Analysis method of sulfate radicals in sulfate and thiosulfate mixture
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A thiosulfate and sulfate technology, applied in the field of chemical analysis, can solve the problems of prolonged analysis time, difficult popularization and application, increased measurement steps, etc., and achieves the effects of simple operation, fast analysis, and accurate results
Inactive Publication Date: 2011-08-03
DALIAN RES & DESIGN INST OF CHEM IND
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Ion chromatography can simultaneously determine sulfate and thiosulfate in the mixture. Although the method has little interference and strong specificity, it is difficult to be widely used in general laboratories due to expensive equipment and high operating conditions; gravimetric method, photometric method , Barium-magnesium mixture EDTA titration method and benzidine hydrochloride precipitation method due to serious interference phenomenon, all need to decompose and remove thiosulfate, thus increasing the measurement steps and prolonging the analysis time
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Embodiment 1
[0048] a) Preparation and calibration of lead nitrate standard solution
[0049] Weigh 24072g of lead nitrate, dissolve it with a small amount of water, add 1mL of 1:1 lead nitrate, and dilute to 1L with 50% ethanol solution.
[0050] Pipette 5mL of sulfate standard solution with a concentration of 001041mol / L, put it in a 100mL beaker, add 40ml of 70% ethanol solution, put a stirring bar, place it on an electromagnetic stirrer, and use 1mol / L Adjust the pH value of the nitric acid solution to 4-5, insert the 305-type lead ion selective electrode and the 851-type silver-silver chloride electrode, and carry out automatic potentiometric titration with the lead nitrate standard solution under constant stirring, and the lead nitrate standard consumed at the equivalent point The volume of the solution is 7174mL, see the titration curve figure 1 .
[0051] Calculate lead nitrate standard solution concentration according to above-mentioned formula 1, C (PbNO 3 )=0.007255mol / L.
...
Embodiment 2
[0058] a) Preparation and calibration of lead nitrate standard solution
[0059] With embodiment 1.
[0060] b) Analysis of Sulfate
[0061] Weigh 3.8681g of the mixture of sulfate and thiosulfate, dissolve it to a 500mL volumetric flask, dilute with water to the mark, and shake well to obtain solution A.
[0062] Use a pipette to pipette 20mL of solution A, put it in a 250mL Erlenmeyer flask, add 10mL of acetic acid-sodium acetate buffer solution (PH≈6), 1.0g of potassium iodide, and use iodine standard solution Titration, near the end point, add 1mL~2mL starch indicator solution, continue titration until the solution turns blue and does not fade within 30s, which is the end point, and the volume of iodine standard solution consumed is 3.10ml.
[0063] Use a pipette to pipette 20mL of solution A, place it in a 100mL volumetric flask, dilute with water to the mark, and shake well to obtain solution B. Use a pipette to take 5mL of solution B, put it in a 100mL beaker, add 4...
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Abstract
The invention belongs to the field of chemical analysis and relates to an analysis method of sulfate radicals in a sulfate and thiosulfate mixture. The method provided by the invention comprises the following steps: a) preparing and calibrating a lead nitrate standard solution, preparing an ethanol aqueous solution of lead nitrate, shifting the sulfate radical standard solution with known volume and concentration, using the aqueous solution added with ethanol as a medium, adjusting the pH value to be 4-5, inserting a lead ion-selective electrode and a silver-silver chloride electrode, carrying out automatic potentiometric titration by utilizing the lead nitrate standard solution and computing the concentration of the lead nitrate standard solution; and b) measuring the content of the thiosulfate by directly utilizing iodine standard solution titration to analyze the sulfate radicals, using the aqueous solution added with the ethanol into the solution to be measured as the medium, adjusting the pH value to be 4-5, inserting the lead ion-selective electrode and the silver-silver chloride electrode, carrying out the automatic potentiometric titration by utilizing the lead nitrate standard solution and measuring the total content of the sulfate and the thiosulfate, thereby computing the content of the sulfate radicals.
Description
technical field [0001] The invention belongs to the field of chemical analysis, and relates to a method for analyzing sulfate radicals in a mixture of sulfate and thiosulfate. Background technique [0002] Commonly used analysis methods for sulfate include ion chromatography, gravimetric analysis, photometry, barium-magnesium mixture EDTA titration, and benzidine hydrochloride precipitation method. If sulfate is mixed with thiosulfate, thiosulfate will interfere with the determination of sulfate. Ion chromatography can simultaneously determine sulfate and thiosulfate in the mixture. Although the method has little interference and strong specificity, it is difficult to be widely used in general laboratories due to expensive equipment and high operating conditions; gravimetric method, photometric method , Barium-magnesium mixture EDTA titration method and benzidine hydrochloride precipitation method have serious interference phenomena, all of which need to decompose and remov...
Claims
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