CN112683615A - Method for measuring chloride ion content of concrete raw material - Google Patents

Method for measuring chloride ion content of concrete raw material Download PDF

Info

Publication number
CN112683615A
CN112683615A CN202011471104.2A CN202011471104A CN112683615A CN 112683615 A CN112683615 A CN 112683615A CN 202011471104 A CN202011471104 A CN 202011471104A CN 112683615 A CN112683615 A CN 112683615A
Authority
CN
China
Prior art keywords
raw material
chloride
concrete raw
silver
concentration
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN202011471104.2A
Other languages
Chinese (zh)
Inventor
郭睿
王军
赵日煦
高飞
吴媛媛
王婵
王淑
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Wuhan Cscec Western Construction Engineering Quality Inspection Co ltd
China West Construction Group Co Ltd
China Construction Ready Mixed Concrete Co Ltd
Original Assignee
Wuhan Cscec Western Construction Engineering Quality Inspection Co ltd
China West Construction Group Co Ltd
China Construction Ready Mixed Concrete Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Wuhan Cscec Western Construction Engineering Quality Inspection Co ltd, China West Construction Group Co Ltd, China Construction Ready Mixed Concrete Co Ltd filed Critical Wuhan Cscec Western Construction Engineering Quality Inspection Co ltd
Priority to CN202011471104.2A priority Critical patent/CN112683615A/en
Publication of CN112683615A publication Critical patent/CN112683615A/en
Pending legal-status Critical Current

Links

Landscapes

  • Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)

Abstract

The invention discloses a method for measuring the chloride ion content of a concrete raw material, which comprises the steps of adding a to-be-measured concrete raw material into a nitric acid solution, and heating for 1-2 min; accurately adding excessive silver nitrate solution, stirring and heating to precipitate all chloride ions in the raw materials in a form of silver chloride; filtering to remove silver chloride precipitate and undissolved raw materials to obtain supernatant; preparing silver ion standard solutions with different concentrations, and establishing a standard curve with the concentration as a horizontal coordinate and the electric signal value CPS as a vertical coordinate by using an inductively coupled plasma emission spectrum; and measuring the concentration of silver ions in the clear liquid by using the inductively coupled plasma emission spectrum and the standard curve, and obtaining the content of chloride ions in the concrete raw material by a calculation formula. The invention is suitable for raw materials such as concrete cement, mineral admixture, sand, stone, additive and the like, and the test method is simple and easy to operate.

Description

Method for measuring chloride ion content of concrete raw material
Technical Field
The invention belongs to the technical field of concrete materials, and particularly relates to a method for measuring the content of chloride ions in a concrete raw material.
Background
The chloride ion content is an important factor affecting the durability of concrete. The content of chloride ions in concrete is too high, so that the steel bars in the concrete are easy to generate electrochemical reaction to cause corrosion of the steel bars, thereby causing the volume expansion and loosening of the concrete and damaging the concrete structure. The chloride ions in the concrete mainly come from raw materials such as cement, water, sand, additives and the like used in mixing, so the control of the content of the chloride ions in the concrete must be started from the raw materials. The selection of a suitable chloride ion content test method is an extremely important part of the whole quality control link.
At present, different methods are used for testing the chloride ion content in different concrete raw materials at home and abroad. The chloride ion determination method described in the standard GB/T176 cement chemical analysis method mainly comprises a mercury nitrate titration method, an ammonium thiocyanate volumetric method, an ion chromatography method, a potentiometric titration method and the like; the chloride ion content test method in coarse and fine aggregates is also described in the standard GB/T568-2019, mainly potassium chromate indicating silver nitrate titration. However, in the above three chemical analysis methods, the reagents used, such as mercury nitrate, ammonium thiocyanate, potassium chromate, etc., are highly toxic or first-order carcinogenic chemical reagents, and there is a certain risk in the experimental operation; the ion chromatography is a common trace anion detection method, has the advantages of small interference, wide detection range and more accurate quantification, but is time-consuming in the chromatographic separation process and only suitable for sample detection with less batch; the potentiometric titration method has high efficiency, can avoid errors caused by manual operation, but the titrating pipeline of the potentiometric titrator is easy to block, and the generated silver chloride floccule has great influence on the sensitivity and stability of the measuring electrode.
Disclosure of Invention
The invention aims to provide a method for measuring the content of chloride ions in a concrete raw material, so as to avoid the problems of danger brought to testers by toxic chemicals in an indicator titration method, errors brought by manual operation of a potentiometric titration method and low testing efficiency of an ion chromatography method, and improve the accuracy and the testing efficiency of a measuring result.
In order to achieve the purpose, the technical scheme is as follows:
the method for measuring the chloride ion content of the concrete raw material comprises the following steps:
(1) adding a to-be-detected concrete raw material into a nitric acid solution, and heating for 1-2 min;
(2) accurately adding excessive silver nitrate solution, stirring and heating to precipitate all chloride ions in the raw materials in a form of silver chloride;
(3) filtering to remove silver chloride precipitate and undissolved raw materials to obtain supernatant;
(4) preparing silver ion standard solutions with different concentrations, and establishing a standard curve with the concentration as a horizontal coordinate and the electric signal value CPS as a vertical coordinate by using an inductively coupled plasma emission spectrum;
(5) and measuring the concentration of silver ions in the clear liquid by using the inductively coupled plasma emission spectrum and the standard curve, and obtaining the content of chloride ions in the concrete raw material by a calculation formula.
According to the scheme, the concrete raw material is one or a mixture of cement, mineral admixture, sand, stone and additive.
According to the scheme, in the step 1, the concentration of nitric acid is 30-50 vt%, and the heating temperature is 60-100 ℃;
according to the scheme, the concentration of the silver nitrate solution in the step 2 is 5.0g/L, and the heating temperature is 100 ℃;
according to the scheme, the calculation formula in the step 5 is as follows:
XCl -=100×35.45[c1v1-c2m2/1000]/1000×107.87m1
wherein m is1-concrete raw material mass, g; v. of1-silver nitrate solution volume, mL; c. C1-silver nitrate solution concentration, mg/mL; m is2-supernatant mass, g; c. C2-silver ion concentration in the clear solution,. mu.g/g; xCl -Chloride ion content, wt%.
Compared with the prior art, the invention has the beneficial effects that:
(1) according to the method for testing the content of the chloride ions in the concrete admixture, an advanced precision testing instrument is adopted to inductively couple the plasma emission spectrum, so that errors caused by manual operation in a potentiometric titration method are reduced, and the accuracy of a test result and the test efficiency are improved.
(2) The invention has simple testing principle, avoids using highly toxic or first-grade carcinogenic chemical reagents such as mercury nitrate, ammonium thiocyanate, potassium chromate and the like, and effectively avoids the danger of toxic chemicals to testers.
(3) The invention is suitable for raw materials such as concrete cement, mineral admixture, sand, stone, additive and the like, and the test method is simple and easy to operate.
(4) The sand and the stone are heated by nitric acid, so that the time for dissolving out chloride ions in the original test method is shortened.
Detailed Description
The following examples further illustrate the technical solutions of the present invention, but should not be construed as limiting the scope of the present invention.
Preparing silver ion standard solutions with the concentrations of 1.0 mug/g, 10.0 mug/g and 100.0 mug/g respectively, creating an inductively coupled plasma emission spectrum silver element testing method, optimizing instrument parameters, and establishing a standard curve with the concentration (mug/g) as a horizontal coordinate and an electric signal value CPS as a vertical coordinate; meanwhile, 5.0mg/mL silver nitrate solution is prepared for standby.
Example 1
Accurately weighing 3.8991g of concrete raw material portland cement, placing the concrete raw material portland cement into a 500mL beaker, adding 50mL of water, stirring to completely disperse a sample, adding 50mL of 30 vt% nitric acid solution under stirring, heating and slightly boiling at 100 ℃ for 2min, taking down, accurately transferring 1.0mL of 5.0mg/mL silver nitrate solution into the solution by using a pipette, stirring and boiling at 100 ℃ for 2min, adding a little filter paper, filtering by using quick filter paper which is washed by 2% nitric acid solution in advance, collecting filtrate into a 250mL conical flask (with the mass of 116.34g) with the mass weighed in advance, washing the beaker, a glass rod and the filter paper until the total volume of the filtrate and the washing liquid reaches about 200mL to be measured, and weighing the total mass of the solution and the conical flask (with the mass of 316.87 g). The concentration of the solution to be measured is 15.392 mug/g by the inductive coupling plasma emission spectrum of the established method, and the content of chloride ions in the portland cement is 0.0161 percent according to the formula calculation.
Comparative example 1
4.8733g of the same sample as in example 1 was weighed, placed in a 500mL beaker, 50mL of water was added, the sample was stirred to completely disperse, 50mL of nitric acid solution (1+2) was added under stirring, and the mixture was boiled and slightly boiled for 2 min. Taking down, adding 5.0mL of 0.05mol/L silver nitrate standard solution, stirring uniformly, boiling for 2min, adding a little filter paper, filtering with quick filter paper washed by nitric acid (1+100) in advance, collecting filtrate in a 250mL conical flask, washing a beaker, a glass rod and the filter paper by nitric acid (1+100) until the total volume of the filtrate and the washing liquid reaches about 200mL, and cooling the solution to 25 ℃ in a dark place. 5mL of ferric ammonium sulfate indicator solution was added and the solution was titrated with 0.05mol/L of ammonium thiocyanate standard solution to give a reddish brown color and did not disappear upon shaking, at which time the volume of ammonium thiocyanate consumed was 5.4 mL. A blank test was performed as described above without the addition of sample, and the volume of ammonium thiocyanate standard titration solution used for the blank titration was recorded as 5.0 mL. The chloride ion content of this sample was 0.0156%.
Example 2
4.5335g of concrete raw material mineral powder is accurately weighed and placed in a 500mL beaker, 50mL of water is added, the sample is completely dispersed by stirring, 50mL of 40 vt% nitric acid solution is added under stirring, the mixture is heated and slightly boiled for 2min at 100 ℃, the mixture is taken down, 1.0mL of 5.0mg/mL silver nitrate solution is accurately transferred by a pipette and added, the mixture is stirred and boiled for 1min at 100 ℃, a little filter paper is added, the mixture is filtered by quick filter paper which is washed by 2% nitric acid solution in advance, the filtrate is collected in a 250mL conical flask (with the mass of 115.65g) with the mass of 115.65g, the beaker, the glass rod and the filter paper are washed until the total volume of the filtrate and the washing liquid reaches about 200mL, and the total mass of the solution and the conical flask is weighed (with the mass of 316.03 g). The concentration of the solution to be measured is 14.741 mug/g by the inductive coupling plasma emission spectrum of the established method, and the content of the chloride ions in the mineral powder is 0.0148% according to the formula.
Example 3
4.1129g of concrete raw material fly ash is accurately weighed and placed in a 500mL beaker, 50mL of water is added, the sample is stirred to be completely dispersed, 50mL of 40 vt% nitric acid solution is added under stirring, the mixture is heated and slightly boiled for 1min at 100 ℃, the mixture is taken down, 1.0mL of 5.0mg/mL silver nitrate solution is accurately transferred and added by a pipette, the mixture is stirred and boiled for 1min at 100 ℃, a little filter paper is added, the mixture is filtered by quick filter paper which is washed by 2% nitric acid solution in advance, the filtrate is collected in a 250mL conical flask (with the mass of 117.33g) with the mass of 117.33g, the beaker, the glass rod and the filter paper are washed until the total volume of the filtrate and the washing liquid reaches about 200mL, and the total mass of the solution and the conical flask is weighed (with the mass of 317.81 g). The concentration of the solution to be measured is 19.514 mug/g by using the inductively coupled plasma emission spectrum of the established method, and the content of chloride ions in the fly ash is 0.00865 percent according to the formula calculation.
Example 4
The concrete raw material machine-made sand 500.0g is accurately weighed and placed in a ground bottle, 500mL of distilled water is measured by a volumetric flask and injected into the ground bottle, 50mL of 50 vt% nitric acid solution is accurately added under stirring, and the ground bottle is placed on an electric hot plate and heated at 60 ℃ to fully dissolve chloride. After cooling, the clarified solution at the upper part of the ground bottle is filtered, then 50mL of filtrate is accurately transferred by a pipette and placed in a 250mL clean beaker, 5.0mL of 5.0mg/mL silver nitrate solution is accurately transferred by a pipette and added thereto, stirring and boiling is carried out for 2min at 100 ℃, a little filter paper is added, filtration is carried out by using quick filter paper which is washed by 2% nitric acid solution in advance, the filtrate is collected in a 250mL conical flask (with the mass of 116.90g) with the mass of which is weighed in advance, the beaker, the glass rod and the filter paper are washed until the total volume of the filtrate and the washing solution reaches about 200mL, and the total mass of the solution and the conical flask is weighed (with the mass of 317.51 g). The concentration of the solution to be measured is 15.221 mug/g by the inductively coupled plasma emission spectrum of the established method, and the chloride ion content of the machine-made sand is 0.0158 percent according to the formula calculation.
Example 5
500.5g of concrete raw material crushed stone is accurately weighed and placed in a ground bottle, 500mL of distilled water is measured by a volumetric flask and injected into the ground bottle, 50mL of 50 vt% nitric acid solution is accurately added, and the ground bottle is placed on an electric hot plate and heated at 60 ℃ to fully dissolve chloride. After cooling, the upper part of the ground bottle is filtered with clear solution, then 100mL of filtrate is accurately transferred by a pipette and placed in a 250mL clean beaker, 10.0mL of 5.0mg/mL silver nitrate solution is accurately transferred by a pipette and added thereto, stirring and boiling is carried out for 2min at 100 ℃, a little filter paper is added, filtration is carried out by using quick filter paper which is washed by 2% nitric acid solution in advance, the filtrate is collected in a 250mL conical flask (with the mass of 113.86g) with the mass of which is weighed in advance, the beaker, the glass rod and the filter paper are washed until the total volume of the filtrate and the washing solution reaches about 200mL, and the total mass of the solution and the conical flask is weighed (with the mass of 314.23 g). The concentration of the solution to be measured is 12.265 mug/g by the inductive coupling plasma emission spectrum of the established method, and the chloride ion content of the macadam is 0.0172 percent according to the formula calculation.
Example 6
2.3347g of concrete raw material polycarboxylate superplasticizer is accurately weighed and placed in a beaker, 50mL of distilled water and 4mL of 50 vt% nitric acid solution are added, and the beaker is placed on an electric hot plate and heated and stirred at 60 ℃ until the concrete raw material polycarboxylate superplasticizer is completely dissolved. Sucking 1.0mL of 5.0mg/mL silver nitrate solution by a pipette, adding the silver nitrate solution into the silver nitrate solution, stirring the mixture evenly and boiling the mixture for 2min, adding a little of filter paper, filtering the mixture by using quick filter paper which is washed by 2% nitric acid solution in advance, collecting filtrate into a 250mL conical flask (with the mass of 115.60g) with the mass of the filtrate weighed in advance, washing a beaker, a glass rod and the filter paper until the total volume of the filtrate and the washing solution reaches about 200mL to be tested, and weighing the total mass of the solution and the conical flask (with the mass of 315.92 g). The concentration of the solution to be measured is determined to be 22.523 mu g/g by inductively coupled plasma emission spectroscopy of the established method, and the content of chloride ions in the polycarboxylate superplasticizer is 0.00680 percent according to the formula.
Comparative example 2
Blank test: adding 200mL of water and 4mL of nitric acid (1+1) into a beaker, accurately transferring 10mL of 0.1000mol/L NaCl solution by using a pipette, slowly dropwise adding 0.1003mol/L silver nitrate solution under electromagnetic stirring under the condition of not adding a sample, and recording the potential and the corresponding reading of a burette until the potential is mutated for the first time; after the equivalence point is exceeded, a second 10mL of 0.1000mol/L NaCl solution is pipetted into the same solution and the standard AgNO is continued3The solution was titrated to potential for a second mutation. Performing parallel test twice, and calculating AgNO by using a quadratic derivative method3Volume V of solution consumption01And V0210.26mL and 20.24mL, respectively.
Sample testing: 4.9379g of the same polycarboxylate superplasticizer sample as in example 6 was accurately weighed and placed in a beaker, 200mL of water and 4mL of nitric acid (1+1) were added, 10mL of 0.1000mol/L NaCl solution was accurately removed with a pipette, 0.1003mol/L silver nitrate solution was slowly added dropwise with electromagnetic stirring, the potential and the corresponding burette reading were recorded until the potential mutated for the first time, and AgNO consumption at the first end point was obtained3The volume of the solution was 10.36mL, then 10mL of 0.1000mol/L NaCl solution was added to the beaker, titration was continued until the potential mutated a second time, and the AgNO consumption at the second endpoint was recorded3The volume of the solution was 20.32mL, and the chloride ion content of the admixture sample was 0.00661% according to the calculation formula.

Claims (5)

1. The method for measuring the content of chloride ions in the concrete raw material is characterized by comprising the following steps of:
(1) adding a to-be-detected concrete raw material into a nitric acid solution, and heating for 1-2 min;
(2) accurately adding excessive silver nitrate solution, stirring and heating to precipitate all chloride ions in the raw materials in a form of silver chloride;
(3) filtering to remove silver chloride precipitate and undissolved raw materials to obtain supernatant;
(4) preparing silver ion standard solutions with different concentrations, and establishing a standard curve with the concentration as a horizontal coordinate and the electric signal value CPS as a vertical coordinate by using an inductively coupled plasma emission spectrum;
(5) and measuring the concentration of silver ions in the clear liquid by using the inductively coupled plasma emission spectrum and the standard curve, and obtaining the content of chloride ions in the concrete raw material by a calculation formula.
2. The method for measuring the chloride ion content of a concrete raw material according to claim 1, wherein the concrete raw material is one or a mixture of cement, mineral admixture, sand, stone and admixture.
3. The method for measuring the chloride ion content of the concrete raw material according to claim 1, wherein the concentration of the nitric acid in the step 1 is 30 to 50 vt%, and the heating temperature is 60 to 100 ℃.
4. The method for measuring the chloride ion content of a concrete raw material according to claim 1, wherein the silver nitrate solution in the step 2 has a concentration of 5.0g/L and a heating temperature of 100 ℃.
5. The method for measuring the chloride ion content of a concrete raw material according to claim 1, wherein the calculation formula in step 5 is as follows:
Figure FDA0002833778130000011
wherein m is1-concrete raw material mass, g; v. of1-silver nitrate solution volume, mL; c. C1-silver nitrate solution concentration, mg/mL; m is2-supernatant mass, g; c. C2-silver ion concentration in the clear solution,. mu.g/g;
Figure FDA0002833778130000012
chloride ion content, wt%.
CN202011471104.2A 2020-12-14 2020-12-14 Method for measuring chloride ion content of concrete raw material Pending CN112683615A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202011471104.2A CN112683615A (en) 2020-12-14 2020-12-14 Method for measuring chloride ion content of concrete raw material

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202011471104.2A CN112683615A (en) 2020-12-14 2020-12-14 Method for measuring chloride ion content of concrete raw material

Publications (1)

Publication Number Publication Date
CN112683615A true CN112683615A (en) 2021-04-20

Family

ID=75447776

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202011471104.2A Pending CN112683615A (en) 2020-12-14 2020-12-14 Method for measuring chloride ion content of concrete raw material

Country Status (1)

Country Link
CN (1) CN112683615A (en)

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103728289A (en) * 2013-12-16 2014-04-16 金川集团股份有限公司 Method for rapidly measuring gold and silver in crude copper
CN105403556A (en) * 2015-11-02 2016-03-16 第一拖拉机股份有限公司 Method for determining chlorine ion content in engine coolant of tractor
CN106290316A (en) * 2016-08-16 2017-01-04 湖北兴发化工集团股份有限公司 A kind of analysis method of Dimethyldichlorosilane hydrolysate intermediate ion

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103728289A (en) * 2013-12-16 2014-04-16 金川集团股份有限公司 Method for rapidly measuring gold and silver in crude copper
CN105403556A (en) * 2015-11-02 2016-03-16 第一拖拉机股份有限公司 Method for determining chlorine ion content in engine coolant of tractor
CN106290316A (en) * 2016-08-16 2017-01-04 湖北兴发化工集团股份有限公司 A kind of analysis method of Dimethyldichlorosilane hydrolysate intermediate ion

Similar Documents

Publication Publication Date Title
CN103196776A (en) Measuring method of catalytic cracking slurry solid content
CN103926300A (en) Improved method for determining free chlorine ions in cement paste or mortar
CN113720804B (en) Method for rapidly detecting residual quantity of flocculant in sand for concrete
CN105203475A (en) Method of determining chemical oxygen demand in chlorine-containing water sample
CN104034722A (en) Method for measuring substance content of composite silicon carbide
Shan et al. A facile, fast responsive and highly selective mercury (II) probe characterized by the fluorescence quenching of 2, 9-dimethyl-1, 10-phenanthroline and two new metal–organic frameworks
CN117368339A (en) Detection method for flocculant residue in machine-made sand
CN112683615A (en) Method for measuring chloride ion content of concrete raw material
CN109613169A (en) A kind of method of lead molybdate precipitating in ferro-molybdenum chemical analysis
CN111650194A (en) Method for determining phosphorus content in iron ore by bismuth-phosphorus-molybdenum blue
CN109060990A (en) A method of different shape phosphate in measurement water-soluble poly ammonium phosphate
CN115979976A (en) Method for detecting flocculating agent in washing machine-made sand
CN113281458A (en) Analysis method for free total calcium content of steel slag
CN104407095A (en) Method for measuring magnesium ion in sulfate-process titanium dioxide concentrated solution
CN100535637C (en) Continuous detecting method for lead-cadmium in plastic sample
CN112129744A (en) Chemical phase analysis method for lithium in ore
CN113418970A (en) Method for measuring fluorine in magnesium refractory material
CN107478585B (en) Method for testing free silicon dioxide in mica powder
CN110850025A (en) Method for determining chloride ion content in industrial iron oxide by automatic potentiometric titration
CN112710650A (en) Method for rapidly and accurately measuring main chemical component content of cement
CN113447479A (en) Method for measuring copper content in copper concentrate by photometric titration
CN109596607A (en) A kind of method of chloride ion in measurement silver cyanide
CN113030067B (en) Method for rapidly identifying rare earth grade of weathering crust elution-deposited rare earth ore in field
CN116878984A (en) Sample pretreatment method for measuring chloride ion content in cement clinker and application thereof
CN114518428B (en) Method for detecting content of free chloride ions in ultrahigh-strength cement-based material

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
RJ01 Rejection of invention patent application after publication
RJ01 Rejection of invention patent application after publication

Application publication date: 20210420