Preservation method and automatic analysis method of trace divalent sulfide ions in water samples

An automatic analysis, divalent sulfur technology, applied in the analysis of materials, material analysis through observation of the influence of chemical indicators, preparation of test samples, etc., can solve the problem of low automation, large errors, and short life of ion electrodes Selectivity and other issues, to achieve the effect of simple and fast storage method and simplified storage conditions

Inactive Publication Date: 2017-08-25
SICHUAN UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Among them, only high-performance liquid chromatography is an automatic analysis method. Other analysis methods are not highly automated and require cumbersome manual operations. Larger, the ion electrode used in the electrochemical analysis of sulfur ions has a short life and poor selectivity, while the indirect flame atomic absorption method, chemiluminescence method, fluorescence method and high performance liquid chromatography are more expensive due to the required instruments Therefore, if a low-cost automatic analysis method for trace divalent sulfide ions can be developed, it will have positive significance for reducing the analysis cost

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  • Preservation method and automatic analysis method of trace divalent sulfide ions in water samples
  • Preservation method and automatic analysis method of trace divalent sulfide ions in water samples
  • Preservation method and automatic analysis method of trace divalent sulfide ions in water samples

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Experimental program
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Effect test

Embodiment 1

[0031] In this implementation, the stability of divalent sulfide ions under different pH conditions is investigated, and the storage method of divalent sulfide ions in water samples is determined.

[0032] 1. Specimen Preparation

[0033] (1) Static divalent sulfide ion sample: 0.75g Na 2 S·9H 2 Dissolve O in deionized deionized water, dilute to 100mL volumetric flask with deoxygenated deionized water to obtain the mother liquor, and place it in a refrigerator at 4°C to refrigerate; dilute the newly prepared mother liquor with deionized water, and adjust the pH value with sodium hydroxide standard solution , to obtain pH values ​​of 7, 8, 9, 10, 11, 12, 13, 13.3, 13.47, 13.6, 13.69 and a concentration of 0.5 mg / L divalent sulfide ion solution, respectively recorded as 1 # ~ 11 # test Samples were tested at room temperature for 24 hours.

[0034] (2) Newly prepared divalent sulfide ion sample: add 0.75g Na 2 S·9H 2 O was dissolved in deoxygenated deionized water, and the v...

Embodiment 2

[0046] In this implementation, investigate the catalytic ability of divalent sulfide ion to potassium periodate oxidation indigo carmine, the steps are as follows:

[0047] 1. Preparation of sample solution

[0048] (1) Preparation of divalent sulfur standard sample: 0.75g Na 2 S·9H 2 O was dissolved in deoxygenated deionized water, then sodium hydroxide was added to a concentration of 0.1mol / L, and the mother liquor was obtained by distilling the volume into a 100mL volumetric flask with deoxygenated deionized water, and stored in a refrigerator at 4°C for later use; the mother liquor was deoxygenated with Dilute with deionized water, add sodium hydroxide to a final concentration of 0.1mol / L, and prepare a standard sample with a divalent sulfide ion concentration of 0.5mg / L.

[0049] (2) 10mmol / L KIO 4 Solution preparation: 2.23g KIO 4 Dissolve in deionized water and dilute to the mark of the 1000mL volumetric flask.

[0050] (3) Preparation of 5mmol / L indigo carmine sol...

Embodiment 3

[0058] In this embodiment, the standard sample is tested to investigate the influence of different inorganic acids on the oxidation of indigo carmine catalyzed by potassium periodate with divalent sulfur ions. The steps are as follows:

[0059] 1. Preparation of standard samples

[0060] (1) Add 0.75g Na 2 S·9H 2 Dissolve O in deoxygenated deionized water, then add sodium hydroxide to a concentration of 0.1 mol / L, dilute to 100mL volumetric flask with deoxygenated deionized water to obtain the mother liquor, and store it in a refrigerator at 4°C for later use;

[0061] (2) Dilute the mother liquor with deoxygenated deionized water, add sodium hydroxide to a final concentration of 0.1mol / L, and prepare a standard sample with a divalent sulfide ion concentration of 0.5mg / L.

[0062] 2. Preparation of oxidizing solution O

[0063] Take KIO with a concentration of 0.01mol / L 4 Aqueous solution 120mL, the final concentration acidity is 0.48mol / L H + Add different inorganic acids ...

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Abstract

The invention discloses a preservation method of trace divalent sulfide ions in a water sample. The preservation method comprises the following operating steps: collecting a water sample containing divalent sulfide ions, immediately adding sodium hydroxide into the water sample until the concentration of hydroxy radicals in the water sample reaches 0.1-0.2 mol / L, and leaving to stand for no more than 24 h' s preservation at the room temperature. The invention further discloses an automatic analysis method of trace divalent sulfide ions in the water sample; the automatic analysis method uses analytical instruments comprising a first low pressure pump, a second low pressure pump, an injection valve, a first mixer, a second mixer, a reactor, an optical flow-through cell, an optical detector and a computer processing system and further comprises the following steps: (1) determining a base line; (2) determining a spectrogram of divalent sulfide ions in a test sample; (3) drawing a standard work curve; (4) calculating the concentration of divalent sulfide ions to be measured in the test sample according to the peak height value of the spectrogram of the divalent sulfide ions and the regression equation of the working curve. According to the preservation method and the automatic analysis method of trace divalent sulfide ions in the water sample, provided by the invention, preservation operations of divalent sulfide ions in the water sample are simplified, and low-cost automatic analysis of divalent sulfide ions is also realized.

Description

technical field [0001] The invention belongs to the field of analysis and detection of sulfides, in particular to a method for storing trace divalent sulfur ions in water samples and an automatic analysis method for trace divalent sulfur ions in water samples. Background technique [0002] Sulphides in water include dissolved H 2 S, HS - , S 2- And the soluble sulfides, acid-soluble metal sulfides and unionized organic and inorganic sulfides in the suspension. Volcanic eruption, reduction of sulfide bacteria, printing and dyeing, tanning, coal coke, medicine, oil refining and paper making will all produce sulfide. The harm of sulfide in water to the environment is mainly manifested in the following aspects: (1) Toxicity: hydrogen sulfide is a very strong neurotoxic gas. When the content of hydrogen sulfide in water exceeds 0.5mg / L, it is harmful to fish and aquatic organisms. It is poisonous. If sulfide is contained in farmland irrigation water, it will cause the root sy...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N35/08G01N21/78G01N1/28
CPCG01N1/28G01N21/78G01N35/085
Inventor 张新申赵正喜莫珊高跃昕
Owner SICHUAN UNIV
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