Concentration column and application thereof in analysis of trace elements in seawater

A technology of trace elements and enrichment columns, which is applied in the direction of analyzing materials, using radiation for material analysis, and using radiation diffraction for material analysis, etc. It can solve problems such as seawater analysis and matrix interference, and achieve improved accuracy and high saturation magnetic intensity. , easy desorption effect

Active Publication Date: 2020-11-06
浙江省舟山海洋生态环境监测站
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the high-salt matrix in seawater is easy to deposit on the rectangular tube, sampling cone, etc., and the polyatomic ions formed by the

Method used

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  • Concentration column and application thereof in analysis of trace elements in seawater
  • Concentration column and application thereof in analysis of trace elements in seawater
  • Concentration column and application thereof in analysis of trace elements in seawater

Examples

Experimental program
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Example Embodiment

[0047] Example 1:

[0048] The preparation method of concentrated column packing comprises the following steps:

[0049] S1, adding 1.35g FeCl 3 ·6H 2 O is dissolved in 42mL ethylene glycol, then 3.6g sodium acetate and 1.0g polyethylene glycol are added, stirred evenly, reacted at 200℃ for 6h, naturally cooled to room temperature, the product is separated by a magnet, then washed with absolute ethanol and water for three times, and dried to prepare Fe. 3 O 4 Nanoparticles;

[0050] S2, adding 8g Fe 3 O 4 Nanoparticles were dispersed in 2400mL absolute ethyl alcohol by ultrasonic wave, then 40mL 25％% ammonia water and 43mL tetraethyl orthosilicate were added in turn under stirring conditions, and the total reaction time was controlled for 8 hours. The product was separated by a magnet, then washed with absolute ethyl alcohol and water for 3 times, and dried to obtain Fe. 3 O 4 @SiO 2 Magnetic ball;

[0051] S3, adding 6g Fe 3 O 4 @SiO 2 Magnetic spheres are dispersed in 20mL DMF b...

Example Embodiment

[0073] Example 2:

[0074] A concentration column comprises: the concentration column filler is the concentration column filler of Example 1.

Example Embodiment

[0075] Example 3:

[0076] Method for analyzing trace elements in seawater

[0077] 1. Instruments and reagents

[0078] Nexion-300D inductively coupled plasma mass spectrometer, including PC3 low-temperature atomization chamber and seaFAST seawater preconcentration column (200μL, PerkinElmer Company); SC-DX seaFAST SP2 seawater preconcentration system and trace metal filter column (0.5mm id) were purchased from Elemental Scientific company.

[0079] Multi-element mixed standard and internal standard (PerkinElmer Company, USA); CASS-5 and NASS-6 reference standards of trace metal elements in seawater (National Research Council of Canada); GBW080040 is the seawater standard substance (State Oceanic Administration No.2 Institute); High purity NaCl solution (10% ~ 11%, American Elemental Scientific Company); Ppt HNO 3 (Fisher Scientific Company). Milli-Q ultrapure water was used in the experiment, and the other reagents used were excellent grade pure. Ammonium acetate Buffer solution...

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Abstract

The invention discloses a concentration column and application thereof in analysis of trace elements in seawater, which belong to the technical field of trace metal element analysis. Concentration column filler filled in an inner cavity of a column body of the concentration column is obtained by the following method: Fe3O4 nanoparticles are prepared by adopting a hydrothermal synthesis method; theFe3O4 nano particles are coated with SiO2 by adopting a sol-gel method, so as to obtain Fe3O4@SiO2 magnetic spheres; and the surfaces of Fe3O4@SiO2 magnetic spheres are modified with trimellitic anhydride and dithiothreitol to obtain the concentration column filler. The concentration column has good affinity, selectivity and capture capability on many heavy metal elements, high adsorption capacity and rapid adsorption and elution kinetics. With the combination of the online pre-concentration of the concentration column and the ICP-MS, the trace elements in the seawater can be simultaneously analyzed, such that the more trace elements can be enriched and separated, and the accuracy is high.

Description

technical field [0001] The invention belongs to the technical field of trace metal element analysis, and in particular relates to a concentration column and its application in the analysis of trace elements in seawater. Background technique [0002] For the analysis of trace heavy metals in seawater, the commonly used methods mainly include atomic absorption method (AAS), atomic fluorescence method (AFS), electrochemical method, spectrophotometry, inductively coupled plasma emission spectrometry (ICP-AES), inductive Coupled plasma mass spectrometry (ICP-MS), etc. AAS is the analysis method for most heavy metal elements in my country's current marine monitoring specifications. This method requires pre-enrichment and matrix separation by means of liquid-liquid extraction, which is cumbersome to operate, easy to contaminate, and cannot achieve simultaneous determination of multiple elements. AFS is mainly used to determine arsenic, mercury, selenium and other elements in seaw...

Claims

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Application Information

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IPC IPC(8): G01N27/62G01N1/40G01N23/04G01N23/20G01N21/35G01R33/12
CPCG01N1/405G01N21/35G01N23/04G01N23/20G01N27/62G01N2021/3595G01R33/1215
Inventor 母清林佘运勇孙毅魏娜
Owner 浙江省舟山海洋生态环境监测站
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