CN106885753B - The method that minusing measures periclase degree of hydration in cement - Google Patents
The method that minusing measures periclase degree of hydration in cement Download PDFInfo
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- CN106885753B CN106885753B CN201710183560.9A CN201710183560A CN106885753B CN 106885753 B CN106885753 B CN 106885753B CN 201710183560 A CN201710183560 A CN 201710183560A CN 106885753 B CN106885753 B CN 106885753B
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- G01N5/00—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid
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Abstract
The invention discloses the methods of periclase degree of hydration in a kind of minusing measurement cement, comprising the following steps: (1) prepares cement-hydrate to be measured；(2) preparation mixing net slurry waits for that test sample and net slurry to be measured wait for test sample；(3) mass percentage to test sample middle reaches from calcium oxide is obtained to calculate to Ca in test sample (OH)2Mass percentage；(4) the gross mass percentage composition that periclase in cement-hydrate to be measured is calculated to test sample percent weight loss is measured using thermogravimetry respectively；(5) it by cement-hydrate percent weight loss to be measured, is scaled the periclase mass percentage of aquation in cement-hydrate to be measured；(6) calculate aquation to regulation age when cement in periclase degree of hydration.The method of the present invention can accurately, effectively measure periclase degree of hydration in cement, with the presence or absence of the stability problem of MgO when convenient for more accurately evaluating high-magnesia cement aquation to a certain age.
Description
Technical field
The present invention relates to building material technical fields, more particularly to periclase aquation journey in a kind of minusing measurement cement
The method of degree.
Background technique
The study found that the periclase hydration through high-temperature calcination is very slow, it is caused during generating magnesium hydroxide
Volume expansion occurs slower.The characteristics of numerous scientific and technical personnel are according to mass concrete proposes to adopt by 30 years of researches
Concrete is set to generate body during temperature drop using the delayed microswelling characteristic of MgO concrete itself with MgO concrete technology
Product expansion, compensation temperature drop are shunk, and improve the anti-crack ability of concrete, and it is pre- wholly or largely to cancel mass concrete with realization
The conventional temperature controls measures such as cold aggregate, mix on the rocks, pre-buried cooling water pipe, jointing and blocking reach high-quality, quick, economy pours greatly
The purpose of volume concrete, therefore, high-magnesia cement obtain research and extension application.
With the presence or absence of MgO when periclase degree of hydration can evaluate hydrated cementitious to a certain age to a certain extent in cement
Stability problem.Usually calculate the degree of hydration of periclase indirectly by the measuring method of periclase mass percentage.Cause
This, the mass percentage of periclase is particularly important in accurate quantitative analysis cement or hydrated product.However, due to continuous mode
There is interference, the so far quantitative determination in the world in relation to periclase in clinker to the measurement of periclase in middle solid solution state magnesia
There are no standards to follow.The more universal periclase quantitative approach chemical method of domestic and international application mainly has BT method, ANM at present
Method, TK method etc., but these methods are not completely separated solid solution state MgO in extraction process, i.e., cannot effectively distinguish solid solution MgO
With the mass percentage of periclase.In addition to chemical method, there are also conductance methods, XRD method etc. for periclase quantitative approach.Electricity
Inducing defecation by enema and suppository is easy to be influenced by factors such as temperature, concentration, voltage, electric current, two electrode spacings and electrode insertion depths, and conductivity is surveyed
Magnitude error is larger, keeps the periclase mass percentage deviation true value of measurement larger；XRD method equally exists X-ray diffraction
The influence of instrument systematic error, the drafting of standard curve, the selection of pure object phase etc. factor equally makes the periclase quality hundred of measurement
Divide content deviation true value larger, measurement results reliability is relatively low.These methods influence periclase quality percentage to some extent and contain
The measurement true value of amount, and then cause periclase degree of hydration evaluation deviation in cement larger.
Summary of the invention
The embodiment of the present invention provides the method for periclase degree of hydration in a kind of minusing measurement cement, can it is accurate, have
Periclase degree of hydration in effect ground measurement cement, convenient for whether there is when more accurately evaluating high-magnesia cement aquation to a certain age
The stability problem of MgO.
The embodiment of the present invention provides a kind of method that minusing measures periclase degree of hydration in cement, including following step
It is rapid:
(1) prepare cement-hydrate to be measured: the cement paste for choosing aquation to regulation age tries the fresh test block in internal portion
It carries out grinding, mix, take at least 3 equal portions as cement-hydrate to be measured；
(2) preparation mixing net slurry waits for that test sample and net slurry to be measured wait for test sample: by 1 part of cement-hydrate to be measured, periclase benchmark
Substance, water are mixed evenly according to the weight ratio of a:1:b, and demoulding obtains the first examination after mixing net slurry sample is made and conserves
Block；1 part of cement-hydrate and water to be measured are mixed evenly according to the weight ratio of a:b, after net slurry sample maintenance to be measured is made
Demoulding obtains the second test block；Wherein a value is between 9~24, and b value is between 3~10；
By first test block and the second test block respectively carry out pressure steam obtain mixing net slurry wait for that test sample and net slurry to be measured wait for
Test sample；
(3) mass percentage to test sample middle reaches from calcium oxide is obtained, is calculated according to formula (I) to Ca in test sample
(OH)2Mass percentage；Described to test sample includes that cement-hydrate to be measured, mixing net slurry wait for that test sample and net slurry to be measured wait for
Test sample；
(4) percent weight loss to test sample within the scope of 300 DEG C~500 DEG C is measured using thermogravimetry respectively, according to
Formula (II) calculates the gross mass percentage composition of periclase in cement-hydrate to be measured, wherein Mg (OH)2Mass percentage
The mass percentage for being scaled MgO is included in；
Wherein: ω is the gross mass percentage composition of periclase in cement-hydrate to be measured；
ω1Ca in test sample (OH) is waited for for mixing net slurry2Mass percentage；
ω2Ca in test sample (OH) is waited for for net slurry to be measured2Mass percentage；
ω3Weightless mass percent of the test sample within the scope of 300 DEG C~500 DEG C is waited for for mixing net slurry；
ω4Weightless mass percent of the test sample within the scope of 300 DEG C~500 DEG C is waited for for net slurry to be measured；
(5) the weightless mass percent by cement-hydrate to be measured within the scope of 300 DEG C~500 DEG C, is scaled the matter of MgO
Percentage composition is measured, as the periclase mass percentage of aquation in cement-hydrate to be measured；It is calculated according to formula (III)；
Wherein: ω5For Ca (OH) in cement-hydrate to be measured2Mass percentage；
ω6For the average value of weightless mass percent of the cement-hydrate to be measured within the scope of 300 DEG C~500 DEG C；
ω7For the periclase quality mass percentage of aquation in cement-hydrate to be measured；(6) aquation to regulation age
When cement in the degree of hydration of periclase be calculated by formula (IV)；
Wherein: α be aquation to regulation age when cement in periclase degree of hydration；
ω7For the periclase mass percentage of aquation in cement-hydrate to be measured；
ω is the gross mass percentage composition of periclase in cement-hydrate to be measured.
Further, the cement-hydrate to be measured, mixing net slurry wait for test sample and net slurry to be measured wait for test sample do respectively to
Few 3 parallel determinations are averaged.
Further, it is described by first test block and the second test block respectively carry out pressure steam obtain mixing net slurry it is to be measured
Sample and net slurry to be measured wait for including the following steps: the first test block and the second test block by test sample that boiling boils 3~5 hours in water respectively, then
It pushes and steams 3~5 hours in 210 DEG C~220 DEG C temperature and/or 1.8~2.2MPa pressure；Test block exterior portion is rejected, and is chosen
Internal fresh test block progress grinding obtains mixing net slurry and waits for that test sample and net slurry to be measured wait for test sample.
Further, the time of maintenance described in step (2) is 24 hours~72 hours.
Further, the mass percentage to test sample middle reaches from calcium oxide is obtained using in GB/T 176-2008
The measurement of glycide method.
Further, the periclase primary standard substance active principle is magnesia, and fineness is 45 μm~80 μm.
According to the above aspect of the present invention, measuring method of the present invention at least can achieve following effect:
The method of periclase degree of hydration can be to avoid being dissolved the dry of state magnesia in measurement cement of the invention in cement
It disturbs, while eliminating during thermogravimetric analysis magnesium hydroxide weightlessness and calcium hydroxide weightlessness crossing instances to periclase measurement result
It influences, accuracy is high, and stability when convenient for more accurately evaluating high-magnesia cement aquation to different larval instar with the presence or absence of MgO is asked
Topic.
Specific embodiment
Present invention is further described in detail combined with specific embodiments below, but not as a limitation of the invention.
A kind of method that minusing measures periclase degree of hydration in cement, comprising the following steps:
(1) prepare cement-hydrate to be measured: the cement paste for choosing aquation to regulation age tries the fresh test block in internal portion
It carries out grinding, mix, take at least 3 equal portions as cement-hydrate to be measured；
(2) preparation mixing net slurry waits for that test sample and net slurry to be measured wait for test sample: by 1 part of cement-hydrate to be measured, periclase benchmark
Substance, water are mixed evenly according to the weight ratio of a:1:b, and demoulding obtains the first examination after mixing net slurry sample is made and conserves
Block；1 part of cement-hydrate and water to be measured are mixed evenly according to the weight ratio of a:b, after net slurry sample maintenance to be measured is made
Demoulding obtains the second test block；Wherein a value is between 9~24, and b value is between 3~10；
By first test block and the second test block respectively carry out pressure steam obtain mixing net slurry wait for that test sample and net slurry to be measured wait for
Test sample；
(3) mass percentage to test sample middle reaches from calcium oxide is obtained, is calculated according to formula (I) to Ca in test sample
(OH)2Mass percentage；Described to test sample includes that cement-hydrate to be measured, mixing net slurry wait for that test sample and net slurry to be measured wait for
Test sample；
(4) percent weight loss to test sample within the scope of 300 DEG C~500 DEG C is measured using thermogravimetry respectively, according to
Formula (II) calculates the gross mass percentage composition of periclase in cement-hydrate to be measured, wherein Mg (OH)2Mass percentage
The mass percentage for being scaled MgO is included in；
Wherein: ω is the gross mass percentage composition of periclase in cement-hydrate to be measured；
ω1Ca in test sample (OH) is waited for for mixing net slurry2Mass percentage；
ω2Ca in test sample (OH) is waited for for net slurry to be measured2Mass percentage；
ω3Weightless mass percent of the test sample within the scope of 300 DEG C~500 DEG C is waited for for mixing net slurry；
ω4Weightless mass percent of the test sample within the scope of 300 DEG C~500 DEG C is waited for for net slurry to be measured；
(5) the weightless mass percent by cement-hydrate to be measured within the scope of 300 DEG C~500 DEG C, is scaled the matter of MgO
Percentage composition is measured, as the periclase mass percentage of aquation in cement-hydrate to be measured；It is calculated according to formula (III)；
Wherein: ω5For Ca (OH) in cement-hydrate to be measured2Mass percentage；
ω6For the average value of weightless mass percent of the cement-hydrate to be measured within the scope of 300 DEG C~500 DEG C；
ω7For the periclase quality mass percentage of aquation in cement-hydrate to be measured；(6) aquation to regulation age
When cement in the degree of hydration of periclase be calculated by formula (IV)；
Wherein: α be aquation to regulation age when cement in periclase degree of hydration；
ω7For the periclase mass percentage of aquation in cement-hydrate to be measured；
ω is the gross mass percentage composition of periclase in cement-hydrate to be measured.
Use " pressure steams test " method of the invention, it is ensured that the complete aquation of periclase in cement-hydrate to be measured；
Using " pressure steams test and thermogravimetry combines " method, it is possible to prevente effectively from being dissolved state magnesia in cement-hydrate to be measured
Interference；It, can simultaneously using the minusing of " magnesium hydroxide and calcium hydroxide resultant and calcium hydroxide mass percentage subtract each other "
To effectively eliminate during thermogravimetric analysis magnesium hydroxide weightlessness and calcium hydroxide weightlessness crossing instances to periclase measurement result
It influences.The method accuracy of periclase degree of hydration is high in minusing measurement cement of the invention, high convenient for more accurately evaluation
With the presence or absence of the stability problem of MgO when magnesium hydrated cementitious is to different larval instar.
Above scheme can complete the measurement of periclase degree of hydration in cement, provide preferred side on this basis
Case:
Preferably, the cement-hydrate to be measured, mixing net slurry wait for test sample and net slurry to be measured wait for test sample do respectively to
Few 3 parallel determinations are averaged.
Preferably, it is described by first test block and the second test block respectively carry out pressure steam obtain mixing net slurry it is to be measured
Sample and net slurry to be measured wait for including the following steps: the first test block and the second test block by test sample that boiling boils 3~5 hours in water respectively, then
It pushes and steams 3~5 hours in 210 DEG C~220 DEG C temperature and/or 1.8~2.2MPa pressure；Test block exterior portion is rejected, and is chosen
Internal fresh test block progress grinding obtains mixing net slurry and waits for that test sample and net slurry to be measured wait for test sample.
Preferably, the time of maintenance described in step (2) is 24 hours~72 hours.
Preferably, obtaining the mass percentage to test sample middle reaches from calcium oxide using in GB/T 176-2008
The measurement of glycide method.
Preferably, the periclase primary standard substance active principle is magnesia, fineness is 45 μm~80 μm.It is prepared
Method is as follows:
(1) calcination 30min~120min obtains calcination sample under conditions of magnesia raw material being placed in 900 DEG C~1400 DEG C；
(2) the calcination sample is cooled to room temperature in 5min~30min；
(3) calcination sample grinding after cooling is obtained into periclase primary standard substance to 45 μm~80 μm.
Wherein, magnesia raw material are one or more of group such as magnesium carbonate, magnesium phosphate, magnesium sulfate, magnesium silicate, magnesium hydroxide
It closes.Magnesia material purity is chemical pure or excellent pure grade.
Embodiment 1-3 high-magnesia cement quantitative determines important parameter
3 kinds of difference MgO mass hundred that 1-3 of the embodiment of the present invention uses Jia Hua special cement limited liability company to produce respectively
Periclase water in cement when the low-heat portland cement of point content (being followed successively by 4.27%, 4.92%, 5.71%) carries out aquation 1 year
The quantitative determination of change degree.1-3 high-magnesia cement of embodiment of the present invention quantitative determination important parameter is shown in Table 1.
1 high-magnesia cement of table quantitative determines important parameter
Compared with the prior art, the advantages of the present invention are as follows: the side of periclase degree of hydration in measurement cement of the invention
Method can be to avoid the interference of solid solution state magnesia in cement, while eliminating magnesium hydroxide endothermic peak and hydrogen-oxygen during thermogravimetric analysis
Change the influence of calcium endothermic peak cross-pair periclase measurement result, accuracy is high, arrives convenient for more accurately evaluating high-magnesia cement aquation
With the presence or absence of the stability problem of MgO when different larval instar.
Illustrate: content, percentage composition and percentage mentioned in the present invention etc., in the case where not clearly indicating,
It is defaulted as mass percentage.
Above embodiments are only exemplary embodiment of the present invention, are not used in the limitation present invention, protection scope of the present invention
It is defined by the claims.Those skilled in the art can within the spirit and scope of the present invention make respectively the present invention
Kind modification or equivalent replacement, this modification or equivalent replacement also should be regarded as being within the scope of the present invention.
Claims (6)
1. a kind of method of periclase degree of hydration in minusing measurement cement, it is characterised in that: the following steps are included:
(1) prepare cement-hydrate to be measured: the cement paste for choosing aquation to regulation age tries the fresh test block in internal portion and carries out
Grinding, mixing take at least 3 equal portions as cement-hydrate to be measured；
(2) preparation mixing net slurry waits for that test sample and net slurry to be measured wait for test sample: by 1 part of cement-hydrate to be measured, periclase primary standard substance,
Water is mixed evenly according to the weight ratio of a:1:b, and demoulding obtains the first test block after mixing net slurry sample is made and conserves；By 1
Part cement-hydrate to be measured and water are mixed evenly according to the weight ratio of a:b, demould after net slurry sample maintenance to be measured is made
To the second test block；Wherein a value is between 9~24, and b value is between 3~10；
By first test block and the second test block respectively carry out pressure steam obtain mixing net slurry wait for that test sample and net slurry to be measured wait for test sample；
(3) mass percentage to test sample middle reaches from calcium oxide is obtained, is calculated according to formula (I) to Ca in test sample (OH)2
Mass percentage；Described to test sample includes that cement-hydrate to be measured, mixing net slurry wait for that test sample and net slurry to be measured wait for test sample；
(4) percent weight loss to test sample within the scope of 300 DEG C~500 DEG C is measured using thermogravimetry respectively, according to formula
(II) the gross mass percentage composition of periclase in cement-hydrate to be measured is calculated, wherein Mg (OH)2Mass percentage conversion
It is included in for the mass percentage of MgO；
Wherein: ω is the gross mass percentage composition of periclase in cement-hydrate to be measured；
ω1Ca in test sample (OH) is waited for for mixing net slurry2Mass percentage；
ω2Ca in test sample (OH) is waited for for net slurry to be measured2Mass percentage；
ω3Weightless mass percent of the test sample within the scope of 300 DEG C~500 DEG C is waited for for mixing net slurry；
ω4Weightless mass percent of the test sample within the scope of 300 DEG C~500 DEG C is waited for for net slurry to be measured；
(5) the weightless mass percent by cement-hydrate to be measured within the scope of 300 DEG C~500 DEG C is scaled the quality hundred of MgO
Point content, as the periclase mass percentage of aquation in cement-hydrate to be measured；It is calculated according to formula (III)；
Wherein: ω5For Ca (OH) in cement-hydrate to be measured2Mass percentage；
ω6For the average value of weightless mass percent of the cement-hydrate to be measured within the scope of 300 DEG C~500 DEG C；
ω7For the periclase mass percentage of aquation in cement-hydrate to be measured；(6) aquation to regulation age when cement in
The degree of hydration of periclase is calculated by formula (IV)；
Wherein: α be aquation to regulation age when cement in periclase degree of hydration；
ω7For the periclase mass percentage of aquation in cement-hydrate to be measured；
ω is the gross mass percentage composition of periclase in cement-hydrate to be measured.
2. the method for periclase degree of hydration in minusing measurement cement according to claim 1, which is characterized in that described
Cement-hydrate to be measured, mixing net slurry wait for that test sample and net slurry to be measured wait for that test sample does at least 3 times parallel determinations respectively and is averaged.
3. the method for periclase degree of hydration in minusing measurement cement according to claim 1, which is characterized in that described
By first test block and the second test block respectively carry out pressure steam obtain mixing net slurry wait for that test sample and net slurry to be measured wait for test sample packet
Include following steps: boiling boils 3~5 hours in water respectively for the first test block and the second test block, then 210 DEG C~220 DEG C temperature and/
Or 1.8~2.2MPa pressure is pushed and is steamed 3~5 hours；Test block exterior portion is rejected, and chooses internal fresh test block and carries out grinding
It obtains mixing net slurry and waits for that test sample and net slurry to be measured wait for test sample.
4. the method for periclase degree of hydration in minusing measurement cement according to claim 1, which is characterized in that step
(2) time of maintenance described in is 24 hours~72 hours.
5. the method for periclase degree of hydration in minusing measurement cement according to claim 1, which is characterized in that obtain
The mass percentage to test sample middle reaches from calcium oxide is using glycide method measurement in GB/T 176-2008.
6. the method for periclase degree of hydration in minusing measurement cement according to claim 1, which is characterized in that described
Periclase primary standard substance active principle be magnesia, fineness be 45 μm~80 μm.
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| CN109374613B (en) * | 2018-11-27 | 2021-06-04 | 湖北建研科峰工程质量检测有限公司 | Method for detecting content of periclase in cement clinker |
| CN111537384B (en) * | 2020-04-24 | 2023-02-03 | 中铁（天津）隧道工程勘察设计有限公司 | Method for determining hydration degree of gypsum rock |
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