CN110794084A - Method for measuring calcium chlorate content - Google Patents
Method for measuring calcium chlorate content Download PDFInfo
- Publication number
- 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
- Authority
- CN
- China
- Prior art keywords
- solution
- calcium chlorate
- content
- calcium
- determining
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- 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
Landscapes
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Molecular Biology (AREA)
- Physics & Mathematics (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
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 formulaCalculating 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 formulaCalculating 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 formulaCalculating 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.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201911133105.3A CN110794084A (en) | 2019-11-19 | 2019-11-19 | Method for measuring calcium chlorate content |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201911133105.3A CN110794084A (en) | 2019-11-19 | 2019-11-19 | Method for measuring calcium chlorate content |
Publications (1)
Publication Number | Publication Date |
---|---|
CN110794084A true CN110794084A (en) | 2020-02-14 |
Family
ID=69445503
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN201911133105.3A Pending CN110794084A (en) | 2019-11-19 | 2019-11-19 | Method for measuring calcium chlorate content |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN110794084A (en) |
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 |
Citations (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
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 |
CN101975777A (en) * | 2010-10-28 | 2011-02-16 | 四川大学 | Automatic analysis method of chlorate in water sample |
CN102353669A (en) * | 2011-06-16 | 2012-02-15 | 占春瑞 | Reagents and method for quickly detecting chlorate in firework drug |
CN103091450A (en) * | 2013-01-02 | 2013-05-08 | 河北钢铁股份有限公司承德分公司 | Method for rapidly determining content of total iron in nitrided ferrovanadium |
CN104165888A (en) * | 2014-08-13 | 2014-11-26 | 国家电网公司 | Method for determining content of sodium chlorate in industrial alkali liquor |
CN105403661A (en) * | 2015-12-18 | 2016-03-16 | 深圳市清时捷科技有限公司 | Five-step iodometric method |
CN105606761A (en) * | 2015-12-23 | 2016-05-25 | 深圳市清时捷科技有限公司 | Reaction endpoint judgment device and five-step iodometry |
CN109580605A (en) * | 2018-12-04 | 2019-04-05 | 攀枝花钢企欣宇化工有限公司 | The measuring method of sodium chlorate in sodium hydroxide solution |
-
2019
- 2019-11-19 CN CN201911133105.3A patent/CN110794084A/en active Pending
Patent Citations (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
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 |
CN101975777A (en) * | 2010-10-28 | 2011-02-16 | 四川大学 | Automatic analysis method of chlorate in water sample |
CN102353669A (en) * | 2011-06-16 | 2012-02-15 | 占春瑞 | Reagents and method for quickly detecting chlorate in firework drug |
CN103091450A (en) * | 2013-01-02 | 2013-05-08 | 河北钢铁股份有限公司承德分公司 | Method for rapidly determining content of total iron in nitrided ferrovanadium |
CN104165888A (en) * | 2014-08-13 | 2014-11-26 | 国家电网公司 | Method for determining content of sodium chlorate in industrial alkali liquor |
CN105403661A (en) * | 2015-12-18 | 2016-03-16 | 深圳市清时捷科技有限公司 | Five-step iodometric method |
CN105606761A (en) * | 2015-12-23 | 2016-05-25 | 深圳市清时捷科技有限公司 | Reaction endpoint judgment device and five-step iodometry |
CN109580605A (en) * | 2018-12-04 | 2019-04-05 | 攀枝花钢企欣宇化工有限公司 | The measuring method of sodium chlorate in sodium hydroxide solution |
Non-Patent Citations (3)
Title |
---|
E.B.阿列克谢也夫斯基 等: "《定量分析 上册》", 30 November 1953, 商务印书馆 * |
上海第一医学院 主编: "《分析化学》", 30 November 1980, 人民卫生出版社出版 * |
中华人民共和国国家质量监督检验检疫总局 等: "《中华人民共和国国家标准》", 15 March 2004 * |
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 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
Diehl et al. | Eriochrome black t and its calcium and magnesium derivatives | |
CN106093287B (en) | The assay method of ammonium nitrogen content in a kind of urea ammonium nitrate solution | |
CN106290334B (en) | The chemistry in detecting of cobalt and manganese content in cobalt manganese raw material | |
CN101995383A (en) | Method for measuring copper ion content of solution | |
CN103439454B (en) | Method for measuring vanadium pentoxide content by potentiometric titration | |
CN101609049A (en) | The method of nickel and cobalt content in a kind of titrimetry test nickel compound | |
CN111735907B (en) | Method for measuring chloride ion content in industrial lanthanum oxide by potentiometric titration | |
CN110794084A (en) | Method for measuring calcium chlorate content | |
CN109633079A (en) | A method of vanadium and ammonium content in detection metavanadate solution | |
CN114805178A (en) | Fluorescent probe for detecting bisulfite ions, preparation thereof and application thereof in food detection | |
Safavi et al. | Kinetic spectrophotometric determination of traces of sulfide | |
CN109406433A (en) | Method for detecting nitric acid content in aluminum etching solution | |
CN101576481B (en) | Method for measuring contents of anionic surface active substances by methylene blue spectrometry | |
CN108267444A (en) | Method for testing chelating ability of chelating acid to metal calcium ions | |
CN102539352B (en) | Determination method of cyanogen in thiocyanate | |
CN108613936B (en) | Method for rapidly analyzing nickel in copper-nickel sulfide ore | |
CN111351784A (en) | Method for analyzing sulfate ions in lithium ion battery preparation process | |
CN103592411B (en) | A kind of method of testing of capsule core release amount of concrete chemical self-repair microcapsule | |
CN113687016B (en) | Method for detecting chloride ion content in cyclobenzaprine hydrochloride | |
CN111366489B (en) | Semi-quantitative detection method for lithium content in primary mixed material sample of ternary cathode material | |
Rosenthal et al. | Acid-Base Equilibria in Concentrated Salt Solutions. Acid-Base Titrations and Measurements of pH and H0. | |
CN113358812A (en) | Quantitative analysis method for isocyanic acid radical in melamine tail gas | |
CN104155406A (en) | Method for measuring contents of ferrous ions and zinc chloride in plating aid for hot-dip galvanizing | |
CN107402205B (en) | method for continuously measuring sodium hydroxide, sodium silicate and sodium carbonate in zincate galvanizing solution | |
RU2367944C1 (en) | Method for sulphate-ions determination in solutions |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
PB01 | Publication | ||
PB01 | Publication | ||
SE01 | Entry into force of request for substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
RJ01 | Rejection of invention patent application after publication |
Application publication date: 20200214 |
|
RJ01 | Rejection of invention patent application after publication |