CN110794084A - Method for measuring calcium chlorate content - Google Patents
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- CN110794084A CN110794084A CN201911133105.3A CN201911133105A CN110794084A CN 110794084 A CN110794084 A CN 110794084A CN 201911133105 A CN201911133105 A CN 201911133105A CN 110794084 A CN110794084 A CN 110794084A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
- G01N31/16—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using titration
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Abstract
The invention belongs to the technical field of analytical chemistry, and particularly relates to a method for determining the content of calcium chlorate. Aiming at the problem that no method capable of accurately determining the content of calcium chlorate exists in the prior art, the invention provides a method for determining the content of calcium chlorate, which comprises the following steps: adding sodium hydroxide into the calcium chlorate solution, adjusting the pH value, using calcium ions in the solution for precipitation, then filtering out the precipitate by using filter paper, taking the filtrate for next analysis, adding strong acid into the filtrate, reacting sodium chlorate in the filtrate with excessive ferrous sulfate in an acidic medium, dripping the excessive ferrous sulfate back by using a potassium dichromate standard solution, and indirectly calculating the content of sodium chlorate in the solution. The determination method can completely eliminate the influence of calcium ions on the titration end point, improve the accuracy of assay analysis, fill the blank of calcium chlorate content determination, and have good application prospect.
Description
Technical Field
The invention belongs to the technical field of analytical chemistry, and particularly relates to a method for determining the content of calcium chlorate.
Background
Calcium chlorate (Ca (ClO)3)2) Is an inorganic salt, white to light yellow crystals, and is usually a dihydrate needle-like crystal. Calcium chlorate is a strong oxidant, mainly used as an oxidantHerbicides and defoliants. It is also used in insecticides, pesticides, photography, fireworks, etc. The determination of the content has important significance for guiding production and use. At present, no method capable of accurately measuring the content of calcium chlorate exists.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: no method capable of accurately measuring the content of calcium chlorate exists in the prior art.
The technical scheme for solving the technical problems comprises the following steps: provides a method for measuring the content of calcium chlorate. The method comprises the following steps:
a. preparing a calcium chlorate solution, adding a sodium hydroxide solution into the calcium chlorate solution, adjusting the pH value of the solution to 11-12 to precipitate calcium ions in the solution, filtering the solution, and taking filtrate to be tested;
b. taking the filtrate with the volume V, adding strong acid into the filtrate, then adding excessive ferrous sulfate solution, after the reaction is finished, adding sodium diphenylamine sulfonate indicator, titrating by using a potassium dichromate standard solution until the solution is purple, and titrating the volume V of the potassium dichromate standard solution1；
c. B, measuring blank solution according to the steps a and b, wherein the titration volume of the blank potassium dichromate standard solution is VBlank space；
d. According to the formula
Calculating to obtain the mass volume concentration of the calcium chlorate in the sample;
wherein C represents the concentration of the potassium dichromate standard solution.
In the method for measuring the content of the calcium chlorate, the concentration of the calcium chlorate solution in the step a is 1-450 g/L.
In the method for measuring the content of the calcium chlorate, the mass concentration of the sodium hydroxide solution in the step a is 48-50%.
In the method for determining the content of calcium chlorate, the strong acid in the step b is a mixed solution of sulfuric acid and phosphoric acid.
Further, in the mixed solution, the volume ratio of the sulfuric acid to the phosphoric acid is 4: 1.
Further, the sulfuric acid is 1: 1 sulfuric acid.
In the method for measuring the content of calcium chlorate, the concentration of the ferrous sulfate solution in the step b is 0.1 +/-0.01 mol/L, and the concentration of the potassium dichromate standard solution is 0.1 +/-0.01 mol/L.
Compared with the prior art, the invention has the beneficial effects that:
the invention creatively provides a method for measuring the content of calcium chlorate, which is characterized in that sodium hydroxide is added to adjust the pH value so as to precipitate calcium ions and eliminate the interference of the calcium ions. And measuring the chlorate content in the filtrate by adopting an oxidation-reduction indirect titration method, thereby calculating the calcium chlorate content. The determination method provided by the invention is specially used for calcium chlorate, fills the blank of calcium chlorate content determination, has accurate and effective determination results, and has good application prospects.
Detailed Description
The invention provides a method for measuring the content of calcium chlorate, which comprises the following steps:
a. preparing a calcium chlorate solution, adding a sodium hydroxide solution into the calcium chlorate solution, adjusting the pH value of the solution to 11-12 to precipitate calcium ions in the solution, filtering the solution, and taking filtrate to be tested;
b. taking the filtrate with the volume V, adding strong acid into the filtrate, then adding excessive ferrous sulfate solution, after the reaction is finished, adding sodium diphenylamine sulfonate indicator, titrating by using a potassium dichromate standard solution until the solution is purple, and titrating the volume V of the potassium dichromate standard solution1；
c. B, measuring blank solution according to the steps a and b, wherein the titration volume of the blank potassium dichromate standard solution is VBlank space；
d. According to the formula
Calculating to obtain the mass volume concentration of the calcium chlorate in the sample;
wherein C represents the concentration of the potassium dichromate standard solution.
In the method for measuring the content of the calcium chlorate, the concentration of the calcium chlorate solution in the step a is 1-450 g/L.
In the method for measuring the content of the calcium chlorate, the mass concentration of the sodium hydroxide solution in the step a is 48-50%.
In the method for determining the content of calcium chlorate, the strong acid in the step b is a mixed solution of sulfuric acid and phosphoric acid.
Further, in the mixed solution, the volume ratio of the sulfuric acid to the phosphoric acid is 4: 1.
Further, the sulfuric acid is 1: 1 sulfuric acid.
In the method for measuring the content of calcium chlorate, the concentration of the ferrous sulfate solution in the step b is 0.1 +/-0.01 mol/L, and the concentration of the potassium dichromate standard solution is 0.1 +/-0.01 mol/L.
The following examples are intended to illustrate specific embodiments of the present invention without limiting the scope of the invention to the examples.
Chemical products such as calcium chlorate and the like adopted in the embodiment are all common commercial products.
The calcium chlorate used is analytically pure and is prepared into 10g/L calcium chlorate solution.
EXAMPLES determination of the calcium chlorate solution content by the method of the invention
Collecting calcium chlorate solution 100ml (preparation concentration is 10g/L), adding 50% sodium hydroxide, adjusting pH to 11.3, filtering off white precipitate with qualitative filter paper, collecting filtrate 2ml, adding FeSO 25ml4，(1：1H2SO4)20ml，H3PO4In a 5ml Erlenmeyer flask, shake well. Closing the bottle cap, and standing for 10 min. Adding 3-5 drops of diphenylamine sodium sulfonate indicator, and titrating to purple by using a potassium dichromate standard solution. Meanwhile, distilled water was used for a blank experiment. According to the formulaThe volume concentration of calcium chlorate in the sample was calculated. The actual measurement results were calculated as follows:
in the embodiment, the actually measured calcium chlorate is 10.13g/L, the theoretical concentration is 10g/L, the result deviation is small, and the accuracy is high.
Claims (7)
1. The method for measuring the content of calcium chlorate is characterized by comprising the following steps of:
a. preparing a calcium chlorate solution, adding a sodium hydroxide solution into the calcium chlorate solution, adjusting the pH value of the solution to 11-12 to precipitate calcium ions in the solution, filtering the solution, and taking filtrate to be tested;
b. taking the filtrate with the volume V, adding strong acid into the filtrate, then adding excessive ferrous sulfate solution, after the reaction is finished, adding sodium diphenylamine sulfonate indicator, titrating by using a potassium dichromate standard solution until the solution is purple, and titrating the volume V of the potassium dichromate standard solution1；
c. B, measuring blank solution according to the steps a and b, wherein the titration volume of the blank potassium dichromate standard solution is VBlank space；
d. According to the formula
Calculating to obtain the mass volume concentration of the calcium chlorate in the sample;
wherein C represents the concentration of the potassium dichromate standard solution.
2. The method for determining the calcium chlorate content of claim 1, wherein the method comprises the following steps: the concentration of the calcium chlorate solution in the step a is 1-450 g/L.
3. The method for determining the calcium chlorate content of claim 1, wherein the method comprises the following steps: and c, the mass concentration of the sodium hydroxide solution in the step a is 48-50%.
4. The method for determining the calcium chlorate content of claim 1, wherein the method comprises the following steps: and the strong acid in the step b is a mixed solution of sulfuric acid and phosphoric acid.
5. The method for determining the calcium chlorate content of claim 1, wherein the method comprises the following steps: in the mixed solution, the volume ratio of sulfuric acid to phosphoric acid is 4: 1.
6. The method for determining the calcium chlorate content of claim 1, wherein the method comprises the following steps: the sulfuric acid is 1: 1 sulfuric acid.
7. The method for determining the calcium chlorate content of claim 1, wherein the method comprises the following steps: the concentration of the ferrous sulfate solution in the step b is 0.1 +/-0.01 mol/L, and the concentration of the potassium dichromate standard solution is 0.1 +/-0.01 mol/L.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111638211A (en) * | 2020-06-11 | 2020-09-08 | 山东信发化工有限公司 | Method for detecting chlorate in brine of electrolytic cell |
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- 2019-11-19 CN CN201911133105.3A patent/CN110794084A/en active Pending
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| CN101907616A (en) * | 2010-08-27 | 2010-12-08 | 长沙兴嘉生物工程股份有限公司 | Method for determining residual quantity of oxidant in inorganic salt |
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| CN111638211A (en) * | 2020-06-11 | 2020-09-08 | 山东信发化工有限公司 | Method for detecting chlorate in brine of electrolytic cell |
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