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A kind of solid phase extraction column and its preparation method and application

A solid-phase extraction column, seafood technology, applied in the field of analytical chemistry and environmental monitoring trace material pre-concentration, to achieve the effect of low cost, high enrichment factor and high chemical stability

Active Publication Date: 2021-01-19
HUAIHAI INST OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Therefore, it is favored and can be used in the fields of catalysis, electricity, molecular recognition and biology, but it has not been reported as a solid phase extraction agent for the simultaneous enrichment and detection of various heavy metals in water.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] The preparation method of solid phase extraction column, comprises the following steps

[0033] (1) Synthesis of layered material tin hydrogen phosphate

[0034] 0.30mol / L of SnCl at room temperature 4 Add dropwise to 0.60mol / L H 3 PO 4 After the reaction, the solution was transferred to a hydrothermal reactor, and crystallized at 180°C for 36 hours to obtain a gel; then the gel was washed with deionized water until no Cl was detected in the washing solution. -1 and PO4 3- , then vacuum-dried at 60°C, ground, passed through a 0.096mm standard sieve, and stored in a desiccator for later use;

[0035] (2) Preparation of tin hydrogen phosphate solid phase extraction column

[0036] First fill a sieve plate in the 6mL injection-type empty column tube, put the layered material tin hydrogen phosphate prepared in step (1), spread it evenly, add another sieve plate, and compress the packed layered material phosphoric acid Hydrogen tin, prepared as a solid phase extraction...

Embodiment 2

[0038] Weigh 43.1059g of sandfish in a crucible, carbonize it on an adjustable electric plate on a low fire until there is no smoke, move it into a horse-boiling furnace for ashing at 500±25°C for 6-8 hours, and cool down. Add 1 mL of mixed acid of nitric acid and perchloric acid (ratio: 9:1) and heat it on an adjustable electric stove over low heat, repeat several times until the digestion is complete, let it cool, dissolve the ash with nitric acid (0.5mol / L), and dissolve the ash in the test Filter the sample digestion liquid into a 100ml volumetric flask, wash the porcelain crucible several times with water, combine the washing liquid into the volumetric flask and set the volume to the mark. The pipette pipettes 50mL sandfish digestion liquid, adjusts pH to be 5.3 with the NaOH of 1mol / L, passes through the solid-phase extraction column (prepared in embodiment 1) with the flow velocity of 5ml / min, then uses 8mL 3mol / L hydrochloric acid to The heavy metals on the solid-phase...

Embodiment 3

[0040]Take by weighing 25.1269g laver in the crucible, carry out digestion with the same method as example 2 to obtain the digestion solution 100ml. Pipette pipette 50mL laver digestion solution, adjust pH to 5.2 with 1mol / L NaOH, pass through the solid phase extraction column (prepared in Example 1) with 5ml / min flow rate, then use 8mL 3mol / L hydrochloric acid to solid phase The heavy metals on the extraction column were analyzed, and the flow rate of the analytical agent was controlled by a vacuum pump to be 5mL / min. The analytical solution was collected in a test tube, and copper, lead and zinc were determined by flame atomic absorption. The result was that the content of copper was 4.005×10 -3 1mg / g, the recovery rate of standard addition is 101.06-106.6%, and the content of lead is 3.1470×10 -3 mg / g, the standard recovery rate is 89.56-98.56%, and the zinc content is 1.626×10 -3 mg / g, the recovery rate of standard addition was 94.23-102.32%.

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Abstract

The invention discloses a solid phase extraction column for trace determination on heavy metal in a marine food product and a preparation method of the solid phase extraction column. An adsorbent of the solid phase extraction column is tin hydrogen phosphate. Screened by a lot of experiments, tin hydrogen phosphate is preferably a solid phase extraction adsorption medium for heavy metal ion enrichment and trace determination, the cost is lower, the adsorption capacity is great, an enrichment factor is high, enrichment performance is stable, multiple types of heavy metal ions (including lead ion, copper ion, arsenic, zinc and the like) can be enriched at the same time, the detection sensitivity and accuracy of the heavy metal ions in the marine food product can be improved, and tin hydrogenphosphate is insoluble in water and organic solvents, is resistant to strong acid and certain alkalinity, is high in chemical stability, can be reused, and has important social and economic effects.

Description

technical field [0001] The invention relates to a heavy metal treatment method, in particular to a solid-phase extraction column using tin hydrogen phosphate as an adsorbent and its preparation method and application, belonging to the field of pre-enrichment of trace substances in analytical chemistry and environmental monitoring. Background technique [0002] With the acceleration of economic development, marine development activities such as port construction, coastal industry, and offshore aquaculture in coastal cities have achieved unprecedented development, which has also brought adverse effects on the environment of coastal waters. In turn, seawater pollution impairs the quality of aquaculture products. Among them, heavy metals are important pollutants that affect the quality of aquatic products. Heavy metal ions have the characteristics of wide distribution, long duration, and not easy to decompose in material circulation and energy exchange. They can be enriched in ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01D15/10B01D15/22B01J20/02B01J20/30G01N1/40
CPCB01D15/10B01D15/22B01J20/0251B01J20/0292G01N1/405
Inventor 张成燕朱明志王艺慧朱彤杨莹
Owner HUAIHAI INST OF TECH
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