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Method for combining technologies of polymer carbon nano tube chromatographic column and ion chromatographic column switching

An ion chromatographic column and carbon nanotube technology, which is applied in the field of polymer carbon nanotube chromatographic column and ion chromatographic column switching technology. Realize, increase analysis cost and other issues, achieve the effect of shortening time, saving analysis time, and simple method

Inactive Publication Date: 2010-10-20
ZHEJIANG UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Commonly used ion chromatography column switching pretreatment columns are often ion exclusion columns and ion exchange columns. The former is often used to eliminate the matrix of weakly ionized compounds, such as organic acids and weak acid matrices. However, for the weakly ionized inorganic anions commonly found in these matrices, For example, the detection of fluoride ion and phosphate ion is difficult to achieve
The latter is used to eliminate high-concentration organic solvents and high-salt matrices, but cannot be directly measured for water-insoluble solvents, and additional sample preparation steps are required
In addition, all these online sample pretreatment systems cannot realize the analysis and detection of organic solvents, organic acids and organic acid salts samples on the same pretreatment column, and need to change the pretreatment column according to the nature of the sample, which undoubtedly increases the analysis time. cost

Method used

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  • Method for combining technologies of polymer carbon nano tube chromatographic column and ion chromatographic column switching
  • Method for combining technologies of polymer carbon nano tube chromatographic column and ion chromatographic column switching
  • Method for combining technologies of polymer carbon nano tube chromatographic column and ion chromatographic column switching

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] The production process of the polymer carbon nanotube composite chromatographic filler is as follows, and the steps are:

[0045] (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.

[0046] (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 monom...

Embodiment 2

[0049] The specific detection steps of polymer carbon nanotube composite chromatography combined with ion chromatography are as follows:

[0050] (1) Set the system according to figure 2 Connected. The first pump 1 is connected to the first six-way valve 3; the enrichment column 10 is connected to the second six-way valve 4; the second six-way valve 4 is connected to the guard column 11, ion exclusion column 12, waste liquid bottle 7, The pump 2 is connected; the analysis column 12 is connected with the guard column 11 and the suppressor 5 respectively; the suppressor 5 is connected with the analysis column 12 and the conductivity detector 6 respectively; the quantitative loop 8 is on the first six-way valve 3, and the pretreatment The columns 13 are respectively connected with the first six-way valve 3 and the second six-way valve 4 . Pumps 1 and 2 are filled with mobile phase and turned on. The mobile phase of pump 1 is deionized water at a flow rate of 0.65mL / min, and th...

Embodiment 3

[0055] This example is to analyze eight common inorganic anion mixed standard samples using column switching technology

[0056] Instruments used: ion chromatograph; conductivity detector; chromatographic workstation; two six-way valves; chromatographic pump; high-purity nitrogen cylinder; analytical column; guard column; enrichment column; anion self-regeneration suppressor. Pretreatment column: use the polymer carbon nanotube composite filler in Example 1 to fill in a 4.6×150mm stainless steel column.

[0057] Eluent: analytical column eluent: 4.5mM Na 2 CO 3 and 0.8mM NaHCO 3 , the flow rate is 1.0mL / min; polymer carbon nanotube pretreatment column eluent: H 2 O, the flow rate is 0.65 mL / min.

[0058] Analysis steps:

[0059] (1) Baseline surveying and mapping

[0060] 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 con...

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Abstract

The invention discloses a method for combining technologies of a polymer carbon nano tube chromatographic column and an ion chromatographic column switching, which is carried out in an ion chromatographic column switching system, adopts a polymer carbon nano tube chromatographic column to carry out on-line pretreatment on a sample and to combine with the technolog of ion chromatographic column switching. The analysis steps orderly comprise baseline mapping, sample loading to a dosing ring, matrix elimination, target ion enrichment, separation analysis of target ion and regeneration of a preliminary treatment column. The invention has low cost, simple manufacturing process and excellent property, can be effectively used for separation analysis of various organic compounds such as organic solvent, organic acid, organic acid salts and the like.

Description

technical field [0001] The invention relates to a method for combining a polymer carbon nanotube chromatographic column and an ion chromatographic column switching technology, in particular to an analysis method for using a polymer carbon nanotube chromatographic column for on-line sample pretreatment and ion chromatographic detection. Background technique [0002] Trace ionic impurities in organic compounds often have a great impact on the yield and purity of products, especially for industries such as the semiconductor industry that have very strict control of impurities. Direct injection of such organic compounds on ion chromatography to detect trace ions contained in them will bring two problems. One is that high concentrations of organic compounds will contaminate and damage the ion chromatography column, and the other is excessive matrix concentration. It will affect the detection of trace target ions. Therefore, the detection of trace ions in organic compounds requir...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/60G01N30/08
Inventor 钟莺莺朱岩
Owner ZHEJIANG UNIV