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A sample pretreatment method suitable for fast detection of heavy metal ions in water

A technology for pretreatment of heavy metal ions and samples, which is used in the preparation, sampling, and measurement devices of samples for testing.

Inactive Publication Date: 2019-04-30
RES CENT FOR ECO ENVIRONMENTAL SCI THE CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, these methods have disadvantages such as complicated pretreatment and low enrichment coefficient

Method used

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  • A sample pretreatment method suitable for fast detection of heavy metal ions in water
  • A sample pretreatment method suitable for fast detection of heavy metal ions in water
  • A sample pretreatment method suitable for fast detection of heavy metal ions in water

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0062]Add 1g of powdered calcium sulfide to 100mL of flue gas purification copper-containing waste liquid (acidified with sulfuric acid (3g / LH2SO4) in advance), stir for 15 minutes, centrifuge, dry in an oven, compact with a hydraulic press, and use LIBS to measure the heavy metal content in the solid . The detection limit of direct detection of copper in liquid is 0.4mg / L, and the detection limit of enriched calcium sulfide is 6.5μg / L. The detection limit after enrichment was 62 times lower than direct detection.

Embodiment 2

[0064] Add 2g of powdered calcium sulfide to 100mL zinc sulphate waste liquid produced in the zinc smelting industry that has been acidified with sulfuric acid (2g / L H2SO4) in advance, stir for 10 minutes, centrifuge, dehydrate and dry with ethanol, compact with a hydraulic press, and measure the solid by XRF heavy metal content in. The detection limit of direct detection of lead in liquid is 0.7mg / L, and the detection limit of calcium sulfide enrichment is 3.5μg / L. The detection limit after enrichment is 200 times lower than direct detection.

Embodiment 3

[0066] Formulate calcium sulfide into a 100g / L emulsion, take 10mL of calcium sulfide emulsion and add it to 100mL of heavy metal wastewater with high organic matter (pre-acidified with sulfuric acid (5g / L H2SO4)), stir for 10 minutes, centrifuge, freeze-dry, and compact with a hydraulic press , using LIBS to determine the content of heavy metals in solids. The detection limit of direct detection of cadmium in liquid is 13.5mg / L, and the detection limit of enriched calcium sulfide is 13.5μg / L. The detection limit after enrichment is 1000 times lower than direct detection.

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Abstract

The invention relates to a sample pretreatment method suitable for fast detection of heavy metal ions in water. The method comprises the following steps: adding a moderate amount of sulfuric acid to asolution containing heavy metal; adding a certain amount of calcium sulfide, and stirring for a certain time; then, neutralizing the solution with alkali; carrying out solid-liquid separation; dryingthe obtained solid; and directly pressing the dried solid and carrying out detection through fast solid detection technology. Through the sample pretreatment method for converting liquid into solid,the difficulty that it is difficult to detect heavy metals in liquid samples directly and quickly is solved, enrichment detection of heavy metal in solution is realized, and detection limit and accuracy are improved; and the method has the advantages of simple operation and low cost and the like.

Description

technical field [0001] The invention relates to a sample pretreatment method suitable for rapid detection of heavy metals in water, in particular to a sample pretreatment method for solidifying and enriching heavy metals in water and using them for rapid detection of solid detection instruments. Background technique [0002] The detection of heavy metals in various types of water has defects such as complicated pretreatment and long detection time, which makes it difficult to meet the rapid detection requirements of heavy metals under certain conditions (such as emergency wastewater). One of the effective methods for rapid qualitative and quantitative detection of heavy metals is to use non-contact spectroscopic techniques such as laser-induced plasma spectroscopy (LIPS) and X-ray fluorescence spectroscopy (XRF) for detection, which has the advantages of short analysis time and simultaneous detection of multiple heavy metals. advantages in online analysis. However, techniqu...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N1/28
CPCG01N1/28G01N1/286
Inventor 彭先佳孔令昊胡星云
Owner RES CENT FOR ECO ENVIRONMENTAL SCI THE CHINESE ACAD OF SCI
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