Measurement method for whole vanadium in soil

A determination method and soil technology, applied in the measurement of color/spectral characteristics, etc., can solve the problems of inability to study the content of V in soil, environmental effects of pollution levels, lack of analysis methods for V in soil, and difficulty in popularization and application. Friendly, reliable measurement principle, accurate test results

Inactive Publication Date: 2013-02-13
SHANDONG NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In my country, there are only methods for the determination of vanadium in silicate rocks (GB / T14506.22-1993) and methods for the determination of vanadium in coal (GB / T19226-2003). There is no standard method for the determination of vanadium in soil, and there is a lack of V in soil Without analytical methods, it is impossible to study the content of V in soil, pollution degree, environmental effects, etc.; (2) The instruments involved in the catalytic kinetic method, fluorescence analysis method, wavelet transform method and ICP method currently used in the determination of trace V in water are in the Environmental monitoring stations and soil laboratories are not commonly equipped. Even if these methods can be applied to the determination of V in soil after modification, it is difficult to popularize and apply them; (3) The spectrophotometric method can successfully measure trace V in water. Monitoring stations and soil laboratories are generally equipped, but the three-phase coexistence of soil solid, liquid and gas, and the complex system of organic, inorganic, biological and other types of co-existence, when extracting V in the soil, many interference factors in the extraction solution affect the spectrophotometry law application, it is necessary to effectively mask and eliminate interference

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  • Measurement method for whole vanadium in soil
  • Measurement method for whole vanadium in soil
  • Measurement method for whole vanadium in soil

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Embodiment 1: Determine the measurement conditions and parameters of V

[0033] (1) Absorption spectrum analysis

[0034] Take 10μg of vanadium (V) standard solution and dilute it to a 25mL volumetric flask to obtain a standard concentration of vanadium of 0.4μg·mL -1 , scan the absorption spectrum of the complex of vanadium (V) and PAN in the wavelength range of 540-630nm; the maximum absorption peak is around 575nm, such as figure 1 shown;

[0035] (2) Acidity

[0036] Comparing the color reaction in hydrochloric acid, sulfuric acid, and nitric acid medium, it is found that the sensitivity in hydrochloric acid medium is the highest. When the amount of hydrochloric acid is in the range of 0-1mL, the absorbance increases with the increase of acidity. Within the range, the absorbance of the complex is stable and reaches the maximum. The absorbance of different vanadium standard solutions is different, and the absorbance also increases with the increase of the solubili...

Embodiment 2

[0052] Embodiment 2: Determine the precision and accuracy of total vanadium determination in soil

[0053] (1) Precision

[0054] Take 20 different soil samples for 20 consecutive measurements and record the statistical values ​​of the measurement results as shown in Table 2. The average value of the soil samples is 60.61-93.75 μg·g -1 , the coefficient of variation is in the range of 2.8 to 4.4, the average coefficient of variation is 3.8%, the standard deviation is in the range of 2.2 to 3.8, the average standard deviation is 2.8%; the relative standard deviation for the determination of vanadium in soil samples is less than 4%, and the variation The coefficient is about 6%, the precision is good, and the effect of repeated determination of a single sample is good;

[0055] Table 2PAN colorimetric method measures the precision of soil total vanadium

[0056]

[0057] (2) Accuracy

[0058] It can be seen from the standard recovery experiment that, as shown in Table 3, t...

Embodiment 3

[0065] Embodiment 3: measurement result comparison

[0066] By utilizing ICP measurement result to compare with the measurement result of the PAN spectrophotometry of the present embodiment, two kinds of method measurement results are similar, utilize the present embodiment method to be feasible, as shown in table 5;

[0067] Table 5 Comparison of PAN colorimetric method and ICP method for determination of vanadium in soil

[0068]

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Abstract

The invention belongs to the technical field of soil analysis measurement and relates to a method for measuring whole vanadium in soil. The method comprises the steps of weighting and placing a soil sample into a conical bottle, adding aqua regia, heating the soil sample dry on an electric furnace with a ventilation cabinet, taking down the soil sample, cooling the soil sample, adding perchloric acid, heating again to emitting white smoke, removing nitric acid after the soil sample is in ropiness, taking down the soil sample to cool, adding diluted hydrochloric acid to dissolve, filtering with distilled water to be arranged in a measuring flask in a constant volume mode, shaking up, standing, obtaining vanadium-contained soil solution to be measured, placing the vanadium-contained soil solution into a colorimetric tube, sequentially adding a color developing agent, hydrogen dioxide solution and hydrochloric acid solution, then sequentially adding a screening agent to stand and shake up to be placed, measuring absorbance of colored complex at the 575nm wave length position with a cuvette, recording measurement results, analyzing and calculating. The method is simple in technical process, reliable in measurement principle, accurate in measurement effect and data, friendly in measurement environment, and widely suitable for measuring various kinds of vanadium-contained soil.

Description

Technical field: [0001] The invention belongs to the technical field of soil analysis and testing, and relates to a method for measuring the total amount of vanadium in the soil, in particular to a method for determining the total amount of vanadium in the soil by using aqua regia-high chlorine digestion, and using 1-(2-pyridylazo)-2-naphthalene Phenol (PAN) is used as the color reagent, and the surfactant sodium dodecyl sulfonate (SDBS) is used as the sensitizer to measure the pollution status of heavy metal vanadium in the soil environment by spectrophotometry. Background technique: [0002] Vanadium (V) is a new metal discovered by Swedish chemist Sefstrom N G from Scandinavian iron ore in 1805. It is named Vanadium following the name "Vanadis" of the Scandinavian legend of love and goddess. Due to its high melting point and the ratio of elastic modulus to density similar to that of steel materials, vanadium is widely used in structural materials. According to the statis...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N21/31
Inventor 成杰民白贯荣王晓凤
Owner SHANDONG NORMAL UNIV
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