CN109752403A - SO in a kind of synchronous detection concrete material42-And Cl-The method of ion concentration distribution - Google Patents

SO in a kind of synchronous detection concrete material42-And Cl-The method of ion concentration distribution Download PDF

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CN109752403A
CN109752403A CN201910022160.9A CN201910022160A CN109752403A CN 109752403 A CN109752403 A CN 109752403A CN 201910022160 A CN201910022160 A CN 201910022160A CN 109752403 A CN109752403 A CN 109752403A
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concrete material
ion concentration
test specimen
concentration distribution
synchronous detection
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高建明
朱健健
贺知章
陈菲
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Southeast University
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Southeast University
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Abstract

The invention discloses SO in a kind of synchronous detection concrete material4 2‑And Cl‑The method of ion concentration distribution, this method be radiated using different elements come secondary x rays have specific energy effect, collected signal is converted into the type and content of various elements in sample using X-ray fluorescence spectrometer (XRF), obtains SO in specific concrete material4 2‑And Cl‑Ion concentration.This method can synchronize detection SO4 2‑And Cl‑Ion concentration reduces the workload of experiment；It is detected and analyzed secondly, this method can directly adopt sample solid powder, reduces experimental procedure and improves the accuracy of experiment and the accuracy of result.

Description

SO in a kind of synchronous detection concrete material42-And Cl-The method of ion concentration distribution
Technical field
The present invention relates to SO in a kind of synchronous detection concrete material4 2-And Cl-The method of ion concentration distribution belongs to mixed Solidifying soil material field.
Background technique
Concrete structure structure will often touch the sulfate such as sewage, ocean and marshland in use and villaumite is mixed There are environment, sulfate can generate physico-chemical attack in inside configuration, generate expanded product, destroy concrete structure for conjunction； Villaumite intrusion concrete makes concrete reinforcing steel intensity impaired, destruction concrete structure durability, therefore concrete under salt environment Interior SO4 2-And Cl-Ion concentration is required to measure and be analyzed with concentration curve, reasonably to plan that concrete life designs It is estimated with structure durability.
Common concrete SO at this stage4 2-Ion concentration detection method are as follows: barium sulfategravimetry, EDTA volumetric method, than turbid Method and colorimetric method.Barium sulfategravimetry and EDTA volumetric method have preferable accuracy, but its operating procedure is complicated；Turbidimetry and ratio Color method operating process is relatively simple, accuracy Shortcomings.Cl-Ion measurement method has silver nitrate titration method and constant-current titration Method etc., silver nitrate titration method and potentiometric titration are directed to increase experimental implementation complexity with prescribed concentration assisted solution is determined And Experimental measurement error.Due to SO4 2-And Cl-Ion concentration measuring method is different, and when measurement needs separately to carry out, if desired together When detect the concentration of two kinds of ions, step is complicated and inconvenient.SO in concrete at this stage4 2-And Cl-Ion concentration detection, It is big to be related to test sample, repetition step is more, and experimentation is difficult to be precisely controlled.X-ray fluorescence spectra analytic approach (XRF) method can be with Two kinds of ions synchronize detection simultaneously and directly adopt sieving powder sample and analyzed and tested, and can effectively overcome experimental implementation The complexity problem not accurate enough with detection numerical value, can easily measure SO under mass concrete salt corrosion4 2-And Cl-Ion The problems such as concentration curve.
Summary of the invention
Technical problem: it is an object of the invention to provide SO in a kind of synchronous detection concrete material4 2-And Cl-Ion concentration point The method of cloth, this method overcome SO in existing concrete material4 2-And Cl-Precision and operation convenience in ion detection method It is difficult to the problem of taking into account, SO in efficient exactly simultaneous detection sample4 2-And Cl-The concentration distribution of ion.
Technical solution: the present invention provides SO in a kind of synchronous detection concrete material4 2-And Cl-Ion concentration distribution Method, method includes the following steps:
1) it prepares concrete material to be detected and dries, be cut into several concrete material test specimens later；
2) the concrete material test specimen for taking step 1) to prepare, is put into prepared standard salt attack solution and erodes；
3) it will be taken out in step 2) by standard salt corrosion test specimen, take its powder inside shape sample to be sieved after dry, Zhi Hou The powdered samples that 1~2h is dried are dried at a temperature of 105 DEG C ± 5 DEG C；
4) the powdered samples tabletting of step 3) drying is analyzed by X-ray fluorescence spectra later at cylindrical type bulk The secondary x rays that method analysis measurement Cl and S element is launched, and its energy and wavelength characteristic are measured, it is scaled Cl and S member later The mass percent of cellulose content, and it is further converted into S element oxide and Cl content form, transformation result is denoted as in test specimen Portion SO4 2-And Cl-Concentration；
5) SO of different location in test specimen is utilized4 2-And Cl-Ion concentration information draws test specimen ion concentration distribution figure, Middle abscissa is test specimen interior location, ordinate SO4 2-And Cl-Ion concentration.
Wherein:
Concrete material to be detected is prepared described in step 1) and is dried refers to according to match ratio formation of concrete material, Demoulding is put into standard curing room and conserves to specified age after 24 ± 2h of curing in the mold, take out later concrete material be placed in 40~ Dry 24~48h under the conditions of 60 DEG C of temperature.
It is cut into described in step 1) in several concrete material test specimens, cutting mode is longitudinally cutting or laterally cuts It cuts, the number of concrete material test specimen is greater than 3 parts.
The water-cement ratio of the concrete material is 0.2~0.7.
The standard curing room is conserved to specified age >=28 day, and the condition in standard curing room is temperature 20 ± 1 DEG C, relative humidity (RH) 95% or more.
In being put into described in step 2) in prepared standard salt attack solution in eroding, salt corrosion solution be containing SO4 2-And Cl-The mixing salt solution of ion, erosion process are constant-temperature constant-humidity environment.
SO in the standard salt attack solution4 2-And Cl-The concentration of ion is 0.1wt%~30wt%；The constant temperature In constant humidity environment, temperature >=0 DEG C, humidity >=20%RH.
Described in step 3) will in step 2) by standard salt corrosion test specimen take out, test specimen by its intensity after standard salt corrosion not Lower than the 60% of initial strength, mass loss≤5%.
It is taken described in step 3) in the sieving of its powder inside shape sample, the partial size of powdered samples is less than 0.074mm.
The powdered samples tabletting of step 3) drying is referred to and existed using tablet press machine at cylindrical type bulk described in step 4) Tabletting is carried out under the conditions of strength of pressed pieces >=20MPa, cylindrical type is block-like with a thickness of 10~40mm.
In X-ray fluorescence spectra analytic approach described in step 4), Xray fluorescence spectrometer set voltage as 220V/50~ 60Hz, helium pressure is maintained at the pressure regulating value of 0~0.025MPa in environment, and X-ray tube voltage and current setting value is 40 ± 1kV/40±1MA。
The mass percent that Cl and S constituent content is scaled described in step 4), which refers to, utilizes Fluorescence Spectrometer OXSAS points Analysis software converts.
The synchronization detects SO in concrete material4 2-And Cl-In the method for ion concentration distribution, initial SO inside test specimen4 2- And Cl-The measuring method of concentration is as follows:
1. concrete material test specimen powder inside shape sample is taken to be sieved, 1~2h is dried at a temperature of 105 DEG C ± 5 DEG C later The powdered samples dried；
2. 1. powdered samples tabletting that step is dried is analyzed by X-ray fluorescence spectra later at cylindrical type bulk The secondary x rays that method analysis measurement Cl and S element is launched, and its energy and wavelength characteristic are measured, it is scaled Cl and S member later The mass percent of cellulose content, and it is further converted into S element oxide and Cl content form, transformation result is denoted as inside test specimen Initial SO4 2-And Cl-Concentration.
The utility model has the advantages that compared with prior art, beneficial effects of the present invention are as follows:
(1) detection method provided by the invention can simultaneously, synchronize and detect SO in concrete sample4 2-And Cl-Ion is dense Degree distribution, experimental implementation process are simple and convenient, it is no longer necessary to successively detect SO4 2-And Cl-Ion concentration overcomes concrete SO4 2-And Cl-Ion concentration detects that sample demand is big and the operational error of sample nature unevenness；
(2) detection method provided by the invention has higher accuracy, it is no longer necessary to be configured to specify by sample dissolution dense Spend solution, by directly detect sieving after powder sample, reduce in similar detection method configure sample standard solution generate Error has higher detection accuracy；
(3) similarly suitable other of detection method provided by the invention corrode the erosion of the salt such as salt such as magnesium sulfate, sodium carbonate, real Proved recipe method is identical, ion parameters is detected in setting by changing, having higher concrete material, other corrode ion concentration The applicability of detection.
Detailed description of the invention
Fig. 1 is SO in synchronous detection concrete material provided by the invention4 2-And Cl-The work of the method for ion concentration distribution Skill flow chart；
Fig. 2 is SO in the concrete material for using distinct methods to measure in embodiment 14 2-And Cl-Ion concentration distribution figure；
Fig. 3 is SO in the concrete material for using distinct methods to measure in embodiment 24 2-And Cl-Ion concentration distribution figure；
Fig. 4 is SO in the concrete material for using distinct methods to measure in embodiment 34 2-And Cl-Ion concentration distribution figure；
Fig. 5 is SO in the concrete material for using distinct methods to measure in embodiment 44 2-And Cl-Ion concentration distribution figure.
Specific embodiment
The present invention will be further described With reference to embodiment:
Embodiment 1:
SO in a kind of synchronous detection concrete material4 2-And Cl-The method of ion concentration distribution, this method include following step It is rapid:
1) it is prepared concrete material (40mm × 40mm × 160mm) according to table 1, rear demoulding is put into standard to curing in the mold for 24 hours (20 DEG C of temperature, relative humidity (RH) 95% or more) maintenance 56d of fog room take out concrete material later and are placed in 60 DEG C of temperature Under the conditions of dry 48h, longitudinally cutting later is 5 concrete material test specimens, longitudinal size be respectively as follows: 30mm, 30mm, 30mm, 30mm、30mm、40mm。
1 Mortar Mixing Ratio Design and Experiment of table
2) part steps 1 are taken) the concrete material test specimen of preparation, and drilling machine takes powdered samples inside test specimen, receives Collect powdered samples and cross 200 meshes (sieve diameter 0.074mm), dries the powder that 2h is dried at a temperature of 105 DEG C later Last shape sample；
3) the powdered samples tabletting of step 2) drying is blocky (thickness 30mm) at cylindrical type, it is glimmering by X-ray later (Xray fluorescence spectrometer sets voltage as 220V/ to the secondary x rays that light spectra methods analysis measurement Cl and S element is launched 50~60Hz, helium pressure is maintained at the pressure regulating value of 0.025MPa in environment, and X-ray tube voltage and current setting value is 40kV/40Ma), and its energy and wavelength characteristic are measured, is scaled the mass percent of Cl and S constituent content later, go forward side by side one Step is converted to S element oxide and Cl content form, and transformation result is denoted as initial SO inside test specimen4 2-And Cl-Concentration；
4) part steps 1 are taken) the concrete material test specimen of preparation, it is put into configured standard sodium chloride and sodium sulphate and corrodes (5%Na in solution2SO4+ 2%NaCl mass fraction), (35 DEG C of temperature, RH 30%) erodes in climatic chamber；
5) it is taken out after erosion age reaches 150 days by standard salt corrosion test specimen, dry 48h under the conditions of 60 DEG C of temperature Sampling, drying process and the step 3) in step 2) are repeated afterwards, and last transformation result is denoted as test specimen erosion and specified for age 150 days The SO of position4 2-And Cl-Ion concentration；
6) SO of different location in test specimen is utilized4 2-And Cl-Ion concentration information draws test specimen ion concentration distribution figure, Middle abscissa is test specimen interior location, ordinate SO4 2-And Cl-Ion concentration.
Same powder is used into traditional silver nitrate titration method and colorimetric method for determining SO simultaneously4 2-And Cl-Ion concentration carries out Ion concentration compares (as shown in Figure 2).
Embodiment 2:
SO in a kind of synchronous detection concrete material4 2-And Cl-The method of ion concentration distribution, this method include following step It is rapid:
1) concrete material (40mm × 40mm × 160mm) is prepared according to table 2, demoulding is put into standard after curing in the mold 22h (19 DEG C of temperature, relative humidity (RH) 95% or more) maintenance 56d of fog room take out concrete material later and are placed in 40 DEG C of temperature Under the conditions of dry 36h, longitudinally cutting later is 5 concrete material test specimens, longitudinal size be respectively as follows: 30mm, 30mm, 30mm, 30mm、30mm、40mm。
2 Mortar Mixing Ratio Design and Experiment of table
2) part steps 1 are taken) the concrete material test specimen of preparation, and drilling machine takes powdered samples inside test specimen, receives Collect powdered samples and cross 200 meshes (sieve diameter 0.074mm), dries what 1.5h was dried at a temperature of 100 DEG C later Powdered samples；
3) the powdered samples tabletting of step 2) drying is blocky (thickness 30mm) at cylindrical type, it is glimmering by X-ray later (Xray fluorescence spectrometer sets voltage as 220V/ to the secondary x rays that light spectra methods analysis measurement Cl and S element is launched 50~60Hz, helium pressure is maintained at the pressure regulating value of 0.025MPa in environment, and X-ray tube voltage and current setting value is 39kV/39Ma), and its energy and wavelength characteristic are measured, is scaled the mass percent of Cl and S constituent content later, go forward side by side one Step is converted to S element oxide and Cl content form, and transformation result is denoted as initial SO inside test specimen4 2-And Cl-Concentration；
4) part steps 1 are taken) the concrete material test specimen of preparation, it is put into configured standard sodium chloride and sodium sulphate and corrodes (5%Na in solution2SO4+ 5%NaCl mass fraction), (35 DEG C of temperature, humidity 30%) erodes in climatic chamber；
5) it is taken out after erosion age reaches 150 days by standard salt corrosion test specimen, dry 36h under the conditions of 40 DEG C of temperature Sampling, drying process and the step 3) in step 2) are repeated afterwards, and last transformation result is denoted as test specimen erosion and specified for age 150 days The SO of position4 2-And Cl-Ion concentration；
6) SO of different location in test specimen is utilized4 2-And Cl-Ion concentration information draws test specimen ion concentration distribution figure, Middle abscissa is test specimen interior location, ordinate SO4 2-And Cl-Ion concentration.
Same powder is used into traditional silver nitrate titration method and colorimetric method for determining SO simultaneously4 2-And Cl-Ion concentration carries out Ion concentration compares (as shown in Figure 3).
Embodiment 3:
SO in a kind of synchronous detection concrete material4 2-And Cl-The method of ion concentration distribution, this method include following step It is rapid:
1) concrete material (40mm × 40mm × 160mm) is prepared according to table 2, demoulding is put into standard after curing in the mold 26h (21 DEG C of temperature, relative humidity (RH) 95% or more) maintenance 56d of fog room take out concrete material later and are placed in 50 DEG C of temperature Under the conditions of it is dry longitudinally cutting later is 5 concrete material test specimens for 24 hours, longitudinal size be respectively as follows: 30mm, 30mm, 30mm, 30mm、30mm、40mm。
2) part steps 1 are taken) the concrete material test specimen of preparation, and drilling machine takes powdered samples inside test specimen, receives Collect powdered samples and cross 200 meshes (sieve diameter 0.074mm), dries what 1.5h was dried at a temperature of 100 DEG C later Powdered samples；
3) the powdered samples tabletting of step 2) drying is blocky (thickness 30mm) at cylindrical type, it is glimmering by X-ray later (Xray fluorescence spectrometer sets voltage as 220V/ to the secondary x rays that light spectra methods analysis measurement Cl and S element is launched 50~60Hz, helium pressure is maintained at the pressure regulating value of 0.025MPa in environment, and X-ray tube voltage and current setting value is 41kV/41Ma), and its energy and wavelength characteristic are measured, is scaled the mass percent of Cl and S constituent content later, go forward side by side one Step is converted to S element oxide and Cl content form, and transformation result is denoted as initial SO inside test specimen4 2-And Cl-Concentration；
4) part steps 1 are taken) the concrete material test specimen of preparation, it is put into configured standard sodium chloride and sodium sulphate and corrodes (5%Na in solution2SO4+ 2%NaCl mass fraction), (20 DEG C of temperature, humidity 80%) erodes in climatic chamber；
5) it is taken out after erosion age reaches 150 days by standard salt corrosion test specimen, is dried for 24 hours under the conditions of 50 DEG C of temperature Sampling, drying process and the step 3) in step 2) are repeated afterwards, and last transformation result is denoted as test specimen erosion and specified for age 150 days The SO of position4 2-And Cl-Ion concentration；
6) SO of different location in test specimen is utilized4 2-And Cl-Ion concentration information draws test specimen ion concentration distribution figure, Middle abscissa is test specimen interior location, ordinate SO4 2-And Cl-Ion concentration.
Same powder is used into traditional silver nitrate titration method and colorimetric method for determining SO simultaneously4 2-And Cl-Ion concentration carries out Ion concentration compares (as shown in Figure 4).
Embodiment 4:
SO in a kind of synchronous detection concrete material4 2-And Cl-The method of ion concentration distribution, this method include following step It is rapid:
1) it is prepared concrete material (40mm × 40mm × 160mm) according to table 2, rear demoulding is put into standard to curing in the mold for 24 hours (20 DEG C of temperature, relative humidity (RH) 95% or more) maintenance 56d of fog room take out concrete material later and are placed in 60 DEG C of temperature Under the conditions of dry 48h, longitudinally cutting later is 5 concrete material test specimens, longitudinal size be respectively as follows: 30mm, 30mm, 30mm, 30mm、30mm、40mm。
2) part steps 1 are taken) the concrete material test specimen of preparation, and drilling machine takes powdered samples inside test specimen, receives Collect powdered samples and cross 200 meshes (sieve diameter 0.074mm), dries what 1.5h was dried at a temperature of 100 DEG C later Powdered samples；
3) the powdered samples tabletting of step 2) drying is blocky (thickness 30mm) at cylindrical type, it is glimmering by X-ray later (Xray fluorescence spectrometer sets voltage as 220V/ to the secondary x rays that light spectra methods analysis measurement Cl and S element is launched 50~60Hz, helium pressure is maintained at the pressure regulating value of 0.025MPa in environment, and X-ray tube voltage and current setting value is 40kV/40Ma), and its energy and wavelength characteristic are measured, is scaled the mass percent of Cl and S constituent content later, go forward side by side one Step is converted to S element oxide and Cl content form, and transformation result is denoted as initial SO inside test specimen4 2-And Cl-Concentration；
4) part steps 1 are taken) the concrete material test specimen of preparation, it is put into configured standard sodium chloride and sodium sulphate and corrodes (5%Na in solution2SO4+ 5%NaCl mass fraction), (20 DEG C of temperature, humidity 80%) erodes in climatic chamber；
5) it is taken out after erosion age reaches 150 days by standard salt corrosion test specimen, dry 48h under the conditions of 60 DEG C of temperature Sampling, drying process and the step 3) in step 2) are repeated afterwards, and last transformation result is denoted as test specimen erosion and specified for age 150 days The SO of position4 2-And Cl-Ion concentration；
6) SO of different location in test specimen is utilized4 2-And Cl-Ion concentration information draws test specimen ion concentration distribution figure, Middle abscissa is test specimen interior location, ordinate SO4 2-And Cl-Ion concentration.
Same powder is used into traditional silver nitrate titration method and colorimetric method for determining SO simultaneously4 2-And Cl-Ion concentration carries out Ion concentration compares (as shown in Figure 5).
It should be pointed out that this experimental method is not under the conditions of departing from basic experiment operating principle and operating procedure, it is corresponding to test Parameter includes: cement-based material sample dimensions, test specimen cutting mode, curing age, concentration of erosion solution configuration and corrodes age Modification can be made also to be considered as among protection scope of the present invention.Part is not described in the implementation case to be all made of first often Standard technique is advised to realize.

Claims (10)

1. SO in a kind of synchronous detection concrete material4 2-And Cl-The method of ion concentration distribution, it is characterised in that: this method packet Include following steps:
1) it prepares concrete material to be detected and dries, be cut into several concrete material test specimens later；
2) the concrete material test specimen for taking step 1) to prepare, is put into prepared standard salt attack solution and erodes；
3) it will be taken out in step 2) by standard salt corrosion test specimen, take its powder inside shape sample to be sieved after dry, later at 105 DEG C The powdered samples that 1~2h is dried are dried at a temperature of ± 5 DEG C；
4) the powdered samples tabletting of step 3) drying is passed through into X-ray fluorescence spectra analytic approach point at cylindrical type bulk later The secondary x rays that analysis measurement Cl and S element is launched, and its energy and wavelength characteristic are measured, it is scaled Cl and S element later and contains The mass percent of amount, and it is further converted into S element oxide and Cl content form, transformation result is denoted as SO inside test specimen4 2- And Cl-Concentration；
5) SO of different location in test specimen is utilized4 2-And Cl-Ion concentration information draws test specimen ion concentration distribution figure, wherein horizontal Coordinate is test specimen interior location, ordinate SO4 2-And Cl-Ion concentration.
2. SO in a kind of synchronous detection concrete material as described in claim 14 2-And Cl-The method of ion concentration distribution, It is characterized in that: preparing concrete material to be detected described in step 1) and drying refers to according to water-cement ratio formation of concrete material Expect, demoulding is put into standard curing room and conserves to specified age after 24 ± 2h of curing in the mold, takes out concrete material later and is placed in Dry 24~48h under the conditions of 40~60 DEG C of temperature.
3. SO in a kind of synchronous detection concrete material as claimed in claim 24 2-And Cl-The method of ion concentration distribution, Be characterized in that: the water-cement ratio of the concrete material is 0.2~0.7.
4. SO in a kind of synchronous detection concrete material as claimed in claim 24 2-And Cl-The method of ion concentration distribution, Be characterized in that: the standard curing room is conserved to specified age >=28 day, and the condition in standard curing room is temperature 20 ± 1 DEG C, 95% or more relative humidity.
5. SO in a kind of synchronous detection concrete material as described in claim 14 2-And Cl-The method of ion concentration distribution, Be characterized in that: in being put into described in step 2) in prepared standard salt attack solution in eroding, salt corrosion solution be containing There is SO4 2-And Cl-The mixing salt solution of ion, erosion process are constant-temperature constant-humidity environment.
6. SO in a kind of synchronous detection concrete material as claimed in claim 54 2-And Cl-The method of ion concentration distribution, It is characterized in that: SO in the standard salt attack solution4 2-And Cl-The concentration of ion is 0.1wt%~30wt%；The perseverance In constant temperature and humidity environment, temperature >=0 DEG C, humidity >=20%RH.
7. SO in a kind of synchronous detection concrete material as described in claim 14 2-And Cl-The method of ion concentration distribution, It is characterized in that: will be taken out in step 2) by standard salt corrosion test specimen described in step 3), test specimen is by its intensity after standard salt corrosion Not less than the 60% of initial strength, mass loss≤5%.
8. SO in a kind of synchronous detection concrete material as described in claim 14 2-And Cl-The method of ion concentration distribution, It is characterized in that: being taken described in step 3) in the sieving of its powder inside shape sample, the partial size of powdered samples is less than 0.074mm.
9. SO in a kind of synchronous detection concrete material as described in claim 14 2-And Cl-The method of ion concentration distribution, It is characterized in that: the powdered samples tabletting of step 3) drying being referred at cylindrical type bulk and utilize tablet press machine described in step 4) Tabletting is carried out under the conditions of strength of pressed pieces >=20MPa, cylindrical type is block-like with a thickness of 10~40mm.
10. SO in a kind of synchronous detection concrete material as described in claim 14 2-And Cl-The method of ion concentration distribution, Be characterized in that: in X-ray fluorescence spectra analytic approach described in step 4), Xray fluorescence spectrometer set voltage as 220V/50~ 60Hz, helium pressure is maintained at the pressure regulating value of 0~0.025MPa in environment, and X-ray tube voltage and current setting value is 40 ± 1kV/40±1MA。
CN201910022160.9A 2019-01-10 2019-01-10 SO in a kind of synchronous detection concrete material42-And Cl-The method of ion concentration distribution Pending CN109752403A (en)

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