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Method for abstracting and enriching organic phosphorus in substrate sludge

An organic phosphorus and sediment technology, applied in the preparation of test samples, etc., can solve the problems of organic phosphorus content that cannot meet the measurement requirements, low spectral resolution and signal-to-noise ratio, etc., to reduce the time required for measurement, reduce the Measuring the effect of costs

Inactive Publication Date: 2013-08-21
HEBEI UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0002] At present, NaOH-EDTA extraction method is generally used for NMR analysis of phosphorus in sediment, which is limited to the content of organic phosphorus in the extract. of 31 P-NMR measurement takes a long time, usually 12-72h, and the resolution and signal-to-noise ratio of the spectrum are low

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  • Method for abstracting and enriching organic phosphorus in substrate sludge
  • Method for abstracting and enriching organic phosphorus in substrate sludge
  • Method for abstracting and enriching organic phosphorus in substrate sludge

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0060] Implementation example 1 and implementation example 2 adopt the same sample, by comparing the spectrogram 2 detected by the traditional method and the spectrogram 3 detected by the foam separation method, it can be known that under the condition that the signal-to-noise ratio and the resolution do not decrease, the foam separation method ( The measurement takes 8h) compared with the traditional method (the measurement takes 12h), and the time required is shortened to 2 / 3 of the original, which shortens the time required for the measurement and reduces the test cost.

[0061] Foam separation method is used for the enrichment of sediment phosphorus, as shown in Figure 3, the spectrogram is at the chemical shift of 1.14ppm, and the phosphoric acid diester signal peak that cannot be detected by traditional methods is detected, so the foam separation method is used to extract and an effective method for enriching organic phosphorus in sediment.

Embodiment 3

[0063] (1) bottom mud sample adopts the sample of implementation example 1

[0064] (2) freeze-drying of sample: with implementation example 1

[0065] (3) Extraction of organic phosphorus in sediment

[0066] Take 300g of the dried mud sample obtained in step (2), add it to 3L of 0.25mol / L NaOH solution, place the solution on a constant temperature shaker at 25°C, and shake and extract for 12h;

[0067] (4) Remove impurities in the solution

[0068] Centrifuge the bottom sludge mixture prepared in step (3) at 4000rpm / min for 30min to remove most of the bottom sludge impurities, then centrifuge the supernatant solution obtained by centrifugation at 10000rpm / min for 30min, then filter it with a 0.45μm filter membrane and collect filtrate;

[0069] (5) the adjustment of filtrate pH: with implementation example 1;

[0070] (6) Separation of organophosphorus in the extract: with implementation example 1

[0071] (7) organophosphorus solution freeze-drying again: with implemen...

Embodiment 4

[0076] (1) bottom mud sample adopts implementation example 1 sample

[0077] (2) freeze-drying of sample: with implementation example 1

[0078] (3) Extraction of organic phosphorus in the bottom mud: with implementation example 1

[0079] (4) remove impurities in the solution: with implementation example 1

[0080] (5) Adjustment of filtrate pH

[0081] The filtrate contains a large amount of sodium hydroxide, and the pH is strongly alkaline, which is not conducive to the formation of foam. The pH of the solution needs to be adjusted, and the pH value of the solution is adjusted to 6.0 with 3mol / L HCl;

[0082] (6) Separation of organophosphorus in the extract: with implementation example 1

[0083] (7) organophosphorus solution freeze-drying again: with implementation example 1

[0084] (8) nuclear magnetic resonance measurement of sample: with implementation example 1

[0085] (9) Measurement results

[0086] The measurement results show that compared with the traditi...

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Abstract

The invention discloses a method for carrying out the abstraction and the enrichment of organic phosphorus in substrate sludge by adopting a foam separating device, which comprises the following steps: (1), collecting a substrate sludge sample; (2), carrying out freeze drying on the sludge sample; (3), extracting the organic phosphorus in the substrate sludge; (4), removing impurities in a mixed solution; (5), regulating the pH of a filtrate; (6), separating the foam from the organic phosphorus in the filtrate; and (7), carrying out vacuum freeze drying on an organic phosphorus solution from which foam is separated and collected again. Compared with the traditional method, the capability of a foam separating method for enriching the organic phosphorus is stronger; the content of the organic phosphorus in the sample for the nuclear magnetic resonance analysis for the organic phosphorus in the substrate sludge is higher; furthermore, a phosphodiester signal peak is detected in the organic phosphorus enriched by the foam separating method, but the traditional method cannot detect the phosphodiester signal peak; and further, the time needed for measurement is shortened to be 2 / 3 of that of the traditional method.

Description

technical field [0001] The invention belongs to a method for extracting and enriching organic phosphorus in bottom mud, in particular to a method for separating and enriching organic phosphorus in bottom mud by using a foam separation device. Background technique [0002] At present, NaOH-EDTA extraction method is generally used for NMR analysis of phosphorus in sediment, which is limited to the content of organic phosphorus in the extract. of 31 P-NMR measurement takes a long time, usually 12-72h, and the resolution and signal-to-noise ratio of the spectrum are low. [0003] Organic phosphorus in sediment mainly includes phosphate monoester, phosphate diester (DNA-P, phosphonate), etc., among which phosphate monoester and phosphate diester are the main components of biological cell membranes. Surface activity, phosphonic acid contains hydrophobic aliphatic chain hydrocarbons and hydrophilic phosphate head, and is also amphoteric. Although DNA-A is a hydrophilic polymer, t...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N1/28G01N1/40G01N1/34
Inventor 齐树亭潘腾飞
Owner HEBEI UNIV OF TECH
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