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Method for analyzing and detecting trace metal ion impurities in dimethyl diallyl ammonium chloride monomers

A technology of dimethyl diallyl ammonium chloride and trace metals, which is applied in the preparation of test samples, measurement of color/spectral properties, etc., can solve the problems of difficulty in ensuring the accuracy and limitation of metal ion content determination results, and the like, Achieve the effect of avoiding operational difficulties and result errors, improving accuracy, and high analytical precision

Active Publication Date: 2017-03-22
NANJING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, because the DMDAAC solution has a certain viscosity, especially when the monomer mass fraction is higher, the solution viscosity is larger, so the liquid absorption amount and liquid absorption rate during the sample test will be affected by the viscosity of the solution, and then have an impact on the measurement sensitivity. It is difficult to guarantee the accuracy of the determination results of metal ion content, which limits the practical application of this detection method.

Method used

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  • Method for analyzing and detecting trace metal ion impurities in dimethyl diallyl ammonium chloride monomers
  • Method for analyzing and detecting trace metal ion impurities in dimethyl diallyl ammonium chloride monomers
  • Method for analyzing and detecting trace metal ion impurities in dimethyl diallyl ammonium chloride monomers

Examples

Experimental program
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Embodiment 1

[0035] (1) Preparation of mixed standard working solution

[0036] Accurately pipette certain volumes of Fe, Cu, and Ni single element standard solutions (500 mg / L) respectively, and sequentially add them to high-purity DMDAAC monomer solutions with a mass fraction of 30%, and prepare mass concentrations of 0.05, 0.10, 0.30, 0.50, 0.70, 0.90, 1.00mg / L series of standard working solutions for monomers containing metal ions.

[0037] (2) Complexation reaction

[0038] Take 20mL of different mass concentrations of the metal ion-containing monomer standard working solution in a 50mL separatory funnel, adjust its pH to 1 with nitric acid solution, add 2.0mL complexing agent (the ratio of the amount of substances is 1:1: 1 ammonium pyrrolidinedithiocarbamate, sodium diethyldithiocarbamate and 1,10-phenanthrene phenanthroline), shake and mix to make it fully complexed.

[0039] (3) Extraction and separation

[0040] Use a pipette to accurately pipette 5 mL of methyl isobutyl keton...

Embodiment 2

[0060] (1) Preparation of mixed standard working solution

[0061] Accurately pipette certain volumes of Fe, Cu, and Ni single element standard solutions (500 mg / L) respectively, and sequentially add them to high-purity DMDAAC monomer solutions with a mass fraction of 45%, and prepare mass concentrations of 0.05, 0.10, 0.20, 0.40, 0.60, 0.80, 1.00mg / L series of standard working solutions for monomers containing metal ions.

[0062] (2) Complexation reaction

[0063] Get 20mL of different mass concentrations of the metal ion-containing monomer standard working solution in a 50mL separatory funnel, adjust its pH to 3 with nitric acid solution, add 2.5mL complexing agent (the ratio of the amount of substance is 1:1: 1 ammonium pyrrolidinedithiocarbamate, sodium diethyldithiocarbamate and 1,10-phenanthrene phenanthroline), shake and mix to make it fully complexed.

[0064] (3) Extraction and separation

[0065] Use a pipette to accurately pipette 8 mL of methyl isobutyl ketone ...

Embodiment 3

[0083] (1) Preparation of mixed standard working solution

[0084] Accurately pipette a certain volume of Fe, Cu, Ni single element standard solution (500mg / L) respectively, and sequentially add to the high-purity DMDAAC monomer solution with a mass fraction of 60%, and prepare a mass concentration of 0.05, 0.10, 0.20, 0.40, 0.80, 1.00mg / L series of standard working solutions for monomers containing metal ions.

[0085] (2) Complexation reaction

[0086] Take 20mL of different mass concentrations of the metal ion-containing monomer standard working solution in a 50mL separatory funnel, adjust its pH to 6 with nitric acid solution, add 3.0mL complexing agent (the ratio of the amount of substances is 1:1: 1 ammonium pyrrolidinedithiocarbamate, sodium diethyldithiocarbamate and 1,10-phenanthrene phenanthroline), shake and mix to make it fully complexed.

[0087] (3) Extraction and separation

[0088] Use a pipette to accurately pipette 10 mL of methyl isobutyl ketone into the ...

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Abstract

The invention discloses a method for analyzing and detecting trace metal ion impurities in dimethyl diallyl ammonium chloride (DMDAAC) monomers. According to the method, an organic solvent chelating extraction-flame atomic absorption spectroscopy method is adopted to measure the contents of multiple trace metal ions in DMDAAC monomers of a DMDAAC monomer solution with a high salt content, and avoids the difficult operation and result errors caused by direct injection of a sample with a high salt content. By utilizing the synergistic effect of a complexing agent, three metal ions (Fe, Cu, and Ni) can be complexed, extracted, separated, analyzed, and tested at the same time. The provided method has the advantages that the operation is simple and convenient, the analysis precision is high, and the contents of several trace metal ion impurities in DMDAAC monomers can be accurately, rapidly, and reliably analyzed and detected. The provide method has an important scientific meaning and industrial practical value for industrial manufacturing of high purity DMDAAC monomers, establishment of national / international standards of DMDAAC monomers, and research on the activity of DMDAAC monomers in polymerization reactions.

Description

technical field [0001] The invention belongs to the technical field of impurity analysis in cationic quaternary ammonium salt monomers, and in particular relates to an analysis and detection method for trace inorganic metal ion impurities (Fe, Cu, Ni) in dimethyl diallyl ammonium chloride monomers. Background technique [0002] Dimethyldiallylammonium Chloride (DMDAAC) is a quaternary ammonium cationic monomer with two unsaturated double bonds, and its homopolymer and copolymer obtained by free radical polymerization have The macromolecular chain has the advantages of high or adjustable positive charge density, good water solubility, stable cationic structural unit, easy control of relative molecular mass, high efficiency and non-toxicity, etc., and is widely used in petroleum exploration, textile printing and dyeing, papermaking, daily chemical industry and water processing and many other fields. [0003] DMDAAC monomer is generally obtained by nucleophilic substitution re...

Claims

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Application Information

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IPC IPC(8): G01N21/33G01N1/28
Inventor 张跃军刘程王维新刘冬鹏
Owner NANJING UNIV OF SCI & TECH
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