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A kind of analysis and detection method and application of complexing agent trisodium nitrilotriacetate in water

A technology of trisodium nitrilotriacetate and a detection method, which is applied in the field of water quality detection, can solve the problems of complex detection process and long analysis time of nitrilotriacetic acid and its salts, and achieve good extraction and derivation effects and accurate analysis results , the effect of simplifying the operation

Active Publication Date: 2022-07-29
QINGDAO TECHNOLOGICAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The analysis and detection methods of reported nitrilotriacetic acid and its salts are: high performance liquid chromatography, ion chromatography, etc., but the inventors found that the method for pretreatment in the prior art is mainly solid phase extraction, The substance must be derivatized to be suitable for high-performance liquid chromatography, which leads to the problems of complicated detection process and long analysis time of nitrilotriacetic acid and its salts

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  • A kind of analysis and detection method and application of complexing agent trisodium nitrilotriacetate in water
  • A kind of analysis and detection method and application of complexing agent trisodium nitrilotriacetate in water
  • A kind of analysis and detection method and application of complexing agent trisodium nitrilotriacetate in water

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] The analysis and detection method of trisodium nitrilotriacetate in water sample specifically includes the following steps:

[0046] Add 2g Al(NO 3 ) 3 ·9H 2 O and 6 g of terephthalic acid, 20 mL of ultrapure water, and 50 mL of N,N-dimethylformamide were stirred at 40 °C for about 2 h. Pour the above-prepared mixture into a 100 mL reaction kettle, place the reaction kettle in a 130°C oven for 48 hours, take it out, wash the material three times with N,N-dimethylformamide and ethanol respectively, and dry at 100°C overnight to obtain White powder MIL-53. Take 20 mg of metal-organic framework material (MIL-53) into a water sample with a pH of 7 (the concentration of the complexing agent trisodium nitrilotriacetate in the water sample is 500 μg / L). Centrifuge at the speed of / min for 10min, discard the supernatant, add 0.5mL of 0.02mol / L Cu 2+ , after ultrasonication for 10min, the eluate was centrifuged at 12000r / min for 10min, the supernatant was taken out, and th...

Embodiment 2

[0048] In this example, the main factors affecting the extraction recovery rate of trisodium nitrilotriacetate are explored, and the optimal values ​​of each factor when the extraction recovery rate is the highest are calculated, and then the optimal value of each factor is determined. The relevant parameters of the working curve of sodium and the detection limit and precision of the method, the specific process includes the following steps:

[0049] S1, calculate the optimal value of each factor when the extraction recovery rate of trisodium nitrilotriacetate is the highest:

[0050] (1) Investigation of the amount of eluent on extraction recovery

[0051] like Figure 5 As shown in the figure, the present invention explores the effect of the amount of eluent on the extraction recovery, keeping other experimental conditions unchanged. 2+ placed in a water sample, when Cu 2+ When the dosage was increased from 100 μL to 500 μL, the peak area of ​​the target substance changed...

Embodiment 3

[0066] Determination of the residual amount of trisodium nitrilotriacetate in seawater, domestic sewage, factory wastewater 1, and factory wastewater 2: After collecting 4 kinds of water samples, filter them with a 0.45 μm filter membrane, and use the method described in Example 1 to filter the water samples. Carry out the measurement, and carry out the accuracy test with the method described in Example 2, then prepare the actual water sample whose concentration of trisodium nitrilotriacetate is 1000 μg / L and carry out the standard addition recovery test, the concentration point is measured 3 times, and calculated 3 times The average value, relative standard deviation and recovery rate of standard addition; among them, trisodium nitrilotriacetate was not detected in seawater and domestic sewage blank; trisodium nitrilotriacetate was detected in factory wastewater, and the experimental results are shown in Table 3 ; As can be seen from the table, the recovery rate of standard ad...

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Abstract

The invention relates to the field of water quality detection, in particular to an analysis and determination method and application of trisodium nitrilotriacetate, a complexing agent in water. The invention utilizes metal-organic frameworks, separates interfering ions in water by dispersing solid-phase extraction technology, enriches trisodium nitrilotriacetate in water, uses eluent to realize simultaneous elution and derivatization, and combines high performance liquid chromatography to realize seawater and life. Determination of complexing agent trisodium nitrilotriacetate in sewage, industrial wastewater and other water bodies. The invention develops the analysis and detection method of the complexing agent in water, which not only saves the derivatization and elution steps of sample pretreatment, but also enables the elution and derivatization to be carried out simultaneously, reduces the pretreatment time, and can effectively improve the anti-matrix interference ability of the detector, reduce the The detection limit of complexing agent in water was obtained. Using the invention to detect factory sewage, the extraction effect and reproducibility are good, and the results are satisfactory, and the invention is suitable for water quality detection of high-concentration complexing agents.

Description

technical field [0001] The invention relates to the field of water quality detection, in particular to an analysis and determination method and application of trisodium nitrilotriacetate, a complexing agent in water. Background technique [0002] The information disclosed in this Background section is only for enhancement of understanding of the general background of the invention and should not necessarily be taken as an acknowledgement or any form of suggestion that this information forms the prior art already known to a person of ordinary skill in the art. [0003] Nitrilotriacetic acid (or nitrilotriacetic acid, NTA) and its salts are compounds that are mostly used in industrial production. They are mainly used as chelating agents for metal ions. They can rapidly complex with metal ions to form chelating compounds, and are stable and stable. It has strong properties and good water solubility. It has been used in the production of washing products and as a complexing agen...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/06G01N30/74
CPCG01N30/06G01N30/74
Inventor 田永程嘉雯李玉彤韩小璇马继平
Owner QINGDAO TECHNOLOGICAL UNIVERSITY
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