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Method for determining trace low-valent phosphate in natural water

A determination method and phosphate technology, applied in the field of water treatment, can solve the problems of long time unsuitable for low-valent phosphate detection, high detection limit, complicated operation, etc.

Inactive Publication Date: 2012-06-27
NANJING UNIV
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  • Summary
  • Abstract
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  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The main defect of this type of method is that the detection limit is too high (ppm level) and the operation is cumbersome, and the time is long, which is not suitable for the detection of trace (ppt level) low-priced phosphate in natural water bodies.
The second is to use today's advanced instrument analysis methods such as high performance liquid chromatography, IC-ICP-ES and other chromatographic instruments for determination, and such methods are mainly used for the separation and determination of low-priced phosphate in geothermal water, high performance liquid chromatography For the determination of low-priced phosphate in the water body of Taihu Lake, the detection limit is too high, and although the detection limit of IC-ICP-ES technology can meet the requirements of natural water bodies, the cost is too high, which is not conducive to popularization

Method used

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  • Method for determining trace low-valent phosphate in natural water
  • Method for determining trace low-valent phosphate in natural water
  • Method for determining trace low-valent phosphate in natural water

Examples

Experimental program
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Effect test

Embodiment 1

[0077] The concentration of low-priced phosphate was determined according to this method from the overlying water of the bottom mud of Dapu Harbor (N1), Meiliang Bay (N2) and Gonghu Bay (N3) in Taihu Lake, Jiangsu Province.

[0078] A. Collection of samples to be tested

[0079] Use a water collector to collect the overlying water from the surface of the bottom mud, then put it into a brown HDPE bottle, add an appropriate amount of chloroform and dilute nitric acid solution to adjust the pH value to be acidic, and store it in a sealed refrigerator. Take it to the laboratory immediately for analysis.

[0080] B. Sample pretreatment and determination

[0081] Take an appropriate amount of water sample, pass through a 0.22 μm water-based microporous membrane, and then pass the filtrate through an OnGuard Ag column (2.5cc P / N057090, Dionex) and an OnGuard Ba column (2.5cc P / N 057094, Dionex) to remove high-concentration Chloride ion (Cl - ) and sulfate (SO 4 2- ), and then th...

example 2

[0093] Example 2. from surface water (river, well water) in a certain area of ​​Jiangsu, according to the method measurement results:

[0094] Table 3 Determination results of phosphite in surface water of Jinjiang, Jiangsu

[0095]

[0096] Note: Well water samples were not detected

example 3

[0097] Example 3. From the interstitial water of different layers of sediment in Gonghu Bay, Taihu Lake, Jiangsu, the measurement results according to this method:

[0098] First, use a columnar mud sampler (Institute of Geography and Limnology, Chinese Academy of Sciences) to collect 50-60cm columnar mud samples, divide them into layers of 20cm, store them in cold storage, and extract water samples from sediment gaps by centrifugation. CT15RT desktop high-speed refrigerated centrifuge settings: Speed: 5000r / min; Time: 20min; T: 4°C. Take an appropriate amount of water sample, pass through a 0.22μm water-based microporous membrane, and then pass the filtrate through an OnGuard Ag column (2.5cc P / N 057090, Dionex) and an OnGuard Ba column (2.5cc P / N 057094, Dionex) to remove high-concentration Chloride ions (Cl - ) and sulfate (SO 4 2- ), and then the extracted water sample enters the ion chromatography system through a 500μL sampling loop for analysis and determination acco...

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Abstract

The invention provides a method for determining trace low-valent phosphate in natural water. The determination detection limit of the method on low-valent phosphate reaches 10<-3> micrometers, which is sufficient to meet the detection requirement for low-valent phosphate in natural water, while the detection limit of existing domestic determination methods for low-valent phosphate is about 0.5 micrometers. Compared with other detection methods, the method of the invention has the advantages of high sensitivity, low detection limit, rapid pretreatment, and simplicity. The specific determining steps of the method include: A. off-line pretreatment; and B. gradient elution. After various negative ions in a water sample to be determined are separated by a separation column, the elution solution and the sample enter an ASRS suppressor and are inhibited to lower background noise, and finally enter a conductance cell for detecting the conductivity of ions in the sample. The Chromeloen 6.5PS2 workstation can draw a spectrum according to the conductance signals received by a data collection system, and a chromatographic workstation is employed to automatically record the area of a characteristic peak, then the actual concentration of low-valent phosphate in the sample can be calculated according to a formula.

Description

technical field [0001] The invention is based on the technology of separating and detecting hypophosphite and phosphite in natural water bodies by using a multi-stage gradient leaching method in an ICS2000 system equipped with a suppressed conductance detector, and belongs to the field of water treatment. Background technique [0002] Phosphorus is an essential element for life on earth and exists in every cell. However, in the past few centuries, the traditional theory believes that phosphorus enters biological cells through positive pentavalent phosphate, and fully oxidized orthophosphate is involved in the formation of phosphorus. Forms of biogeochemical cycles. Modern geochemical and microbiological studies have shown that in the early Earth, the geochemical cycle of phosphorus was dominated by more soluble and easier-to-produced low-priced phosphates (including hypophosphite and phosphite) and represented primitive The presence of low-priced phosphates has been detecte...

Claims

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Application Information

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IPC IPC(8): G01N30/88
Inventor 耿金菊韩超任洪强谢显传王晓蓉
Owner NANJING UNIV
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