CN112557583A - Method for detecting chloride ion content in concrete admixture by potentiometric titration - Google Patents
Method for detecting chloride ion content in concrete admixture by potentiometric titration Download PDFInfo
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- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 title claims abstract description 40
- 238000000034 method Methods 0.000 title claims abstract description 35
- 238000003918 potentiometric titration Methods 0.000 title claims abstract description 16
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract description 146
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims abstract description 86
- 239000000243 solution Substances 0.000 claims abstract description 86
- 229910001961 silver nitrate Inorganic materials 0.000 claims abstract description 73
- 239000011780 sodium chloride Substances 0.000 claims abstract description 43
- 239000012086 standard solution Substances 0.000 claims abstract description 39
- 238000004448 titration Methods 0.000 claims abstract description 30
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 23
- 238000003756 stirring Methods 0.000 claims abstract description 17
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 15
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229920002472 Starch Polymers 0.000 claims abstract description 12
- 235000019698 starch Nutrition 0.000 claims abstract description 12
- 239000008107 starch Substances 0.000 claims abstract description 12
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229940075397 calomel Drugs 0.000 claims abstract description 7
- 239000008367 deionised water Substances 0.000 claims abstract description 7
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 7
- ZOMNIUBKTOKEHS-UHFFFAOYSA-L dimercury dichloride Chemical compound Cl[Hg][Hg]Cl ZOMNIUBKTOKEHS-UHFFFAOYSA-L 0.000 claims abstract description 7
- 229910052709 silver Inorganic materials 0.000 claims abstract description 7
- 239000004332 silver Substances 0.000 claims abstract description 7
- 239000012488 sample solution Substances 0.000 claims description 6
- 238000005303 weighing Methods 0.000 claims description 6
- 239000011259 mixed solution Substances 0.000 claims description 4
- 239000000523 sample Substances 0.000 claims description 3
- 239000000654 additive Substances 0.000 abstract description 15
- 230000000996 additive effect Effects 0.000 abstract description 12
- 238000001514 detection method Methods 0.000 abstract description 11
- 238000002156 mixing Methods 0.000 abstract description 2
- 230000008859 change Effects 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 6
- 238000005259 measurement Methods 0.000 description 5
- 239000011521 glass Substances 0.000 description 3
- 239000002253 acid Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000013043 chemical agent Substances 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000010276 construction Methods 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- XOFYZVNMUHMLCC-ZPOLXVRWSA-N prednisone Chemical compound O=C1C=C[C@]2(C)[C@H]3C(=O)C[C@](C)([C@@](CC4)(O)C(=O)CO)[C@@H]4[C@@H]3CCC2=C1 XOFYZVNMUHMLCC-ZPOLXVRWSA-N 0.000 description 2
- 229910001294 Reinforcing steel Inorganic materials 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 125000001931 aliphatic group Chemical group 0.000 description 1
- 239000002981 blocking agent Substances 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 238000004255 ion exchange chromatography Methods 0.000 description 1
- 150000002790 naphthalenes Chemical class 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 238000000527 sonication Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
- G01N31/16—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using titration
- G01N31/162—Determining the equivalent point by means of a discontinuity
- G01N31/164—Determining the equivalent point by means of a discontinuity by electrical or electrochemical means
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- Health & Medical Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Physics & Mathematics (AREA)
- Electrochemistry (AREA)
- Molecular Biology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention discloses a method for measuring the content of chloride ions in an additive by potentiometric titration. The method specifically comprises the following steps: mixing 1-5 g of an additive with 5-10 mL of nitric acid solution, 100-300 mL of deionized water and 0.5-1 mL of ethylene glycol solution, and then ultrasonically dissolving for 5-10 min; adding a starch solution, taking a silver electrode as an indicating electrode and a calomel electrode as a reference electrode, adding sodium chloride standard solution with the same volume twice, titrating with silver nitrate solution under the stirring condition to the end point, and respectively obtaining the volume of the consumed silver nitrate solution at the end point of the titration twice; obtaining the volume of the consumed silver nitrate solution and the concentration of the silver nitrate solution at the end point of two titrations through blank test titration; and calculating to obtain the content of the chloride ions in the additive. The method has the advantages of high potentiometric titration accuracy, low repeatability limit of 0.03%, low detection cost, no special requirement on detection equipment, and wide popularization in industrial application.
Description
Technical Field
The invention belongs to the technical field of building engineering materials, and particularly relates to a method for detecting the content of chloride ions in a concrete admixture by a potentiometric titration method.
Background
In order to improve certain properties of concrete, such as reducing the amount of water for mixing, or improving the fluidity of concrete, or reducing the setting time of concrete, it is often necessary to add a small amount of chemical agents to concrete during construction, and these chemical agents added to concrete to perform different functions are collectively called concrete admixture. The common additives in the market at present comprise water reducing agents, expanding agents, retarders, water-blocking agents, air-entraining agents and the like, and the additives comprise naphthalene series, aliphatic series, polycarboxylic acids and the like.
An important parameter in the chemical detection indexes of the concrete admixture is the content of chloride ions, and the chloride ions can corrode a reinforcing steel bar material due to high content of the chloride ions, so that the concrete structure is damaged, and serious safety accidents are caused. In order to prevent the harm caused by over-high chloride ions of the concrete, the content of the chloride ions in the concrete raw materials needs to be strictly controlled within a standard range so as to meet the safety requirement of concrete construction. For the determination of trace chloride ions in the concrete admixture, commonly used determination methods include ion chromatography, direct chloride ion selective electrode method or potentiometric titration method, but these methods have the problems of high cost, complex operation, low accuracy and the like.
Disclosure of Invention
The invention aims to provide a method for detecting the content of chloride ions in a concrete admixture by a potentiometric titration method, which has the advantages of high potentiometric titration accuracy, low repeatability limit, low detection cost, no special requirement on detection equipment and wide popularization in industrial application.
In order to solve the technical problems, the invention provides the following technical scheme:
the method for detecting the content of chloride ions in the concrete admixture by a potentiometric titration method is provided, and comprises the following steps:
(1) weighing 1-5 g of concrete admixture, adding 5-10 mL of nitric acid solution and 100-300 mL of deionized water, then adding 0.5-1 mL of ethylene glycol solution, and ultrasonically dissolving for 5-10 min;
(2) adding a sodium chloride standard solution and a starch solution into the mixed solution obtained in the step (1), taking a silver electrode as an indicating electrode and a calomel electrode as a reference electrode, and titrating by using a silver nitrate solution under the stirring condition of 500-1Adding the sodium chloride standard solution with the same volume as the sodium chloride standard solution added for the first time, titrating to a second end point to obtain a silver nitrate consumption volume V at the second titration end point2；
(3) Blank test: the steps (1) and (2) are repeated without adding additives to obtain silver nitrate volumes V consumed at two titration end points in the blank test01And V02And calculating to obtain the concentration c of the silver nitrate solution;
(4) and (3) calculating the result:
volume of silver nitrate consumed by chloride ions in concrete admixture
In the formula:
V1the volume of the silver nitrate solution consumed after the sample solution is added with the sodium chloride standard solution for the first time is mL;
V2the volume of the silver nitrate solution consumed by the sample solution after the sodium chloride standard solution is added for the second time is mL;
V01the volume of the silver nitrate solution consumed in mL after the first addition of the sodium chloride standard solution in the blank test;
V02-the total volume of silver nitrate solution consumed in mL after the second addition of the standard sodium chloride solution in the blank test;
chloride ion content in concrete admixture
In the formula:
c, concentration of silver nitrate solution, wherein the unit is mol/L;
Xcl-chloride ion content in the concrete admixture,%;
v, the volume of a silver nitrate solution consumed by chloride ions in the concrete admixture is mL;
m is the mass of the concrete admixture sample and the unit is g.
According to the scheme, in the step (2), when the titration is close to the equivalent point, 0.1mL of silver nitrate solution is quantitatively added every time, the value of the derivative delta E/delta V is calculated once, the titration can be stopped when the value of the delta E/delta V is reduced, and the volume of the consumed silver nitrate solution at the end point of the titration is recorded as (V)Final (a Chinese character of 'gan'))nAnd calculating the volume V of the consumed silver nitrate solution at the end pointFinal (a Chinese character of 'gan')The following formula:
in the formula:
(Vfinal (a Chinese character of 'gan'))n-2Volume (V) recorded at the end of titrationFinal (a Chinese character of 'gan'))nSubtract 0.2 mL;
(Δ2E/ΔV2)n-1is (V)Final (a Chinese character of 'gan'))n-1Corresponding to the calculated second-level differential quotient value (V)Final (a Chinese character of 'gan'))n-1Volume (V) recorded at the end of titrationFinal (a Chinese character of 'gan'))nSubtract 0.1 mL;
(Δ2E/ΔV2)nat the end of titration (V)Final (a Chinese character of 'gan'))nAnd corresponding to the calculated second-level differential quotient value.
According to the scheme, in the step (3), the concentration of the silver nitrate solution
In the formula:
c, concentration of silver nitrate solution, wherein the unit is mol/L;
c' -the concentration of the sodium chloride standard solution, the unit is mol/L;
v' -volume of sodium chloride standard solution added in a single time, in mL;
V0volume of silver nitrate solution consumed in mL, V, for a single addition of sodium chloride standard solution0＝V02-V01。
According to the scheme, in the step (2), the volume of the sodium chloride standard solution is 10mL, and the concentration is 0.1000 mol/L.
According to the scheme, in the nitric acid solution in the step (1), the volume ratio of nitric acid to water is 1: 1.
According to the scheme, the starch solution added in the step (1) is 2-10mL, and the concentration is 8-12 g/L.
According to the scheme, the concentration of silver nitrate in the step (1) is 0.09000-0.1100 mol/L.
The invention has the beneficial effects that:
1. the invention provides a method for measuring the content of chloride ions in a concrete additive by potentiometric titration, which can ensure that the chloride ions in the additive can be dissolved out more completely and SO can be removed by adding nitric acid4 2-Interference of (2); the ultrasonic dissolution is also more beneficial to the complete dissolution of chloride ions in the additive, and the more accurate numerical value of chloride ions measured by potentiometric titration is ensured; in addition, the ethylene glycol is added into the additive solution to prevent the volatilization of the additive, the starch is added to inhibit the generation of floccules, and the starch can play a role in inhibiting the generation of flocculent precipitates to prevent the precipitates from wrapping electrodes and influencing the measurement of potential; the proper stirring speed is required to be adjusted in the titration process; the invention reduces the interference of external factors as much as possible by adopting various measures, thereby improvingThe accuracy of the results was determined.
2. The method converts the measurement of the concentration of the chloride ions into the measurement of the potential, the response of the potential to the trace chloride ions is more sensitive, and the potentiometric titration accuracy is improved by measures of adding acid, ultrasonically dissolving, adding glycol and starch, controlling the stirring speed and the like; the repeatability limit of the invention is as low as 0.03%, the detection cost is low, no special requirements are required for detection equipment, and the invention can be widely popularized in industrial application.
Detailed Description
To further clarify the objects, technical solutions and advantages of the present invention, the technical solutions, embodiments and features mentioned in the examples will be clearly and completely described below in conjunction with the specific examples of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments of the present invention without any inventive step, are within the scope of the present invention.
Blank test
200mL of water and 5mL of nitric acid (1+1) were added to a clean 400mL beaker, the pH of the solution was adjusted to acidity, and the solution was sonicated on a sonication instrument for 10 min. Adding 10mL of 0.1000mol/L sodium chloride standard solution and 10mL of 10g/L starch solution by a pipette, electromagnetically stirring at the speed of 500r/min, titrating by using a silver nitrate solution with the concentration of about 0.1000mol/L, when the potential value reaches 200mV, the potential can obviously change along with the change of silver nitrate, at the moment, the equivalent point is approached, recording the volume V and the potential value E of consumed silver nitrate solution once when the reading of a burette changes by 0.10mL, calculating the micro quotient value, stopping titration when the micro quotient is reduced once, namely the end point is reached, and calculating the volume V consumed by the silver nitrate solution at the first end point01。
Adding 10mL of 0.1000mol/L sodium chloride standard solution into the same solution by a pipette, continuously titrating by using silver nitrate solution to a second end point, and calculating to obtain the volume V consumed by the silver nitrate solution at the second end point of the blank test02。
Table 1 lists the values of the silver nitrate solution burette readings V and the corresponding point potentials E near the two equivalence points in the blank test byCalculating the consumed volume V of the silver nitrate solution at two end points by a secondary microexperience method01And V02：
TABLE 1
Adding 10mL of silver nitrate volume consumed by 0.1000mol/L sodium chloride
Adding 20mL of silver nitrate volume consumed by 0.1000mol/L sodium chloride
10mL of 0.1000mol/L sodium chloride standard solution consumes the volume of silver nitrate solution
V0＝V02-V01＝20.37-10.48＝9.89(mL)
In the formula:
V010mL of a volume of the silver nitrate solution consumed by the 0.01000mol/L sodium chloride standard solution in mL;
V01-the volume of the silver nitrate solution consumed in a blank test in mL of 200mL of water, 5mL of nitric acid (1+1) and 10mL of 0.1000mol/L of sodium chloride standard solution;
V02volume of silver nitrate solution consumed in mL for 200mL of water, 5mL of nitric acid (1+1), and 20mL of 0.1000mol/L of sodium chloride standard solution in a blank.
Concentration of silver nitrate solution
In the formula:
c, concentration of silver nitrate solution, wherein the unit is mol/L;
c' -the concentration of the sodium chloride standard solution is 0.1000 mol/L;
v' -volume of single addition of standard solution of sodium chloride, 10 mL.
③ volume of silver nitrate consumed by chloride ions in the admixture
In the formula:
V1the volume of the silver nitrate solution consumed by adding 10mL of 0.01000mol/L sodium chloride standard solution into the sample solution is mL;
V2the volume of silver nitrate solution consumed by adding 20mL of 0.01000mol/L sodium chloride standard solution to the sample solution in mL.
Chloride ion content in admixture
In the formula:
c, concentration of silver nitrate solution, wherein the unit is mol/L;
Xcl-chloride ion content in the admixture,%;
v, the volume of silver nitrate solution consumed by chloride ions in the additive is mL;
m is the sample mass of the admixture in g.
Example 1
A method for detecting the content of chloride ions in a concrete admixture by using a potentiometric titration method comprises the following steps:
(1) weighing 1g of the additive into a 400mL beaker, adding 200mL of deionized water and 5mL of nitric acid (1+1), then adding 1mL of ethylene glycol, uniformly stirring by using a glass rod, and then dissolving for 10min by ultrasonic waves;
(2) adding 10mL of 0.1000mol/L sodium chloride standard solution and 10mL of 10g/L starch solution into a beaker, adding an electromagnetic stirring bar into the beaker, placing the beaker on an electromagnetic stirrer, adjusting a potentiometer to a point gear, taking a silver electrode as an indicating electrode and a calomel electrode as a reference electrode, starting the stirrer, performing electromagnetic stirring at the speed of 500r/min, and slowly titrating by using a silver nitrate solution with the concentration of 0.1011 mol/L;
(3) near equivalence points, the burette reading records the volume of silver nitrate solution consumed V and the point value E for each 0.10mL change. After the first end point is reached, 10mL of 0.1000mol/L sodium chloride standard solution is added, and titration is continued by using silver nitrate solution until a second equivalence point appears;
(4) after titration, the chloride ion content is calculated according to the formula (1) and the formula (2), and the obtained detection results are shown in table 2.
Example 2
A method for detecting the content of chloride ions in a concrete admixture by using a potentiometric titration method comprises the following steps:
(1) weighing 4g of an additive into a 400mL beaker, adding 200mL of deionized water and 8mL of nitric acid (1+1), then adding 1mL of ethylene glycol, uniformly stirring by using a glass rod, dissolving for 10min by ultrasonic waves, and filtering by using quick qualitative filter paper;
(2) adding 10mL of 0.1000mol/L sodium chloride standard solution and 2mL of 10g/L starch solution into a beaker, adding an electromagnetic stirring bar into the beaker, placing the beaker on an electromagnetic stirrer, adjusting a potentiometer to a point gear, taking a silver electrode as an indicating electrode and a calomel electrode as a reference electrode, starting the stirrer, performing electromagnetic stirring at the speed of 500r/min, and slowly titrating by using a silver nitrate solution with the concentration of 0.01011 mol/L;
(3) near equivalence points, the burette reading records the volume of silver nitrate solution consumed V and the point value E for each 0.10mL change. After the first end point is reached, 10mL of 0.1000mol/L sodium chloride standard solution is added, and titration is continued by using silver nitrate solution until a second equivalence point appears;
(4) after titration, the chloride ion content is calculated according to the formula (1) and the formula (2), and the obtained detection results are shown in table 2.
Example 3
A method for detecting the content of chloride ions in a concrete admixture by using a potentiometric titration method comprises the following steps:
(1) weighing 5g of an additive to a 400mL beaker, adding 200mL of deionized water and 10mL of nitric acid (1+1), then adding 1mL of ethylene glycol, uniformly stirring by using a glass rod, dissolving for 10min by ultrasonic waves, and filtering by using quick qualitative filter paper;
(2) adding 10mL of 0.1000mol/L sodium chloride standard solution and 12mL of 10g/L starch solution into a beaker, adding an electromagnetic stirring bar into the beaker, placing the beaker on an electromagnetic stirrer, adjusting a potentiometer to a point gear, taking a silver electrode as an indicating electrode and a calomel electrode as a reference electrode, starting the stirrer, performing electromagnetic stirring at the speed of 500r/min, and slowly titrating by using a silver nitrate solution with the concentration of 0.01011 mol/L;
(3) near equivalence points, the burette reading records the volume of silver nitrate solution consumed V and the point value E for each 0.10mL change. After the first end point is reached, 10mL of 0.1000mol/L sodium chloride standard solution is added, and titration is continued by using silver nitrate solution until a second equivalence point appears;
(4) after titration, the chloride ion content is calculated according to the formula (1) and the formula (2), and the obtained detection results are shown in table 2.
Comparative example 1
(1) Weighing 1g of the admixture into a 400mL beaker, and adding 200mL of deionized water and 4mL of nitric acid (1+ 1);
(2) adding 10mL of 0.1000mol/L sodium chloride standard solution into a beaker, adding an electromagnetic stirring bar into the beaker, putting the beaker on an electromagnetic stirrer, adjusting a potentiometer to a point gear, taking a silver electrode as an indicating electrode and a calomel electrode as a reference electrode, starting the stirrer, electromagnetically stirring at the speed of 500r/min, and slowly titrating with a silver nitrate solution with the concentration of 0.01011 mol/L;
(3) near the equivalence point, the burette reading is recorded at each 0.10mL change, the consumption volume V and the point value E. After the first end point is reached, 10mL of 0.1000mol/L sodium chloride standard solution is added, and titration is continued by using silver nitrate solution until a second equivalence point appears;
(4) after the titration is finished, the content of chloride ions is calculated, and the obtained detection results are shown in table 2.
Comparative example 2
The content of chloride ions in 4g of the admixture was measured in accordance with the method of comparative example 1 described above, and the results of the measurement are shown in Table 2.
Comparative example 3
The content of chloride ions in 5g of the admixture was measured in accordance with the method of comparative example 1 described above, and the results of the measurement are shown in Table 2.
TABLE 2 chloride ion content in examples 1-3 and comparative examples 1-3
The above embodiments are only preferred technical solutions of the present invention, and do not limit the present invention; any modification or simple modification or replacement of the above embodiment within the spirit of the present invention will still fall within the protection scope of the present invention.
Claims (7)
1. A method for detecting the content of chloride ions in a concrete admixture by a potentiometric titration method is characterized by comprising the following steps:
(1) weighing 1-5 g of concrete admixture, adding 5-10 mL of nitric acid solution and 100-300 mL of deionized water, then adding 0.5-1 mL of ethylene glycol solution, and ultrasonically dissolving for 5-10 min;
(2) adding a sodium chloride standard solution and a starch solution into the mixed solution obtained in the step (1), stirring the mixed solution under the condition of 500-600r/min by taking a silver electrode as an indicating electrode and a calomel electrode as a reference electrode, and titrating the mixed solution by using a silver nitrate solution to obtain a volume V of consumed silver nitrate when the first titration end point is reached1Adding the sodium chloride standard solution with the same volume as the sodium chloride standard solution added for the first time, titrating to a second end point to obtain a silver nitrate consumption volume V at the second titration end point2；
(3) Blank test: the concrete admixture is not added, and the steps (1) and (2) are repeated to obtain silver nitrate volumes V respectively consumed at two titration end points in the blank test01And V02And calculating to obtain the concentration c of the silver nitrate solution;
(4) and (3) calculating the result:
volume of silver nitrate consumed by chloride ions in concrete admixture
In the formula:
V1the volume of the silver nitrate solution consumed after the sample solution is added with the sodium chloride standard solution for the first time is mL;
V2the volume of the silver nitrate solution consumed by the sample solution after the sodium chloride standard solution is added for the second time is mL;
V01the volume of the silver nitrate solution consumed in mL after the first addition of the sodium chloride standard solution in the blank test;
V02-the total volume of silver nitrate solution consumed in mL after the second addition of the standard sodium chloride solution in the blank test;
chloride ion content in concrete admixture
In the formula:
c, concentration of silver nitrate solution, wherein the unit is mol/L;
Xcl-chloride ion content in the concrete admixture,%;
v, the volume of a silver nitrate solution consumed by chloride ions in the concrete admixture is mL;
m is the mass of the concrete admixture sample and the unit is g.
2. The method according to claim 1, wherein in step (2), when the titration is close to the equivalence point, 0.1mL of silver nitrate solution is added in each time, and the value of the derivative Δ E/. DELTA.V is calculated, and the titration is stopped when the value of Δ E/. DELTA.V is reduced, and the titration is terminated at the end pointThe volume of silver nitrate solution consumed was recorded as (V)Final (a Chinese character of 'gan'))nAnd calculating the volume V of the consumed silver nitrate solution at the end pointFinal (a Chinese character of 'gan')The following formula:
in the formula:
(Vfinal (a Chinese character of 'gan'))n-2Volume (V) recorded at the end of titrationFinal (a Chinese character of 'gan'))nSubtract 0.2 mL;
(Δ2E/ΔV2)n-1is (V)Final (a Chinese character of 'gan'))n-1Corresponding to the calculated second-level differential quotient value (V)Final (a Chinese character of 'gan'))n-1Volume (V) recorded at the end of titrationFinal (a Chinese character of 'gan'))nSubtract 0.1 mL;
(Δ2E/ΔV2)nat the end of titration (V)Final (a Chinese character of 'gan'))nAnd correspondingly calculating the obtained secondary differential quotient value.
3. The method as claimed in claim 1, wherein the concentration of the silver nitrate solution in the step (3)
In the formula:
c, concentration of silver nitrate solution, wherein the unit is mol/L;
c' -the concentration of the sodium chloride standard solution, the unit is mol/L;
v' -volume of sodium chloride standard solution added in a single time, in mL;
V0volume of silver nitrate solution consumed in mL, V, for a single addition of sodium chloride standard solution0＝V02-V01。
4. The method according to claim 1, wherein in the step (2), the sodium chloride standard solution is added in a volume of 10mL and at a concentration of 0.1000 mol/L.
5. The method of claim 1, wherein the volume ratio of nitric acid to water in the nitric acid solution in step (1) is 1: 1.
6. The method according to claim 1, wherein the starch solution added in step (1) is 2-10mL and has a concentration of 8-12 g/L.
7. The method as claimed in claim 1, wherein the concentration of silver nitrate in the step (1) is 0.09000-0.1100 mol/L.
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Cited By (2)
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| CN113447608A (en) * | 2021-06-25 | 2021-09-28 | 山东科技大学 | Method for adjusting band gap of mixed halogen perovskite and application |
| CN113687016A (en) * | 2021-09-09 | 2021-11-23 | 南通联亚药业有限公司 | Method for detecting chloride ion content in cyclobenzaprine hydrochloride |
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