CN106885753A - The method that minusing determines periclase degree of hydration in cement - Google Patents
The method that minusing determines periclase degree of hydration in cement Download PDFInfo
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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 a kind of method that minusing determines periclase degree of hydration in cement, comprise the following steps：(1) cement-hydrate to be measured is prepared；(2) prepare the net slurry of mixing and treat that test sample and net slurry to be measured treat test sample；(3) treat that test sample middle reaches calculate from the weight/mass percentage composition of calcium oxide described in obtaining and treat Ca (OH) in test sample2Weight/mass percentage composition；(4) determined respectively using thermogravimetry and treat test sample percent weight loss, calculate the gross mass percentage composition of periclase in cement-hydrate to be measured；(5) by cement-hydrate percent weight loss to be measured, it is scaled the periclase weight/mass percentage composition of aquation in cement-hydrate to be measured；(6) aquation to the degree of hydration of periclase in cement during regulation age is calculated.The inventive method can accurately, effectively determine periclase degree of hydration in cement, be easy to more accurately evaluate high-magnesia cement aquation to stability problem during a certain age with the presence or absence of MgO.
Description
Technical field
The present invention relates to building material technical field, more particularly to a kind of minusing determines periclase aquation journey in cement
The method of degree.
Background technology
Research finds that the periclase hydration through high-temperature calcination is very slow, causes during magnesium hydroxide is generated
Volumetric expansion occurs slower.Numerous scientific and technical personnel, by 30 years of researches, propose to adopt according to the characteristics of mass concrete
MgO concrete technologies are used, using the delayed microswelling characteristic of MgO concrete itself, makes concrete that body is produced during temperature drop
Product expands, and compensation temperature drop shrinks, and improves the anti-crack ability of concrete, to realize that wholly or largely cancellation mass concrete is pre-
The conventional temperature control measures such as cold aggregate, mix on the rocks, pre-buried cooling water pipe, jointing and blocking, reach high-quality, quick, economy and pour greatly
The purpose of volume concrete, therefore, high-magnesia cement obtains research and extension application.
In cement periclase degree of hydration can evaluate to a certain extent hydrated cementitious to during a certain age whether there is MgO
Stability problem.Generally the degree of hydration of periclase is calculated indirectly by the assay method of periclase weight/mass percentage composition.Cause
This, the weight/mass percentage composition of periclase is particularly important in accurate quantitative analysis cement or hydrated product.However, due to continuous mode
There is interference in middle solid solution state magnesia, to the measure of periclase so far in the world about the quantitative determination of periclase in clinker
Also no standard can be followed.The current more universal periclase quantitative approach chemical method of domestic and international application mainly has BT methods, ANM
Method, TK methods etc., but these methods are not completely separated solid solution state MgO in extraction process, i.e., can not effectively distinguish solid solution MgO
With the weight/mass percentage composition of periclase.In addition to chemical method, periclase quantitative approach also has conductance method, XRD method etc..Electricity
Inducing defecation by enema and suppository is easily influenceed by factors such as temperature, concentration, voltage, electric current, two electrode spacings and electrode insertion depths, and electrical conductivity is surveyed
Value error is larger, makes the periclase weight/mass percentage composition deviation true value of measurement larger；XRD method equally exists X-ray diffraction
The influence of instrument system error, the drafting of standard curve, the selection of pure thing phase etc. factor, equally makes the periclase quality hundred of measurement
Point content deviation true value is larger, and measurement results reliability is relatively low.These methods influence periclase quality percentage to contain to some extent
The measure true value of amount, and then it is larger to cause periclase degree of hydration in cement to evaluate deviation.
The content of the invention
The embodiment of the present invention provides a kind of method that minusing determines periclase degree of hydration in cement, can accurately, have
Effect ground determines periclase degree of hydration in cement, is easy to 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 determines periclase degree of hydration in cement, including following step
Suddenly：
(1) cement-hydrate to be measured is prepared：Choose aquation and try the fresh test block in internal portion to the cement paste of regulation age
Carry out grinding, mix, take at least 3 equal portions as cement-hydrate to be measured；
(2) prepare the net slurry of mixing and treat that test sample and net slurry to be measured treat test sample：By 1 part of cement-hydrate to be measured, periclase benchmark
Material, water are according to a:1:Than mixing and stirring, the demoulding obtains the first examination to the weight of b after the net slurry samples of mixing and maintenance is obtained
Block；By 1 part of cement-hydrate to be measured and water according to a:The weight of b than mixing and stirring, after net slurry samples maintenance to be measured is obtained
The demoulding obtains the second test block；Between 9~24, b values are between 3~10 for wherein a values；
Described the first test block and the second test block carried out into pressure steaming respectively obtain mixing net slurry to treat that test sample and net slurry to be measured are treated
Test sample；
(3) weight/mass percentage composition of the test sample middle reaches from calcium oxide is treated described in obtaining, is calculated according to formula (I) and is treated Ca in test sample
(OH)2Weight/mass percentage composition；Described treats that test sample includes that the net slurry of cement-hydrate to be measured, mixing treats that test sample and net slurry to be measured are treated
Test sample；
(4) percent weight loss for treating test sample in the range of 300 DEG C~500 DEG C is determined respectively using thermogravimetry, according to
Formula (II) calculates the gross mass percentage composition of periclase in cement-hydrate to be measured, wherein Mg (OH)2Weight/mass percentage composition
The weight/mass percentage composition for being scaled MgO is counted；
Wherein：ω is the gross mass percentage composition of periclase in cement-hydrate to be measured；
ω1Starched for mixing is net and treat Ca (OH) in test sample2Weight/mass percentage composition；
ω2For net slurry to be measured treats Ca (OH) in test sample2Weight/mass percentage composition；
ω3For the net slurry of mixing treats weightless mass percent of the test sample in the range of 300 DEG C~500 DEG C；
ω4For net slurry to be measured treats weightless mass percent of the test sample in the range of 300 DEG C~500 DEG C；
(5) the weightless mass percent by cement-hydrate to be measured in the range of 300 DEG C~500 DEG C, is scaled the matter of MgO
Amount percentage composition, as the periclase weight/mass percentage composition of aquation in cement-hydrate to be measured；Calculated according to formula (III)；
Wherein：ω5It is Ca (OH) in cement-hydrate to be measured2Weight/mass percentage composition；
ω6It is the average value of weightless mass percent of the cement-hydrate to be measured in the range of 300 DEG C~500 DEG C；
ω7It is the periclase quality weight/mass percentage composition of aquation in cement-hydrate to be measured；(6) aquation to regulation age
When cement in the degree of hydration of periclase calculated by formula (IV)；
Wherein：α is degree of hydration of the aquation to periclase in cement during regulation age；
ω7It is the periclase weight/mass percentage composition of aquation in cement-hydrate to be measured；
ω is the gross mass percentage composition of periclase in cement-hydrate to be measured.
Further, described cement-hydrate to be measured, the net slurry of mixing treat test sample and net slurry to be measured treat test sample do respectively to
Few 3 parallel determinations are averaged.
Further, it is described described the first test block and the second test block are carried out pressure steaming respectively to obtain mixing to starch to be measured only
Sample and net slurry to be measured treat that test sample comprises the following steps：Boiling boils 3~5 hours in water respectively for first test block and the second test block, then
Steaming is pushed in 210 DEG C~220 DEG C temperature and/or 1.8~2.2MPa pressure 3~5 hours；Test block Outboard Sections are rejected, and is chosen
Internal fresh test block carries out grinding and obtains mixing net slurry to treat that test sample and net slurry to be measured treat test sample.
Further, the time for being conserved described in step (2) is 24 hours~72 hours.
Further, treat weight/mass percentage composition of the test sample middle reaches from calcium oxide using in GB/T 176-2008 described in obtaining
Glycide method is determined.
Further, described periclase primary standard substance active principle is magnesia, and fineness is 45 μm~80 μm.
By such scheme, assay method of the present invention can at least reach following effect：
The method of periclase degree of hydration can avoid the dry of solid solution state magnesia in cement in measure cement of the invention
Disturb, while eliminating, magnesium hydroxide during thermogravimetric analysis is weightless and calcium hydroxide weightlessness crossing instances are to periclase measurement result
Influence, accuracy is high, is easy to more accurately to evaluate high-magnesia cement aquation and is asked to stability during different larval instar with the presence or absence of MgO
Topic.
Specific embodiment
The present invention is described in further detail with reference to specific embodiment, but it is not as a limitation of the invention.
A kind of method that minusing determines periclase degree of hydration in cement, comprises the following steps：
(1) cement-hydrate to be measured is prepared：Choose aquation and try the fresh test block in internal portion to the cement paste of regulation age
Carry out grinding, mix, take at least 3 equal portions as cement-hydrate to be measured；
(2) prepare the net slurry of mixing and treat that test sample and net slurry to be measured treat test sample：By 1 part of cement-hydrate to be measured, periclase benchmark
Material, water are according to a:1:Than mixing and stirring, the demoulding obtains the first examination to the weight of b after the net slurry samples of mixing and maintenance is obtained
Block；By 1 part of cement-hydrate to be measured and water according to a:The weight of b than mixing and stirring, after net slurry samples maintenance to be measured is obtained
The demoulding obtains the second test block；Between 9~24, b values are between 3~10 for wherein a values；
Described the first test block and the second test block carried out into pressure steaming respectively obtain mixing net slurry to treat that test sample and net slurry to be measured are treated
Test sample；
(3) weight/mass percentage composition of the test sample middle reaches from calcium oxide is treated described in obtaining, is calculated according to formula (I) and is treated Ca in test sample
(OH)2Weight/mass percentage composition；Described treats that test sample includes that the net slurry of cement-hydrate to be measured, mixing treats that test sample and net slurry to be measured are treated
Test sample；
(4) percent weight loss for treating test sample in the range of 300 DEG C~500 DEG C is determined respectively using thermogravimetry, according to
Formula (II) calculates the gross mass percentage composition of periclase in cement-hydrate to be measured, wherein Mg (OH)2Weight/mass percentage composition
The weight/mass percentage composition for being scaled MgO is counted；
Wherein：ω is the gross mass percentage composition of periclase in cement-hydrate to be measured；
ω1Starched for mixing is net and treat Ca (OH) in test sample2Weight/mass percentage composition；
ω2For net slurry to be measured treats Ca (OH) in test sample2Weight/mass percentage composition；
ω3For the net slurry of mixing treats weightless mass percent of the test sample in the range of 300 DEG C~500 DEG C；
ω4For net slurry to be measured treats weightless mass percent of the test sample in the range of 300 DEG C~500 DEG C；
(5) the weightless mass percent by cement-hydrate to be measured in the range of 300 DEG C~500 DEG C, is scaled the matter of MgO
Amount percentage composition, as the periclase weight/mass percentage composition of aquation in cement-hydrate to be measured；Calculated according to formula (III)；
Wherein：ω5It is Ca (OH) in cement-hydrate to be measured2Weight/mass percentage composition；
ω6It is the average value of weightless mass percent of the cement-hydrate to be measured in the range of 300 DEG C~500 DEG C；
ω7It is the periclase quality weight/mass percentage composition of aquation in cement-hydrate to be measured；(6) aquation to regulation age
When cement in the degree of hydration of periclase calculated by formula (IV)；
Wherein：α is degree of hydration of the aquation to periclase in cement during regulation age；
ω7It is the periclase weight/mass percentage composition of aquation in cement-hydrate to be measured；
ω is the gross mass percentage composition of periclase in cement-hydrate to be measured.
It is of the invention to use " pressure steams experiment " method, it is ensured that the complete aquation of periclase in cement-hydrate to be measured；
Using " pressure steams experiment and thermogravimetry is combined " method, it is possible to prevente effectively from solid solution state magnesia in cement-hydrate to be measured
Interference；Simultaneously using the minusing of " magnesium hydroxide and calcium hydroxide resultant are subtracted each other with calcium hydroxide weight/mass percentage composition ", can
Effectively to eliminate, magnesium hydroxide during thermogravimetric analysis is weightless and calcium hydroxide weightlessness crossing instances are to periclase measurement result
Influence.The method accuracy that minusing of the invention determines periclase degree of hydration in cement is high, is easy to more accurately evaluate height
Magnesium hydrated cementitious are to stability problem during different larval instar with the presence or absence of MgO.
Above scheme can complete the measure of periclase degree of hydration in cement, and preferred side is given on this basis
Case：
Preferably, described cement-hydrate to be measured, the net slurry of mixing treat test sample and net slurry to be measured treat test sample do respectively to
Few 3 parallel determinations are averaged.
Preferably, described described the first test block and the second test block to be carried out pressure steaming respectively obtain mixing to starch to be measured only
Sample and net slurry to be measured treat that test sample comprises the following steps：Boiling boils 3~5 hours in water respectively for first test block and the second test block, then
Steaming is pushed in 210 DEG C~220 DEG C temperature and/or 1.8~2.2MPa pressure 3~5 hours；Test block Outboard Sections are rejected, and is chosen
Internal fresh test block carries out grinding and obtains mixing net slurry to treat that test sample and net slurry to be measured treat test sample.
Preferably, the time conserved described in step (2) is 24 hours~72 hours.
Preferably, treating weight/mass percentage composition of the test sample middle reaches from calcium oxide using in GB/T 176-2008 described in obtaining
Glycide method is determined.
Preferably, described 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 into 900 DEG C~1400 DEG C；
(2) described calcination sample is cooled to room temperature in 5min~30min；
(3) by the calcination sample grinding after cooling to 45 μm~80 μm, that is, periclase primary standard substance is obtained.
Wherein, magnesia raw material are the groups of one or more such as magnesium carbonate, magnesium phosphate, magnesium sulfate, magnesium silicate, magnesium hydroxide
Close.Magnesia material purity is chemical pure or top pure grade.
Embodiment 1-3 high-magnesia cement quantitative determines important parameter
3 kinds of difference MgO mass hundred that embodiment of the present invention 1-3 is produced using Jia Hua special cements limited company respectively
The low-heat portland cement of point content (being followed successively by 4.27%, 4.92%, 5.71%) carries out during aquation 1 year periclase water in cement
The quantitative determination of change degree.Embodiment of the present invention 1-3 high-magnesia cement quantitative determination important parameter is shown in Table 1.
The high-magnesia cement of table 1 quantitative determines important parameter
Compared with prior art, the advantage of the invention is that：The side of periclase degree of hydration in measure cement of the invention
Method can 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, be easy to more accurately to evaluate high-magnesia cement aquation and arrive
With the presence or absence of the stability problem of MgO during different larval instar.
Explanation：Content, percentage composition and percentage for being mentioned in the present invention etc., in the case where not clearly indicating,
It is defaulted as weight/mass percentage composition.
Above example is only exemplary embodiment of the invention, is 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 make respectively in essence of the invention and protection domain to the present invention
Modification or equivalent are planted, this modification or equivalent also should be regarded as being within the scope of the present invention.
Claims (6)
1. a kind of method that minusing determines periclase degree of hydration in cement, it is characterised in that：Comprise the following steps：
(1) cement-hydrate to be measured is prepared：Choose aquation is carried out to the fresh test block in the internal portion of cement paste examination of regulation age
Grinding, mixing, take at least 3 equal portions as cement-hydrate to be measured；
(2) prepare the net slurry of mixing and treat that test sample and net slurry to be measured treat test sample：By 1 part of cement-hydrate to be measured, periclase primary standard substance,
Water is according to a:1:Than mixing and stirring, the demoulding obtains the first test block to the weight of b after the net slurry samples of mixing and maintenance is obtained；By 1
Part cement-hydrate to be measured is with water according to a:Than mixing and stirring, the demoulding is obtained the weight of b after net slurry samples maintenance to be measured is obtained
To the second test block；Between 9~24, b values are between 3~10 for wherein a values；
Described the first test block and the second test block carried out into pressure steaming respectively obtain mixing net slurry to treat that test sample and net slurry to be measured treat test sample；
(3) weight/mass percentage composition of the test sample middle reaches from calcium oxide is treated described in obtaining, is calculated according to formula (I) and is treated Ca (OH) in test sample2
Weight/mass percentage composition；Described treats that test sample includes that the net slurry of cement-hydrate to be measured, mixing treats that test sample and net slurry to be measured treat test sample；
(4) percent weight loss for treating test sample in the range of 300 DEG C~500 DEG C is determined respectively using thermogravimetry, according to formula
(II) the gross mass percentage composition of periclase in cement-hydrate to be measured, wherein Mg (OH) are calculated2Weight/mass percentage composition conversion
For the weight/mass percentage composition of MgO is counted；
Wherein：ω is the gross mass percentage composition of periclase in cement-hydrate to be measured；
ω1Starched for mixing is net and treat Ca (OH) in test sample2Weight/mass percentage composition；
ω2For net slurry to be measured treats Ca (OH) in test sample2Weight/mass percentage composition；
ω3For the net slurry of mixing treats weightless mass percent of the test sample in the range of 300 DEG C~500 DEG C；
ω4For net slurry to be measured treats weightless mass percent of the test sample in the range of 300 DEG C~500 DEG C；
(5) the weightless mass percent by cement-hydrate to be measured in the range of 300 DEG C~500 DEG C, is scaled the quality hundred of MgO
Point content, as the periclase weight/mass percentage composition of aquation in cement-hydrate to be measured；Calculated according to formula (III)；
Wherein：ω5It is Ca (OH) in cement-hydrate to be measured2Weight/mass percentage composition；
ω6It is the average value of weightless mass percent of the cement-hydrate to be measured in the range of 300 DEG C~500 DEG C；
ω7It is the periclase quality weight/mass percentage composition of aquation in cement-hydrate to be measured；(6) aquation to regulation age when water
The degree of hydration of periclase is calculated by formula (IV) in mud；
Wherein：α is degree of hydration of the aquation to periclase in cement during regulation age；
ω7It is the periclase weight/mass percentage composition 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 that minusing according to claim 1 determines periclase degree of hydration in cement, it is characterised in that described
Cement-hydrate to be measured, the net slurry of mixing treat that test sample and net slurry to be measured treat that test sample does at least 3 times parallel determinations and averages respectively.
3. the method that minusing according to claim 1 determines periclase degree of hydration in cement, it is characterised in that described
The pressure steaming that carries out described the first test block and the second test block respectively obtain mixing net slurry and treat that test sample and net slurry to be measured treat test sample bag
Include following steps：Boiling boils 3~5 hours in water respectively for first test block and the second test block, then 210 DEG C~220 DEG C temperature and/
Or 1.8~2.2MPa pressure pushes steaming 3~5 hours；Rejecting test block Outboard Sections, and choose internal fresh test block carries out grinding
Obtain mixing slurry only and treat that test sample and net slurry to be measured treat test sample.
4. the method that minusing according to claim 1 determines periclase degree of hydration in cement, it is characterised in that step
(2) time conserved described in is 24 hours~72 hours.
5. the method that minusing according to claim 1 determines periclase degree of hydration in cement, it is characterised in that obtain
It is described to treat that test sample middle reaches are determined from the weight/mass percentage composition of calcium oxide using glycide method in GB/T 176-2008.
6. the method that minusing according to claim 1 determines periclase degree of hydration in cement, it is characterised in that described
Periclase primary standard substance active principle be magnesia, fineness be 45 μm~80 μm.
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| CN111537384A (en) * | 2020-04-24 | 2020-08-14 | 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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