CN106969996B - The method that minusing quantitative determines periclase mass percentage in cement - Google Patents
The method that minusing quantitative determines periclase mass percentage in cement Download PDFInfo
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Abstract
The invention discloses the methods of periclase mass percentage in a kind of minusing quantitative determination cement, comprising the following steps: (1) prepare blended cement net slurry and wait for that test sample and cement paste to be measured wait for test sample: (2) obtain the mass percentage to test sample middle reaches from calcium oxide and calculate to Ca in test sample (OH)2Mass percentage；(3) percent weight loss to test sample is measured using thermogravimetry respectively, calculates the mass percentage of periclase in cement to be measured.The method of the present invention, which can accurately, effectively quantify periclase mass percentage in cement, convenient for more accurately evaluating the expansion characteristics of high-magnesia cement makes it meet different engineerings to its expansile requirement.
Description
Technical field
The present invention relates to periclase quality in building material technical field more particularly to a kind of minusing quantitative determination cement
The method of percentage composition.
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.
MgO exists in the form of two kinds to be dissolved and dissociate in clinker.Wherein solid solution state MgO is without expansion, with free
MgO existing for crystal habit (also referred to as periclase), own vol can expand about 117% in slow hydration process, have the later period
Micro-expansibility.Therefore, the late expansion characteristic of accurate evaluation high-magnesia cement, it is necessary to which periclase in high-magnesia cement is quantified.
There is interference to the measurement of periclase due to being dissolved state magnesia in continuous mode, so far in the world in relation to magnesium square in clinker
There are no standards to follow for the quantitative determination of stone.The more universal periclase quantitative approach chemical method of domestic and international application is main at present
There are BT method, ANM method, TK method etc., but these methods are not completely separated solid solution state MgO in extraction process, i.e., it cannot be effective
Distinguish the mass percentage of solid solution MgO and periclase.In addition to chemical method, there are also conductance methods, XRD for periclase quantitative approach
Method etc..Conductance method is easy the shadow by factors such as temperature, concentration, voltage, electric current, two electrode spacings and electrode insertion depths
It rings, conductivity measurements error is larger, keeps the periclase mass percentage deviation true value of measurement larger；XRD method is equally deposited
In the influence of X-ray diffractometer systematic error, the drafting of standard curve, the selection of pure object phase etc. factor, equally make measurement
Periclase mass percentage deviation true value is larger, and measurement results reliability is relatively low.
Summary of the invention
The embodiment of the present invention provides the method for periclase mass percentage in a kind of minusing quantitative determination cement, can be with
The mass percentage of periclase in cement is accurately, effectively quantified, convenient for more accurately evaluating the expansion characteristics of high-magnesia cement,
It is set to meet different engineerings to its expansile requirement.
The embodiment of the present invention provides a kind of method that minusing quantitative determines periclase mass percentage in cement, including
Following steps:
(1) it prepares blended cement net slurry and waits for that test sample and cement paste to be measured wait for test sample: by 1 part of cement to be measured, periclase base
Quasi- substance, water are mixed evenly according to the weight ratio of a:1:b, and demoulding obtains the after blended cement net slurry sample is made and conserves
One test block；1 part of cement and water to be measured are mixed evenly according to the weight ratio of a:b, cement paste sample maintenance to be measured is made
Demoulding obtains the second test block afterwards；Wherein a value is between 9~24, and b value is between 3~10；
It first test block and the second test block is carried out to pressure steams to obtain blended cement net slurry and wait for test sample and water to be measured respectively
Cement paste waits for test sample；
(2) 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 includes that blended cement net slurry waits for that test sample and cement paste to be measured wait for test sample to test sample；
(3) 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 mass percentage of periclase in cement to be measured；
Wherein: ω is the mass percentage of periclase in cement to be measured；
ω1Ca in test sample (OH) is waited for for blended cement net slurry2Mass percentage；
ω2Ca in test sample (OH) is waited for for cement paste 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 blended cement net slurry；
ω4Weightless mass percent of the test sample within the scope of 300 DEG C~500 DEG C is waited for for cement paste to be measured.
Further, the blended cement net slurry waits for that test sample and cement paste to be measured wait for that test sample does at least 3 times respectively and puts down
Row measurement is averaged.
Further, described to carry out first test block and the second test block respectively to press to steam obtaining blended cement net slurry
Wait for including the following steps: the first test block and the second test block by test sample that boil 3~5 small for boiling in water respectively to test sample and cement paste to be measured
When, it then 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 it chooses internal fresh test block and carries out grinding and obtain blended cement net slurry waiting for that test sample and cement paste to be measured wait for test sample.
Further, the time of maintenance described in step (1) 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.
It at least can achieve following effect by above scheme the method for the present invention:
The method of periclase mass percentage can be to avoid solid solution state oxygen in cement in quantitative determination cement of the invention
Change the interference of magnesium, while eliminating magnesium hydroxide weightlessness and calcium hydroxide weightlessness crossing instances during thermogravimetric analysis and periclase is surveyed
Determine the influence of result, accuracy is high, convenient for more accurately evaluating the expansion characteristics of cement, instructs the practical application of cement in engineering
Demand.
Specific embodiment
Present invention is further described in detail combined with specific embodiments below, but not as a limitation of the invention.
The embodiment of the present invention provides a kind of method that minusing quantitative determines periclase mass percentage in cement, including
Following steps:
(1) it prepares blended cement net slurry and waits for that test sample and cement paste to be measured wait for test sample: by 1 part of cement to be measured, periclase base
Quasi- substance, water are mixed evenly according to the weight ratio of a:1:b, and demoulding obtains the after blended cement net slurry sample is made and conserves
One test block；1 part of cement and water to be measured are mixed evenly according to the weight ratio of a:b, cement paste sample maintenance to be measured is made
Demoulding obtains the second test block afterwards；Wherein a value is between 9~24, and b value is between 3~10；
It first test block and the second test block is carried out to pressure steams to obtain blended cement net slurry and wait for test sample and water to be measured respectively
Cement paste waits for test sample；
(2) 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 includes that blended cement net slurry waits for that test sample and cement paste to be measured wait for test sample to test sample；
(3) 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 mass percentage of periclase in cement to be measured；
Wherein: ω is the mass percentage of periclase in cement to be measured；
ω1Ca in test sample (OH) is waited for for blended cement net slurry2Mass percentage；
ω2Ca in test sample (OH) is waited for for cement paste 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 blended cement net slurry；
ω4Weightless mass percent of the test sample within the scope of 300 DEG C~500 DEG C is waited for for cement paste to be measured.
Use " pressure steams test " method of the invention, it is ensured that the complete aquation of periclase in cement to be measured；Using " pressure
Steam test and thermogravimetry combine " method, it is possible to prevente effectively from being dissolved the interference of state magnesia in cement；It uses simultaneously
The minusing of " magnesium hydroxide and calcium hydroxide resultant and calcium hydroxide mass percentage subtract each other ", can effectively eliminate thermogravimetric point
The influence of magnesium hydroxide weightlessness and calcium hydroxide weightlessness crossing instances to periclase measurement result during analysis.Of the invention quantifies
The method accuracy for measuring periclase mass percentage in cement is high, convenient for more accurately evaluating the expansion characteristics of cement, refers to
Lead the practical application request of cement in engineering.
Above scheme can complete the measurement of periclase mass percentage in cement, provide on this basis preferably
Scheme:
Preferably, the blended cement net slurry waits for that test sample and cement paste to be measured wait for that test sample does at least 3 times respectively and puts down
Row measurement is averaged.
Preferably, described carry out first test block and the second test block to press to steam obtaining blended cement net slurry respectively
Wait for including the following steps: the first test block and the second test block by test sample that boil 3~5 small for boiling in water respectively to test sample and cement paste to be measured
When, it then 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 it chooses internal fresh test block and carries out grinding and obtain blended cement net slurry waiting for that test sample and cement paste to be measured wait for test sample.
Preferably, the time of maintenance described in step (1) 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 1-4, high-magnesia cement quantitative determine important parameter
4 kinds of difference MgO mass hundred that 1-4 of the embodiment of the present invention uses Jia Hua special cement limited liability company to produce respectively
The low-heat portland cement of point content (being followed successively by 4.04%, 4.87%, 5.92%, 7.05%) carries out determining for periclase in cement
It is fixed to measure.1-4 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: periclase quality percentage in quantitative determination cement of the invention
The method of content can be to avoid the interference of solid solution state magnesia in cement, while eliminating magnesium hydroxide heat absorption during thermogravimetric analysis
The influence at peak and calcium hydroxide endothermic peak cross-pair periclase measurement result, accuracy is high, convenient for more accurately evaluating cement
Expansion characteristics instruct the practical application request of cement in engineering.
Content, percentage composition and percentage mentioned in the present invention etc. are defaulted as mass percentage, in above-mentioned side
The transformation for selecting conventional reagent or means to carry out on the basis of case is within the scope of the present invention.
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 mass percentage in minusing quantitative determination cement, it is characterised in that: including following step
It is rapid:
(1) it prepares blended cement net slurry and waits for that test sample and cement paste to be measured wait for test sample: by 1 part of cement to be measured, periclase primary standard substance
Matter, water are mixed evenly according to the weight ratio of a:1:b, and demoulding obtains the first examination after blended cement net slurry sample is made and conserves
Block；1 part of cement and water to be measured are mixed evenly according to the weight ratio of a:b, taken off after cement paste sample maintenance to be measured is made
Mould obtains the second test block；Wherein a value is between 9~24, and b value is between 3~10；
It first test block and the second test block is carried out to pressure steams to obtain blended cement net slurry and wait for that test sample and cement to be measured are net respectively
Slurry is to test sample；
(2) 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 includes that blended cement net slurry waits for that test sample and cement paste to be measured wait for test sample to test sample；
(3) 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) mass percentage of periclase in cement to be measured is calculated；
Wherein: ω is the mass percentage of periclase in cement to be measured；
ω1Ca in test sample (OH) is waited for for blended cement net slurry2Mass percentage；
ω2Ca in test sample (OH) is waited for for cement paste 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 blended cement net slurry；
ω4Weightless mass percent of the test sample within the scope of 300 DEG C~500 DEG C is waited for for cement paste to be measured.
2. the method for periclase mass percentage, feature in minusing quantitative determination cement according to claim 1
It is, the blended cement net slurry waits for that test sample and cement paste to be measured wait for that test sample does at least 3 times parallel determinations respectively and is averaged
Value.
3. the method for periclase mass percentage, feature in minusing quantitative determination cement according to claim 1
It is, it is described first test block and the second test block are carried out to pressure to steam to obtain blended cement net slurry and wait for test sample and to be measured respectively
Cement paste waits for including the following steps: the first test block and the second test block by test sample that boiling is boiled 3~5 hours in water respectively, then 210
DEG C~220 DEG C of temperature and/or 1.8~2.2MPa pressure pushes and steams 3~5 hours；Test block exterior portion is rejected, and is chosen internal new
Fresh test block progress grinding obtains blended cement net slurry and waits for that test sample and cement paste to be measured wait for test sample.
4. the method for periclase mass percentage, feature in minusing quantitative determination cement according to claim 1
It is, the time of maintenance described in step (1) is 24 hours~72 hours.
5. the method for periclase mass percentage, feature in minusing quantitative determination cement according to claim 1
It is, obtains the mass percentage to test sample middle reaches from calcium oxide and surveyed using glycide method in GB/T 176-2008
It is fixed.
6. the method for periclase mass percentage, feature in minusing quantitative determination cement according to claim 1
It is, the periclase primary standard substance active principle is magnesia, and fineness is 45 μm~80 μm.
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