-dinitro benzene, nitrotoluene, nitrophenol and nitrobenzene Langmuir and the Freundlich adsorption isothermal on multi-walled carbon nano-tubes, calculate simultaneously the thermodynamic parameters such as free energy change Δ G, enthalpy change Δ H, Entropy Changes Δ S, thereby characterized the absorption property of multi-walled carbon nano-tubes to nitroaromatic.By Batch Equilibrium Method is a kind of method of measuring absorption property, but has Separation of Solid and Liquid difficulty, complex steps, the shortcoming such as waste time and energy.Existing chemicals of a great variety, carbon nano-tube is difficult to measure one by one to the absorption property of variety classes organic compound, has restricted carbon nano-tube and has controlled and the application of chemical analysis field polluting.
By measuring the chromatogram retention factors, the method that obtains thermodynamic parameter and adsorption isothermal is simple.Document " Journal of chromatographyA.2007; 1145:133 ~ 140 " adopts van ' t Hoff equation, a series of palycyclic aromatic PAHs have been calculated at the anti-phase fixedly phase of phenyl class (C18, C18Aqua, Propyl-phenyl, Synergi polar-RP) the upper thermodynamic parameter that keeps has compared palycyclic aromatic at the anti-phase fixing retention behavior of going up mutually of difference.Document " Journal ofchromatographyA.2005; 1099:1 ~ 42 " points out to utilize chromatography can accurately obtain the adsorption isothermal of one matter, comprising: frontal analysis Frontal Analysis, Capillary Electrophoresis frontal analysis Capillary Electrophoresis Frontal Analysis, impulse method Pulse Methods, unique point elution method Elution by Characteristic Points.In the stratographic analysis field, the adsorption isothermal that chromatography obtains can be used for prediction overload spectrogram, estimate surface property (the Journal of chromatographyA.2002 of chromatographic column fixed phase, 978:81 ~ 107), in the Pharmaceutical Analysis field, frontal analysis is usually used in measuring the binding ability (Electrophoresis.2008 of medicine-plasma proteins, 29:2876 ~ 2883), wherein, frontal analysis have advantages of to detector sensitivity and chromatogram column efficiency require lowly, be to be widely used in the chromatographic process of measuring the one matter adsorption isothermal.At present, there is no based on the carbon nano-tube chromatographic column, adopt van ' t Hoff equation and liquid chromatography frontal analysis to measure the report of carbon nanotube adsorption performance.Therefore, set up a kind of thermodynamic parameter that multiple organic compound keeps and method of adsorption isothermal of fast, efficiently obtaining based on chromatography on carbon nano-tube, significant.
Summary of the invention
The invention provides thermodynamic parameter that a kind of quick acquisition organic compound keeps and the method for adsorption isothermal on carbon nano-tube.The method has advantages of accurately, quick, reagent dosage is few, pollution-free, be easy to Separation of Solid and Liquid, have important references value to estimating the carbon nanotube adsorption performance, significant in the application in the fields such as water pollution improvement, sample pre-treatments and analytical test as sorbing material for carbon nano-tube.
Technical scheme of the present invention is as follows:
The first step: preparation carbon nano-tube liquid-phase chromatographic column, choose 4.6 * 50mm stainless steel column chromatography post, the loading of carbon nano-tube is controlled at the 250mg left and right, and excessive carbon nano-tube can cause post to press too high and absorption-desorption overlong time, affects separating effect.Concrete preparation method is as follows:
(1) dress post: adopt the high-pressure homogenization method to load, at first stainless steel chromatogram post is carried out leak test and cleaning; Unload the column cap of the empty chromatographic column entrance of cleaning-drying, chromatographic column is received on the pre-column that is connected with the homogenate tank; Keep column jecket to be on vertical direction, guarantee that airtight performance is good, avoid high pressure lower prop Joint's falling off.
(2) preparation homogenate: take the 250mg carbon nano-tube in the glass conical flask of 50ml, can choose the carbon nano-tube of purity 95%, external diameter 3 ~ 10nm, length 5 ~ 20nm; Prepare the carbon nano-tube homogenate with dimethyl formamide as spreading agent, be placed in the ultrasonic 10min of ultrasound bath, obtain the carbon nano-tube homogenate that fully disperses.
(3) chromatography column: the wall carbon nano tube homogenate is poured into rapidly in the homogenate tank, then with displacement fluid, the homogenate tank is filled up, use the Pneumatic constant press pump to prepare the carbon nano-tube liquid-phase chromatographic column, until the homogenate that flows out surpasses 80ml, close the Pneumatic constant press pump, treat that the homogenate tank drops to normal pressure naturally; Unload chromatographic column, mounted sieve and chromatographic column joint, mark chromatographic column importer to; Chromatographic column is accessed high performance liquid chromatography, replacement solvent balance chromatographic column.
Second step: in the carbon nano-tube liquid chromatography packed column access high performance liquid chromatography with preparation, flow velocity 0.15ml/min, sample concentration 1g/L, sample size 1 μ L, record detector signal, according to following formula (1), measure the retention time of organic compound on the carbon nano-tube liquid-phase chromatographic column calculate Retention factor k '
k′=(t
R-t
0)/t
0 (1)
Wherein k' is the retention factors of organic compound on chromatographic column; t
R, t
0It is respectively retention time and the dead time of organic compound.
Calculate the reservation thermodynamic parameter of organic compound on the carbon nano-tube liquid-phase chromatographic column according to van ' t Hoff equation (2)
Wherein Δ H ° and Δ S ° is respectively that solute is at Entropy Changes and the enthalpy change of alternate migration; T is thermodynamic temperature; R is mol gas constant; φ is the fixedly phase of chromatographic column and the volume ratio of mobile phase.Adopt weight method, can calculate φ by formula (3)
V wherein
sAnd V
mRespectively stationary phase volume and mobile phase volume.
According to equation (4), calculate Gibbs free energy (Δ G °)
ΔG°=ΔH°-TΔS° (4)
Adopt high performance liquid chromatography-frontal analysis, according to the saturated extent of adsorption (q of equation (5) unit of account volume carbon nano-tube
*)
F wherein
vFlow velocity for mobile phase; t
eq.Be the time of equivalent area; t
hBe the residence time in post; t
eBe pump dead time outside chromatographic column between detecting device; V
cFree column volume for chromatographic column; C
eBe liquid equilibrium concentration (g/L).
According to q
*And C
e, adopt Linear equation (6) and Freundlich equation (7) match adsorption isothermal
q
*=K
LC
e+a (6)
Wherein, K
LAnd K
FBe respectively Linear and Freundlich adsorption equilibrium costant; N is the Freundlich index; A is constant.
Beneficial effect of the present invention is as follows:
1. the carbon nano-tube liquid-phase chromatographic column of preparation has more excellent stability, absorption property that can the multiple organic compound of analytical test.
2. use high performance liquid chromatography simple to operate, be easy to Separation of Solid and Liquid, the carbon nano-tube liquid-phase chromatographic column of preparation can Reusability, reduces a large amount of uses of medicine and solvent, avoids environmental pollution.
3. the thermodynamic parameter and the adsorption isothermal that can the quick obtaining organic compound keep on carbon nano-tube of the method, estimate carbon nano-tube to the absorption property of organic compound.
Description of drawings
Fig. 1 (a) is under the same terms, and toluene repeats sample introduction at the liquid chromatogram of multi-walled carbon nano-tubes liquid-phase chromatographic column upward stability through three times.
Fig. 1 (b) is under the same terms, and toluene repeats sample introduction at the liquid chromatogram of multi-walled carbon nano-tubes liquid-phase chromatographic column upward stability through three times.
Fig. 2 acetonitrile mutually in organism in the strength retention lnk' of the multi-walled carbon nano-tubes liquid-phase chromatographic column variation with temperature 1/T.
The Freundlich adsorption isothermal of Sulfamethoxazole on the multi-walled carbon nano-tubes liquid-phase chromatographic column that Fig. 3 obtains according to breakthrough curve.
The concentration that Fig. 4 frontal analysis is measured is 3.00 * 10
-3The breakthrough curve schematic diagram of the Sulfamethoxazole solution of g/L.
Embodiment
The leak test of packed column and cleaning: choose 4.6 * 50mm stainless steel column chromatography post, void column should guarantee that two ends are smooth and without burr; Column jecket outlet is blocked submerge, carrier gas passes into the import of stainless steel column under condition of high voltage, and whether observe packed column has bubble to emerge, if bubble this packed column gas leakage of explanation of emerging is arranged, can not use; Use washed with methanol, remove the surperficial grease of column jecket, then rinse well with tap water, use at last distilled water, acetone rinsing, finish-drying is standby in baking oven.
Chromatography column: adopt high-pressure homogenization method chromatography column, take the 250mg multi-walled carbon nano-tubes in the glass conical flask of 50ml, can choose the multi-walled carbon nano-tubes of purity 95%, external diameter 3 ~ 10nm, length 5 ~ 20nm; Add the 30ml dimethyl formamide in conical flask, be placed in the ultrasonic 10min of ultrasound bath, obtain the fully multi-walled carbon nano-tubes homogenate of dispersion, homogenate is poured into rapidly in the homogenate tank, then with acetone, the homogenate tank is filled up, open immediately the Pneumatic constant press pump after sealing, stuffing pressure 0 ~ 50MPa, the homogenate that flows out surpasses 80ml, close the Pneumatic constant press pump, treat that the homogenate tank drops to normal pressure naturally, unloads chromatographic column, mounted sieve and chromatographic column joint, the import of the good multi-walled carbon nano-tubes liquid-phase chromatographic column of mark.
Chromatographic column balance: with multi-walled carbon nano-tubes liquid-phase chromatographic column access high performance liquid chromatography, under 25 ℃, use 100% acetonitrile as mobile phase, with flow velocity balance chromatographic column 10 ~ 12h of 0.1ml/min, until system's baseline stability.
Detection of Stability: take methyl alcohol as solvent, the benzene of configuration 1g/L, the solution of toluene are under 25 ℃ of conditions, use 100% acetonitrile as mobile phase, flow velocity 0.2ml/min, sample size 1 μ L uses diode array detector (DAD detecting device), ultraviolet detects wavelength 210nm, record the chromatographic peak of benzene, toluene, triplicate sample introduction, the reappearance of the chromatographic peak of observation test sample, result shows that the reappearance of chromatographic peak of benzene, toluene is better, as Fig. 1 (a), Fig. 1 (b).
After system's baseline stability, under 20 ℃ of conditions, take 100% acetonitrile as mobile phase, flow velocity 0.15ml/min, sample size 1 μ L uses diode array detector (DAD detecting device), and it is 254nm that ultraviolet detects wavelength, as the dead time label, measure the dead time t of multi-walled carbon nano-tubes liquid-phase chromatographic column with acetone
0, take methyl alcohol as solvent, the phenol solution of configuration 1g/L, it is 230nm that ultraviolet detects wavelength, other conditions are identical, measure the retention time t of phenol on the multi-walled carbon nano-tubes liquid-phase chromatographic column
R, according to formula (1) calculate the Retention factor k of 25 ℃ of lower phenol '.
The temperature of setting column oven is 25 ℃, 30 ℃, 35 ℃, 40 ℃, 45 ℃ respectively, other conditions are constant, measure the k' of phenol on multi-walled carbon nano-tubes under different temperatures, lnk' and 1/T linear fit with six temperature spots obtaining, obtain Δ H ° for-8.58kJ/mol and Δ S ° are-8.79J/molk, when calculating 25 ℃ according to equation (3), the Δ G of phenol ° is-5.96kJ/mol.
After system's baseline stability, under 20 ℃ of conditions, take 100% acetonitrile as mobile phase, flow velocity 0.15ml/min, sample size 1 μ L uses diode array detector (DAD detecting device), and it is 254nm that ultraviolet detects wavelength, with acetone as the dead time label, t when measuring multi-walled carbon nano-tubes liquid-phase chromatographic column dead
0, take methyl alcohol as solvent, the sulfadimidine solution of configuration 1g/L, it is 265nm that ultraviolet detects wavelength, other conditions are identical, measure the retention time t of sulfadimidine on the multi-walled carbon nano-tubes liquid-phase chromatographic column
R, according to formula (1) calculate 25 ℃ of lower sulfadimidines Retention factor k '.
The temperature of setting column oven is 25 ℃, 30 ℃, 35 ℃, 40 ℃, 45 ℃ respectively, other conditions are constant, measure the k' of sulfadimidine on multi-walled carbon nano-tubes under different temperatures, lnk' and 1/T linear fit with six temperature spots obtaining, obtain Δ H ° for-16.29kJ/mol and Δ S ° are-31.54J/molk, when calculating 25 ℃ according to equation (3), the Δ G of sulfadimidine ° is-6.88kJ/mol.
Embodiment 4
After system's baseline stability, under 20 ℃ of conditions, take 100% methyl alcohol as mobile phase, flow velocity 0.15ml/min, sample size 1 μ L uses diode array detector (DAD detecting device), and it is 254nm that ultraviolet detects wavelength, as the dead time label, measure the dead time t of multi-walled carbon nano-tubes liquid-phase chromatographic column with acetone
0, take methyl alcohol as solvent, the toluene solution of configuration 1g/L, it is 210nm that ultraviolet detects wavelength, other conditions are identical, measure the retention time t of toluene on the multi-walled carbon nano-tubes liquid-phase chromatographic column
R, according to formula (1) calculate the Retention factor k of 25 ℃ of Toluenes '.
The temperature of setting column oven is 25 ℃, 30 ℃, 35 ℃, 40 ℃, 45 ℃ respectively, other conditions are constant, measure the k' of different temperatures Toluene on multi-walled carbon nano-tubes, lnk' and 1/T linear fit with six temperature spots obtaining, obtain Δ H ° for-6.54kJ/mol and Δ S ° are-5.57J/molk, when calculating 25 ℃ according to equation (3), the Δ G of toluene ° is-4.88kJ/mol.
After system's baseline stability, under 20 ℃ of conditions, take 100% methyl alcohol as mobile phase, flow velocity 0.15ml/min, sample size 1 μ L uses diode array detector (DAD detecting device), and it is 254nm that ultraviolet detects wavelength, as the dead time label, measure the dead time t of multi-walled carbon nano-tubes liquid-phase chromatographic column with acetone
0, take methyl alcohol as solvent, the bromobenzene solution of configuration 1g/L, it is 230nm that ultraviolet detects wavelength, other conditions are identical, measure the retention time t of bromobenzene on the multi-walled carbon nano-tubes liquid-phase chromatographic column
R, according to formula (1) calculate 25 ℃ of lower bromobenzenes Retention factor k '.
The temperature of setting column oven is 25 ℃, 30 ℃, 35 ℃, 40 ℃, 45 ℃ respectively, other conditions are constant, measure the k' of bromobenzene on multi-walled carbon nano-tubes under different temperatures, lnk' and 1/T linear fit with six temperature spots obtaining, obtain Δ H ° for-11.22kJ/mol and Δ S ° are-18.51J/molk, when calculating 25 ℃ according to equation (3), the Δ G of bromobenzene ° is-5.70kJ/mol.
Embodiment 6
Use 4.6 * 50mm multi-walled carbon nano-tubes liquid-phase chromatographic column, the free column volume V of chromatographic column
cBe 0.83ml; Use two kinds of different solvents of density of pure water and acetonitrile, adopt mobile phase volume V in weight method computer chromatography post
mBe 0.78ml, flow velocity is under the condition of 0.15ml/min, calculates residence time t in post
hBe 5.20min; At identical flow velocity, do not connect under the condition of chromatographic column, take acetone as probe molecule, record pump dead time t outside chromatographic column between detecting device
eBe 4.95min.
Take methyl alcohol as solvent, configuration concentration is 4.00 * 10
-3The Sulfamethoxazole stock solution of g/L and 0.1g/L, as mobile phase, Sulfamethoxazole and methyl alcohol mix by a certain percentage, and can to obtain concentration range be 2.00 * 10 with Sulfamethoxazole solution and methanol solvate
-5The Sulfamethoxazole solution of ~ 0.1g/L.Under 30 ℃, flow velocity with 0.15ml/min passes through chromatographic column, uses diode array detector (DAD detecting device), and it is 254nm that ultraviolet detects wavelength, record the breakthrough curve of Sulfamethoxazole, corresponding Sulfamethoxazole concentration is its equilibrium concentration C until detector signal tends towards stability
e, and think that multi-walled carbon nano-tubes is saturated to the absorption arrival of Sulfamethoxazole at this moment.Calculate the saturated extent of adsorption q of Sulfamethoxazole on the unit volume multi-walled carbon nano-tubes under specific concentrations according to equation (5)
*For example: when mobile phase by 75% 4.00 * 10
-3The solution of the Sulfamethoxazole of g/L and 25% methyl alcohol form, and can obtain concentration after mixing is 3.00 * 10
-3The Sulfamethoxazole solution of g/L, the breakthrough curve of Sulfamethoxazole under this concentration of detector recording, be 71.62min when the time, breakthrough curve forms, the detection signal that records this moment is 104.20mAu, this moment, multi-walled carbon nano-tubes was saturated to the absorption arrival of Sulfamethoxazole, the equilibrium concentration (C of corresponding Sulfamethoxazole
e=3.00 * 10
-3G/L).Breakthrough curve (Fig. 3) left side represents the amount of multi-walled carbon nano-tubes absorption Sulfamethoxazole, the right side represents that Sulfamethoxazole flows out the amount of chromatographic column with mobile phase, by the integration of chromatographic work station to breakthrough curve right side area, can obtain the amount that Sulfamethoxazole flows out chromatographic column is 2.46 * 10
5MAus, according to the equivalent area principle, under the constant condition of equilibrium concentration, can converse the saturated equivalent time of multi-walled carbon nano-tubes absorption is 32.27min, calculates under this concentration conditions the q of multi-walled carbon nano-tubes to Sulfamethoxazole according to equation (5)
*Be 4.06 * 10
-4G/L.
According to the q that records
*And C
e, by equation (7), match Freundlich adsorption isothermal (Fig. 4) obtains q
*=0.171C
e 1.032, R
2=0.999, K
FBe 0.171 (g/L)
(1-n)
Claims (1)
- One kind obtain organic compound on the carbon nanometer the reservation thermodynamic parameter and the method for adsorption isothermal, it is characterized in that comprising the following steps:The first step: preparation carbon nano-tube liquid-phase chromatographic column, choose 4.6 * 50mm chromatographic column, adopt the filling of high-pressure homogenization method, the loading of carbon nano-tube is controlled at 250mg; Use dimethyl formamide to prepare the carbon nano-tube homogenate as solvent, homogenate is poured into rapidly in the homogenate tank, then with displacement fluid, the homogenate tank is filled up, open immediately the Pneumatic constant press pump after sealing, chromatography column, unload chromatographic column, mounted sieve and chromatographic column joint, the import of the good chromatographic column of mark; Chromatographic column is connected high performance liquid chromatography, choose acetonitrile as replacement solvent, with the flow velocity balance chromatographic column of 0.1ml/min; Record at last the chromatographic peak that specimen keeps on chromatographic column through repeating sample introduction, the stability of check carbon nano-tube post separating property;Second step: the carbon nano-tube liquid-phase chromatographic column access high performance liquid chromatography with above-mentioned preparation, record the liquid chromatogram detector signal;The flow velocity that mobile phase is set is 0.15ml/min, sample size 1 μ L, and sample concentration 1g/L measures the chromatographic retention of organic compound in the carbon nano-tube chromatographic column under different temperatures, the calculating Retention factor k '; According to equation (1) and equation (2), calculate the reservation thermodynamic parameter of compound in the carbon nano-tube chromatographic column;ΔG°＝ΔH°-TΔS° (2)Wherein, Δ H ° and Δ S ° is respectively that solute is at Entropy Changes and the enthalpy change of alternate migration; Δ G ° is Gibbs free energy; T is thermodynamic temperature; R is mol gas constant; φ is the volume ratio of fixing and mobile phase in chromatographic column;Adopt high performance liquid chromatography-frontal analysis, obtain the breakthrough curve of compound under different liquid concentrations, according to the saturated extent of adsorption q of equation (3) unit of account volume carbon nano-tube *According to Linear equation (4) and Freundlich equation (5) match adsorption isothermal, calculate adsorption equilibrium costant;F wherein vFlow velocity for mobile phase; t eq.Be the time of equivalent area; t hBe the residence time in post; t eBe pump dead time outside chromatographic column between detecting device; V cFree column volume for chromatographic column; C eBe liquid equilibrium concentration (g/L);q *＝K LC e+a (4)Wherein, K LAnd K FBe respectively Linear and Freundlich adsorption equilibrium costant; N is the Freundlich index; A is constant.
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| CN112313511A (en) * | 2018-04-20 | 2021-02-02 | 詹森生物科技公司 | Column identification in a manufacturing Process for preparing an anti-IL 12/IL23 antibody composition |
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| CN108318595B (en) * | 2018-01-15 | 2020-11-06 | 北京建筑大学 | Method for measuring adsorption equilibrium constant in colloidal solution |
| CN112313511A (en) * | 2018-04-20 | 2021-02-02 | 詹森生物科技公司 | Column identification in a manufacturing Process for preparing an anti-IL 12/IL23 antibody composition |
| CN113804810A (en) * | 2020-06-15 | 2021-12-17 | 浙江科技学院 | Chromatographic separation column and method for detecting VOCs gas chromatography |
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