Combination method of polymer carbon nanotube chromatographic column and ion chromatography single pump column switching technology
A technology for switching ion chromatography columns and single-pump columns, which is applied in the field of ion chromatography single-pump column switching, can solve problems such as long retention time and limited application range, and achieve the effects of accelerating analysis speed, saving analysis time, and simplifying equipment
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Embodiment 1
[0033] Embodiment 1: the making process of polymer carbon nanotube composite chromatographic filler is as follows, and its steps are:
[0034] (1) Synthesize 1.8 μm monodisperse polystyrene seed by dispersion polymerization method earlier, monomer concentration is 20%, stabilizer concentration is 3%, initiator consumption is 4% of monomer, and reaction medium is 95% ethanol aqueous solution, The reaction temperature was 70°C, the stirring speed was 250 rpm, and the reaction time was 24 hours.
[0035] (2) 50 mg of multi-walled carbon nanotubes were oxidized with 200 mL of concentrated sulfuric acid / concentrated nitric acid=3:1 (v / v) mixed acid solution, ultrasonicated at 35° C. for 6 hours, washed until neutral and then dried. Then, monodisperse polystyrene-divinylbenzene-carbon nanotube composite microspheres with a crosslinking degree of 55% were prepared by seed swelling method. The concentration of the monomer is 10%, the content of carbon nanotubes accounts for 1% of the...
Embodiment 2
[0037] Example 2: The specific detection steps of polymer carbon nanotube composite chromatography and ion chromatography single-pump column switching are as follows:
[0038] 1) Set the system according to figure 1 Well connected: the pump 1 is connected to the eluent generator 2, then the eluent passes through the six-way valve 3, connects the guard column 12 and the analysis column 13, passes through the suppressor 6, enters the detector 7 for detection, and then passes through the ten-way valve 4 is connected with the pretreatment column 11, and finally enters the waste liquid bottle 10. A 200 μL quantitative loop 5 is connected to the ten-way valve 4 , and the entire system is protected by nitrogen gas, 14 is a nitrogen cylinder, and a concentration column 8 is connected to the six-way valve 3 . After pump 1 was filled with mobile phase, it was turned on at a flow rate of 0.5 mL / min. The nitrogen gas 14 for protection is opened to a pressure of about 5 psi. Detector 7 ...
Embodiment 3
[0044] Embodiment 3: This embodiment is to analyze seven kinds of common inorganic anion mixed standard samples with column switching technology
[0045] Instruments used: ion chromatograph; chromatographic pump; conductivity detector; chromatographic workstation; one six-way valve; one ten-way valve; high-purity nitrogen cylinder; analytical column; guard column; enrichment column; 200 μL injection volume; electrochemical Self-regenerating suppressor.
[0046] Pretreatment column: use the polymer carbon nanotube composite filler in Example 1 to fill in a 4.6×150mm stainless steel column.
[0047] Eluent: H 2 O, KOH eluent generator concentration: 18mM, suppressor current: 90mA, flow rate 0.65mL / min.
[0048] Analysis steps:
[0049] (1) Baseline surveying and mapping
[0050] The eluent is pumped into the chromatographic separation column to achieve equilibrium, and the eluent output from the chromatographic separation column is converted into an electrical signal by the ...
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