Automatic Analysis Method of Trace Divalent Nickel in Water Samples

An automatic analysis, divalent nickel technology, applied to the analysis of materials, instruments, etc., can solve the problems of poor absorbance, operator injury, high detection limit, etc., to improve the analysis speed, simplify the analysis operation, and eliminate the effect of absorbance difference

Inactive Publication Date: 2016-08-24
SICHUAN UNIV
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Problems solved by technology

However, this method has the following disadvantages: (1) due to the use of gallic acid to mask iron, the complex of gallic acid and iron is black, causing the sample to absorb at all wavelengths and cannot be directly analyzed. In order to avoid the complex formed by gallic acid and iron Compounds interfere with the analysis of target substances, while avoiding the damage of EDTA to cobalt and nickel colored complexes, the organic extractant benzene-n-butanol must be used for extraction and separation. The extraction operation must be performed manually, and online automatic analysis cannot be realized. agent will cause harm to the operator
(2) This method is a colorimetric analysis method, which requires manual operation, and it is prone to differences in absorbance between samples due to different degrees of color reaction or extraction, thereby affecting the accuracy of the analysis
(3) The detection limit of this method is very high, which can only realize the analysis of constant or trace nickel, but cannot directly analyze trace nickel, and cannot be used for the analysis of trace nickel water samples
[0004] Inductively coupled plasma-atomic emission spectrometry (ICP-AES) and inductively coupled plasma mass spectrometry (ICP-MS) have also been applied to the determination of nickel, and when used for the determination of nickel in human urine and biological samples, ICP- AES detection limit is 10 -3 μg / g, when determining nickel in cigarette paper, the detection limit of ICP-MS is 10 -6 μg / g (Li Ru et al., 2010), but the operation of inductively coupled plasma spectrometry is cumbersome, especially the equipment used in this method is very expensive, which seriously limits their wide use
At the same time, when ICP-MS is used for sample analysis of high-calcium matrix, it will cause serious interference to the detection of trace nickel, and there is a problem of low recovery rate (He Guangtao et al., 2009)

Method used

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  • Automatic Analysis Method of Trace Divalent Nickel in Water Samples
  • Automatic Analysis Method of Trace Divalent Nickel in Water Samples
  • Automatic Analysis Method of Trace Divalent Nickel in Water Samples

Examples

Experimental program
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Embodiment 1

[0029]Since the method of the present invention does not use pretreatment operations such as organic solvent extraction, some ions in the environmental water sample may interfere with the measurement of Ni(II). In this embodiment, first understand whether the interfering ions will interfere with the measurement of Ni(II) .

[0030] 1. Chromogenic solution R 1 preparation

[0031] Take 9mL of cetyltrimethylammonium bromide (CTMAB) aqueous solution with a concentration of 0.01g / L, 15mL of NH with pH=10 3 -NH 4 Cl buffer solution, 6 mL of 2-(5-bromo-2-pyridylazo)-5-diethylaminophenol (5-Br-PADAP) with a concentration of 2×10 -4 g / L 5-Br-PADAP ethanol solution, 3 mL of 0.25 g / L triethanolamine (TEA) aqueous solution, 5 mL of 0.1 g / L potassium sodium tartrate aqueous solution were added to a 50 mL volumetric flask, and deionized water was added Set the volume to the mark, and ultrasonically treat for 30 minutes to obtain the chromogenic solution R 1 , in the chromogenic soluti...

Embodiment 2

[0042] In this embodiment, the standard sample is tested to investigate the precision of the method of the present invention. The steps are as follows:

[0043] 1. Preparation of standard samples

[0044] (1) Weigh 0.4785g NiSO 4 ·7H 2 O in a beaker, dissolved in deionized water, then added nitric acid to a final concentration of 5mmol / L, then distilled to a 100mL volumetric flask with deionized water, refrigerated in a refrigerator for later use, and the solution was calibrated as Ni(II) ) concentration is the mother liquor of 1g / L;

[0045] (2) Dilute the mother liquor with simulated environmental water (20mg / L Ca 2+ , 10mg / L Mg 2+ , 100mg / L HCO 3 - ), dilute with nitric acid until the final concentration of nitric acid is 5 mmol / L, and prepare a standard sample with a Ni(II) concentration of 25 μg / L.

[0046] 2. Chromogenic solution R 1 preparation

[0047] Take 9mL CTMAB concentration and be the CTMAB aqueous solution of 0.01g / L, 15mL the NH of pH=10 3 -NH 4 Cl...

Embodiment 3

[0057] In this embodiment, the tested sample is simulated environmental water plus Ni(II) standard sample. Its analysis steps are as follows:

[0058] 1. Preparation of standard samples

[0059] (1) Weigh 0.4785g NiSO 4 ·7H 2 O in a beaker, dissolved in deionized water, then added nitric acid to a final concentration of 5mmol / L, then distilled to a 100mL volumetric flask with deionized water, refrigerated in a refrigerator for later use, and the solution was calibrated as Ni(II) ) concentration is the mother liquor of 1g / L;

[0060] (2) Prepare a series of standard samples: Dilute the mother liquor prepared in step (1) with deionized water, add nitric acid until the final concentration of nitric acid is 5 mmol / L, and prepare 1# to 15# standard samples. Ni(Ⅱ) in each standard sample ) concentrations are 5μg / L, 10μg / L, 25μg / L, 50μg / L, 100μg / L, 125μg / L, 150μg / L, 175μg / L, 200μg / L, 225μg / L, 250μg / L, 275μg / L, 300μg / L, 350μg / L, 400μg / L, and the concentration of nitric acid in 1...

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Abstract

The invention provides an automatic analysis method for trace divalent nickel in a water sample. By using analysis instruments including a sample flow path, a propellant liquid flow path, a developing liquid flow path, a masking agent flow path, an injection valve, a mixer, a first reactor, a second reactor, an optical flow cell, an optical detector, a computer processing system and a low-pressure pump, the automatic analysis method comprises the following steps: (1) drawing a baseline; (2) drawing a spectrogram of divalent nickel in a test sample; (3) drawing a standard working curve; and (4) according to the peak height value of the divalent nickel spectrogram and the standard working curve, calculating the concentration of the to-be-tested divalent nickel in the test sample. The propellant liquid is HNO3 water solution, the masking agent is ethylenediamine tetraacetic acid disodium water solution, and the developing liquid is a mixed solution prepared from cetrimonium bromide, 2-(5-bromo-2-pyridylazo)-5-diethylaminophenol, alcohol, potassium sodium tartrate tetrahydrate, triethanolamine, NH3-NH4Cl buffering solution and deionized water. The method is simple to operate, fast in analysis speed, low in analysis cost and low in detection limit.

Description

technical field [0001] The invention belongs to the field of detection and analysis of heavy metal nickel in environmental water bodies, in particular to an automatic analysis method for trace divalent nickel in water samples. Background technique [0002] Nickel is widely used in electroplating, stainless steel, magnets, coins, batteries, medical metal materials, and catalysts for hydrogenation reactions. Nickel is also the active center of certain enzymes. It is an essential trace element and is of great significance to life activities. Nickel compounds can enter the body through various routes, interact with biomolecules in tissue cells through the body's membrane barrier, and accumulate in the liver, kidney, lung, cardiovascular system, and blood, leading to various toxic effects. The health standard for the limit of nickel in food in my country recommends that the per capita daily intake is 0.440 mg, and the guideline value of nickel concentration recommended by the Wor...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N35/00
Inventor 张新申赵正喜高跃昕莫珊
Owner SICHUAN UNIV
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