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Preparation method of sol for rapidly detecting sulfur ions in environmentally friendly manner and application of sol

A technology of sulfide ions and sols, which is applied in the measurement of color/spectral characteristics, analysis by making materials undergo chemical reactions, and material analysis by observing the impact on chemical indicators, etc., can solve the problem of inability to achieve rapid detection and cumbersome operations , time-consuming and other problems, to achieve the effect of low test cost, simple preparation method and high commercial value

Active Publication Date: 2019-06-18
QINGDAO UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Sulfur dioxide is also widely used in food processing, such as sulfur fumigation and bleaching of food, but if the residual sulfur exceeds the specified content, it will cause threats and harm to the health and safety of consumers
The gravimetric method is the sulfide precipitation method, so that S 2- Lead sulfide, cadmium sulfide, copper sulfide, etc. are produced, and then acid-dissolved to form hydrogen sulfide after filtration. The iodine method is used for determination, which is cumbersome to operate and has a relatively high detection limit.
Instrumental methods include chemiluminescence, fluorescence photometry, electrochemical method, and ion chromatography-electrochemical method. These are large-scale instruments, expensive, and require professional operation.
[0008] Chinese Patent No. 2016106737364 discloses a rapid detection test paper for sulfide in water and its preparation method. It uses a paper strip soaked in a mixed solution of lead acetate and p-amino-N,N-dimethylaniline to detect water quality. The test paper can detect the water quality in 5 minutes. Rapid detection of sulfide indicators in water quality, but the detection limit can only reach 1mg / L
[0009] Chinese Patent No. 2016109425881 discloses a test paper for the detection of sulfur-containing substances. A paper strip soaked in a mixed solution of 5-25% ferric chloride solution and 1-10% potassium permanganate is used to detect sulfur ions in food for 2 hours. The detection can be completed, but the minimum detection limit is 0.1mg / L

Method used

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  • Preparation method of sol for rapidly detecting sulfur ions in environmentally friendly manner and application of sol
  • Preparation method of sol for rapidly detecting sulfur ions in environmentally friendly manner and application of sol
  • Preparation method of sol for rapidly detecting sulfur ions in environmentally friendly manner and application of sol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] A kind of preparation process of the sol of green rapid detection sulfur ion, comprises the steps:

[0043](1) Weigh 0.100 g of sodium carboxymethylcellulose (CMC), add 99.9 mL of distilled water, and configure a CMC solution with a mass fraction of 0.1%, which is designated as solution A;

[0044] (2) measure 0.01moL (1.70g) silver nitrate, 0.02moL ammoniacal liquor (1.50mL25% ammoniacal liquor) and 98.5mL distilled water, be made into the silver ammonium ion solution that concentration is 0.10mol / L, record as solution B;

[0045] (3) Add 50 μL of solution B to 50 μL of solution A under stirring at room temperature, stir at 50°C for 20 minutes, then add 50 μL of sodium ascorbic acid (Vc) with a concentration of 0.12 mol / L, and continue stirring for 25 minutes. The bright yellow CMC / AgNPs sol can be obtained.

[0046] (4) Store the prepared sol in the dark.

[0047] The prepared above-mentioned sol was used for S 2- Qualitative, the qualitative process includes:

[...

Embodiment 2

[0056] A kind of preparation process of the sol of green rapid detection sulfur ion, comprises the steps:

[0057] (1) Weigh 0.200g of sodium carboxymethylcellulose (CMC), add 99.8mL of distilled water to form a CMC solution with a mass fraction of 0.2%, and call it solution A;

[0058] (2) measure 0.02moL (3.40g) silver nitrate, 0.04moL ammoniacal liquor (3.00mL25% ammoniacal liquor) and 97.0mL distilled water, be made into the silver ammine ion solution that concentration is 0.20mol / L, denote as solution B;

[0059] (3) Add 80 μL of solution B to 70 μL of solution A under stirring at room temperature, stir at 80°C for 10 minutes, then add 50 μL of glucose solution with a concentration of 0.2 mol / L, and continue stirring for 35 minutes. Yellow CMC / AgNPs sol.

[0060] (4) Store the prepared sol in the dark.

[0061] The prepared above-mentioned sol was used for S 2- Qualitative, the qualitative process includes:

[0062] (1) Take 5 mL of CMC / AgNPs sol and dilute it 2 times...

Embodiment 3

[0069] A kind of preparation process of the sol of green rapid detection sulfur ion, comprises the steps:

[0070] (1) Weigh 0.150g of sodium carboxymethylcellulose (CMC), add 99.85mL of distilled water to form a CMC solution with a mass fraction of 0.15%, and call it solution A;

[0071] (2) Measure 0.005moL (0.850g) of silver nitrate, 0.01moL of ammonia water (0.75mL of 25% ammonia water) and 99.25mL of distilled water to form a silver ammonium ion solution with a concentration of 0.05mol / L, which is designated as solution B;

[0072] (3) Add 30 μL of solution B to 40 μL of solution A under stirring at room temperature, stir at 30°C for 20 minutes, then add 50 μL of hydrazine solution with a concentration of 0.05 mol / L, and continue stirring for 15 minutes. After the reaction is complete, you can get Bright yellow CMC / AgNPs sol.

[0073] (4) Store the prepared sol in the dark.

[0074] The prepared above-mentioned sol was used for S 2- Qualitative, the qualitative process...

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Abstract

The invention discloses a preparation method of sol for rapidly detecting sulfur ions in an environmentally friendly manner and belongs to technical field of trace sulfur ion measurement. Carboxy methyl celluloses (CMC) and a silver-ammonia complex are adopted as raw materials, an in-situ oxidation reduction method is adopted, and therefore, CMC / AgNPs sol is prepared. The invention also disclosesapplication of the sol to the qualitative determination of S<2-> and the quantitative determination of the concentration of the S<2->. The environmentally friendly natural polymer material CMC and theinorganic silver are used as the raw materials for preparing the sol; the prepared sol is highly selective to the S<2->, is not interfered by other ions and has high sensitivity; the detection limitof the sol can reach microgramma-grade and is larger than or equal to 7.68 microgramma / L; and the method is suitable for the timely, in-situ and rapid detection of sulfur ions in detection objects such as water and food. The sol is environmentally friendly, low in testing cost and has a high commercial value.

Description

technical field [0001] The invention relates to the technical field of trace sulfide ion determination, in particular to a green sol preparation method for rapid detection of sulfide ions and an application thereof. Background technique [0002] Elemental sulfur is basically non-toxic, and can be used as an additive in traditional Chinese medicine and daily necessities. It is often used as a fungicide and insecticide in agriculture, and can also be used as a mercury scavenger. It has many uses. However, sulfides are very toxic, a small amount can cause headaches, and severe ones can cause death. Hydrogen sulfide is a strong neurotoxin and has a strong stimulating effect on mucous membranes. Low concentrations of hydrogen sulfide can irritate the respiratory tract and eyes, and cause headaches. When the concentration reaches 1mg / L or higher, it is life-threatening. When the concentration is 0.00041mg / L, the odor can be smelled, when the concentration is 120-280mg / L, it can ...

Claims

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Application Information

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IPC IPC(8): G01N21/78G01N21/31
Inventor 薛云徐胜军赵昔慧孙恒李群
Owner QINGDAO UNIV
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