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Method for preparing water body phosphate oxygen isotope sample through in-situ enrichment

An oxygen isotope and in-situ enrichment technology, which is applied in the preparation of test samples, sampling, and measuring devices, can solve the problems of consuming a lot of time and reagent materials, the workload of water collection, and the large error of results, etc., and achieve saving Effects of time and economic cost, reduction of water harvesting workload, and simplification of difficulty or steps

Pending Publication Date: 2020-02-14
INST OF GEOCHEM CHINESE ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, it is common to first convert the phosphate in the water to be tested into high-purity, stable Ag. 3 PO 4 Solid sample, then tested for Ag by EA-IRMS high temperature pyrolysis method 3 PO 4 Medium delta 18 o P , there are defects such as cumbersome operation, time-consuming and laborious:
[0004] 1) PO in natural water bodies 4 The content is low, and a large amount of raw water needs to be collected to enrich the sufficient amount of PO required for the test 4 , the workload of water collection is heavy and the cost is high
[0005] 2) It is necessary to perform cumbersome process operations such as filtration, impurity removal, and passive phosphorus concentration on raw water, and it is easy to cause phosphorus loss
[0006] 3) The raw water collection process is instantaneous sampling, and the obtained δ 18 o P The composition represents the δ at a certain moment 18 o P Composition information has a certain degree of randomness, so it is difficult to accurately reflect the dynamic change information of phosphate in raw water
[0007] 4) Impurities such as dissolved organic matter DOM and various anions / cations in raw water will seriously interfere with δ 18 o P Purification operation and test analysis, it needs to be completely removed, otherwise it will affect the δ 18 o P Accuracy of test results
Overall, δ 18 o P The separation and purification operation is a series of continuous and complex multi-step impurity removal and PO 4 extraction process (e.g. CePO 4 step washing Cl - The number of times is even as high as more than ten times), which not only consumes a lot of time and reagent materials, but also easily leads to low phosphorus recovery and fractionation of oxygen isotopes, which eventually leads to Ag 3 PO 4 The error of the sample result is large

Method used

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  • Method for preparing water body phosphate oxygen isotope sample through in-situ enrichment
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  • Method for preparing water body phosphate oxygen isotope sample through in-situ enrichment

Examples

Experimental program
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Effect test

Embodiment 1

[0042] 1) Cover the Zr-Oxide gel membrane with a diameter of 10cm with a nylon mesh, and immerse it in the in-situ water body to be tested for phosphate enrichment until the required detection time period is reached;

[0043] 2) Take out the Zr-Oxide gel film and place it in 20 mL of 1mol / L sodium hydroxide solution for continuous shaking for 24 hours, and pass it through a 0.45 μm filter membrane to obtain a phosphorus-containing eluent;

[0044] 3) Adjust the pH value of the above-mentioned phosphorus-containing eluent to 5.8, then add cerium nitrate solution to adjust the pH value to 5.5, and get the cerium phosphate precipitate; the cerium nitrate solution is prepared from 0.5g cerium nitrate hexahydrate and 2mL water;

[0045] 4) Add 15 mL of 0.2 mol / L nitric acid to the above cerium phosphate precipitate, and then add 5 mL of Biorad AG 50W-X8 cation exchange resin after the cerium phosphate precipitate is completely dissolved and shake continuously for 12 hours to remove ...

Embodiment 2

[0049] In order to further eliminate Cl - Content, on the basis of Example 1, also can be in step 4) in, before adding the nitric acid of 15mL 0.2mol / L, wash the cerium phosphate precipitate three times continuously with the buffer solution that pH value is 5.6 earlier, described buffer solution consists of It is prepared by mixing 1L of pure water with 0.2mL of 99.8% glacial acetic acid and then adding 1mol / L of potassium acetate.

[0050] from Figure 1~3 It can be seen that the Ag prepared by the method of the present invention 3 PO 4 The sample has good purity and only contains a very small amount of Ag ((this is because Ag 3 PO 4 It has the characteristics of easily decomposing a small amount of nano-silver when exposed to light, but does not affect the δ 18 o P Composition test results). Water body δ at three phosphorus concentration levels 18 o P The composition information is relatively close, and they are all added from the same phosphorus source (KH 2 PO 4...

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Abstract

The invention, which belongs to the environment-friendly monitoring method field, relates to a method for preparing a water body phosphate oxygen isotope sample through in-situ enrichment. The methodcomprises the following steps: immersing a Zr-Oxide gel film into a water body, fishing out the Zr-Oxide gel film after a period of time, putting the Zr-Oxide gel film into a sodium hydroxide solution, carryin gout oscillating for 24 hours, and carrying out filtering to obtain a phosphorus-containing eluent; adjusting the pH value of the eluent to 5.8 and adding a cerous nitrate solution to adjustthe pH value to 5.5; adding nitric acid into a cerium phosphate precipitate, adding cation exchange resin after dissolving of the cerium phosphate precipitate, and carrying out oscillation for 12h; filtering the solution after cation exchange resin processing into a black centrifuge tube, adjusting the pH value to 8.5 by using ammonia water, adding a silver nitrate solution, carrying out centrifuging to obtain a silver phosphate precipitate; washing the silver phosphate precipitate with pure water, adding hydrogen peroxide to react for more than 3 hours, carrying out centrifuging to retain the precipitate, washing the centrifugal precipitate with pure water, and carrying out freezing and drying. Therefore, large-volume sampling can be avoided effectively; and the difficulty or steps of filtration and impurity removal can be reduced or simplified obviously. The method is a novel method for preparing a water body phosphate oxygen isotope sample.

Description

technical field [0001] The invention relates to a method for preparing a water body phosphate oxygen isotope sample, in particular to a method for preparing a water body phosphate oxygen isotope sample by in-situ enrichment; it belongs to an environmental protection monitoring method. Background technique [0002] Phosphate (PO 4 ) is a key pollutant that causes eutrophication in rivers, lakes and other water bodies. Sources of phosphate in water include not only exogenous industrial and agricultural wastewater, domestic sewage, and atmospheric dry and wet deposition, but also endogenous degradation of biological residues and release of phosphorus from sediments. The dynamic changes of different phosphate source types and input quantities will produce different environmental effects. Phosphate oxygen isotope (δ 18 o P ) as a new and effective tracer tool has gradually attracted widespread attention, and has been applied to the source analysis and biogeochemical research ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N1/40
CPCG01N1/4005G01N1/4044G01N1/405G01N2001/4011
Inventor 王敬富刘勇陈敬安丁士明金祖雪王燕
Owner INST OF GEOCHEM CHINESE ACADEMY OF SCI
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