CN103163237B - 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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- CN103163237B CN103163237B CN201310043531.4A CN201310043531A CN103163237B CN 103163237 B CN103163237 B CN 103163237B CN 201310043531 A CN201310043531 A CN 201310043531A CN 103163237 B CN103163237 B CN 103163237B
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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 reservation thermodynamic parameter and adsorption isothermal by the retention time of organic compound in carbon nano-tube chromatographic column under mensuration different temperatures, belong to 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 to original position reparation and the sample analysis of environmental pollution control, pollution at environmental area, 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 Novel adsorption filler.Therefore, the Fast Measurement of carbon nano-tube to organic compound absorption, contributes to carbon nano-tube application in wastewater treatment and chemical analysis field as adsorbent.
Retaining thermodynamic parameter, saturated extent of adsorption and adsorption equilibrium costant is to evaluate the important parameter (Journal ofcolloid and interface science.2011,360:760 ~ 767) of absorption property.Control and these parameters of chemical analysis technology field can be evaluated the information such as absorption property and range of application (Journal of chromatographyA.2007,1145:133 ~ 140) of adsorbent polluting.Document " Journal of colloid and interface science.2009; 330:1 ~ 8 ", adopt By Batch Equilibrium Method to measure adsorpting data, matching 1,3-dinitro benzene, nitrotoluene, nitrophenol and nitrobenzene Langmuir and the Freundlich adsorption isothermal on multi-walled carbon nano-tubes, calculate the thermodynamic parameters such as free energy change Δ G, enthalpy change Δ H, Entropy Changes Δ S simultaneously, 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 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 are calculated at the anti-phase fixing phase (C18 of phenyl class, C18Aqua, Propyl-phenyl, Synergi polar-RP) the upper thermodynamic parameter retaining, 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 stratographic analysis field, the adsorption isothermal that chromatography obtains can be used for prediction overload spectrogram, evaluate surface property (the Journal of chromatographyA.2002 of chromatographic column fixed phase, 978:81 ~ 107), in 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 one matter adsorption isothermal.At present, there is no based on 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 retains in carbon nano-tube and method of adsorption isothermal of fast, efficiently obtaining based on chromatography, significant.
Summary of the invention
The invention provides thermodynamic parameter that a kind of quick acquisition organic compound retains in carbon nano-tube and the method for adsorption isothermal.The method has advantages of accurately, quick, reagent dosage is few, pollution-free, be easy to Separation of Solid and Liquid, there is important references value to evaluating 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 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 high-pressure homogenization method to load, first stainless steel chromatogram post is carried out to 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 being connected with homogenate tank; Keep column jecket in vertical direction, ensure that airtight performance is good, avoid high pressure lower prop Joint's falling off.
(2) prepare homogenate: take 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 carbon nano-tube homogenate using dimethyl formamide as spreading agent, be placed in the ultrasonic 10min of ultrasound bath, obtain the carbon nano-tube homogenate fully disperseing.
(3) chromatography column: wall carbon nano tube homogenate is poured into rapidly in homogenate tank, then with displacement fluid, homogenate tank is filled up, use Pneumatic constant press pump to prepare carbon nano-tube liquid-phase chromatographic column, until the homogenate flowing out exceedes 80ml, close Pneumatic constant press pump, treat that 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 to high performance liquid chromatography, replacement solvent balance chromatographic column.
Second step: by the carbon nano-tube liquid chromatography packed column access high performance liquid chromatography of 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 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 in 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 carbon nano-tube liquid-phase chromatographic column according to van ' t Hoff equation (2)
Wherein Δ H ° and Δ S ° is respectively Entropy Changes and the enthalpy change of solute in alternate migration; T is thermodynamic temperature; R is mol gas constant; φ is the fixing phase of chromatographic column and the volume ratio of mobile phase.Adopt weight method, can calculate φ by formula (3)
Wherein V
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
*)
Wherein F
vfor the flow velocity of mobile phase; t
eq.for the time of equivalent area; t
hfor the residence time in post; t
efor pump dead time outside chromatographic column between detecting device; V
cfor the free column volume of chromatographic column; C
efor liquid equilibrium concentration (g/L).
According to q
*and C
e, adopt Linear equation (6) and Freundlich equation (7) matching adsorption isothermal
q
*=K
LC
e+a (6)
Wherein, K
land K
fbe respectively Linear and Freundlich adsorption equilibrium costant; N is 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 preferably 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 method can quick obtaining organic compound retains in carbon nano-tube thermodynamic parameter and adsorption isothermal, evaluate the absorption property of carbon nano-tube to organic compound.
Brief description of the drawings
Fig. 1 (a) is under the same terms, and toluene repeats the liquid chromatogram of sample introduction in 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 the liquid chromatogram of sample introduction in multi-walled carbon nano-tubes liquid-phase chromatographic column upward stability through three times.
Fig. 2 acetonitrile mutually in organism variation with temperature 1/T at the strength retention lnk' of multi-walled carbon nano-tubes liquid-phase chromatographic column.
The Freundlich adsorption isothermal of the Sulfamethoxazole that Fig. 3 obtains according to breakthrough curve on multi-walled carbon nano-tubes liquid-phase chromatographic column.
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
Embodiment 1
The leak test of packed column and cleaning: choose 4.6 × 50mm stainless steel column chromatography post, void column should ensure that two ends are smooth and without burr; Column jecket outlet is blocked and submerged, and 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 there is bubble to emerge, this packed column gas leakage is described, can not use; By washed with methanol, remove column jecket surface grease, then rinse well with tap water, finally use distilled water, acetone rinsing, in baking oven, finish-drying is for subsequent use.
Chromatography column: adopt high-pressure homogenization method chromatography column, take 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; In conical flask, add 30ml dimethyl formamide, be placed in the ultrasonic 10min of ultrasound bath, obtain the multi-walled carbon nano-tubes homogenate fully disperseing, homogenate is poured into rapidly in homogenate tank, then with acetone, homogenate tank is filled up, after sealing, open immediately Pneumatic constant press pump, stuffing pressure 0 ~ 50MPa, the homogenate flowing out exceedes 80ml, close Pneumatic constant press pump, treat that 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: by multi-walled carbon nano-tubes liquid-phase chromatographic column access high performance liquid chromatography, at 25 DEG C, use 100% acetonitrile as mobile phase, with flow velocity balance chromatographic column 10 ~ 12h of 0.1ml/min, until system baseline stability.
Detection of Stability: taking methyl alcohol as solvent, the benzene of configuration 1g/L, the solution of toluene, under 25 DEG C of conditions, use 100% acetonitrile as mobile phase, flow velocity 0.2ml/min, sample size 1 μ L, use diode array detector (DAD detecting device), ultraviolet detects wavelength 210nm, record the chromatographic peak of benzene, toluene, sample introduction in triplicate, 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).
Embodiment 2
After system baseline stability, under 20 DEG C of conditions, taking 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, using acetone as dead time label, measure the dead time t of multi-walled carbon nano-tubes liquid-phase chromatographic column
0, taking 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 multi-walled carbon nano-tubes liquid-phase chromatographic column
r, according to formula (1) calculate the Retention factor k of phenol at 25 DEG C '.
The temperature of setting column oven is 25 DEG C, 30 DEG C, 35 DEG C, 40 DEG C, 45 DEG C respectively, other conditions are constant, measure the k' of phenol on multi-walled carbon nano-tubes under different temperatures, by the lnk' of six temperature spots that obtain and 1/T linear fit, obtain Δ H ° for-8.58kJ/mol and Δ S ° are-8.79J/molk, while calculating 25 DEG C according to equation (3), the Δ G of phenol ° is-5.96kJ/mol.
Embodiment 3
After system baseline stability, under 20 DEG C of conditions, taking 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, using acetone as dead time label, t while measuring multi-walled carbon nano-tubes liquid-phase chromatographic column dead
0, taking 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 multi-walled carbon nano-tubes liquid-phase chromatographic column
r, according to formula (1) calculate sulfadimidine at 25 DEG C Retention factor k '.
The temperature of setting column oven is 25 DEG C, 30 DEG C, 35 DEG C, 40 DEG C, 45 DEG C respectively, other conditions are constant, measure the k' of sulfadimidine on multi-walled carbon nano-tubes under different temperatures, by the lnk' of six temperature spots that obtain and 1/T linear fit, obtain Δ H ° for-16.29kJ/mol and Δ S ° are-31.54J/molk, while calculating 25 DEG C according to equation (3), the Δ G of sulfadimidine ° is-6.88kJ/mol.
Embodiment 4
After system baseline stability, under 20 DEG C of conditions, taking 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, using acetone as dead time label, measure the dead time t of multi-walled carbon nano-tubes liquid-phase chromatographic column
0, taking 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 multi-walled carbon nano-tubes liquid-phase chromatographic column
r, according to formula (1) calculate 25 DEG C of Toluenes Retention factor k '.
The temperature of setting column oven is 25 DEG C, 30 DEG C, 35 DEG C, 40 DEG C, 45 DEG C respectively, other conditions are constant, measure the k' of different temperatures Toluene on multi-walled carbon nano-tubes, by the lnk' of six temperature spots that obtain and 1/T linear fit, obtain Δ H ° for-6.54kJ/mol and Δ S ° are-5.57J/molk, while calculating 25 DEG C according to equation (3), the Δ G of toluene ° is-4.88kJ/mol.
After system baseline stability, under 20 DEG C of conditions, taking 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, using acetone as dead time label, measure the dead time t of multi-walled carbon nano-tubes liquid-phase chromatographic column
0, taking 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 multi-walled carbon nano-tubes liquid-phase chromatographic column
r, according to formula (1) calculate bromobenzene at 25 DEG C Retention factor k '.
The temperature of setting column oven is 25 DEG C, 30 DEG C, 35 DEG C, 40 DEG C, 45 DEG C respectively, other conditions are constant, measure the k' of bromobenzene on multi-walled carbon nano-tubes under different temperatures, by the lnk' of six temperature spots that obtain and 1/T linear fit, obtain Δ H ° for-11.22kJ/mol and Δ S ° are-18.51J/molk, while calculating 25 DEG C 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
cfor 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
mfor 0.78ml, under the condition that flow velocity is 0.15ml/min, calculate residence time t in post
hfor 5.20min; At identical flow velocity, do not connect under the condition of chromatographic column, taking acetone as probe molecule, record pump dead time t outside chromatographic column between detecting device
efor 4.95min.
Taking methyl alcohol as solvent, configuration concentration is 4.00 × 10
-3the Sulfamethoxazole stock solution of g/L and 0.1g/L, using Sulfamethoxazole solution and methanol solvate as mobile phase, Sulfamethoxazole and methyl alcohol mix by a certain percentage, and can to obtain concentration range be 2.00 × 10
-5the Sulfamethoxazole solution of ~ 0.1g/L.At 30 DEG C, 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, until the Sulfamethoxazole concentration that detector signal tends towards stability corresponding is its equilibrium concentration C
e, and think that now multi-walled carbon nano-tubes arrives saturated to the absorption of Sulfamethoxazole.Calculate the saturated extent of adsorption q of Sulfamethoxazole on unit volume multi-walled carbon nano-tubes under certain concentration 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 composition, after mixing, can obtain concentration 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, now multi-walled carbon nano-tubes is 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, right side represents that Sulfamethoxazole flows out the amount of chromatographic column with mobile phase, integration by chromatographic work station to breakthrough curve right side area, the amount that can obtain Sulfamethoxazole outflow chromatographic column is 2.46 × 10
5mAus, according to equivalent area principle, under the constant condition of equilibrium concentration, can conversing multi-walled carbon nano-tubes, to adsorb saturated equivalent time be 32.27min, calculate 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 recording
*and C
e, by equation (7), matching 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)
1. obtain the reservation thermodynamic parameter of organic compound in carbon nano-tube and a 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 carbon nano-tube homogenate for solvent, homogenate is poured into rapidly in homogenate tank, then with displacement fluid, homogenate tank is filled up, after sealing, open immediately Pneumatic constant press pump, chromatography column, unload chromatographic column, mounted sieve and chromatographic column joint, the import of the good chromatographic column of mark; Chromatographic column is connected to high performance liquid chromatography, choose acetonitrile as replacement solvent, with the flow velocity balance chromatographic column of 0.1mL/min; The chromatographic peak that finally record test sample retains in chromatographic column through repeating sample introduction, the stability of inspection carbon nano-tube post separating property;
Second step: by the carbon nano-tube liquid-phase chromatographic column access high performance liquid chromatography of above-mentioned preparation, record 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 carbon nano-tube chromatographic column under different temperatures, calculating Retention factor k '; According to equation (1) and equation (2), calculate the reservation thermodynamic parameter of compound in carbon nano-tube chromatographic column;
ΔG°＝ΔH°-TΔS° (2)
Wherein, Δ H ° and Δ S ° is respectively enthalpy change and the Entropy Changes of solute in 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) matching adsorption isothermal, calculate adsorption equilibrium costant;
Wherein F
vfor the flow velocity of mobile phase; t
eq.for the time of equivalent area; t
hfor the residence time in post; t
efor pump dead time outside chromatographic column between detecting device; V
cfor the free column volume of chromatographic column; C
efor 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 Freundlich index; A is constant.
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