A kind of concentration column and its application in the analysis of trace elements in seawater

A trace element, concentration column technology, applied in the analysis of materials, material analysis using radiation, material analysis using radiation diffraction, etc., can solve problems such as seawater analysis, matrix interference, etc., to achieve improved accuracy, high saturation magnetic intensity , the effect of easy desorption

Active Publication Date: 2021-03-16
浙江省舟山海洋生态环境监测站
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  • Summary
  • 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 high-salt matrix, such as ArO + , ArCl + , ArNa + , ClO + matrix interference, etc., so that seawater cannot be directly analyzed by ICP-MS

Method used

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  • A kind of concentration column and its application in the analysis of trace elements in seawater
  • A kind of concentration column and its application in the analysis of trace elements in seawater
  • A kind of concentration column and its application in the analysis of trace elements in seawater

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Embodiment 1

[0048] The preparation method of concentration column packing comprises:

[0049] S1, 1.35g FeCl 3 ·6H 2 O was dissolved in 42mL of ethylene glycol, then 3.6g of sodium acetate and 1.0g of polyethylene glycol were added, stirred evenly, and reacted at 200°C for 6h, naturally cooled to room temperature, and the product was separated with a magnet, and then mixed with absolute ethanol and Washed three times with water, dried, and prepared Fe 3 o 4 Nanoparticles;

[0050] S2, add 8g Fe 3 o 4 Nanoparticles were ultrasonically dispersed in 2400mL of absolute ethanol, and then 40mL of 25% ammonia water and 43mL of ethyl orthosilicate were added sequentially under stirring conditions, and the total reaction time was controlled to be 8h. Water was washed 3 times, and dried to obtain Fe 3 o 4 @SiO 2 magnetic ball;

[0051] S3, 6g Fe 3 o 4 @SiO 2 Ultrasonically disperse the magnetic balls in 20 mL of DMF, add 1.4 g of trimellitic anhydride, react at 178 ° C for 3 h, stop he...

Embodiment 2

[0074] A concentrating column, comprising, the concentrating column packing is the concentrating column packing of embodiment 1.

Embodiment 3

[0076] A method for analyzing trace elements in seawater

[0077] 1. Instruments and reagents

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

[0079] Multi-metal element mixed standard and internal standard (PerkinElmer, USA); CASS-5 and NASS-6 seawater trace metal element reference standard samples (National Research Council, Canada); GBW080040 is seawater standard material (Second Institute of State Oceanic Administration); Pure NaCl solution (10% ~ 11%, Elemental Scientific, USA); ppt grade HNO 3 (Fisher Scientific Corporation). The experimental water was Milli-Q ultrapure water, and the rest of the reagents used were of superior grade. Ammonium acetate buffer solution (Buffer), the preparation method is ...

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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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Patent Type & Authority Patents(China)
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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