CN115468951A - Method for testing relative content of cement in cement mixture - Google Patents
Method for testing relative content of cement in cement mixture Download PDFInfo
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- CN115468951A CN115468951A CN202211305235.2A CN202211305235A CN115468951A CN 115468951 A CN115468951 A CN 115468951A CN 202211305235 A CN202211305235 A CN 202211305235A CN 115468951 A CN115468951 A CN 115468951A
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Abstract
The invention belongs to the technical field of cement content determination, and particularly relates to a method for testing the relative content of cement in a cement mixture. According to the components of the cement mixture to be detected, samples with different cement contents are prepared in advance, disodium ethylene diamine tetraacetate is used for titrating the samples respectively, the dosage of the disodium ethylene diamine tetraacetate is determined, and a standard curve of the mass percentage of the cement and the dosage of the disodium ethylene diamine tetraacetate is constructed; substituting the set value of the cement content into the standard curve to determine the required dosage of the disodium ethylene diamine tetraacetate under the set value of the cement content; premixing a cement mixture to be detected and an ammonium chloride solution, and performing solid-liquid separation to obtain a supernatant; and mixing the supernatant with the ethylene diamine tetraacetic acid, the sodium hydroxide solution and the calcium red indicator which are determined to be used in the set value of the cement content, and observing the difference between the determined color and the set value of the cement content. The test method provided by the invention is simple and easy to operate and short in test time.
Description
Technical Field
The invention belongs to the technical field of cement content determination, and particularly relates to a qualitative testing method for cement content in a cement mixture.
Background
For cement-based mixture, the cement in the mixture mainly plays a role of a binder, so that loose sand and stone materials in the mixture can be hardened and generate strength; therefore, the regulation and control of the cement content in the mixture in the construction process are very important.
However, the conventional method for determining the cement content needs many detection devices, mainly comprises a burette, an iron support, a conical flask and the like, is not easy to operate in a complicated construction site, has a long determination period, and cannot timely determine whether the cement content in the cement mixture meets the construction requirements.
Disclosure of Invention
The invention aims to provide a method for testing the relative content of cement in a cement mixture.
In order to achieve the above purpose, the invention provides the following technical scheme:
the invention provides a method for testing the relative content of cement in a cement mixture, which comprises the following steps:
preparing samples with different cement contents in advance according to the components of the cement mixture to be detected, titrating the samples respectively by using disodium ethylene diamine tetraacetate, determining the using amount of the disodium ethylene diamine tetraacetate, and constructing a standard curve of the mass percentage of the cement and the using amount of the disodium ethylene diamine tetraacetate;
substituting a set value of the cement content into the standard curve, and determining the dosage of the required disodium ethylene diamine tetraacetate under the set value of the cement content;
premixing a cement mixture to be detected and an ammonium chloride solution, and performing solid-liquid separation to obtain a supernatant;
and mixing the supernatant with the disodium ethylene diamine tetraacetate, the sodium hydroxide solution and the calcium red indicator which are determined by the dosage under the set value of the cement content, and observing the color of the obtained mixed solution:
when the color of the mixed solution is red, the cement content in the cement mixture to be detected is higher than the set value of the cement content;
and when the color of the mixed solution is blue, the cement content in the cement mixture to be detected is equal to or lower than the set value of the cement content.
Preferably, the dosage ratio of the ammonium chloride in the cement mixture to be tested and the ammonium chloride solution is 1000g:4.16mol.
Preferably, the ratio of the amount of sodium hydroxide in the supernatant to the amount of sodium hydroxide in the sodium hydroxide solution is 10mL:0.0225mol.
Preferably, the dosage ratio of the supernatant to the calcium red indicator is 10mL: 0.2-0.3 g.
Preferably, the ethylene diamine tetraacetic acid with the determined dosage is added in the form of an ethylene diamine tetraacetic acid solution under the set value of the cement content;
the molar concentration of the ethylene diamine tetraacetic acid in the ethylene diamine tetraacetic acid solution is 0.0001mol/L.
The invention provides a method for testing the relative content of cement in a cement mixture, which comprises the following steps: preparing samples with different cement contents in advance according to the components of the cement mixture to be detected, titrating the samples respectively by using disodium ethylene diamine tetraacetate, determining the dosage of the disodium ethylene diamine tetraacetate, and constructing a standard curve of the mass percentage of the cement and the dosage of the disodium ethylene diamine tetraacetate; substituting the set value of the cement content into the standard curve to determine the required dosage of the disodium ethylene diamine tetraacetate under the set value of the cement content; premixing a cement mixture to be detected and an ammonium chloride solution, and performing solid-liquid separation to obtain a supernatant; and mixing the supernatant with the disodium ethylene diamine tetraacetate, the sodium hydroxide solution and the calcium red indicator which are determined by the cement content set value, and observing the color of the obtained mixed solution: when the color of the mixed solution is red, the cement content in the cement mixture to be detected is higher than the set value of the cement content; and when the color of the mixed solution is blue, the cement content in the cement mixture to be detected is equal to or lower than the set value of the cement content. The invention determines the difference between the cement content in the cement mixture to be detected and the set value of the cement content by observing the color change. The testing method provided by the invention does not need a complicated testing instrument and has short testing time; meanwhile, the method is not influenced by the environment, and can be used for qualitatively testing the cement content of the cement mixture to be tested on any complex construction site.
Drawings
FIG. 1 is a standard curve of the mass percent of cement obtained in example 1 versus the volume of a disodium ethylenediaminetetraacetate solution;
FIG. 2 is a standard curve of the mass percent of cement obtained in example 2 versus the volume of the disodium EDTA solution.
Detailed Description
The invention provides a method for testing the relative content of cement in a cement mixture, which comprises the following steps:
preparing samples with different cement contents in advance according to the components of the cement mixture to be detected, titrating the samples respectively by using disodium ethylene diamine tetraacetate, determining the dosage of the disodium ethylene diamine tetraacetate, and constructing a standard curve of the mass percentage of the cement and the dosage of the disodium ethylene diamine tetraacetate;
substituting a set value of the cement content into the standard curve, and determining the dosage of the required disodium ethylene diamine tetraacetate under the set value of the cement content;
premixing the cement mixture to be detected and an ammonium chloride solution, and performing solid-liquid separation to obtain a supernatant;
and mixing the supernatant with the disodium ethylene diamine tetraacetate, the sodium hydroxide solution and the calcium red indicator which are determined by the dosage under the set value of the cement content, and observing the color of the obtained mixed solution:
when the color of the mixed solution is red, the cement content in the cement mixture to be detected is higher than the set value of the cement content;
and when the color of the mixed solution is blue, the cement content in the cement mixture to be detected is equal to or lower than the set value of the cement content.
In the present invention, all the raw materials are commercially available products well known to those skilled in the art unless otherwise specified.
According to the invention, samples with different cement contents are prepared in advance according to the components of the cement mixture to be detected, disodium ethylene diamine tetraacetate is used for carrying out titration on the samples respectively, the dosage of the disodium ethylene diamine tetraacetate is determined, and a standard curve of the mass percentage content of the cement and the dosage of the disodium ethylene diamine tetraacetate is constructed and obtained.
The invention has no special limitation on the components of the cement mixture to be tested, as long as the cement mixture to be tested contains cement.
In a specific embodiment of the present invention, the components of the cement mixture to be tested preferably include cement, water and an inorganic binder stabilizing material; the mass ratio of the cement to the water to the inorganic binder stabilizing material is preferably 5:100:5.5.
in the present invention, the inorganic binder stabilizing material preferably includes stone chips, a first crushed stone, and a second crushed stone. In the present invention, the particle size of the stone chips is preferably 5mm or less. In the present invention, the particle diameter d of the first crushed stone is preferably: d is more than 5mm and less than 10mm. In the present invention, the second crushed stone preferably has a particle size of 10 to 30mm. In the present invention, the mass ratio of the stone chips, the first crushed stone, and the second crushed stone is preferably 3:4:3 (marked as formula one);
or the components of the cement mixture to be detected comprise cement, water and an inorganic binder stabilizing material; the mass ratio of the cement to the water to the inorganic binder stabilizing material is preferably 5:100:6.
in the present invention, the inorganic binder stabilizing material preferably includes stone chips, a first crushed stone, and a second crushed stone. In the present invention, the particle size of the stone chips is preferably 5mm or less. In the present invention, the particle diameter d of the first crushed stone is preferably: d is more than 5mm and less than 10mm. In the present invention, the second crushed stone preferably has a particle size of 10 to 30mm. In the present invention, the mass ratio of the stone chips, the first crushed stone, and the second crushed stone is preferably 3.5:3:3.5 (noted as formulation two).
In the present invention, the cement content in the sample is preferably 1 to 10%. The method for preparing the samples with different cement contents is not particularly limited, and the method known by the person skilled in the art can be adopted.
The titration process is not particularly limited in the present invention, and those skilled in the art can use the same.
In the present invention, the method for determining the standard curve preferably comprises the steps of:
respectively mixing the samples with different cement contents with an ammonium chloride solution for the first time, and then separating to obtain a first supernatant;
secondly, mixing the first supernatant with a sodium hydroxide solution and a calcium red indicator to obtain a mixed solution;
titrating the mixed solution to blue by using disodium ethylene diamine tetraacetate, and recording the dosage of the disodium ethylene diamine tetraacetate;
and drawing a standard curve of the percentage cement content-disodium ethylene diamine tetraacetate content by taking the cement content as a horizontal coordinate and the disodium ethylene diamine tetraacetate content as a vertical coordinate.
The concentration of the ammonium chloride solution is not particularly limited in the present invention, and those known to those skilled in the art can be used. In the present invention, the amount ratio of ammonium chloride in the sample and the ammonium chloride solution is preferably 1000g:4.16mol.
The first mixing and separating process of the present invention is not particularly limited, and may be performed by a process known to those skilled in the art.
In the present invention, the molar concentration of the sodium hydroxide solution is preferably 0.45mol/L. In the present invention, the ratio of the amount of sodium hydroxide in the first supernatant to the amount of sodium hydroxide in the sodium hydroxide solution is preferably 10mL:0.0225mol. In the present invention, the ratio of the first supernatant to the calcium red indicator is preferably 10mL:0.2 to 0.3g.
In the present invention, the amount of the disodium edetate can be expressed by the amount of the substance of the disodium edetate or the volume of the disodium edetate solution with a specific molar concentration.
In the embodiment of the present invention, it is preferable to draw a standard curve of the percentage cement content to the volume of the disodium ethylenediaminetetraacetate solution by taking the volume of the disodium ethylenediaminetetraacetate solution with a specific molar concentration as a vertical coordinate. In the embodiment of the present invention, the molar concentration of the disodium ethylene diamine tetraacetate solution is preferably 0.0001mol/L.
The process of the second mixing process is not particularly limited in the present invention, and may be performed by a process known to those skilled in the art.
After a standard curve of the cement mass percentage content-disodium ethylene diamine tetraacetate dosage is obtained, the invention substitutes the set value of the cement content into the standard curve to determine the required disodium ethylene diamine tetraacetate dosage under the set value of the cement content.
The method comprises the steps of premixing the cement mixture to be detected and an ammonium chloride solution, and carrying out solid-liquid separation to obtain a supernatant.
The concentration of the ammonium chloride solution is not particularly limited in the present invention, and those known to those skilled in the art can be used. In the invention, the dosage ratio of the ammonium chloride in the cement mixture to be tested and the ammonium chloride solution is preferably 1000g:4.16mol.
In the present invention, the premixing is preferably performed under stirring. The present invention is not limited to the above-mentioned conditions, and the stirring may be carried out by a method known to those skilled in the art. After the premixing, the present invention preferably further comprises allowing the obtained mixed solution to stand. The time for the standing is not particularly limited in the present invention, and those known to those skilled in the art can be used.
The process of the solid-liquid separation is not particularly limited in the present invention, and those well known to those skilled in the art can be used.
After the supernatant is obtained, the supernatant is mixed with the disodium ethylene diamine tetraacetate, the sodium hydroxide solution and the calcium red indicator with the determined dosage under the set value of the cement content, and the color of the obtained mixed solution is observed:
when the color of the mixed solution is red, the cement content in the cement mixture to be detected is higher than the set value of the cement content;
and when the color of the mixed solution is blue, the cement content in the cement mixture to be detected is equal to or lower than the set value of the cement content.
In the invention, the disodium ethylene diamine tetraacetate with a determined dosage is added in the form of disodium ethylene diamine tetraacetate solution under the set value of the cement content; the molar concentration of the ethylene diamine tetraacetic acid in the ethylene diamine tetraacetic acid solution is 0.0001mol/L.
In a specific embodiment of the invention, the molar concentration of the sodium hydroxide solution is preferably 0.45mol/L. In the present invention, the ratio of the amount of sodium hydroxide in the supernatant to the amount of sodium hydroxide in the sodium hydroxide solution is 10mL:0.0225mol. In the present invention, the ratio of the amount of the supernatant to the amount of the calcium red indicator is preferably 10mL: 0.2-0.3 g.
The remixing process is not particularly limited in the present invention and may be performed by a process known to those skilled in the art.
In the invention, calcium ions in the cement to be detected react with ethylene diamine tetraacetic acid disodium, when the calcium ions are excessive, the excessive calcium ions react with a calcium red indicator, and a generated product shows red color, which indicates that the cement content in the cement mixture to be detected is higher than a set value of the cement content; when the calcium ions are insufficient, the free calcium red indicator is displayed as blue, which indicates that the cement content in the cement mixture to be tested is lower than the set value of the cement content; when the calcium ions completely react, the free calcium red indicator is displayed as blue, which indicates that the cement content in the cement mixture to be tested is equal to the set value of the cement content.
In the present invention, when the color of the mixed solution is blue, the present invention preferably includes performing a repeated verification test.
In the present invention, the process of the repeated verification test preferably includes the steps of:
mixing the obtained supernatant, a sodium hydroxide solution and a calcium red indicator to obtain a mixed solution; the color of the mixed solution is red;
titrating the mixed solution by using the disodium ethylene diamine tetraacetate solution with the determined dosage under the set value of the cement content, and observing the color change in the titration process:
when the disodium ethylene diamine tetraacetate solution is not completely dripped, the color of the mixed solution is changed from red to blue, namely the cement content in the cement mixture to be detected is lower than the set value of the cement content;
and after the disodium ethylene diamine tetraacetate solution is completely dripped, the color of the mixed solution is changed from red to blue, namely the cement content in the cement mixture to be detected is equal to the set value of the cement content.
According to the invention, by observing the color change of the mixed liquid, whether the cement content in the cement mixture to be detected meets the requirement of a set value can be rapidly and qualitatively judged; the testing method provided by the invention does not need a complicated testing instrument, the testing process time is about 8min, and the testing time is short; meanwhile, the method is not influenced by the environment, and can be used for qualitatively testing the cement content of the cement mixture to be tested on any complex construction site.
In order to further illustrate the present invention, the following detailed description of the method for testing the relative content of cement in a cement mixture provided by the present invention is made with reference to the accompanying drawings and examples, which should not be construed as limiting the scope of the present invention.
Example 1
According to the components of the formula I, samples with cement mass contents of 0%, 2%, 4%, 6% and 8% are prepared in advance respectively, and the mass of each sample is 1000g;
respectively mixing the samples with an ammonium chloride solution containing 4.16mol of ammonium chloride, standing and separating to obtain supernate;
mixing 10mL of supernate, 50mL of sodium hydroxide solution with the molar concentration of 0.45mol/L and 0.3g of calcium red indicator, titrating the obtained mixed solution by adopting ethylene diamine tetraacetic acid disodium solution with the molar concentration of 0.0001mol/L, and recording the consumption of the ethylene diamine tetraacetic acid disodium solution when the color of the mixed solution is changed into blue;
drawing a standard curve (shown in figure 1) of the cement mass content-disodium ethylene diamine tetraacetate solution volume by taking the cement mass content as a horizontal coordinate and the volume of the disodium ethylene diamine tetraacetate solution as a vertical coordinate;
bringing the set value (5%) of the cement content into a standard curve, and determining that the volume of the required disodium ethylene diamine tetraacetate solution is 11.0mL;
premixing a plurality of parts of cement mixture to be detected with 1000g of ammonium chloride solution containing 4.16mol of ammonium chloride, standing and separating to obtain supernatant;
mixing 10mL of supernate, 11.0mL of disodium ethylene diamine tetraacetate solution with the molar concentration of 0.0001mol/L, 50mL of sodium hydroxide solution with the molar concentration of 0.45mol/L and 0.3g of calcium red indicator, and observing the color of the mixed solution; when the color of the mixed solution is red, the cement content in the cement mixture to be detected is higher than the set value of the cement content; and when the color of the mixed solution is blue, the cement content in the cement mixture to be detected is equal to or lower than the set value of the cement content.
Example 2
According to the components of the formula II, samples with cement mass contents of 0%, 2%, 4%, 6% and 8% are prepared in advance respectively, and the mass of each sample is 1000g;
respectively mixing the samples with an ammonium chloride solution containing 4.16mol of ammonium chloride, standing and separating to obtain supernate;
mixing 10mL of supernatant, 50mL of sodium hydroxide solution with the molar concentration of 0.45mol/L and 0.3g of calcium red indicator, titrating the obtained mixed solution by adopting the disodium ethylenediamine tetraacetate solution with the molar concentration of 0.0001mol/L, and recording the consumption of the disodium ethylenediamine tetraacetate solution when the color of the mixed solution is changed into blue;
drawing a standard curve (shown in figure 2) of the cement mass content-disodium ethylene diamine tetraacetate solution volume by taking the cement mass content as a horizontal coordinate and the disodium ethylene diamine tetraacetate solution volume as a vertical coordinate;
bringing a set value (5%) of the cement content into a standard curve, and determining that the volume of the required disodium ethylene diamine tetraacetate solution is 7.5mL;
premixing a plurality of parts of cement mixture to be detected with 1000g of ammonium chloride solution containing 4.16mol of ammonium chloride, standing and separating to obtain supernatant;
mixing 10mL of supernatant, 7.5mL of ethylene diamine tetraacetic acid solution with the molar concentration of 0.0001mol/L, 50mL of sodium hydroxide solution with the molar concentration of 0.45mol/L and 0.3g of calcium red indicator, and observing the color of the mixed solution; when the color of the mixed solution is red, the cement content in the cement mixture to be detected is higher than the set value of the cement content; and when the color of the mixed solution is blue, the cement content in the cement mixture to be detected is equal to or lower than the set value of the cement content.
Performance testing
Test example 1
Determining that the volume of the disodium ethylene diamine tetraacetate solution is 7.5mL when the cement content is 5% by using the standard curve of the percentage content of the cement and the volume of the disodium ethylene diamine tetraacetate solution obtained in the example 2, and then verifying the stability of the test result of the qualitative test method for the cement content provided by the invention;
the verification method comprises the following steps: according to the components of the formula II, samples with cement contents of 4.8%, 4.9%, 5.0%, 5.1% and 5.1% are prepared respectively, and qualitative test of the cement contents is carried out according to the mode of the example 2; the results obtained with 100 tests performed at each cement content are shown in table 1:
TABLE 1 stability test of test results of the test methods provided by the invention
As can be seen from Table 1, the accuracy of the qualitative test method provided by the invention is 96-98%, and the method can be used as a qualitative test method for the content of cement in a cement mixture in the actual construction process.
Test example 2
Determining that the volume of the disodium ethylene diamine tetraacetate solution is 7.5mL when the cement content is 5% according to the standard curve of the percentage cement content-disodium ethylene diamine tetraacetate solution volume obtained in the example 2, and then performing a random sample verification test;
the verification method comprises the following steps:
samples with different cement contents were prepared according to the ingredients of formulation two, and then qualitative tests were performed on 100 groups of cement contents in the manner of example 2, with the cement contents and corresponding color change results shown in table 2:
table 2 random trial verification test results of the test method provided by the present invention
Note: * Representing an error or outlier;
according to the table 2, the accuracy of the method reaches 96%, and the method can be used as a qualitative test method for the content of the cement in the cement mixture in the actual construction process.
Although the above embodiments have been described in detail, they are only a part of the embodiments of the present invention, not all of the embodiments, and other embodiments can be obtained without inventive step according to the embodiments, and all of the embodiments belong to the protection scope of the present invention.
Claims (5)
1. A method for testing the relative content of cement in a cement mixture is characterized by comprising the following steps:
preparing samples with different cement contents in advance according to the components of the cement mixture to be detected, titrating the samples respectively by using disodium ethylene diamine tetraacetate, determining the using amount of the disodium ethylene diamine tetraacetate, and constructing a standard curve of the mass percentage of the cement and the using amount of the disodium ethylene diamine tetraacetate;
substituting the set value of the cement content into the standard curve to determine the required dosage of the disodium ethylene diamine tetraacetate under the set value of the cement content;
premixing a cement mixture to be detected and an ammonium chloride solution, and performing solid-liquid separation to obtain a supernatant;
and mixing the supernatant with the disodium ethylene diamine tetraacetate, the sodium hydroxide solution and the calcium red indicator which are determined by the dosage under the set value of the cement content, and observing the color of the obtained mixed solution:
when the color of the mixed solution is red, the cement content in the cement mixture to be detected is higher than the set value of the cement content;
and when the color of the mixed solution is blue, the cement content in the cement mixture to be detected is equal to or lower than the set value of the cement content.
2. The test method according to claim 1, wherein the ratio of the amount of ammonium chloride in the cement mixture to be tested and the ammonium chloride solution is 1000g:4.16mol.
3. The test method according to claim 1, wherein the ratio of the amount of sodium hydroxide in the supernatant to the amount of sodium hydroxide in the sodium hydroxide solution is 10mL:0.0225mol.
4. The test method according to claim 1, wherein the ratio of the amount of the supernatant to the amount of the calcium red indicator is 10mL:0.2 to 0.3g.
5. The test method according to claim 6, characterized in that the amount of ethylenediaminetetraacetic acid determined at the cement content set point is added in the form of an ethylenediaminetetraacetic acid solution;
the molar concentration of the ethylene diamine tetraacetic acid in the ethylene diamine tetraacetic acid solution is 0.0001mol/L.
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