CN108956815B - Method for testing chloride ion content in sea sand - Google Patents
Method for testing chloride ion content in sea sand Download PDFInfo
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- CN108956815B CN108956815B CN201810730311.1A CN201810730311A CN108956815B CN 108956815 B CN108956815 B CN 108956815B CN 201810730311 A CN201810730311 A CN 201810730311A CN 108956815 B CN108956815 B CN 108956815B
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Abstract
The invention discloses a method for testing the content of chloride ions in sea sand, which comprises the following steps: (1) taking sea sand and sieving to obtain a sea sand sieving substance which is a sea sand sample; (2) putting a sea sand sample in a proper amount of water, and putting the sea sand sample in an ultrasonic cleaner for ultrasonic treatment for 10-30 min to obtain ultrasonic liquid; (3) distilling and extracting the ultrasonic liquid simultaneously to obtain extract liquor; (4) and (4) carrying out ion chromatography test on the extract liquor, and calculating to obtain the content of chloride ions. According to the invention, the sea sand is pretreated by adopting an ultrasonic-assisted simultaneous distillation extraction method, and chloride ions in the sea sand are fully released through multiple actions of ultrasonic and simultaneous distillation extraction, so that the test result is more accurate. According to the invention, inorganic acid is used as a solvent for distillation and extraction, so that chloride ions in the sea sand are completely dissolved, and the distillation and extraction are prevented from volatilizing, so that the test result is real and reliable, and meanwhile, the distillation and extraction method greatly shortens the test time and improves the test efficiency.
Description
Technical Field
The invention belongs to the technical field of building material detection, and particularly relates to a method for testing the content of chloride ions in sea sand.
Background
The continuous growth of the scale of construction in China leads the demand of the sand for the building to be more and more, and because river sand is limited by resources and environment, the demand of the sand for the building can not be met far away, and sea sand becomes an important part of the sand for the building. Sea sand, the second ocean mineral product second only to petroleum and natural gas, is an important raw material for engineering construction and plays an important role in large-scale engineering construction. The sea sand contains various salts such as chloride salt, sulfate and the like, and when the sea sand is applied to concrete fine aggregates, the components can affect the strength, durability and the like of concrete to different degrees. Therefore, the state has exported relevant standards, such as GB/T14684-2011 construction sand and JGJ 52-2006 Standard for quality and inspection methods of common concrete sand and stone, which are in China, and has proposed normative guidance and requirements for construction sand and inspection methods.
Sea sand is an insoluble solid sample in which the chloride salts are encapsulated. Analysis of water insoluble solids for chloride ions requires treatment of the sample to extract the target component chloride ions, transfer them to an aqueous solution, and then testing them. The pretreatment method for measuring anions in a water-insoluble solid sample generally comprises water or leacheate extraction, microwave digestion, high-temperature hydrolysis and the like, but all the methods have certain defects. Such as water or leacheate, is the most common extraction method, is simple and easy to operate, but cannot ensure that ions to be detected can be completely dissolved in an aqueous solution; microwave digestion is a novel extraction method, the extraction efficiency is high, but the instrument is expensive; the high-temperature hydrolysis method has complicated operation steps and is time-consuming. Sometimes, in order to accelerate the extraction process, the component to be detected is extracted more sufficiently, and better effect is achieved by means of auxiliary means such as heating, temperature rise, ultrasonic oscillation, microwave extraction and the like. Another effective method for measuring anions in water-insoluble solid samples is acid dissolution treatment, but acid dissolution treatment also has certain problems because chlorine ions, fluorine ions and the like are relatively easy to form hydrogen chloride and hydrogen fluoride in an acidic medium, and the hydrogen chloride and the hydrogen fluoride are volatile, which results in low test results. In a sample pretreatment method for determining the content of chloride ions and sulfate radicals in limestone solid disclosed in CN201110310284, a limestone sample is pretreated by perchloric acid, and the obtained treated sample filtrate is subjected to an ion chromatography test. The method for detecting the content of chloride ions in the sea sand disclosed in CN201510059460 comprises the steps of sieving the sea sand, pretreating by heating and ultrasonic oscillation, and then testing by a potentiometric titration method.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a method for testing the content of chloride ions in sea sand.
The technical scheme of the invention is as follows:
a method for testing the content of chloride ions in sea sand comprises the following steps:
(1) taking sea sand, and sieving the sea sand with a sieve with the size of 150-170 mu m to obtain a sea sand sieving substance which is a sea sand sample;
(2) putting a sea sand sample in a proper amount of water, and putting the sea sand sample in an ultrasonic cleaner for ultrasonic treatment for 10-30 min to obtain ultrasonic liquid;
(3) distilling and extracting the ultrasonic liquid simultaneously to obtain extract liquor;
(4) performing ion chromatography test on the extract liquor, and calculating to obtain the content of chloride ions;
the simultaneous distillation and extraction comprises the following steps: accurately weighing a certain amount of ultrasonic liquid, placing the ultrasonic liquid in a first container, weighing 30-70 mL of inorganic acid in a second container, connecting the first container and the second container in a simultaneous distillation device, opening cooling water, heating the first container by an electric heating jacket, heating the second container by a water bath at 60-100 ℃, distilling and extracting for 10-30 min, and collecting an extracting solution of the second container after extraction is finished; replacing the first container and the second container, adding distilled water and fresh inorganic acid, distilling and extracting in the same way, cleaning the instrument, and mixing the two extractive solutions in the second container to obtain extractive solution.
The ion chromatograph adopts a 4 x 250mm IonPac AS17-C anion analysis column and a 4 x 50mm IonPacAG17-C protection column, and adopts an AERS3004mm anion suppressor and a conductivity detector, the temperature of the chromatographic column is 20-40 ℃, the sample injection amount is 10-30 mu L, the flow rate is 0.8-1.2 mL/min, the eluent contains 5mmol/L salicylic acid and 1.2mmol/L boric acid, and the solvent of the eluent is water.
The ion chromatography test described above involves the drawing of a standard working curve and the calculation of chloride ion content, wherein,
the standard working curve is plotted as: transferring 0.00, 2.00, 4.00, 6.00, 8.00 and 10.00mL from 1000mg/L Cl & lt- & gt standard stock solution by using a pipette into a 100mL volumetric flask, diluting with ultrapure water, fixing the volume to a scale, shaking up, placing on an ion chromatograph for testing to obtain the peak area of a chloride ion standard working curve, and drawing a standard working curve of concentration-peak area to obtain a chloride ion standard curve equation;
the test calculation for chloride ion content was: performing ion chromatography test on the extractive solution, performing parallel test for several times, averaging, and substituting into the obtained standard curve to obtain the concentration of chloride ions in the sea sand to be tested, and then according to formula
Obtaining the content of chloride ions in the sea sand to be tested, wherein
The unit of W is,
c is the concentration of chloride ions in the extract in mug/mL,
v is the volume of the extract used, in mL,
m is the sample size of the sea sand sample in g.
In a preferred embodiment of the present invention, the water in the step (2) is distilled water, deionized water or ultrapure water.
In a preferred embodiment of the present invention, the sonication time is 20 min.
In a preferred embodiment of the present invention, the inorganic acid is sulfuric acid (1+1), phosphoric acid or perchloric acid, and the sulfuric acid (1+1) is a solution prepared by mixing sulfuric acid and water in a volume ratio of 1: 1.
In a preferred embodiment of the invention, the volume of the mineral acid is 50 mL.
In a preferred embodiment of the invention, the temperature of the water bath is 80 ℃.
In a preferred embodiment of the invention, the time for the distillative extraction is 20 min.
In a preferred embodiment of the invention, the column temperature is 30 ℃, the sample size is 20 μ L, and the flow rate is 1.0 mL/min.
The invention has the beneficial effects that:
1. according to the invention, the sea sand is pretreated by adopting an ultrasonic-assisted simultaneous distillation extraction method, and chloride ions in the sea sand are fully released through multiple actions of ultrasonic and simultaneous distillation extraction, so that the test result is more accurate.
2. According to the invention, inorganic acid is used as a solvent for distillation and extraction, so that chloride ions in the sea sand are completely dissolved, and the distillation and extraction are prevented from volatilizing, so that the test result is real and reliable, and meanwhile, the distillation and extraction method greatly shortens the test time and improves the test efficiency.
3. The mixed leacheate is used for leaching and analyzing the sample, the separation effect is good, the chloride ions can be effectively separated from other ions, the separation degree is improved, and the result of quantitative analysis is more accurate and reliable. The salicylic acid is acid with strong dissociation capability and strong leaching strength, and after a small amount of boric acid is added, the leaching capability of the leaching solution is improved, so that weakly-retained ions can be better separated, and the method is suitable for measuring the weakly-retained ions, namely chloride ions.
4. The invention applies the ultrasonic-assisted simultaneous distillation extraction-ion chromatography to the test of the chloride ions in the sea sand, widens the test method of the chloride ion content in the sea sand, and provides a new test means for the chloride ion content in the sea sand.
Detailed Description
The technical solution of the present invention is further illustrated and described by the following detailed description.
Example 1
1.1 instruments and reagents
A Switzerland Wantong 883 ion chromatograph system of Switzerland Wantong China Co., Ltd; IonPac AS17-C anion analytical column; IonPac AG17-C guard column; AERS3004mm anion suppressor; electronic analytical balance of mettlerlatio instruments (shanghai) ltd; a chloride ion standard stock solution; sulfuric acid (analytically pure); phosphoric acid (analytically pure); perchloric acid (analytically pure); distilled water, ultrapure water and deionized water are all self-made in laboratories; the samples are sea sand samples No. 1, No. 2 and No. 3, and are purchased from a certain company
1.2 taking No. 1 sea sand and sieving the sea sand by a sieve with the sieve pore size of 160 mu m to obtain a sea sand sieving substance which is a No. 1 sea sand sample;
1.3, putting a No. 1 sea sand sample into a certain amount of distilled water, and putting the sample into an ultrasonic cleaner for ultrasonic treatment for 10min to obtain No. 1 ultrasonic liquid;
1.4 accurately weigh 5.006g of sample of ultrasound solution # 1, place in round bottom flask a, and measure a certain amount of 50mL sulfuric acid (1+1)) in round bottom flask b. Connecting round-bottom flask a and round-bottom flask b to a simultaneous distillation device, turning on cooling water, heating round-bottom flask a with an electric heating jacket, heating round-bottom flask b with a 60 deg.C water bath, distilling and extracting for 30min, and collecting the extractive solution of round-bottom flask b after extraction. Replacing the new round-bottom flask a and the new round-bottom flask b, adding distilled water and fresh inorganic acid respectively, performing distillation extraction in the same manner as above, cleaning the instrument, and combining the two extracts of the round-bottom flask b to obtain the No. 1 extract. (after the extract is acidified by adding a small amount of nitric acid, a silver nitrate solution is added, a white precipitate is generated, indicating that chloride ions exist and indicating that the chloride ions in the sea sand are extracted, and the pretreatment method can be used for measuring the chloride ions in the sea sand.)
1.5 ion chromatography of the extract
Drawing a standard curve: transferring 0.00, 2.00, 4.00, 6.00, 8.00 and 10.00mL of chloride ion standard solution into a 100mL volumetric flask by using a pipette, diluting with ultrapure water, fixing the volume to a scale, shaking up, placing on an ion chromatograph for testing to obtain the peak area of a chloride ion standard working curve, and drawing a standard working curve of concentration-peak area to obtain a chloride ion standard curve equation; the linear regression equation, i.e., the standard curve, is: y 2.01 × C1+0.45, with a correlation coefficient of 0.993.
The chromatographic conditions are as follows: IonPac AS17-C anion analysis column, 4 × 250mm, IonPacAG17-C protective column, 4 × 50mm, AERS3004mm anion inhibitor, conductivity detector, chromatographic column temperature of 20 ℃, sample injection amount of 30 μ L, flow rate of 0.8mL/min, leacheate containing 5mmol/L salicylic acid and 1.2mmol/L boric acid, and solvent of water;
and (3) sample testing: taking the extract to perform ion chromatography test, performing parallel test for 10 times, averaging, and substituting into the obtained standard curve to obtain the concentration of chloride ions in the sea sand to be tested, and then according to the formula
And obtaining the content of the chloride ions in the sea sand to be measured, wherein the unit of W is%, the unit of C is mu g/mL, V is the volume of the liquid to be measured, the unit is mL, m is the sampling amount of the sea sand sample to be measured, the unit is g, and the relative standard deviation of the content of the chloride ions in the sea sand to be measured is 0.010%.
Example 2
1.3, putting a No. 2 sea sand sample into a certain amount of distilled water, and putting the sample into an ultrasonic cleaner for ultrasonic treatment for 20min to obtain No. 2 ultrasonic liquid;
1.4 accurately weigh 7.006g of 2# ultrasound solution sample, place in round bottom flask a, and measure a certain amount of 30mL phosphoric acid in round bottom flask b. Connecting round-bottom flask a and round-bottom flask b to a simultaneous distillation device, turning on cooling water, heating round-bottom flask a with an electric heating jacket, heating round-bottom flask b with a water bath at 80 deg.C, distilling and extracting for 20min, and collecting the extractive solution of round-bottom flask b after extraction. Replacing the new round-bottom flask a and the new round-bottom flask b, adding distilled water and fresh inorganic acid respectively, performing distillation extraction in the same manner as above, cleaning the instrument, and combining the two extracts of the round-bottom flask b to obtain the No. 2 extract.
1.5 ion chromatography of the extract
The chromatographic conditions are as follows: IonPac AS17-C anion analysis column, 4X 250mm, IonPacAG17-C protective column, 4X 50mm, AERS3004mm anion inhibitor, conductivity detector, chromatographic column temperature of 30 ℃, sample injection amount of 20 mu L, flow rate of 1.0mL/min, leacheate containing 5mmol/L salicylic acid and 1.2mmol/L boric acid, and solvent of water.
The rest is the same as in example 1. The content of chloride ions in the sea sand was measured to be 0.032%, and the relative standard deviation was 0.012%.
Example 3
1.3, putting a No. 3 sea sand sample into a certain amount of distilled water, and putting the sample into an ultrasonic cleaner for ultrasonic treatment for 30min to obtain a No. 3 ultrasonic liquid;
1.4 accurately weighing 10.006g of 3# ultrasonic liquid sample, placing in a round-bottom flask a, and measuring a certain amount of 70mL perchloric acid in a round-bottom flask b. Connecting round-bottom flask a and round-bottom flask b into a simultaneous distillation device, turning on cooling water, heating round-bottom flask a with an electric heating jacket, heating round-bottom flask b with a water bath at 100 deg.C, distilling and extracting for 10min, and collecting the extractive solution of round-bottom flask b after extraction. Replacing the new round-bottom flask a and the new round-bottom flask b, adding distilled water and fresh inorganic acid respectively, performing distillation extraction in the same manner as above, cleaning the instrument, and combining the two extracts of the round-bottom flask b to obtain the No. 2 extract.
1.5 ion chromatography of the extract
The chromatographic conditions are as follows: IonPac AS17-C anion analysis column, 4X 250mm, IonPacAG17-C protective column, 4X 50mm, AERS3004mm anion inhibitor, conductivity detector, chromatographic column temperature of 40 ℃, sample injection amount of 10 mu L, flow rate of 1.2mL/min, leacheate containing 5mmol/L salicylic acid and 1.2mmol/L boric acid, and solvent of water.
The rest is the same as in example 1. The measured content of chloride ions in the sea sand was 0.029% with a relative standard deviation of 0.050%.
The above description is only a preferred embodiment of the present invention, and therefore should not be taken as limiting the scope of the invention, which is defined by the appended claims.
Claims (7)
1. A method for testing the content of chloride ions in sea sand is characterized by comprising the following steps: the method comprises the following steps:
(1) taking sea sand, and sieving the sea sand with a sieve with the size of 150-170 mu m to obtain a sea sand sieving substance which is a sea sand sample;
(2) putting a sea sand sample in a proper amount of water, and putting the sea sand sample in an ultrasonic cleaner for ultrasonic treatment for 10-30 min to obtain ultrasonic liquid;
(3) distilling and extracting the ultrasonic liquid simultaneously to obtain extract liquor;
(4) performing ion chromatography test on the extract liquor, and calculating to obtain the content of chloride ions;
the simultaneous distillation and extraction comprises the following steps: accurately weighing a certain amount of ultrasonic liquid, placing the ultrasonic liquid in a first container, weighing 30-70 mL of inorganic acid in a second container, connecting the first container and the second container in a simultaneous distillation device, opening cooling water, heating the first container by an electric heating jacket, heating the second container by a water bath at 60-100 ℃, distilling and extracting for 10-30 min, and collecting an extracting solution of the second container after extraction is finished; replacing a new first container and a new second container, respectively adding distilled water and fresh inorganic acid, opening cooling water, heating the first container by an electric heating sleeve, heating the second container by a water bath at 60-100 ℃, carrying out distillation extraction for 10-30 min, collecting an extracting solution of the second container after extraction is finished, cleaning an instrument, and combining the extracting solutions in the second container twice to obtain an extracting solution; the inorganic acid is concentrated sulfuric acid, phosphoric acid or perchloric acid with the volume concentration of 50%;
the ion chromatograph adopts a 4 x 250mm IonPac AS17-C anion analysis column and a 4 x 50mm IonPacAG17-C protection column, and adopts an AERS3004mm anion suppressor and a conductivity detector, the temperature of the chromatographic column is 20-40 ℃, the sample injection amount is 10-30 mu L, the flow rate is 0.8-1.2 mL/min, the eluent contains 5mmol/L salicylic acid and 1.2mmol/L boric acid, and the solvent of the eluent is water;
the ion chromatography test described above involves the drawing of a standard working curve and the calculation of chloride ion content, wherein,
the standard working curve is plotted as: pipet from 1000mg/L Cl-Transferring 0.00mL, 2.00 mL, 4.00 mL, 6.00 mL, 8.00 mL and 10.00mL of standard stock solution into a 100mL volumetric flask, diluting with ultrapure water, fixing the volume to a scale, shaking up, placing on an ion chromatograph for testing to obtain the peak area of a standard working curve of the chloride ions, drawing the standard working curve of the concentration-peak area, and obtaining a standard curve equation of the chloride ions;
the test calculation for chloride ion content was: performing ion chromatography test on the extractive solution, performing parallel test for several times, averaging, and substituting into the obtained standard curve to obtain the concentration of chloride ions in the sea sand to be tested, and then according to formula
Obtaining the content of chloride ions in the sea sand to be tested, wherein
C is the concentration of chloride ions in the extract in mug/mL,
v is the volume of the extract used, in mL,
m is the sample size of the sea sand sample in g.
2. The test method of claim 1, wherein: the water in the step (2) is distilled water, deionized water or ultrapure water.
3. The test method of claim 1, wherein: the ultrasonic time is 20 min.
4. The test method of claim 1, wherein: the volume of the inorganic acid is 50 mL.
5. The test method of claim 1, wherein: the temperature of the water bath was 80 ℃.
6. The test method of claim 1, wherein: the time for distillation and extraction is 20 min.
7. The test method of claim 1, wherein: the temperature of the chromatographic column is 30 ℃, the sample injection amount is 20 mu L, and the flow rate is 1.0 mL/min.
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| CN110455983B (en) * | 2019-08-28 | 2020-06-09 | 福州大学 | Detection method for determining content of chloride ions in sea sand |
| CN112255329A (en) * | 2020-09-21 | 2021-01-22 | 上海市食品药品包装材料测试所 | Ion chromatography for determining chloride ions in edetate disodium |
| CN114486873A (en) * | 2022-02-28 | 2022-05-13 | 云南水富云天化有限公司 | Method for measuring content of chloride ions in polyglutamic acid |
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