CN111735787B - Test method for rapidly determining mud content in machine-made sand - Google Patents
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Abstract
The invention belongs to the technical field of material performance detection, and discloses a test method for rapidly determining the mud content in machine-made sand, which aims to solve the problems in the method for determining the existence of harmful clay in fine aggregate in the prior art. The method can effectively distinguish the types of the clay, estimate the content of the clay components, and judge whether the method can be safely used for concrete production according to the size of the fine aggregate MBV, thereby reasonably utilizing the machine-made sand polluted by the clay.
Description
Technical Field
The invention relates to the technical field of material performance detection, in particular to a test method for rapidly determining the mud content in machine-made sand.
Background
The fine aggregate is an important constituent material in concrete, and the fine aggregate used in concrete in the past is mainly natural sand. With the successive implementation of environmental policies, some areas even appear
There is no condition where sand is available, so it is imperative that machine-made sand replace natural sand. However, the machine-made sand tends to mix with harmful clay components during exploitation, transportation and storage, because the harmful clay has larger adsorptivity and volume expansion after water adsorption, thereby seriously affecting workability of concrete and even endangering durability of the concrete. The industry has more testing methods for clay minerals in fine aggregates, and currently commonly adopted methods are mainly a Sand Equivalent (SE) method and a Methylene Blue (MB) method.
Wherein the sand equivalent method has no obvious distinguishing effect on stone powder and clay components, and moreover, the sand equivalent test cannot effectively distinguish expansive clay minerals (montmorillonite) from non-expansive clay minerals (kaolinite). The methylene blue method has better correlation with the clay mineral content in the fine aggregate, but the methylene blue test method provided in the specification is excessively complicated and time-consuming to operate and has limited application range, and the titration end point of the methylene blue method is judged by observing whether a halo appears on filter paper, and fig. 2 shows the experimental result of a certain experimenter after the methylene blue test, wherein 35ml, 40ml and 45ml appear, but the titration end point is determined to be 45ml, so that the human error is larger. Therefore, finding a method for rapidly determining the existence of harmful clay in fine aggregates becomes a key for quality control of fine aggregates.
Disclosure of Invention
The invention aims to solve the problems in the method for determining the existence of harmful clay in fine aggregate in the prior art, and provides a test method for rapidly determining the mud content in machine-made sand, which is simple in test and small in error.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
a test method for rapidly determining the mud content in machine-made sand comprises the following steps:
1) Preparing and crushing a dried machine-made sand sample, then sieving the fine aggregate by a 4.75mm sieve and placing the treated sample into a sealed bag for later use;
2) Weighing 20g of a sample to be measured, weighing 30mL of methylene blue solution with the mass concentration of 0.5%, and then adding the two into a test tube for mixing;
3) Sucking 1-2ml of upper liquid and filtering into a clean test tube;
4) Transferring 130 mu L of the filtrate obtained in the step 3), pouring the filtrate into a test tube with scales, diluting the test tube with water to 45mL, and uniformly mixing;
5) Placing a cuvette containing a standard methylene blue solution with the mass concentration of 0.5% into a sample groove of a colorimeter, and clearing the absorbance of the reference solution by utilizing the colorimeter and selecting a corresponding test mode;
6) Then filling the liquid to be detected in the step 4) into a cuvette and putting the cuvette into a sample tank of a colorimeter, testing the MBV value of the sample, wherein the unit is mg/L, and if the measured MBV is less than 7mg/g, the sample is effective MBV;
7) If the MBV measured in the step 6) is greater than 7mg/g, 20g of the sample consists of 10g of the machine-made sand sample to be tested and 10g of standard sand together, then the test is carried out according to the steps 2) -6), and if the MBV measured in the step 6) is greater than 14mg/g, 20g of the sample consists of 5g of the machine-made sand sample to be tested and 15g of standard sand together, then the test is carried out according to the steps 2) -6).
Further, in the step 2), the concentration of the initial methylene blue solution is corrected by using a colorimeter, and whether the mass concentration of the initial methylene blue solution is 0.5% or not is determined, and the determination steps are as follows:
a) 130 mu L of initial methylene blue solution is removed and poured into a test tube with scales, diluted to 45mL by water and uniformly mixed;
b) Selecting a corresponding test mode on the colorimeter, inserting a cuvette filled with water into a sample groove, covering an instrument cover, and pressing a zeroing key to carry out zeroing;
c) Changing the cuvette in the sample cell in step b) to a cuvette containing the methylene blue reference solution in step a) and testing, wherein the initial methylene blue solution concentration is 0.5% if the cuvette shows a reading of 14.44 ppm;
mass concentration C of the initial methylene blue solution before dilution in step a) initial-actual Obtained by the following equation:
wherein: c (C) method106 Concentration values measured in the colorimeter 610Abs 610nm mode, ppm;
C initial-actual -initial methylene blue solution concentration, mg/g;
d) If the initial methylene blue solution concentration is not 0.5%, the methylene blue test value is corrected by the following formula:
wherein: MBV (MBV) corrected -corrected methylene blue value, mg/g;
C initial-theoretical -theoretical methylene blue solution concentration, 0.5%;
MBV measured -the resulting methylene blue value, mg/g, was tested with the wrong methylene blue concentration.
Further, in the step 3), 1-2ml of the upper liquid is sucked by a syringe, the needle of the syringe is removed, a filter membrane is arranged at the tip of the syringe, and the mixed liquid is filtered into a clean test tube.
Further, 130. Mu.L of the filtered filtrate was removed with a micropipette in step 4) and poured into a graduated tube.
Further, after the liquid in the step 4) is mixed, starting timing by using a stopwatch, simultaneously shaking the plastic test tube filled with the mixed liquid for 1min, then standing for 3min, and then shaking the plastic test tube filled with the mixed liquid again for 1min, wherein the mixing time of the sample and the methylene blue solution is 5min in total.
Further, the colorimeter in step 5) selects a 001 test mode, wherein the formula of the 001 test mode is as follows:
wherein: c (C) 0 -methylene blue standard solution mass concentration, 5g/L;
c, the concentration of methylene blue of the liquid to be tested for absorbance test, mg/L;
m-the mass of the sample to be measured, 20g;
30-the volume of methylene blue standard solution used for the test, mL;
130-micropipette aspirate filtrate volume, μl;
45-volume after dilution of filtrate, mL;
MBV-methylene blue value, which represents the mass of methylene blue adsorbed per kilogram of sample, mg/g.
Compared with the prior art, the invention has the following beneficial effects:
the invention provides a test method for rapidly determining the mud content in machine-made sand, which utilizes a colorimeter to test the absorbance of methylene blue solution after clay absorption, then establishes the connection between the absorbance and the concentration of the methylene blue solution after clay absorption, and finally converts the change of the concentration of the methylene blue solution into MBV. The test method only needs 10 minutes for testing one sample, provides a method for rapidly determining the existence of harmful clay minerals in fine aggregates for laboratory and engineering site tests, has obvious correlation between the content of expansive clay and MBV, and shows that the test method for rapidly determining the content of the clay in machine-made sand is the most effective and rapid method for identifying the clay minerals in the aggregates. The method can effectively distinguish the types of the clay, estimate the content of the clay components, and judge whether the method can be safely used for concrete production according to the size of the fine aggregate MBV, thereby reasonably utilizing the machine-made sand polluted by the clay.
Drawings
FIG. 1 is a standard curve of absorbance of methylene blue solutions;
FIG. 2 is a schematic representation of a methylene blue test of the prior art;
FIG. 3 is a flow chart of a methylene blue test based on sample amount variation;
FIG. 4 is a graph comparing the results of the present invention with those of the conventional test method;
FIG. 5 clay type and content versus MBV.
Detailed Description
The invention will be further described with reference to the drawings and the specific examples.
Experimental materials:
methylene blue (C) 16 H 18 N 3 SCI) solution with a mass concentration of 0.5%, drinking water, machine sand sample, 4.75mm aggregate sieve, analytical balance, micropipette, colorimeter.
The additional device comprises: two plastic test tubes with a graduated scale of 45ml, a 5ml plastic test tube, a 10ml syringe, a 0.2 μm filter, a weighing pan, two pipettes, a micropipette tip, a stopwatch, a disposable latex glove.
Example 1:
before the experiment, the concentration of the initial methylene blue solution is corrected by using a colorimeter to determine whether the mass concentration of the initial methylene blue solution is 0.5 percent, and the determination steps are as follows:
a) 130. Mu.L of the initial methylene blue solution was removed by micropipette and poured into graduated tubes, and the solution was diluted to 45mL with water and mixed well.
b) The 002 test mode is selected on the colorimeter, then a cuvette filled with water is inserted into the sample tank, the instrument cover is covered, and the zeroing key is pressed for zeroing.
Note that: 002 test pattern was set according to the following test:
(1) drawing up standard curve
Firstly, preparing methylene blue solution with mass fraction of 5%, and diluting the prepared methylene blue solution to obtain standard solutions with different methylene blue concentrations of 0, 1.5mg/l, 3mg/l, 4.5mg/l, 6mg/l, 7.5mg/l and 9mg/l respectively. Then, absorbance values at 610nm of each group of methylene blue solutions with different concentrations were measured by a colorimeter, the test results are shown in table 1, and finally, fitting of standard curves was performed, and the fitting results are shown in fig. 1:
TABLE 1 absorbance at 610nm of methylene blue solutions of different concentrations
(1) And setting a 002 test mode in the colorimeter according to a relation between absorbance and methylene blue solution concentration established by the test.
c) The cuvette in the sample cell was replaced with the cuvette containing the methylene blue reference solution in step a) and tested, indicating a starting methylene blue solution concentration of 0.5% if the cuvette shows a reading of 14.44 ppm.
Mass concentration C of the initial methylene blue solution before dilution in step a) initial-actual Obtained by the following equation:
wherein: c (C) method106 Concentration values measured in the colorimeter 610Abs 610nm mode, ppm;
C initial-actual -initial methylene blue solution concentration, mg/g.
d) If the initial methylene blue solution concentration is not 0.5%, the methylene blue test value is corrected by the following formula:
wherein: MBV (MBV) corrected -corrected methylene blue value, mg/g;
C initial-theoretical -theoretical methylene blue solution concentration, 0.5%;
MBV measured -the resulting methylene blue value was tested with the wrong methylene blue concentration.
The experiment is as follows:
1) A200 g sample of dry machine-made sand was prepared and agglomerated fines in the aggregate were crushed using a mortar or pestle or any other method without damaging the aggregate particles.
And then sieving the fine aggregate by a 4.75mm sieve and placing the treated sample into a sealing bag for standby.
2) And (3) adjusting an analytical balance, weighing 20g of a sample to be measured, measuring 30mL of methylene blue solution with the mass concentration of 0.5% by using a plastic test tube with the scale specification of 50mL, adding the two into the test tube, mixing, screwing a test tube cover, starting timing by using a stopwatch, simultaneously shaking the plastic test tube filled with the mixed solution for 1min, standing for 3min, and shaking the plastic test tube filled with the mixed solution again for 1min, wherein the mixing time of the sample and the methylene blue solution is 5min.
3) The plastic test tube cap containing the mixed solution is opened, 1-2ml of the upper layer liquid is sucked by a syringe, the needle of the syringe is taken down, a filter membrane is arranged at the tip of the syringe, and the mixed solution is filtered into a clean 5ml test tube.
4) 130. Mu.L of the filtered filtrate was removed with a micropipette and poured into a clean plastic test tube with a scale of 50mL, and the test tube was gently shaken to mix the solution with water to dilute the solution to 45 mL.
5) And (5) taking down the cover of the colorimeter device, opening the power supply of the colorimeter, and selecting a 001 test mode. (mode of self-setting in colorimeter based on the relationship between absorbance established by the assay and methylene blue solution concentration after adsorption by clay). The formula for the 001 test mode is as follows:
wherein: c (C) 0 -methylene blue standard solution mass concentration, 5g/L;
c, the concentration of methylene blue of the liquid to be tested for absorbance test, mg/L;
m-the mass of the sample to be measured, 20g;
30-the volume of methylene blue standard solution used for the test, mL;
130-micropipette aspirate filtrate volume, μl;
45-volume after dilution of filtrate, mL;
MBV-methylene blue value, which represents the mass of methylene blue adsorbed per kilogram of sample, mg/g.
And then placing a cuvette containing a standard methylene blue solution with the mass concentration of 0.5% into a sample tank of the colorimeter, covering an instrument cover, and then resetting the absorbance of the reference solution by pressing a reset key.
6) And then the liquid to be detected in the step 4) is filled into a cuvette and placed into a sample tank of a colorimeter, and the MBV of the sample is 4.235mg/g. The MBV is less than 7mg/g and is effective MBV.
Example 2:
experimental procedures (1) to (5) were the same as in examples 1 (1) to (5).
6) And then the liquid to be detected in the step 4) is filled into a cuvette and placed into a sample tank of a colorimeter, and the MBV of the sample is 7.635mg/g.
7) The measured MBV is larger than 7mg/g, the weighed 20g sample consists of 10g of machine-made sand sample to be measured and 10g of standard sand, and is mixed with 30g of methylene blue solution with the mass concentration of 0.5%, then the test is carried out according to the steps 3) -6), and finally the MBV of the sample is 8.367mg/g, and the value is smaller than 14mg/g, so that the MBV is effective.
Example 3:
experimental procedures (1) to (5) were the same as in examples 1 (1) to (5).
6) And then the liquid to be detected in the step 4) is filled into a cuvette and placed into a sample tank of a colorimeter, and the MBV of the sample is 13.356mg/g.
7) Because the measured MBV is larger than 7mg/g, the weighed 20g sample consists of 10g of machine-made sand sample to be measured and 10g of standard sand, and is mixed with 30g of methylene blue solution with the mass concentration of 0.5%, and then the test is carried out according to the steps 3) -6), so that the MBV of the sample is 14.257mg/g.
8) The MBV measured at this time is greater than 14mg/g, and the 20g sample weighed consists of 5g of machine-made sand sample to be measured and 15g of standard sand together and mixed with 30g of methylene blue solution with a mass concentration of 0.5%, after which the test is carried out according to steps 3) to 6). The final MBV of the obtained sample was 15.473mg/g.
Comparative example:
the conventional methylene blue method is used in fig. 2. And the same samples are divided into five groups A-E, and are compared by adopting optimized methylene blue for testing, and the test results are shown in Table 2 and FIG. 3. From the graph, it can be known that the test result of the optimized methylene blue method is in a linear relationship with the conventional method, and the fitting degree is 0.995.
Table 2 results of the conventional methylene blue method and the optimized methylene blue method tests.
Red soil and sodium montmorillonite with different percentage contents are respectively added into clean standard sand, 14 groups of sand samples to be tested are added, and the 14 groups of sand samples to be tested are tested by using a test method for rapidly determining the mud content in machine-made sand, wherein the detailed contents are shown in table 3. FIG. 5 is a graph of the relationship between the types and contents of the clay in the fine aggregate and the MBV, from which the obvious correlation between the MBV and the clay content obtained by the test method for rapidly determining the clay content in the machine-made sand can be obtained, and the larger the tested MBV, the higher the clay content in the corresponding fine aggregate is. The method can also obtain the fine aggregate containing different types of clay, and the two types of fine aggregate MBV have larger difference even if the clay content is the same, so that the test method for rapidly determining the clay content in the machine-made sand can effectively distinguish the types of clay and judge the expansive clay mineral (montmorillonite) and the non-expansive clay mineral (kaolinite).
The invention utilizes a colorimeter to test the absorbance of methylene blue solution after being adsorbed by clay, then establishes the relation between the absorbance and the concentration of the methylene blue solution after being adsorbed by clay, and finally converts the change of the concentration of the methylene blue solution into MBV.
Table 3 results of test methods for rapidly determining the mud content in machine-made sand for clay type and content tests.
Claims (5)
1. A test method for rapidly determining the mud content in machine-made sand is characterized by comprising the following steps:
1) Preparing and crushing a dried machine-made sand sample, then sieving the fine aggregate by a 4.75mm sieve and placing the treated sample into a sealed bag for later use;
2) Weighing 20g of a sample to be measured, weighing 30mL of methylene blue solution with the mass concentration of 0.5%, and then adding the two into a test tube for mixing; before mixing, the concentration of the initial methylene blue solution is corrected by a colorimeter, and whether the mass concentration of the initial methylene blue solution is 0.5% or not is determined, wherein the determination steps are as follows:
a) 130 mu L of initial methylene blue solution is removed and poured into a test tube with scales, diluted to 45mL by water and uniformly mixed;
b) Selecting a corresponding test mode on the colorimeter, inserting a cuvette filled with water into a sample groove, covering an instrument cover, and pressing a zeroing key to carry out zeroing;
c) Changing the cuvette in the sample cell in step b) to a cuvette containing the methylene blue reference solution in step a) and testing, wherein the initial methylene blue solution concentration is 0.5% if the cuvette shows a reading of 14.44 ppm;
mass concentration C of the initial methylene blue solution before dilution in step a) initial-actual Obtained by the following equation:
wherein: c (C) method106 Concentration values measured in the colorimeter 610Abs 610nm mode, ppm;
C initial-actual -initial methylene blue solution concentration, mg/g;
d) If the initial methylene blue solution concentration is not 0.5%, the methylene blue test value is corrected by the following formula:
wherein: MBV (MBV) corrected -corrected methylene blue value, mg/g;
C initial-theoretical -theoretical methylene blue solution concentration, 0.5%;
MBV measured -measuring with wrong methylene blue concentrationThe methylene blue value obtained in a test, mg/g;
3) Sucking 1-2ml of upper liquid and filtering into a clean test tube;
4) Transferring 130 mu L of the filtrate obtained in the step 3), pouring the filtrate into a test tube with scales, diluting the test tube with water to 45mL, and uniformly mixing;
5) Placing a cuvette containing a standard methylene blue solution with the mass concentration of 0.5% into a sample groove of a colorimeter, and clearing the absorbance of the reference solution by utilizing the colorimeter and selecting a corresponding test mode;
6) Then filling the liquid to be detected in the step 4) into a cuvette and putting the cuvette into a sample tank of a colorimeter, testing the MBV value of the sample, wherein the unit is mg/L, and if the measured MBV is less than 7mg/g, the sample is effective MBV;
7) If the MBV measured in the step 6) is greater than 7mg/g, 20g of the sample consists of 10g of the machine-made sand sample to be tested and 10g of standard sand together, then the test is carried out according to the steps 2) -6), and if the MBV measured in the step 6) is greater than 14mg/g, 20g of the sample consists of 5g of the machine-made sand sample to be tested and 15g of standard sand together, then the test is carried out according to the steps 2) -6).
2. The test method for rapidly determining the mud content in machine-made sand according to claim 1, wherein the test method comprises the following steps: in the step 3), 1-2ml of upper liquid is sucked by a syringe, the needle of the syringe is taken down, a filter membrane is arranged at the tip of the syringe, and the mixed liquid is filtered into a clean test tube.
3. The test method for rapidly determining the mud content in machine-made sand according to claim 1, wherein the test method comprises the following steps: the filtered filtrate of 130. Mu.L was removed with a micropipette in step 4) and poured into a graduated tube.
4. The test method for rapidly determining the mud content in machine-made sand according to claim 1, wherein the test method comprises the following steps: after the liquid in the step 4) is mixed, starting timing by using a stopwatch, simultaneously shaking the plastic test tube filled with the mixed liquid for 1min, then standing for 3min, and then shaking the plastic test tube filled with the mixed liquid again for 1min, wherein the mixing time of the sample and the methylene blue solution is 5min.
5. The test method for rapidly determining the mud content in machine-made sand according to claim 1, wherein the test method comprises the following steps: the colorimeter in the step 5) selects a 001 test mode, wherein the formula of the 001 test mode is as follows:
wherein: c (C) 0 -methylene blue standard solution mass concentration, 5g/L;
c, the concentration of methylene blue of the liquid to be tested for absorbance test, mg/L;
m-the mass of the sample to be measured, 20g;
30-the volume of methylene blue standard solution used for the test, mL;
130-micropipette aspirate filtrate volume, μl;
45-volume after dilution of filtrate, mL;
MBV-methylene blue value, which represents the mass of methylene blue adsorbed per kilogram of sample, mg/g.
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| CN112461767A (en) * | 2020-11-17 | 2021-03-09 | 中建商品混凝土有限公司 | Automatic high-precision MB value rapid detection device and use method thereof |
| CN112485152A (en) * | 2020-12-11 | 2021-03-12 | 山东交通学院 | Method for judging river sand quality |
| CN112946170A (en) * | 2020-12-23 | 2021-06-11 | 中山艾尚智同信息科技有限公司 | Method for measuring mud content of machine-made sand for building |
| CN113552119A (en) * | 2021-07-20 | 2021-10-26 | 广东华路交通科技有限公司 | Fine aggregate methylene blue value testing method |
| CN113848185B (en) * | 2021-09-30 | 2024-03-01 | 中建西部建设建材科学研究院有限公司 | Sand MB value test system and method |
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