CN110736746A - quick test method for testing chloride ion content in sand - Google Patents
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- CN110736746A CN110736746A CN201911187204.XA CN201911187204A CN110736746A CN 110736746 A CN110736746 A CN 110736746A CN 201911187204 A CN201911187204 A CN 201911187204A CN 110736746 A CN110736746 A CN 110736746A
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- G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
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Abstract
The invention discloses quick testing methods for testing chloride ion content in sand, which comprises the steps of firstly stirring dry sand to be tested uniformly, then weighing 500g as a test sample, then adding the test sample into 500mL of distilled water to prepare a sand-water mixed solution, fully stirring uniformly, standing for 0.5-2 h, preparing silver nitrate reagent with corresponding concentration according to the test temperature and the standing time of the sand-water mixed solution and the qualified chloride ion concentration required by a customer, taking 50mL of supernatant filtrate of the sand-water mixed solution, putting into a conical flask, adding 1mL of potassium chromate indicator with concentration of 5% (W/V) into the conical flask, shaking the conical flask while slowly adding 5mL of silver nitrate reagent with preparation concentration corresponding to the test conditions, observing the color change and recording of the solution in the conical flask, and judging whether the chloride ion content in the sand meets the customer standard or not according to whether the recorded solution color changes into brick red.
Description
Technical Field
The invention belongs to the technical field of material detection, and particularly relates to rapid testing methods for testing the content of chloride ions in sand.
Background
The sea sand is large in reserve, convenient to exploit and far lower in price than the river sand and the ore sand, but the content of chloride ions in the sea sand is relatively high, the untreated sea sand is directly used for reinforced concrete and has considerable harm and always endangers the life and property safety of people.
The existing common chloride ion analysis methods comprise a silver nitrate titration method and an instrument rapid determination method, wherein the silver nitrate titration method has accurate result, but the titration process has fixed technical content, testers need to be trained to carry out post operation, the time required by the titration test is long, the instrument rapid determination method has high dependence on equipment, and for samples with different concentrations, standard solutions with different concentrations need to be selected for calibration, and the error is large and ranges from 3% to 30%.
Disclosure of Invention
The invention aims to solve the technical problem of providing quick test methods for testing the content of chloride ions in sand, which are used for quickly judging whether the content of chloride ions in the tested sand meets the standard required by customers, thereby shortening the detection time and improving the detection accuracy.
In order to achieve the technical effects, the invention adopts the technical scheme that:
A rapid test method for testing the content of chloride ions in sand, which is characterized by comprising the following test steps:
s1, uniformly stirring dry sand to be detected, and weighing 500g of dry sand to be detected as a detection sample;
s2, adding the detection sample into 500mL of distilled water to prepare a sand-water mixed solution, fully stirring uniformly, standing for 0.5-2 h, and shaking for 3-5 times during standing;
s3, preparing a silver nitrate reagent with corresponding concentration according to the detection condition and the qualified chloride ion concentration required by a client; the detection conditions comprise a detection temperature condition of 0-40 ℃ and a standing time condition of the sand-water mixed liquid during detection;
s4, taking 50mL of supernatant filtrate of the sand-water mixed solution obtained in the step S2, and placing the supernatant filtrate into a conical flask;
s5, adding 1mL of potassium chromate indicator with the concentration of 5% (W/V) into the conical flask, shaking the conical flask, slowly adding 5mL of silver nitrate reagent with the preparation concentration corresponding to the detection condition, and observing the color change and record of the solution in the conical flask;
and S6, judging whether the content of the chloride ions in the sand meets the customer standard according to whether the color of the solution recorded in the step is brick red.
, in the step S2, the time interval of shaking the sand-water mixed liquid is 4-5 min each time, and the final time from times of shaking to the standing time is not less than 10 min.
, the time for shaking the sand-water mixture in step S2 is 10-15S.
, in the step S3, when the detection temperature is 20 ℃, the sand-water mixed solution is placed for 2 hours, and the chloride ion concentration calculated by the dry sand mass percentage is 0.06%, the concentration of the prepared silver nitrate reagent is 0.169 mol/L.
, the preparation method of the silver nitrate reagent in the step S3 is that the detection temperature is 20 ℃, the standing time of the sand-water mixed liquid in the step S2 is 2 hours, the chloride ion concentration is 0.06% in terms of dry sand mass percentage, and the silver nitrate concentration is correspondingly reduced or increased by 5% of the initial concentration when the detection temperature is 0-40 ℃ and the detection temperature is 10 ℃ when the detection temperature is reduced or increased.
, the preparation method of the silver nitrate reagent in the step S3 is that the placing time of the sand-water mixed liquid in the step S2 is 2 hours at the detection temperature, the placing time is 0.06 percent of the chloride ion concentration in terms of dry sand mass percentage and the silver nitrate with the concentration of 0.169mol/L is taken as the reference, and the placing time is reduced by 0.5 hour when the placing time of the sand-water mixed liquid is 0.5 to 2 hours, and the silver nitrate concentration is 0.96, 0.92 and 0.846 times of the initial concentration correspondingly.
, the preparation method of the silver nitrate reagent in the step S3 is that the concentration of the chloride ion is reduced by 0.005 and the concentration of the silver nitrate is reduced by 1/12 corresponding to the initial concentration within 0.005-0.06% by mass percentage of the dry sand based on the silver nitrate with the detection temperature of 20 ℃, the standing time of the sand-water mixed liquid in the step S2 of 2 hours, the concentration of the chloride ion in the dry sand of 0.06% by mass percentage and the concentration of the chloride ion of 0.169 mol/L.
Further , the silver nitrate reagent concentration preparation in step S3 can be performed before detection or during the sand-water mixture standing time.
, when the concentration of the silver nitrate reagent is prepared in the step S3, the method further includes the steps of subpackaging the prepared silver nitrate reagent by 5mL as units, and marking the packages of the subpackaged silver nitrate reagent with corresponding detection conditions and chloride ion concentration conditions for detection.
Compared with the prior art, the method has the advantages that the method is used for qualitatively detecting the content of the chloride ions in the tested sand, silver nitrate reagent with a fixed concentration is prepared according to the standing time of the sand-water mixed liquid and the qualified chloride ion concentration required by a customer at the detection temperature of 0-40 ℃, the detection accuracy is improved by correcting the concentration of the silver nitrate reagent, the later engineering quality is guaranteed, the method is simple and convenient to operate, can detect without professional training, is short in test process time consumption and high in accuracy, has an error of 1% -2%, does not need special equipment, is high in maneuverability, is suitable for detecting in places with poor relative operation environments (such as construction sites), can customize the reagent according to the commercial value of a supplier and a supplier, is convenient to carry, and promotes the transaction achievement of the supplier and the supplier.
The above description is only an overview of the technical solutions of the present invention, and in order to make the technical means of the present invention more clearly understood, the embodiments may be implemented according to the content of the description, and in order to make the above and other objects, features, and advantages of the present invention more clearly understood, it is obvious that the described embodiments are some, not all embodiments of of the present invention.
Detailed Description
A rapid test method for testing the content of chloride ions in sand, comprising the following test steps:
s1, uniformly stirring dry sand to be detected, and weighing 500g of dry sand to be detected as a detection sample;
s2, adding the detection sample into 500mL of distilled water to prepare a sand-water mixed solution, fully stirring, standing for 0.5-2 h, shaking for 3-5 times during standing, wherein the time interval of each shaking is 4-5 min, the time of each shaking is 10-15 s, and the time from the last times of shaking to the end of standing is not less than 10 min.
S3, preparing a silver nitrate reagent with corresponding concentration according to the detection conditions and the qualified chloride ion concentration required by a client, subpackaging the prepared silver nitrate reagent by taking 5mL as units, and marking the corresponding detection conditions and the chloride ion concentration conditions for detection on the package of the subpackaged silver nitrate reagent, wherein the detection conditions comprise a detection temperature condition of 0-40 ℃ and a standing time condition of a sand-water mixed solution during detection;
s4, taking 50mL of supernatant filtrate of the sand-water mixed solution obtained in the step S2, and placing the supernatant filtrate into a conical flask;
s5, adding 1mL of potassium chromate indicator with the concentration of 5% (W/V) into the conical flask, shaking the conical flask, slowly adding 5mL of silver nitrate reagent with the preparation concentration corresponding to the detection condition, and observing the color change and record of the solution in the conical flask;
s6, judging whether the content of the chloride ions in the sand meets the customer standard according to whether the color of the solution recorded in the step S5 is brick red, judging the sand to be qualified when the color of the solution is brick red, and otherwise, judging the sand to be unqualified.
The preparation method of the silver nitrate reagent in the step S4 comprises the following steps: the silver nitrate concentration at this time was defined as the initial concentration based on silver nitrate having a chloride ion concentration of 0.06% and a concentration of 0.169mol/L in terms of mass percentage of dry sand at a detection temperature of 20 ℃ and a standing time of the sand-water mixed solution of step S2 of 2 hours. When the detection temperature is 0-40 ℃, the silver nitrate concentration is correspondingly reduced or increased by 5% of the initial concentration when the detection temperature is reduced or increased by 10 ℃; in the sand-water mixed liquid standing time of 0.5-2 h, the silver nitrate concentration is 0.96, 0.92 and 0.846 times of the initial concentration when the standing time is reduced by 0.5 h; and the concentration of the chloride ions is within 0.005-0.06 percent in mass percentage of the dry sand, and the concentration of the silver nitrate is reduced by 1/12 corresponding to the initial concentration when the concentration of the chloride ions is reduced by 0.005.
The following table 1 shows the correction relationship between the partial detection temperature, the standing time of the sand-water mixed solution, and the chloride ion concentration requirement in the sand specified by the customer and the concentration of the silver nitrate reagent (basic test condition: temperature 20 ℃; standing time 2h, chloride ion discrimination concentration 0.06%; assuming that the reference concentration or initial concentration of the silver nitrate reagent is 0.169mol/L as 1), the silver nitrate concentration required under the corresponding detection condition can be calculated according to the table during the detection:
table 1:
in the embodiment, in order to ensure the engineering quality of a certain project, strict clearance is achieved, and sea sand is prevented from being used, indexes of ' quality of chloride ions of sand for reinforced concrete is not more than 0.06% (calculated by mass percentage of dry sand) ' in ' standard of quality of sand and stone for common concrete and inspection method ' proposed by an owner ' are too loose, and therefore, part of sea sand is possibly mixed in.
In order to meet the requirements of customers, the testing environment of the customers is investigated, and silver nitrate reagents with corresponding concentrations (calculated to be 0.001 in the following) are prepared by selecting corresponding correction coefficients:
case 1: during detection, the test environment temperature is 20 ℃; the sand-water mixed solution is placed for 2 hours; the final silver nitrate concentration correction factor is: 1 × 0.167 ═ 0.167, the actual silver nitrate concentration used for the detection was 0.167 × 0.169 ═ 0.028 mol/L.
Case 2: during detection, the test environment temperature is 20 ℃; the standing time of the sand-water mixed solution is 0.5 hour; the final silver nitrate concentration correction factor is: 1 x 0.846 x 0.167 ═ 0.141; the actual concentration of silver nitrate used for the test was 0.141 × 0.169 ═ 0.024 mol/L.
Case 3: during detection, the test environment temperature is 10 ℃; the standing time of the sand-water mixed solution is 0.5 hour; the final silver nitrate concentration correction factor is: 0.95 × 0.846 × 0.167 ═ 0.134; the actual concentration of silver nitrate used for the test was 0.134 × 0.169 — 0.023 mol/L.
The method is used for qualitatively detecting the content of the chloride ions in the test sand, silver nitrate reagent with a fixed concentration is prepared according to the standing time of the sand-water mixed liquid and the qualified chloride ion concentration required by a customer at the detection temperature of 0-40 ℃, the concentration of the silver nitrate reagent is corrected, the accuracy of detection is improved, the later engineering quality is ensured, the operation is simple and convenient, the detection can be carried out without professional training, the test process is short in time consumption and high in accuracy, the detection error is 1-2%, no specific equipment is needed, the maneuverability is high, the method is suitable for detection in places with relatively poor operation environments (such as construction sites), in addition, the reagent can be customized according to the agreed value of supply and demand parties, the reagent is convenient to store and is used for the site detection of the supply and demand parties through the subpackaging and marking of the silver nitrate reagent with the customized concentration, and the transaction achievement of the supply and demand parties is promoted.
The present invention is not limited to the above-described embodiments, and various modifications made without inventive step from the above-described concept will fall within the scope of the present invention for those skilled in the art.
Claims (9)
1, A rapid test method for testing the content of chloride ions in sand, which is characterized by comprising the following test steps:
s1, uniformly stirring dry sand to be detected, and weighing 500g of dry sand to be detected as a detection sample;
s2, adding the detection sample into 500mL of distilled water to prepare a sand-water mixed solution, fully stirring uniformly, standing for 0.5-2 h, and shaking for 3-5 times during standing;
s3, preparing a silver nitrate reagent with corresponding concentration according to the detection condition and the qualified chloride ion concentration required by a client; the detection conditions comprise a detection temperature condition of 0-40 ℃ and a standing time condition of the sand-water mixed liquid during detection;
s4, taking 50mL of supernatant filtrate of the sand-water mixed solution obtained in the step S2, and placing the supernatant filtrate into a conical flask;
s5, adding 1mL of potassium chromate indicator with the concentration of 5% (W/V) into the conical flask, shaking the conical flask, slowly adding 5mL of silver nitrate reagent with the preparation concentration corresponding to the detection condition, and observing the color change and record of the solution in the conical flask;
s6, judging whether the content of the chloride ions in the sand meets the customer standard according to whether the color of the solution recorded in the step S5 is brick red.
2. The method for rapid testing of chloride ion content in sand according to claim 1, wherein the time interval between shaking of sand-water mixture in step S2 is 4-5 min, and the time from shaking times to the end of standing time is not less than 10 min.
3. The method for testing the content of chloride ions in sand according to claim 1, wherein the time for shaking the sand-water mixture in step S2 is 10-15S.
4. The method for rapid testing of chloride ion content in sand according to claim 1, wherein in step S3, when the testing temperature is 20 ℃, the time of leaving the sand-water mixture is 2 hours, and the chloride ion concentration is 0.06% by mass percentage of the dry sand, the concentration of the prepared silver nitrate reagent is 0.169 mol/L.
5. The method for rapidly testing the content of chloride ions in sand according to claim 4, wherein the silver nitrate reagent in step S3 is prepared by decreasing or increasing the silver nitrate concentration by 5% of the initial concentration for 10 ℃ every time the detection temperature is decreased or increased at 0-40 ℃ based on the detection temperature of 20 ℃, the standing time of the sand-water mixed solution in step S2 being 2 hours, the chloride ion concentration being 0.06% by mass percentage of the dry sand, and the silver nitrate concentration being 0.169 mol/L.
6. The method for rapid testing of chloride ion content in sand according to claim 4, wherein the silver nitrate reagent in step S3 is formulated such that the silver nitrate concentration is 0.96, 0.92 or 0.846 times the initial concentration for each 0.5 hour reduction in the standing time of the sand-water mixture within 0.5 to 2 hours, based on the detection temperature of 20 ℃, the standing time of the sand-water mixture in step S2 of 2 hours, the chloride ion concentration of 0.06% in terms of dry sand mass percentage and the silver nitrate concentration of 0.169 mol/L.
7. The method for rapidly testing chloride ion content in sand of claim 4, wherein the silver nitrate reagent of step S3 is prepared by reducing the chloride ion concentration by 0.005 for every 1/12% of the initial concentration of silver nitrate, based on the silver nitrate with the detection temperature of 20 ℃, the standing time of the sand-water mixed solution of step S2 being 2 hours, the chloride ion concentration by 0.06% of the dry sand mass percentage, and the concentration of the chloride ion being 0.169 mol/L.
8. The method for rapid testing of chloride ion content in sand according to claim 1, wherein the silver nitrate reagent concentration preparation in step S3 is either before testing or during the time of sand-water mixture standing.
9. The method for rapidly testing chloride ion content in sand, according to claim 1, wherein the step S3 includes dispensing prepared silver nitrate reagent at mL, and marking the package of the dispensed silver nitrate reagent with corresponding testing conditions and chloride ion concentration conditions for testing.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111487241A (en) * | 2020-04-20 | 2020-08-04 | 河海大学 | Full-automatic sea sand chloride ion content detection device and control method thereof |
| CN112114084A (en) * | 2020-08-19 | 2020-12-22 | 河海大学 | Method for rapidly detecting concentration of chloride ions in concrete mixture |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
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| CN112114084A (en) * | 2020-08-19 | 2020-12-22 | 河海大学 | Method for rapidly detecting concentration of chloride ions in concrete mixture |
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Application publication date: 20200131 |