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A solution and alkali fusion technology, applied in the field of analysis and detection, can solve problems such as polluting the environment, harmful to analysts' health, and inaccurate data
Inactive Publication Date: 2015-03-25
工信华鑫科技有限公司
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This method introduces the highly toxic substance mercuric chloride, which is harmful to the analyst's body, and the discharge seriously pollutes the environment
Moreover, this method is often not easy to control, and it is easy to cause problems such as delayed titration end point and inconspicuous discoloration, resulting in inaccurate data
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Embodiment 1
[0036] Take the GSB H 3005-97 national standard sample as the sample, which contains 56.09% iron.
[0037] 1. Weigh 0.2g of the sample into a corundum crucible, add 2-3g of sodium peroxide, mix well, then add 1g of sodium peroxide to cover, melt in a muffle furnace at 600-700°C for 10min, take it out and cool it, and first use hot water After leaching, add 15ml of hydrochloric acid, heat to near boiling on an electric furnace, add 100g / l tin dichloride dropwise while hot to reduce to light yellow, and cool to room temperature with running water.
[0038] 2. Add 15 drops of 250g / L sodium tungstate to the solution, add titanium trichloride solution dropwise until the tungsten blue, add 2-3 drops of copper sulfate solution, shake to make the tungsten blue disappear, add 10ml sulfur phosphorus mixed acid (2 +3), 10 drops of sodium diphenylamine sulfonate, titrated with potassium dichromate standard solution to purple as the end point.
[0039] 3. The measurement result is 55.90% ...
Embodiment 2
[0041] Take the GBW 07170 national standard sample as the sample, which contains 8.93% iron.
[0042] 1. Weigh 0.2g of the sample into a corundum crucible, add 2-3g of sodium peroxide, mix well, then add 1g of sodium peroxide to cover, melt in a muffle furnace at 600-700°C for 10min, take it out and cool it, and first use hot water After leaching, add 15ml of hydrochloric acid, heat to near boiling on an electric furnace, add 100g / l tin dichloride dropwise while hot to reduce to light yellow, and cool to room temperature with running water.
[0043] 2. Add 15 drops of 250g / L sodium tungstate to the solution, add titanium trichloride solution dropwise until the tungsten blue, add 2-3 drops of copper sulfate solution, shake to make the tungsten blue disappear, add 10ml sulfur phosphorus mixed acid (2 +3), 10 drops of sodium diphenylamine sulfonate, titrated with potassium dichromate standard solution to purple as the end point.
[0044] 3. The measurement result is 8.90% iron c...
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Abstract
The invention relates to a method for measuring total iron, and belongs to the field of analysis and detection. The method comprises the following steps: S1, fusing an iron-containing test sample at high temperature by using alkali, and then leaching by using acid; S2, heating a leaching solution to be nearly boiled, dropping tin chloride (50-150g / L) to until the light yellow color appears, and cooling; S3, dropping a titanium trichloride solution until the tungsten blue color appears by taking sodium tungstate as an indicator; S4, dropping several drops of copper solutions, and shaking to fade the tungsten blue color; S5, adding a right amount of sulfuric-phosphorous mixed acid (2+3), and titrating until the purple color as an end point appears by taking sodium diphenylamine sulfonate (4-10g / L) as an indicator and using a standard potassium dichromate solution. The method disclosed by the invention substitutes that the traditional total iron measurement in which mercuric chloride needs to be applied, so that the environmental pollution is reduced, the reaction is easily controlled by adding the copper solution and mixed sulfuric acid, end point discoloration is relatively obvious, and the method is relatively accurate, fast, simple and convenient.
Description
technical field [0001] The invention belongs to the field of analysis and detection. It relates to a method for determining total iron. Background technique [0002] The current method for determining total iron is first to reduce most of the ferric iron to ferrous iron with tin dichloride, and then oxidize and remove the excess with mercuric chloride. This method introduces the highly toxic substance mercuric chloride, which is harmful to the analyst's body, and the discharge seriously pollutes the environment. Moreover, this method is often difficult to control, and it is easy to cause problems such as delayed titration end point and inconspicuous discoloration, resulting in inaccurate data. Therefore, the current method for the determination of total iron urgently needs to be improved. Contents of the invention [0003] The object of the invention is a method for measuring total iron, the method adopts tin protochloride-titanium trichloride-potassium dichromate titra...
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