CN104502407B - Isothermal-measure testing apparatus for cement initial hydration exothermic characteristic - Google Patents
Isothermal-measure testing apparatus for cement initial hydration exothermic characteristic Download PDFInfo
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- CN104502407B CN104502407B CN201410592377.0A CN201410592377A CN104502407B CN 104502407 B CN104502407 B CN 104502407B CN 201410592377 A CN201410592377 A CN 201410592377A CN 104502407 B CN104502407 B CN 104502407B
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Abstract
An isothermal-measure testing apparatus for cement initial hydration exothermic characteristic is disclosed. A sample cup of the test apparatus is put in a sample cup pool, stirring blades of a water-bath stirrer are arranged to close to radiating fins, the water-bath stirrer is eccentrically arranged in a water-bath kettle, the radiating fins of a semiconductor refrigeration/heating sheet are arranged in the water-bath kettle, one end of hydration injection water pipe is provided with a water injection port inserted by an injector, and the other end is provided with a hydration water outlet; the test apparatus comprises two thermistors, the first thermistor is at the center of the bottom of the sample cup pool and is used for sensing the sample temperature, and the second thermistor is adhered to the lower part at the outer side of the sample cup pool and is immersed into water bath and is used to sense the water bath temperature; and the temperature difference expressed by the two thermistors is taken as representation of the cement initial hydration exothermic characteristic. The test apparatus is capable of completely accurately measuring the first heat-release peak during cement initial hydration.
Description
First, technical field
The present invention relates to hydration heat of cement testing equipment technical field, specifically a kind of initial hydration of cement exothermic character etc.
The assay device of temperature measurement.
2nd, background technology
Initial hydration of cement exothermic character refers to the cement size of aquation release heat and release in 0～tens min
Speed.Found according to conventional research, cement has substantial connection in many properties of initial hydration heat characteristic and cement,
Therefore determine cement to start the exothermic character to tens min in aquation is highly important to understanding and grasping cement performance.
The hydration heat characteristic of cement refers to the size of cement release heat and the speed of release in hydration process, typically passes through
The range of temperature and rate of change of hydrated sample is showing.Conventional hydrated cementitious exothermic character metering system has three kinds,
One kind is isothermal metering system, measures in cement hydration process from sample and spills into the heat of environment, while keeping the temperature of environment
Degree is constant, and this mode obtains rate of heat release of the cement in hydration process, can calculate in specified hydration age through integration
Heat release total amount；One kind is adiabatic metering system,
The heat that cement discharges in hydration process is not outer to be dissipated, and the heat of accumulation rises sample temperature, is measured with this
The size of accumulation heat, by differential rate of heat release of the cement in hydration process can be obtained；One kind is the antipyretic survey of chemical solution
Amount mode, the heat discharged when being dissolved by some chemical reagent according to hydrated sample under each hydration age with it is unhydrated when always dissolve
Heat difference come calculate cement sample specify age under discharge accumulation heat.Chemolysis thermal measurement mode can only be measured
Compared with the hydration heat amount of long-age, and operation is relatively complicated, and chemical reagent corrosivity used are big, dangerous, therefore wait gentle thermal insulation
Both metering systems are more commonly used.
During using isothermal or adiabatic method measurement hydrated cementitious exothermic character, generally require in advance cement according to certain
The ratio of mud stirring that adds water make after cement slurry, just measure the thermal discharge size of slurry, cause stirring pulping process and dress sample
That a few minutes in cannot measure hydration heat characteristic, miss the information of the hot release characteristic of initial hydration of cement.
Heat that cement discharges during initial hydration and less, the change for causing sample temperature be not it is obvious that
Changes of hydrated cementitious sample temperature is directly turned to the sign of hydration heat characteristic, tend to be subject to ambient temperature slowly,
The impact of minor variations, therefore measurement cement, in initial hydration exothermic character, measuring instrument needs accurately temperature control and arranges
Apply.
3rd, the content of the invention
It is an object of the invention to provide a kind of assay device of the temperature measurement such as initial hydration of cement exothermic character, can be reduced
Impact of the aquation water to cement testing sample temperature during water filling, eliminates slow, the minor variations of bath temperature in measurement process
Impact to hydration heat feature measurement, first hydration heat peak that be complete, accurately measuring initial hydration of cement.
The present invention realizes above-mentioned purpose by following technical proposals method：A kind of initial hydration of cement exothermic character isothermal is surveyed
The assay device of amount, including specimen cup, aquation water outlet, specimen cup pond, stirring in water bath device, semiconductor refrigerating/heat piece,
Fin, aquation water water injection pipe, the first critesistor, the second critesistor, water filling port and water-bath kettle, semiconductor refrigerating/
Piece is heated installed in the position of the height of water-bath kettle 1/3rd, aquation water water injection pipe is placed in specimen cup pond Jing after spiralization setting
Lower section, after constant temperature enough long-time aquation coolant-temperature gage can be made to reach unanimity with testing sample temperature.Stirring in water bath device is in
It is eccentrically set in water-bath kettle, the stirring vane of stirring in water bath device is located at the lower limb of the fin contacted with water-bath but does not touch
The aquation spiral-form portion of water water injection pipe, aquation water water injection pipe one end is provided with the water filling port that can be inserted by syringe, separately
One end is provided with aquation water outlet, and the first temperature-sensitive electricity for sensing sample temperature is posted at the center of specimen cup pond inner bottom part
Resistance, the circular metal conducting strip for having a level above the critesistor is close to therewith, when specimen cup inserts specimen cup pond, should
Metal conducting strip can be in close contact with specimen cup bottom, and side-lower posts hot for sensing the second of bath temperature outside specimen cup pond
Quick resistance is simultaneously dipped in water-bath, and using the temperature difference expressed by the first critesistor and the second critesistor as initial hydration of cement
The sign of exothermic character.
The specimen cup carries specimen cup lid.
Two faces of the semiconductor refrigerating/heat piece are glued with fin, fin stretch in water-bath kettle with water
Bath contact, another fin is placed in outside water-bath kettle and is furnished with the electric fan of a direct current 12V.
The water-bath kettle bottom is provided with poppet, and the frame face of poppet is provided with hole, and specimen cup pond is through the hole and is fastened on pad
On frame, specimen cup pond top edge exposes water-bath face about 0.5cm.
The aquation water water injection pipe is the plastic material for meeting medical requirement.
Described specimen cup is in flat cylinder, is the good metal material of heat conduction, for placing testing sample.
The present invention has following outstanding advantages：
1st, in advance cement testing sample need not be prepared into slurry, aquation water is directly injected into sample when starting measurement
In, it is ensured that at the very start being capable of the temperature change that occurs because of aquation of measuring samples in hydrated cementitious.
2nd, initial hydration of cement exothermic character is measured by the way of isothermal filling aquation water, aquation water first passes through water
Bath carries out constant temperature, then just notes in cement sample, and the temperature of aquation water can be treated test sample product temperature by this mode of adding water
The impact of degree is preferably minimized.
3rd, the temperature of measuring samples and water-bath is distinguished by two critesistor, with both difference variations cement is characterized
Initial hydration exothermic character, this method can eliminate in measurement process the slow of bath temperature, minor variations to initial hydration of cement
The impact of exothermic character measurement, completely, accurately measures first hydration heat peak.
4th, illustrate
Fig. 1 is the structural representation of the assay devices of temperature measurement such as initial hydration of cement exothermic character of the present invention.
At the beginning of Fig. 2 is the assay device measurement cement using temperature measurements such as initial hydration of cement exothermic characters of the present invention
The result of beginning hydration heat characteristic.
5th, specific embodiment
Below by embodiment, the invention will be further described.
Embodiment 1
As shown in figure 1, the assay device of the temperature measurement such as initial hydration of cement exothermic character of the present invention, including sample
Cup 1, specimen cup lid 2, aquation water outlet 3, specimen cup pond 4, stirring in water bath device 5, semiconductor refrigerating/heat piece 6, radiating
Piece 7, aquation water water injection pipe 8, the first critesistor 9, the second critesistor 10, water filling port 11 and water-bath kettle 12, quasiconductor
Refrigerating/heating piece 6 is arranged on the position of the height of water-bath kettle 12 about 1/3rd, and two face has aluminium heat sink to be close to therewith
, fin 7 is stretched into and contacted with water-bath in water-bath kettle 12, another fin is placed in outside water-bath kettle and is furnished with a direct current 12V
Electric fan be used for drive away the hot or cold of the fin, three callosities are placed on water-bath kettle bottom, are provided with the frame face of poppet
The hole of suitable diameter, specimen cup pond 4 is through the hole and is fastened on poppet, and the top edge of specimen cup pond 4 exposes water-bath face about
0.5cm, aquation water water injection pipe 8 is placed in the lower section in specimen cup pond 4 Jing after spiralization setting, motor-driven by water-bath kettle top
Stirring in water bath device 5 is stretched in water-bath kettle 12, and paddle is located at the lower limb lower section of fin 7 but does not touch aquation water water injection pipe
The first critesistor 9 is posted at 8 spiral-form portion, the center of the inner bottom part of specimen cup pond 4, there is a level above the critesistor
Circular metal conducting strip be close to therewith, when specimen cup 1 inserts specimen cup pond 4, the metal conducting strip can be with the bottom of specimen cup 1
It is in close contact, the outer side-lower in specimen cup pond 4 posts the second critesistor 10 and is dipped in water-bath.The specimen cup 1 carries sample
Bowl cover 2, cement sample 13 is placed in specimen cup 1, and, near fin 7, stirring in water bath device 5 is in bias for described stirring in water bath device 5
It is arranged in water-bath kettle 12, the fin 7 of semiconductor refrigerating/heat piece 6 is placed in water-bath kettle 12, aquation water water injection pipe 8 one
End is provided with the water filling port 11 that can be inserted by syringe, and the other end is provided with aquation water outlet 3, and the critesistor is two
Only, the first critesistor 9 is located in the middle of the inner bottom part of specimen cup pond 4, and for sensing sample temperature, the second critesistor 10 is affixed on sample
The outer lower portion of product cup pond 4 is simultaneously dipped in water-bath, for sensing bath temperature, and is made with the temperature difference expressed by this two critesistor
For the sign of initial hydration of cement exothermic character.
Described specimen cup 1 is in flat cylinder, is the good metal material of heat conduction, for placing testing sample.
Near fin 7, in being eccentrically set in water-bath kettle 12, this more has stirring in water bath device 5 described stirring in water bath device 5
Being uniformly distributed beneficial to bath temperature.
Described aquation water water injection pipe 8 is twist placed in water-bath kettle 12 in the water-bath of the lower section of specimen cup pond 4, aquation
With water water injection pipe 8 using the plastic material for meeting medical requirement.
The using method of the assay devices of temperature measurement such as initial hydration of cement exothermic character of the present invention, including such as
Lower operating procedure：
(1) semiconductor refrigerating/backing 6, the power supply of stirring in water bath device 5 are opened, arranges what is needed in the range of 20～30 DEG C
Constant temperature water bath temperature, the water-bath after a period of time reaches temperature constant state, and constant-temperature precision is better than ± 0.005 DEG C；
(2) 4.00g is weighed with the balance of one of percentage precision dry by 0.080mm square hole screens, homogenizing and 65～70 DEG C/3h
Cement sample to be measured 13 after dry, during specimen cup 1 is inserted several times, is gently transferred water in the cup mud sample 13 with weighing scoop, makes cup
Interior cement sample 13 is tentatively evenly distributed, and then gently vibrates one side rotary sample cup 1 on one side on smooth desktop, makes sample in cup
Everywhere bulk density is uniform, capillary tube is evenly distributed, the cement powder fixed bed of surfacing for product formation.Weighed sample matter
Amount is selected typically in the range of 4～8g, and should fix the sample amount of weighing so that measurement result has comparability；
(3) volume markings are immersed one and fills aquation use through the syringe insertion water filling port 11 demarcated outlet 3
In the beaker of water, syringe is inserted in water filling port 11, multiple aspirating syringe is so as to without bubble in water injection pipe 8, all fill
Full water water, then that syringe pump is to the corresponding volume markings of 2.0mL and fixed, the ratio of mud now is 0.50.Will
The outlet 3 of water injection pipe removes the beaker for filling aquation water, dries the surface of outlet 3 and the inner surface of specimen cup lid 2.For
It is smoothed out cement " static state " aquation, the ratio of mud should be selected and fixed in the range of 0.40～0.60, so that measurement result
With comparability；
(4) insulation cover 2 of specimen cup 1 is covered, the bottom centre position of specimen cup pond 4 is inserted after the bottom of specimen cup 1 is cleaned,
The bottom of specimen cup 1 is contacted well with the conducting strip surface of the first critesistor 9, cover the insulation cover of water-bath kettle 12；
(5) in the state of water-bath has been enter into constant temperature, specimen cup 1 is inserted behind glass pond 4, by computer data acquiring system
Overall view examines the difference variation trend of bath temperature and cement testing sample temperature, after the constant temperature water bath of 1h or longer time,
When both temperature difference are balanced, injector piston is leggiero promoted to the end, the aquation water of respective volume is injected into be measured
In cement sample 13, cement starts aquation.
(6) cement starts after aquation, the first critesistor of balanced bridge and the bottom of electronic amplification system measuring samples cup 1
9 and the temperature difference that sensed of the second critesistor 10 for being dipped in water-bath of the outer lower portion of specimen cup pond 4, the table in the form of mV values
Up to both temperature difference, and gathered and recorded Jing after digital-to-analogue conversion by computer.The change of the mV values is used for initial hydration of cement
The sign of exothermic character.
Cement initial water is carried out using the assay device of the temperature measurements such as initial hydration of cement exothermic character of the present invention
Change the temperature measurements such as exothermic character and amount to 46min, measurement result is as shown in Figure 2.
Claims (1)
1. the assay device of the temperature measurement such as a kind of initial hydration of cement exothermic character, it is characterised in that use including specimen cup, aquation
Water outlet, specimen cup pond, stirring in water bath device, semiconductor refrigerating/heat piece, fin, aquation water water injection pipe, the first temperature-sensitive
Resistance, the second critesistor, water filling port and water-bath kettle, semiconductor refrigerating/heat piece installed in the height of water-bath kettle 1/3rd
Position, aquation water water injection pipe is placed in the lower section in specimen cup pond Jing after spiralization setting, and stirring in water bath device is in being eccentrically set on
In water-bath kettle, the stirring vane of stirring in water bath device is located at the lower limb of the fin contacted with water-bath but does not touch aquation to be noted with water
The spiral-form portion of water pipe, aquation water water injection pipe one end is provided with the water filling port that can be inserted by syringe, and the other end is provided with water
Change uses water outlet, the center of specimen cup pond inner bottom part to post the first critesistor for sensing sample temperature, the first temperature-sensitive
The circular metal conducting strip for having a level above resistance is close to therewith, when specimen cup inserts specimen cup pond, the metal heat-conducting
Piece can be in close contact with specimen cup bottom, and side-lower posts the second critesistor for sensing bath temperature simultaneously outside specimen cup pond
In being dipped in water-bath, and using the temperature difference expressed by the first critesistor and the second critesistor as initial hydration of cement exothermic character
Sign,
Two faces of the semiconductor refrigerating/heat piece are glued with fin, and a fin is stretched in water-bath kettle and connect with water-bath
Touch, another fin is placed in outside water-bath kettle and is furnished with the electric fan of a direct current 12V,
The water-bath kettle bottom is provided with poppet, and the frame face of poppet is provided with hole, and specimen cup pond is through the hole and is fastened on poppet,
Specimen cup pond top edge exposes the cm of water-bath face 0.5.
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| CN201410592377.0A CN104502407B (en) | 2014-10-28 | 2014-10-28 | Isothermal-measure testing apparatus for cement initial hydration exothermic characteristic |
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| CN201410592377.0A CN104502407B (en) | 2014-10-28 | 2014-10-28 | Isothermal-measure testing apparatus for cement initial hydration exothermic characteristic |
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| CN104458806B (en) * | 2014-10-28 | 2017-03-29 | 广西大学 | The assay device and its test method of the temperature measurements such as initial hydration of cement exothermic character |
| CN108426916A (en) * | 2018-05-07 | 2018-08-21 | 东南大学 | A kind of device and its application method measuring hydrated cementitious rate of heat release and hydration period |
| CN112445248A (en) * | 2019-08-27 | 2021-03-05 | 中国建筑材料科学研究总院有限公司 | Constant temperature control system |
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| CN104458806A (en) * | 2014-10-28 | 2015-03-25 | 广西大学 | Testing device and testing method for cement initial hydration exothermic character isothermal measurement |
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| JP3084472B2 (en) * | 1994-11-21 | 2000-09-04 | セイコーインスツルメンツ株式会社 | Humidity control type thermal analyzer |
| JP3434694B2 (en) * | 1997-12-01 | 2003-08-11 | セイコーインスツルメンツ株式会社 | Differential scanning calorimeter |
| CN2329965Y (en) * | 1998-03-16 | 1999-07-21 | 姜治邦 | Tester for cement hydration heat |
| CN101907588A (en) * | 2010-07-06 | 2010-12-08 | 长沙理工大学 | Mixed sampling device used in micro calorimeter for measuring heat of hydration of cement and other solids |
| CN102494807B (en) * | 2011-12-26 | 2013-06-05 | 上海海洋大学 | Multi-point temperature calibration device for accurately controlling temperature fluctuation of thermostatic water bath box and operation method thereof |
| CN102590263B (en) * | 2012-03-08 | 2014-01-08 | 北京工业大学 | Device and method for measuring phase change latent heat of composite phase change energy storage material |
| CN103072750A (en) * | 2013-01-23 | 2013-05-01 | 沈阳建筑大学 | Waterproof sealing device for cement hydration heat test |
| CN203490187U (en) * | 2013-10-15 | 2014-03-19 | 上海仪电物理光学仪器有限公司 | Medicament melting point apparatus testing device |
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