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Method for quantitatively analyzing content of free ion in soil sediment sample

A quantitative analysis and sediment technology, applied in the analysis of materials, material analysis through optical means, measuring devices, etc., can solve the problems of salt accumulation, corrosion, instrument failure, high background of the instrument, etc., to achieve the elimination of interference, small error, The effect of high accuracy

Active Publication Date: 2017-07-25
INST OF GEOLOGY & GEOPHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, the analysis of free iron content mostly adopts spectrometry or mass spectrometry, and whether it is atomic absorption spectrometry (AAS), inductively coupled plasma spectrometry (ICP-OES) or inductively coupled plasma mass spectrometry (ICP-MS), the The existence of a large amount of sodium ions will cause the failure of the instrument and shorten the service life of the instrument (for example: AAS combustion head salt accumulation, corrosion, ICP-OES rectangular tube salt accumulation, corrosion, ICP-MS sampling cone corrosion, etc.)
, the most important thing is that due to the interference of the high salt content of the sample, the background of the instrument is too high, and the free iron in the sample cannot be accurately determined.
For example, using AAS to directly measure free iron extracts, the error is as high as 11%
However, the colorimetric method is interfered by the sodium citrate contained in the extraction solution, which affects the color development, resulting in very unsatisfactory test results.

Method used

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  • Method for quantitatively analyzing content of free ion in soil sediment sample
  • Method for quantitatively analyzing content of free ion in soil sediment sample
  • Method for quantitatively analyzing content of free ion in soil sediment sample

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0059] Adopt the method of the present invention to analyze the Eocene gypsum rock sedimentary sample of Xining Basin, concrete method is as follows:

[0060] (1) Firstly, free iron was dissolved and extracted from the sample (Eocene gypsum rock sedimentary sample in Xining Basin). Grind the sample to 100 mesh in an agate mortar, accurately weigh 0.1 g of the sample and add 0.2 g of sodium dithionite powder reagent. Then add 10ml sodium citrate (0.3mol L -1 ) and sodium bicarbonate (0.1mol L -1 ) to mix the extracts. The above mixed solution was heated in a water bath at 75 °C for 15 min. The heated solution was centrifuged in a centrifuge for 5min (3600r / min), and 2.0mL of the supernatant was taken and diluted to 100mL for later use.

[0061] (2) Preparation of ion imprinted materials. 4-vinylpyridine (C 7 h 7 N) as a functional monomer, 2,2'-bipyridine (C 10 h 8 N 2 ) is a chelating agent, azobisisobutyronitrile (AIBN, C 8 h 12 N 4 ) as an initiator, Fe 3+ As a...

Embodiment 2

[0074] Adopt the method of the present invention to analyze the silt grade loess sample in Gansu area, analysis process is as follows figure 1 As shown, the specific method is as follows:

[0075] (1) Firstly, dissolving and extracting free iron from soil sediment samples (silt grade loess samples). Grind the sample in an agate mortar to below 100 mesh, and accurately weigh 0.15 g of the sample and add 0.25 g of sodium dithionite powder reagent. Then add 12ml sodium citrate (0.3mol L -1 ) and sodium bicarbonate (0.1molL -1 ) to mix the extracts. The above mixed solution was heated in a water bath at 75 °C for 15 min. The heated solution was centrifuged in a centrifuge for 5min (3600r / min), and 2.0mL of the supernatant was taken and diluted to 100mL for later use.

[0076] (2) Preparation of ion imprinted materials. 4-vinylpyridine (C 7 h 7 N) as a functional monomer, 2,2'-bipyridine (C 10 h 8 N 2 ) is a chelating agent, azobisisobutyronitrile (AIBN, C 8 h 12 N 4 ...

Embodiment 3

[0088] Adopt the method of the present invention to analyze the sediment sample in the Jingbian area of ​​the Loess Plateau, the specific method is as follows:

[0089] (1) Firstly, free iron was dissolved and extracted from soil sediment samples (sediment samples from the Jingbian area of ​​the Loess Plateau). Grind the sample in an agate mortar to below 100 mesh, and accurately weigh 0.2 g of the sample and add 0.3 g of sodium dithionite powder reagent. Then add 15ml sodium citrate (0.3mol L -1 ) and sodium bicarbonate (0.1mol L -1 ) to mix the extracts. The above mixed solution was heated in a water bath at 75 °C for 15 min. The heated solution was centrifuged in a centrifuge for 5min (3600r / min), and 2.0mL of the supernatant was taken and diluted to 100mL for later use.

[0090] (2) Preparation of ion imprinted materials. 4-vinylpyridine (C 7 h 7 N) as a functional monomer, 2,2'-bipyridine (C 10 h 8 N 2 ) is a chelating agent, azobisisobutyronitrile (AIBN, C 8 h...

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Abstract

The invention discloses a method for quantitatively analyzing the content of free ion in a soil sediment sample. The method includes: dissolving and extracting the free ion from the soil sediment sample; preparing an ionic imprinting material; preparing a nonionic imprinting material; performing solid-phase extraction and analytical tests. The method has the advantages that the ionic imprinting high-polymer material is used to perform solid-phase extraction on free ion extract to eliminate the interference of a large amount of sodium ions, the method is small in error and high in accuracy, the solid-phase extraction technology can enrich, separate and purify the sample to eliminate the interference, and a new approach is provided for the accurate testing of the free iron.

Description

technical field [0001] The invention belongs to the technical field of geological soil analysis, in particular to a method for quantitatively analyzing free iron content in soil sediment samples. Background technique [0002] Free iron refers to other forms of iron in soil that are not part of layered silicate minerals, mainly some iron oxides and hydroxides. Its production in soil sediments is mainly formed by the weathering of three types of rocks (magmatic rocks, sedimentary rocks and metamorphic rocks) under different hydrothermal conditions on the surface. The main weathering effects include: physical weathering (disintegration and fragmentation of rocks caused by physical factors, such as wind erosion and glacier abrasion, etc.); chemical weathering (changes in the chemical composition of rocks to produce new substances, such as hydrolysis, oxidation, etc.) and biological weathering Weathering (mechanical destruction or chemical breakdown of rock by biological activit...

Claims

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Application Information

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IPC IPC(8): G01N21/31
CPCG01N21/3103
Inventor 胡彬张春霞薛丁帅郭正堂
Owner INST OF GEOLOGY & GEOPHYSICS CHINESE ACAD OF SCI
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