Quantitative analysis method for measuring trace nickel in water by microwave digestion-flame atomic absorption spectrometry (FAAS)

A technology of microwave digestion and quantitative analysis, which is applied in the preparation of test samples, color/spectral characteristic measurement, etc., can solve the problem of low sensitivity that cannot reach the lower limit of nickel detection, high analysis cost, unfavorable promotion and use, and long analysis time without practical effect and other issues, to achieve the effects of reducing pollution and harm to the human body, saving measurement costs, and low instrument maintenance costs

Inactive Publication Date: 2011-02-09
SHENYANG POLYTECHNIC UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The detection limit is 3.77×10 -3 mg / L, the method has high sensitivity, the operation process is cumbersome and takes a long time, and ice bath and centrifugal extraction are required, and the high analysis cost is not conducive to popularization
[0017] The above methods for determining trace nickel in water may not reach the lower limit of detection of nickel in water due to low sensitivity, or there are many operation steps and the process is cumbersome and the cumulative error is large, or the use of large and expensive instruments leads to high instrument maintenance costs, or the amount of reagents is large However, it pollutes the environment and operators, or takes a long time to analyze and has no practical effect, all of which have different degrees of disadvantages and are not suitable for popularization and application.

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  • Quantitative analysis method for measuring trace nickel in water by microwave digestion-flame atomic absorption spectrometry (FAAS)
  • Quantitative analysis method for measuring trace nickel in water by microwave digestion-flame atomic absorption spectrometry (FAAS)
  • Quantitative analysis method for measuring trace nickel in water by microwave digestion-flame atomic absorption spectrometry (FAAS)

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0081] Determination of nickel content and recovery rate experiment in environmental engineering laboratory wastewater of Shenyang University of Technology:

[0082] (1) Microwave digestion pretreatment of samples: accurately pipette 5.0ml water samples from three waste liquid buckets into microwave digestion tanks (take 3 copies of each sample for parallel test, and take 3 copies for recovery rate experiment at the same time), Add 10.0ml of 70.0% nitric acid, 1.0ml of 40.0% hydrofluoric acid and 1.0ml of 30.0% hydrogen peroxide, cover the lid, insert it into the protective cover, and put a burst membrane on it. At the same time, prepare a blank solution, and then put it into the microwave digestion apparatus Sample digestion. Digestion pressure 2.5MPa, digestion time 15min. After the digestion program is over, when the temperature reaches 40°C, turn on the microwave digestion apparatus and take out the digestion tank; transfer the sample in the digestion tank to a beaker, he...

Embodiment 2

[0092] Determination of nickel content and recovery rate experiment in Taizi River water of Liaoyang City:

[0093] (1) Sample concentration and microwave digestion pretreatment: Accurately remove the detected leaves and debris and filter them through a filter membrane with a pore size of 0.45 μm to remove suspended particles in Taizi River in March, May, and July 2010. 2000.0ml in a 2000ml beaker (take 3 parts of each sample for parallel experiments, and take 3 parts at the same place for recovery experiment), evaporate and concentrate to 10.0ml (n 1 =200). Take 10 digestion tanks, add 5.0ml of concentrated water sample to 9 digestion tanks, add 10.0ml of 70.0% nitric acid, 1.0ml of 40.0% hydrofluoric acid and 1.0ml of 30.0% hydrogen peroxide, cover the lids and insert the protective cover In, and put the burst membrane, while preparing a blank solution. Then put it into a microwave digestion apparatus for sample digestion. The digestion pressure is 2.5MPa, and the digesti...

Embodiment 3

[0102] Determination of nickel content and recovery rate in coal washing water of a coal washing plant in Dengta City

[0103] (1) Sample microwave digestion pretreatment: Accurately pipette 5.0ml of water samples of coal washing water in the morning, middle and evening shifts of three shifts in May, filtered through a filter membrane with a 0.45 μm pore size to remove particles suspended in the water (3 Add 10.0ml of 70.0% nitric acid, 1.0ml of 40.0% hydrofluoric acid and 1.0ml of 30.0% hydrogen peroxide to the digestion tank, cover the lid, insert it into the protective cover, and put the burst membrane on it, and prepare a blank solution at the same time . Then put it into a microwave digestion apparatus for sample digestion, the digestion pressure is 2.5MPa, and the digestion time is 30min. After the digestion program is finished, when the temperature display reaches 38°C, turn on the microwave digestion apparatus, take out the digestion tank and transfer the sample to a ...

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Abstract

The invention relates to a quantitative analysis method for measuring trace nickel in water by microwave digestion-flame atomic absorption spectrometry (FAAS), which is characterized in that: pretreatment is performed on a water sample by combining low-temperature concentration and microwave digestion; nonylphenol polyoxyethylene-10-ether (NP-10) is used as activating agent; and the trace content is obtained from a regression equation or a working curve according to the linear relation between the absorbance difference between the water sample and the blank solution measured by a flame atomic absorption spectrograph and the nickel content. The invention has the advantages of simple microwave digestion pretreatment process, small reagent amount, environmental protection, time saving, high efficiency and the like and is a fast, accurate, flexible and widely-applicable analysis method for measuring trace nickel in water.

Description

1. Technical field: [0001] The invention relates to a quantitative analysis method for determining trace nickel in water, in particular to the microwave digestion treatment technology for trace nickel in water and the method of using nonylphenol polyoxyethylene-10-ether (NP-10) as an activator Flame atomic absorption spectrometry is a test technique for determining trace nickel in water, specifically, it is a FAAS determination method for determining trace nickel in water. 2. Background technology: [0002] Nickel is mainly used in the production of stainless steel and nickel alloys, and is also a common catalyst in chemical production. At the same time, nickel is also an essential trace element for the human body. However, excessive nickel intake in the human body will cause harm to the body, causing skin allergies and nickel Carcinogenic. The maximum allowable concentration of nickel in the drinking water hygiene standard (GB 5749-2006) is 0.02mg / L, therefore, the determi...

Claims

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Application Information

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IPC IPC(8): G01N21/31G01N1/44
Inventor 赵丽杰赵丽萍白晓琳关晓彤李良
Owner SHENYANG POLYTECHNIC UNIV
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