CN111239331A - Method for detecting content of calcium oxide in quick lime - Google Patents
Method for detecting content of calcium oxide in quick lime Download PDFInfo
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- CN111239331A CN111239331A CN202010199460.7A CN202010199460A CN111239331A CN 111239331 A CN111239331 A CN 111239331A CN 202010199460 A CN202010199460 A CN 202010199460A CN 111239331 A CN111239331 A CN 111239331A
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- G—PHYSICS
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- 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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- 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
- G01N31/22—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using chemical indicators
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Abstract
The invention discloses a method for detecting the content of calcium oxide in quick lime, which comprises the following steps: (1) drying a quicklime sample, putting the quicklime sample into a beaker, adding distilled water for wetting, adding concentrated hydrochloric acid, heating to boil to completely dissolve quicklime, and cooling to obtain a free calcium solution; (2) transferring the free calcium solution obtained in the step (1) into a volumetric flask, adding distilled water to a constant volume, shaking up, sequentially adding a triethanolamine solution and a calcium carboxylic acid indicator, shaking up and dropwise adding a sodium hydroxide solution, and then titrating with an EDTA standard solution until the solution is changed from wine red to pure blue; (3) taking a calcium oxide standard substance, and repeating the step (1) and the step (2); (4) the content of calcium oxide was calculated. The method comprises the steps of adding concentrated hydrochloric acid during detection, heating to boil, enabling calcium ions to be fully dissociated, enabling the heated solution to be clear, adding a calcium carboxylic acid indicator in a matched manner, dropping EDTA standard solution at regular time, enabling the solution to have obvious color change, and accurately judging the detection endpoint.
Description
Technical Field
The invention relates to the technical field of chemical inspection, in particular to a method for detecting the content of calcium oxide in quick lime.
Background
In the current standard method for chemical industry inspection, the industrial calcium oxide content inspection is mainly performed by a more authoritative sucrose method in the chemical industry, the reaction mechanism is that calcium oxide and sucrose generate sucrose calcium with higher solubility, phenolphthalein is used as an indicator, and the calcium oxide content is titrated and calculated by using a hydrochloric acid standard solution. In the actual application standard method, because industrial quick lime contains more impurities and the content of calcium oxide is low, the generated calcium sucrose is mixed with the impurities, the color of an inspection end point is turbid or not obvious, the inspection end point judgment and the detection result are influenced, and a plurality of parallel experiments are needed to obtain a relatively accurate inspection result.
Disclosure of Invention
Aiming at the prior art, the invention aims to provide a method for detecting the content of calcium oxide in quick lime.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention provides a method for detecting the content of calcium oxide in quick lime, which comprises the following steps:
(1) drying a quicklime sample, putting the quicklime sample into a beaker, adding distilled water for wetting, adding concentrated hydrochloric acid, heating to completely dissolve the quicklime, and cooling to obtain a free calcium solution;
(2) transferring the free calcium solution obtained in the step (1) into a volumetric flask, adding distilled water to a constant volume, shaking up, sequentially adding a triethanolamine solution and a calcium carboxylic acid indicator, shaking up and dropwise adding a sodium hydroxide solution until the test solution is changed from blue to wine red, and then titrating with an EDTA standard solution until the solution is changed from wine red to pure blue;
(3) taking a calcium oxide standard substance with the same quality as the quicklime sample, and repeating the step (1) and the step (2);
(4) calculating the content of calcium oxide; content of calcium oxide:
in the formula: w- - -the content of calcium oxide in the calcium oxide standard substance, the unit is%;
V1-titrating the calcium oxide standards to consume the volume of EDTA standard solution in ml;
m1-weighing the calcium oxide standard in g;
V2- -the volume of EDTA standard solution consumed by the titration sample in ml;
m2weighing the weight of the sample in g.
Preferably, in the step (1), the drying is carried out at a temperature of 105-110 ℃ to a constant weight, and the moisture is removed by drying.
Preferably, in the step (1), the solid-to-liquid ratio of the quicklime sample to the concentrated hydrochloric acid is 1g to 30 ml.
Preferably, in step (1), cooling is carried out to room temperature. Heating to boiling can dissolve calcium oxide in the quicklime sufficiently, and the solution will be relatively clear.
In the step (1), distilled water is added for wetting, then concentrated hydrochloric acid is added, and the purpose of wetting by adding distilled water is that the dried and constant-weight quicklime is a powdery sample and is fluffy, so that the quicklime can be scattered in air flow to cause component loss, and the quicklime cannot be lost after being wetted by water.
Preferably, in the step (1), the mass concentration of the concentrated hydrochloric acid is 36-38%.
Preferably, in the step (2), the volume ratio of the triethanolamine to the free calcium solution is (1-2): 25.
Preferably, in the step (2), the solid-to-liquid ratio of the calcium carboxylic acid indicator to the free calcium solution is (1-2) g: 250 ml.
Preferably, in the step (2), the mass ratio of the calcium carboxylic acid indicator to the sodium chloride in the calcium carboxylic acid indicator is 1: 99.
Preferably, in the step (2), the sodium hydroxide solution has a mass concentration of 10%.
Preferably, in step (2), the sodium hydroxide solution is added dropwise in an excess amount so that the pH of the solution is 12.5 or more.
Preferably, in the step (2), the mass concentration of the triethanolamine solution is 30-35%.
Preferably, in step (2), the substance of the EDTA standard solution is present in a concentration of 0.05 mol/l.
Preferably, in the step (3), the content of calcium oxide in the calcium oxide standard product is 51.20%.
The invention has the beneficial effects that:
1. the invention innovates the original detection method, adds concentrated hydrochloric acid during detection, then heats and boils to ensure that calcium ions are fully dissociated, the heated solution is clear and not turbid, and is matched with the calcium carboxylic acid indicator, and the EDTA standard solution is used for dripping for timing, so that the solution is changed from wine red into pure blue, the solution color change is obvious, the detection end point judgment is accurate, the problem of inaccurate detection end point judgment during the detection of the original sucrose method is solved, and the detection is simplified and accurate.
2. The content of the calcium oxide in the test sample of the lime can be calculated by substituting the content of the calcium oxide in the calcium oxide standard sample into a formula through the matching detection of the calcium oxide standard sample, and the operation is convenient.
Detailed Description
It should be noted that the following detailed description is exemplary and is intended to provide further explanation of the disclosure. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs.
As introduced in the background art, when the content of calcium oxide in industrial quicklime is detected at present, a sucrose method is generally adopted, sucrose calcium is generated by adding a sucrose solution, phenolphthalein is used as an indicator, and the detection endpoint is turbid in color or not obvious in color development during detection, so that the detection endpoint judgment and the detection result are influenced.
Based on the above, the invention discloses a method for detecting the content of calcium oxide in quick lime, which comprises the steps of adding concentrated hydrochloric acid, heating to boil, fully dissociating calcium ions, ensuring that the heated solution is clear and not turbid, adding a calcium carboxylic acid indicator, and dripping the EDTA standard solution to ensure that the solution is changed from wine red into pure blue, the solution has obvious color change and the detection endpoint is accurately judged.
In order to make the technical solutions of the present application more clearly understood by those skilled in the art, the technical solutions of the present application will be described in detail below with reference to specific embodiments.
The test materials used in the examples of the present invention are all conventional in the art and commercially available.
1. Sample preparation
The sample must be representative and uniform, and the obtained large sample is divided into 100g of samples for detection.
2. Preparation of reagents
2.1 calcium carboxylic acid indicator: mixing a calcium carboxylic acid indicator and sodium chloride dried at 105 ℃ for 2h according to a mass ratio of 1:99 are fully ground and evenly mixed in a mortar, and then are put in a wide-mouth bottle with a ground mouth for standby.
2.2 triethanolamine solution: 250ml of triethanolamine were weighed out and mixed with 750ml of distilled water.
2.3 calcium oxide standard sample: the calcium oxide content was 51.20%, which is a standard sample of Ministry of metallurgy purchased from institute of metallurgy in Shandong province.
2.4 disodium Ethylenediaminetetraacetate (EDTA) standard solution: the mass concentration was 0.05 mol/l.
2.5 sodium hydroxide solution: 10% sodium hydroxide solution.
Example 1: a method for detecting the content of calcium oxide in quick lime comprises the following steps:
(1) drying 0.5g of quicklime sample, placing the dried quicklime sample in a 100ml beaker, adding distilled water for wetting, adding 15ml of concentrated hydrochloric acid, heating to boil to completely dissolve quicklime, and cooling to obtain a free calcium solution; the drying is carried out at the temperature of 100-110 ℃ to constant weight;
(2) taking 25ml of the free calcium solution obtained in the step (1), transferring the free calcium solution into a volumetric flask of 250ml, adding distilled water to a constant volume of 250ml, shaking up, sequentially adding 5ml of triethanolamine solution and 0.1g of calcium carboxylic acid indicator, shaking up and dropwise adding 10% by mass sodium hydroxide solution until the test solution changes from blue to wine red and the sodium hydroxide solution is excessive by 0.5ml so that the pH of the solution is more than 12.5, and then titrating with EDTA standard solution until the solution changes from wine red to pure blue;
(3) taking 0.5g of calcium oxide standard substance, and repeating the step (1) and the step (2);
(4) calculating the content of calcium oxide; content of calcium oxide:
in the formula: w- - -the content of calcium oxide in the calcium oxide standard substance, the unit is%;
V1-titrating the calcium oxide standards to consume the volume of EDTA standard solution in ml;
m1-weighing the calcium oxide standard in g;
V2- -the volume of EDTA standard solution consumed by the titration sample in ml;
m2weighing the weight of the sample in g.
Methodology investigation test:
repeatability and accuracy surveys
By respectively detecting the content of the same batch of calcium oxide with known content by using the method of the application example 1 and the existing sucrose method, the content of the calcium oxide sample is 49.1%.
The test method comprises the following steps: the same sample and the same experimenter use the method of the application example 1 and the existing sucrose method to respectively repeat titration for 5 times, and record the result of each time; the same sample, different experimenters, were titrated 5 times with the method of the present invention and the existing sucrose method, and the results were recorded each time. The results are shown in the following table:
as can be seen from the table above, the calcium oxide content is measured by the method of the invention, different testers operate different times, the measured calcium oxide content results are not very different, and compared with the existing sucrose method, the titration end point of the method of the invention is judged well, so the repeatability of the method of the invention is better.
The closer the calcium oxide content measured by the method of the invention in the example 1 is to the known content value of the calcium oxide sample, so the method of the invention in the example 1 has high accuracy.
The above description is only a preferred embodiment of the present application and is not intended to limit the present application, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, improvement and the like made within the spirit and principle of the present application shall be included in the protection scope of the present application.
Claims (8)
1. A method for detecting the content of calcium oxide in quick lime is characterized by comprising the following steps:
(1) drying a quicklime sample, putting the quicklime sample into a beaker, adding distilled water for wetting, adding concentrated hydrochloric acid, heating to boil to completely dissolve quicklime, and cooling to obtain a free calcium solution;
(2) transferring the free calcium solution obtained in the step (1) into a volumetric flask, adding distilled water to a constant volume, shaking up, sequentially adding a triethanolamine solution and a calcium carboxylic acid indicator, shaking up and dropwise adding a sodium hydroxide solution until the test solution is changed from blue to wine red, and then titrating with an EDTA standard solution until the solution is changed from wine red to pure blue;
(3) taking a calcium oxide standard substance with the same quality as the quicklime sample, and repeating the step (1) and the step (2);
(4) calculating the content of calcium oxide; content of calcium oxide:
in the formula: w- - -the content of calcium oxide in the calcium oxide standard substance, the unit is%;
V1-titrating the calcium oxide standards to consume the volume of EDTA standard solution in ml;
m1-weighing the calcium oxide standard in g;
V2- -the volume of EDTA standard solution consumed by the titration sample in ml;
m2weighing the weight of the sample in g.
2. The detection method according to claim 1, wherein in the step (1), the drying is performed at a temperature of 100 ℃ to 110 ℃ to a constant weight.
3. The method according to claim 1, wherein in the step (1), the solid-to-liquid ratio of the quicklime sample to the concentrated hydrochloric acid is 1g:30 ml.
4. The method according to claim 1, wherein in the step (2), the volume ratio of triethanolamine to the free calcium solution is (1-2): 25.
5. The method according to claim 1, wherein in the step (2), the solid-to-liquid ratio of the calcium carboxylic acid indicator to the free calcium solution is (1-2) g: 250 ml.
6. The preparation method according to claim 1, wherein in the step (2), the mass ratio of the calcium carboxylic acid indicator to the sodium chloride in the calcium carboxylic acid indicator is 1: 99.
7. The production method according to claim 1, wherein in the step (2), the triethanolamine solution has a mass concentration of 30 to 35%.
8. The method according to claim 1, wherein in the step (3), the content of calcium oxide in the calcium oxide standard is 51.20%.
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| CN202010199460.7A CN111239331A (en) | 2020-03-20 | 2020-03-20 | Method for detecting content of calcium oxide in quick lime |
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Cited By (1)
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| CN113640454A (en) * | 2021-07-30 | 2021-11-12 | 华能国际电力股份有限公司上海石洞口第一电厂 | Method for rapidly testing content of calcium oxide in limestone |
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