CN105806659A - Device for obtaining pore solution in cement-based material and method for analyzing components of pore solution - Google Patents
Device for obtaining pore solution in cement-based material and method for analyzing components of pore solution Download PDFInfo
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- CN105806659A CN105806659A CN201610347365.0A CN201610347365A CN105806659A CN 105806659 A CN105806659 A CN 105806659A CN 201610347365 A CN201610347365 A CN 201610347365A CN 105806659 A CN105806659 A CN 105806659A
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- cement
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- hole solution
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/02—Devices for withdrawing samples
- G01N1/10—Devices for withdrawing samples in the liquid or fluent state
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/02—Devices for withdrawing samples
- G01N1/10—Devices for withdrawing samples in the liquid or fluent state
- G01N2001/1031—Sampling from special places
Abstract
The invention provides a device for obtaining a pore solution in a cement-based material and a method for analyzing components of the pore solution.The device comprises a piston, an extruding cavity, a base plate and a support.The extruding cavity is arranged on the base plate, the top face of the base plate is provided with a liquid collecting tank communicated with the extruding cavity, and a liquid discharging channel communicated with the liquid collecting tank is formed in the base plate.The device is characterized in that the liquid discharging channel is arranged obliquely, and a liquid outlet of the liquid discharging channel is formed in the side wall of the base plate.The device is simple in structure, wide in application range and convenient to operate, and the real pore solution is obtained.The method for analyzing the components of the pore solution is specially designed based on common component concentration of the pore solution in the cement-based material and an ion chromatography technique and is simple, quick, convenient and high in accuracy.
Description
Technical field
The invention belongs to civil engineering material technical field, the device that relates to obtaining solution in hardening cement base material and the hole solution component analyzing method based on ion chromatography, specifically a kind of obtain the device of hole solution in cement-based material and the method analyzing hole solution composition.
Background technology
Being typical loose structure with the cement-based material that concrete is representative, hole solution is just present in the intrapore solution containing different kinds of ions composition.Hole solution is the internal important liquid phase environment of cement-based material, and concrete durability and steel bar corrosion play vital impact, and analyzes the ion component of hole solution to research hydrated reaction of cement important in inhibiting.
Material is put in pressurizing unit and is called high pressure extract method by the method for forcing press extruding acquisition pores solution, and the liquid that this method obtains can reflect the situation of hole solution really.
Ion chromatography is a kind of trace wet-chemical analysis new technique proposed in 1975, within 1977, begins in water treatment field and adopts.The application of present ion chromatograph is more and more extensive, and precision is also more and more higher.In the chromatography of ions, various ions are that the basis relative affinity to exchanger resin is exchanged by ion and separates.
The hole solution component analyzing method external standard method of ion chromatography technology.Chromatography of ions is to analyze anion and cationic a kind of liquid-phase chromatography method, has quick and convenient, sensitivity high.Can be used for analyzing Common Anions such as F in aqueous solution-、Cl-、Br-、NO2 -、NO3 -、SO4 2-、PO4 3-With Common Cations Li+、Na+、NH4 +、K+、Mg2+、Ca2+.Different according to INSTRUMENT MODEL, the concentration range of ion chromatography is 1 μ g/L(1～10 μ g/L) to 103mg/L.External standard method is individually to be measured under the chromatographic condition identical with sample by standard sample, the chromatographic peak face obtained
The method that the long-pending chromatographic peak area with tested component carries out contrasting the content trying to achieve tested component.
Existing hole solution pressurizing unit has flaw, and is all not equipped with convenient, specification, accurate hole solution component analyzing method accordingly.Chinese patent (application number CN200410066554.8) invention disclosed patent application, it is long that it collects fluid pipeline path, not simply；Utility model patent disclosed in Chinese patent (application number CN201420844839.9), excessively complicated, collection device is not good, collects too slow, is unfavorable for a large amount of sample analysis；Chinese patent (application number CN201310172200.0) invention disclosed patent application, it takes the particle after the full water of extrded material vacuum, and what obtain is not real hole solution；The leaching liquid of filtering holes solution after the ultrasonic extraction that Chinese patent (application number CN201010127341.7) invention disclosed patent obtains, this method is consuming time oversize, can only detect a kind of ion every time, very numerous and diverse.Therefore, the hole solution urgently researching and developing a kind of purposes pressurizing unit wide, easy and simple to handle and respective standard at present analyzes method.
Summary of the invention
The present invention solves prior art Problems existing, it is provided that a kind of obtain the device of hole solution, simple in construction in cement-based material, purposes is wide, it is simple to operation, it is possible to obtain real hole solution；Also provide for a kind of analysis method of hole solution composition, analyze method simple, convenient, analyze result degree of accuracy high.
It is an object of the invention to be achieved through the following technical solutions: a kind of obtain the device of hole solution in cement-based material, extrusion chamber and the chassis of described piston is can be inserted into including piston, centre, described extrusion chamber is arranged on described chassis, described chassis face arranges the collecting tank that connect internal with described extrusion chamber, described chassis arranges the apocenosis passage connected with described collecting tank, it is characterized in that, described apocenosis passage is obliquely installed, and the liquid outlet of described apocenosis passage is arranged on described chassis side wall.
Improvement to technique scheme: described apocenosis passage is inserted into stainless steel tube, described stainless steel tube the inner is inserted in described collecting tank, and described liquid outlet is stretched out in described stainless steel tube outer end.
Further improvement to technique scheme: described extrusion chamber is cylindrical cavity, described chassis is disc, circular caulking groove is set in the middle part of described base top surface, described circular caulking groove diameter is consistent with the external diameter of described extrusion chamber, described extrusion chamber snaps in described circular caulking groove, described collecting tank is annular and is arranged on described circular middle part, caulking groove bottom surface, the external diameter of described annular collecting tank is equal to the diameter of described extrusion chamber intermediate cylindrical cavity, certain gradient is had in described collecting tank, the least significant end of described collecting tank is inserted in described stainless steel tube the inner.
Further improvement to technique scheme: described piston is cylindrical, described piston upper end arranges the piston cap of cylinder, described piston cap is the diameter cylinder more than described piston diameter, described piston cap bottom surface arranges circular socket, described piston upper end embeds in described circular socket and forms loose fit, because of the bias of die misalignment formation during to avoid to greatest extent pressurizeing.
Further improvement to technique scheme: the bottom on described chassis arranges bearing, and described bearing is cylindrical shape, and described bearing external diameter is less than the external diameter of described base.
A kind of analysis method of hole solution composition, comprises the steps:
(1) required reagent and medicine are prepared:
Ultra-pure water；
Anionic recognition system leacheate 30mM potassium hydroxide solution；
Cation detection system leacheate 20mM Loprazolam solution；
Standard sample, including Cl-、SO4 2-、Na+、K+、Ca2+、Mg2+Common hole solution detection ion list mark solution；
Syringe filter；
Plastic-like QC；
Filter element cap；
(2) according to cement based sample ion concentration range to be measured, take the optimized scope of ion chromatograph into consideration, treat the standard solution of 4 ~ 5 concentration levels of measured ion with the preparation of stepwise dilution method；
(3) cement-based material hole solution is filtered by syringe filter, and with 1:n dilution proportion；
(4) first analyze the standard solution of 4 ~ 5 concentration levels treating measured ion, post analysis hole solution sample to be measured with ion chromatography, directly give test sample concentration x；
(5) according to the following formula by Ca in dilute sample2+Concentration conversion is Ca in hole solution2+Actual concentrations
y=n·x
Wherein, Ca in y hole solution2+Actual concentrations, mg/L；
N extension rate；
Ca in x dilute sample2+Concentration, mg/L.
Improvement to technique scheme: the acquisition methods of cement-based material hole solution in described step (3), the device of hole solution in cement-based material that obtains described in any one of claim 1-6 is placed on pressure testing machine centre position, put into after cylindrical test block surface is dried in described extrusion chamber, put piston, piston cap, then use hydraulic press to start pressurization；Loading speed maintains 5 ~ 6kN/s, is pressurized within the scope of 460kN ~ 750kN gradually, until cement-based material hole solution flows out, collects with polystyrene bottle.
Further improvement to technique scheme: the acquisition methods of cement-based material hole solution in described step (3), in order to obtain more cement-based material hole solution, slowing down loading speed when test block just starts stress until beginning to flow out cement-based material hole solution, recovering normal loading speed afterwards again.
Compared with prior art, advantages of the present invention and having the benefit effect that
(1) device of hole solution in acquisition cement-based material provided by the invention, has certain slope inside collecting tank, it is possible to accelerating liquid flows, and reduces liquid residue in collecting tank；The apocenosis passage connected with collecting tank in base is obliquely installed, the liquid outlet of apocenosis passage is arranged on described base side wall lower limb, apocenosis passage inserts stainless steel tube, energy accelerating liquid flowing velocity, shorten flow path of the liquid, it is effectively prevented from liquid to run off along apocenosis passage sidewall, also allows for using the more hole solution of syringe assisted collection；Circular caulking groove on base can block extrusion chamber, makes the two Relative sliding not occur and produce space in operation, it is to avoid sample particle flows to liquid to obtain liquid clarification；Its simple in construction, compact, purposes is wide, it is simple to operation, it is possible to obtain real hole solution.
(2) the analysis method of hole solution composition provided by the invention, operational approach is simple, convenient, analyzes result accurately, reliably, and a sample can pass through twice analysis, draws the concentration of cationes whole in hole solution and anion.
Accompanying drawing explanation
Fig. 1 is that a kind of device of hole solution that obtains in cement-based material of the present invention is along the cross-sectional view of axis；
Fig. 2 is that a kind of chassis that obtains in cement-based material in the device of hole solution is along the enlarged diagram of axis profile structure.
1. piston cap, 2. piston, 3. extrusion chamber, 4. test block, 5. collecting tank, 6. chassis, 7. bearing, 8. stainless steel tube, 9. apocenosis passage.
Detailed description of the invention
Below in conjunction with the drawings and specific embodiments, the present invention is made further technology to describe.Should be understood that embodiment to be merely to illustrate and do not limit the scope of the invention.
Referring to Fig. 1, Fig. 2, being that the present invention is a kind of obtains the embodiment of the device of hole solution in cement-based material, including piston 2, the middle extrusion chamber 3 inserting described piston 2 and chassis 6, is arranged on described chassis 6 by extrusion chamber 3.Being arranged above with and the collecting tank 5 connected inside extrusion chamber 3 on chassis 6, arrange the apocenosis passage 9 connected with collecting tank 5 in chassis 6, apocenosis passage 9 is obliquely installed, and the liquid outlet of apocenosis passage 9 is arranged on the sidewall on chassis 6.
Specifically: above-mentioned apocenosis passage 9 is inserted into stainless steel tube 8, the inner of stainless steel tube 8 is inserted in collecting tank 5, and described liquid outlet is stretched out in stainless steel tube 8 outer end.
Above-mentioned liquid outlet is positioned at the lower limb of described base 6, and it is 1-2cm that stainless steel tube 8 stretches out the length of liquid outlet.
Being the cylindrical cavity being vertically arranged in the middle of above-mentioned extrusion chamber 3, the cylindrical cavity internal diameter of above-mentioned extrusion chamber is generally the concrete optional 50mm of 40-60mm(), highly it is generally the concrete optional 100mm of 80-120mm().Above-mentioned chassis 6 is disc, arranges circular caulking groove in the middle part of the end face of chassis 6, and circular caulking groove diameter is consistent with the external diameter of extrusion chamber 3, and extrusion chamber 3 snaps in location in circular caulking groove.Collecting tank 5 is for annular and is arranged on circular middle part, caulking groove bottom surface, and collecting tank 5 external diameter of annular is equal to the diameter of extrusion chamber 3 intermediate cylindrical cavity.There is certain slope in above-mentioned collecting tank 5, the inner of stainless steel tube 8 is inserted the least significant end of collecting tank 5.Preferably, the degree of depth of above-mentioned collecting tank least significant end is 8mm, and the degree of depth of most significant end is 5mm.
Above-mentioned piston 2 is cylindrical, described piston 2 upper end arranges the piston cap 1 of cylinder, described piston cap 1 is the diameter cylinder more than described piston 2 diameter, and described piston cap 1 bottom surface arranges circular socket, and described piston 2 upper end embeds in described circular socket and forms loose fit.The bottom on above-mentioned chassis 6 arranges bearing 7, and described bearing 7 is cylindrical shape, and described bearing 7 external diameter is less than the external diameter of described base 6.
Specific embodiment is with acquisition pores solution and analyzes Ca2+Concentration is example.
It is placed on pressure testing machine by device centre position, Ф 50mm × 50mm cylindrical test block 4 surface is put in the extrusion chamber 3 shown in Fig. 1 after drying, puts piston 2, piston cap 1, then use hydraulic press to start pressurization.Loading speed maintains 5 ~ 6kN/s, is pressurized to gradually between about 460kN ~ 750kN, until hole solution flows out, collects with polystyrene bottle.In order to obtain more hole solution, it is possible to slow down loading speed when test block 4 has just started stress until beginning to flow out hole solution, recover normal loading speed afterwards again.Alternatively, it is also possible to shed pressure again maintaining a period of time when hydraulic press reaches maximum pressure, again pressurize again after a while.Often all must clean extrusion equipment cavity and hole slot with pure water after one test block 4 of pressure.General each test block 4 can be pressed and be taken 5 ~ 8ml hole solution.
The detailed description of the invention of the analysis method of a kind of hole solution composition of the present invention, comprises the steps:
(1) required reagent and medicine are prepared:
Ultra-pure water；
Anionic recognition system leacheate 30mM potassium hydroxide solution；
Cation detection system leacheate 20mM Loprazolam solution；
Standard sample, including Cl-、SO4 2-、Na+、K+、Ca2+、Mg2+Ion list mark solution is detected etc. common hole solution；
Syringe filter；
Plastic-like QC；
Filter element cap；
(2) according to cement based sample ion concentration range to be measured, take the optimized scope of ion chromatograph into consideration, treat the standard solution of 4 ~ 5 concentration levels of measured ion with the preparation of stepwise dilution method；
(3) cement-based material hole solution is filtered by syringe filter, and with 1:n dilution proportion；
(4) first analyze the standard solution of 4 ~ 5 concentration levels treating measured ion, post analysis hole solution sample to be measured with ion chromatography, directly give test sample concentration x；
(5) according to the following formula by Ca in dilute sample2+Concentration conversion is Ca in hole solution2+Actual concentrations
y=n·x
Wherein, Ca in y hole solution2+Actual concentrations, mg/L；
N extension rate；
Ca in x dilute sample2+Concentration, mg/L.
The present invention analyzes Ca in hole solution2+The embodiment of concentration:
The analysis method of a kind of hole solution composition of the present invention, analyzes Ca in hole solution in accordance with the following steps2+Concentration:
(1) required reagent and medicine are prepared:
Ultra-pure water；
Loprazolam, for the preparation of leacheate under cation detection system, eluent concentration is 20mM.The storing solution that stock solution can first be made into 1M is standby, takes 100ml and be diluted to 5000ml during preparation leacheate, or takes 20ml and be diluted to 1000ml；
Ca2+Singly mark solution；
Syringe filter；
Plastic-like QC；
Filter element cap.
(2) according to cement based sample ion concentration range to be measured, the chromatographic optimized scope of coupled ion, the standard solution of 4 ~ 5 concentration levels is prepared by stepwise dilution method.Calcium ion list mark concentration: 2mg/L, 10mg/L, 20mg/L, 40mg/L, if stock solution is 100mg/L, then takes 1ml, 5ml, 10ml, 20ml stock solution respectively and is diluted to 50ml with deionized water.
(3) hole solution syringe filter with the microporous filter membrane that aperture is 0.22mm is filtered,
Drawing 0.5ml hole solution with micropipettor, ultra-pure water dilutes 200 times, shakes up as sample solution to be analyzed, is injected in quantitative loop with syringe is placed on analyzing sample solution on the specimen holder of automatic sampler according to the label of arrangement.
(4) Ca is analyzed based on ion chromatography2+Concentration: system, by going out the corresponding relation of peak area under a curve and ion concentration by time electrical conductivity, determines the ion concentration in sample according to the alignment of standard solution.
The chromatograph peak height of component to be determined in per sample or area, can calculate from standard curve and obtain corresponding dilute sample concentration.
y=n·x
Wherein, Ca in y hole solution2+Actual concentrations, mg/L；
N extension rate；
Ca in x dilute sample2+Concentration, mg/L.
Ca in hole solution is calculated according to above-mentioned formula2+Actual concentrations.
Table 1 is test Ca in the present embodiment2+Concentration results.
Table 1
The present invention analyzes the embodiment of the labor method of various compositions in hole solution:
The analysis method of a kind of hole solution composition of the present invention, comprises the steps:
(1) required reagent and medicine are prepared:
Ultra-pure water (18MW), the potassium hydroxide solution of 30mM, this solution is the leacheate under Anionic recognition system；
Loprazolam, for the preparation of leacheate under cation detection system, eluent concentration is 20mM.The storing solution that stock solution can first be made into 1M is standby, takes 100ml and be diluted to 5000ml during preparation leacheate, or takes 20ml and be diluted to 1000ml；
Standard sample, Cl-、SO4 2-、Na+、K+、Ca2+、Mg2+Dan Biao；
Syringe filter (0.22mm)；
Plastic-like QC (5ml)；
Filter element cap.
(2) according to cement based sample ion concentration range to be measured, take the optimized scope of this model chromatography of ions into consideration, prepare the standard solution of 4 ~ 5 concentration levels by stepwise dilution method.
Chloride ion list mark concentration: 5mg/l, 10mg/l, 20mg/l, 50mg/l, 100mg/l, can first be made into the stock solution of 1000mg/l, then adopt separatory method, takes 0.5ml, 1ml, 2ml, 5ml, 10ml stock solution respectively and is diluted to 100ml with deionized water；
Sulfate ion list mark concentration: 5mg/l, 10mg/l, 20mg/l, 50mg/l；If stock solution is 100mg/l, then take 1.25ml, 2.5ml, 5ml, 12.5ml stock solution respectively and be diluted to 25ml with deionized water；
Sodium ion list mark concentration: 2mg/l, 10mg/l, 20mg/l, 40mg/l, if stock solution is 100mg/l, then takes 1ml, 5ml, 10ml, 20ml stock solution respectively and is diluted to 50ml with deionized water；
Potassium ion list mark concentration: 2mg/l, 10mg/l, 20mg/l, 40mg/l, if stock solution is 100mg/l, then takes 1ml, 5ml, 10ml, 20ml stock solution respectively and is diluted to 50ml with deionized water；
Calcium ion list mark concentration: 2mg/l, 10mg/l, 20mg/l, 40mg/l, if stock solution is 100mg/l, then takes 1ml, 5ml, 10ml, 20ml stock solution respectively and is diluted to 50ml with deionized water；
Magnesium ion list mark concentration: 0.5mg/l, 1mg/l, 2mg/l, 5mg/l, if stock solution is 100mg/l, then takes 0.25ml, 0.5ml, 1ml, 2.5ml stock solution respectively and is diluted to 50ml with deionized water；
(3) collect abundant hole solution, filter by the syringe filter with the microporous filter membrane that aperture is 0.22mm；
Drawing 0.5ml hole solution with micropipettor, ultra-pure water (resistivity is more than 18M Ω) is diluted in 100ml volumetric flask, shakes up as sample solution to be analyzed；Analysis sample solution is injected in quantitative loop (can analyze multiple) with syringe simultaneously, is placed on the specimen holder of automatic sampler according to the label of arrangement,；
(4) standard solution configured and hole solution are analyzed (for DionexICS-1500 ion chromatograph) by following operating process:
The first step, confirms that the amount of solution in leacheate bottle is more than 1L, opens nitrogen cylinder switch, 0.1MPa is transferred to by dividing potential drop table；Regulate air relief valve to about 3 ~ 6psi；
Second step, opens the on and off switch of ICS-1500 main frame；
3rd step, opens automatic sampler switch；
4th step, opens computer, double-clicks Chromeleon(chameleon software) work station icon, open control panel, now workstation system and main frame are in " Remote " (remotely controlling) state automatically.In EluentLevel(leacheate level) place's input actual volume；
5th step, clicks PumpSetting(pump and arranges) button, the page clicks On(turn on pump after occurring), rotate the WasteValve(waist valve in left side counterclockwise simultaneously) start aerofluxus, click Off(after 3 minutes and close pump) close afterwards, aerofluxus terminates；Again On(turn on pump is clicked), open suppressor electric current (leacheate species concentrations can be inputted in " SignalParameter " (signal parameter) interface, system automatically calculate current value and open suppressor) simultaneously；
6th step, sets 30 ° of C of column temperature, sets pond 35 ° of C of temperature；
7th step, during system balancing, it is necessary to check that whether parameters is normal: the fluctuation of system pressure should be less than ± 10psi；The background conductance of anion should lower than 30mS；Cationic background conductance should lower than 10mS.Now can open the DataAcquisition(data acquisition on control panel), carry out baseline operation, after about 30 minutes, stop walking baseline after baseline stability, proceed by analysis test；
8th step, first the standard solution of 4 ~ 5 concentration levels of preparation is placed on specimen holder with special sample feeding pipe and filter element cap, then specimen holder is put in automatic sampler, after successively the specimen holder placing sample cell is put in automatic sampler (noting: need after analyzing 30 samples continuously again to demarcate)；
9th step, clicks Batch(batch) button, select the Sequence sequence table woven in advance, this document is that sample sequence off-balancesheet is removed in the inside with packaging file, also has relevant program file and method file.System, by going out the corresponding relation of peak area under a curve and ion concentration by time electrical conductivity, determines the ion concentration in sample according to the alignment of standard solution；
Tenth step, stops after data acquisition until system, reserves the 30min time and allows leacheate continue to flow in systems with detergent line；Click " Shutdown " (closedown) button afterwards and close closed system；
14th step, closes computer, automatic sampler, main frame, a water-adding system power supply in order, finally closes nitrogen cylinder main valve.
The chromatograph peak height of component to be determined in per sample or area, can calculate from standard curve and obtain corresponding concentration (system provides automatically).
In the analysis method of hole solution composition of the present invention, the acquisition methods of cement-based material hole solution is preferably used the present invention and obtains the device of hole solution in cement-based material, can collecting real hole solution faster, more, operational approach is simple, convenient, analyzes result accurately, reliably.
Certainly, described above is not limitation of the present invention, and the present invention is also not limited to the example above.Those skilled in the art in the essential scope of the present invention, change, remodeling, interpolation or the replacement made, also should belong to protection scope of the present invention.
Claims (9)
1. one kind obtains the device of hole solution in cement-based material, including piston, extrusion chamber, chassis and bearing, described extrusion chamber is arranged on described chassis, described chassis face arranges the collecting tank that connect internal with described extrusion chamber, described inside chassis arranges the apocenosis passage connected with described collecting tank, it is characterized in that, described apocenosis passage is obliquely installed, and the liquid outlet of described apocenosis passage is arranged on described chassis side wall.
2. the device of hole solution in the acquisition cement-based material described in claim 1, it is characterised in that described apocenosis passage is inserted into stainless steel tube, and described stainless steel tube the inner is inserted in described collecting tank, and described liquid outlet is stretched out in described stainless steel tube outer end.
3. the device of hole solution in the acquisition cement-based material described in claim 1 or 2, it is characterized in that, it is cylindrical cavity in the middle of described extrusion chamber, described chassis is disc, circular caulking groove is set in the middle part of described chassis face, described circular caulking groove diameter is consistent with the external diameter of described extrusion chamber, described extrusion chamber snaps in described circular caulking groove, described collecting tank is annular and is arranged on described circular middle part, caulking groove bottom surface, the external diameter of described annular collecting tank is identical with the internal diameter of described extrusion chamber intermediate cylindrical cavity, certain gradient is had in described collecting tank, the least significant end of described collecting tank is inserted in described stainless steel tube the inner.
4. the device of hole solution in the acquisition cement-based material described in claim 3, it is characterized in that, described piston is cylindrical, described piston upper end arranges the piston cap of cylinder, described piston cap is the diameter cylinder more than described piston diameter, described piston cap bottom surface arranges circular socket, and described piston upper end embeds in described circular socket.
5. the device of hole solution in the acquisition cement-based material described in claim 1 or 2, it is characterised in that the bottom on described chassis arranges bearing, and described bearing is cylindrical shape, and described bearing external diameter is less than the external diameter of described base.
6. the device of hole solution in the acquisition cement-based material described in claim 3, it is characterised in that the bottom on described chassis arranges bearing, and described bearing is cylindrical shape, and described bearing external diameter is less than the external diameter of described base.
7. the analysis method of a hole solution composition, it is characterised in that comprise the steps:
(1) required reagent and medicine are prepared:
Ultra-pure water；
30mM potassium hydroxide leacheate；
20mM Loprazolam leacheate；
Standard sample, including Cl-、SO4 2-、Na+、K+、Ca2+、Mg2+Ion list mark solution contained by common cement-based material hole solution；
Syringe filter；
Plastic-like QC；
Filter element cap；
(2) according to cement based sample ion concentration range to be measured, take the optimized scope of this model chromatography of ions into consideration, treat the standard solution of 4 ~ 5 concentration levels of measured ion with the preparation of stepwise dilution method；
(3) cement-based material hole solution is filtered by syringe filter, and with 1:n dilution proportion；
(4) first analyze the standard solution of 4 ~ 5 concentration levels treating measured ion, post analysis hole solution sample to be measured with ion chromatography, directly give test sample concentration；
(5) Ca in dilute sample2+Concentration and Ca in hole solution2+Actual concentrations conversion relation is as follows:
y=n·x
Wherein, Ca in y hole solution2+Actual concentrations, mg/L；
N extension rate；
Ca2+ concentration, mg/L in x dilute sample.
8. the analysis method of the hole solution composition described in claim 7, it is characterized in that, the acquisition methods of cement-based material hole solution in described step (3), the device of hole solution in cement-based material that obtains described in any one of claim 1-6 is placed on pressure testing machine centre position, put into after cylindrical test block surface is dried in described extrusion chamber, put piston, piston cap, then use hydraulic press to start pressurization；Loading speed maintains 5 ~ 6kN/s, is pressurized within the scope of 460kN ~ 750kN gradually, until cement-based material hole solution flows out, collects with polystyrene bottle.
9. the analysis method of the hole solution composition described in claim 8, it is characterized in that, the acquisition methods of cement-based material hole solution in described step (3), in order to obtain more cement-based material hole solution, slowing down loading speed when test block just starts stress until beginning to flow out cement-based material hole solution, recovering normal loading speed afterwards again.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106840796A (en) * | 2017-01-22 | 2017-06-13 | 东南大学 | A kind of low water binder ratio concrete liquid phase extraction element and method |
| CN107621483A (en) * | 2017-08-16 | 2018-01-23 | 西安建筑科技大学 | A kind of method of testing of micro concrete hole solution pH value |
| CN107702954A (en) * | 2017-08-16 | 2018-02-16 | 西安建筑科技大学 | A kind of pressing device and method of the true hole solution of micro concrete |
| CN108613895A (en) * | 2018-04-13 | 2018-10-02 | 浙江大学 | A kind of sulphate aluminium cement hardened paste Pore Solution composition measuring method |
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| CN107621483A (en) * | 2017-08-16 | 2018-01-23 | 西安建筑科技大学 | A kind of method of testing of micro concrete hole solution pH value |
| CN107702954A (en) * | 2017-08-16 | 2018-02-16 | 西安建筑科技大学 | A kind of pressing device and method of the true hole solution of micro concrete |
| CN108613895A (en) * | 2018-04-13 | 2018-10-02 | 浙江大学 | A kind of sulphate aluminium cement hardened paste Pore Solution composition measuring method |
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