CN106018157A - Detection method for ingredients of ash calcium powder - Google Patents
Detection method for ingredients of ash calcium powder Download PDFInfo
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- CN106018157A CN106018157A CN201610298595.2A CN201610298595A CN106018157A CN 106018157 A CN106018157 A CN 106018157A CN 201610298595 A CN201610298595 A CN 201610298595A CN 106018157 A CN106018157 A CN 106018157A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N5/00—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid
- G01N5/04—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid by removing a component, e.g. by evaporation, and weighing the remainder
Abstract
The invention provides a detection method for ingredients of ash calcium powder. The detection method comprises the following steps that a CaO sample is analyzed with a thermogravimetric analysis method, and the content of Ca(OH)2 in the CaO sample is obtained; an ash calcium powder sample is put into a thermogravimetric meter, the temperature of the ash calcium powder sample is increased to 900-1100 DEG C from the room temperature, calculation is carried out based on a calculation method according to the weight loss of the ash calcium powder sample in the temperature range and the content of Ca(OH)2 in the CaO sample, and the content of Ca(OH)2, CaO and CaCO3 are obtained. According to the detection method, the contents of all ingredients in the ash calcium powder are obtained through the thermogravimetric analysis method; in the detection process, the problem that the accuracy of the contents of CaO and Ca(OH)2 in the ash calcium powder is influenced due to the fact that CaO in the ash calcium powder is converted into Ca(OH)2 due to moisture absorption is considered, so that the content of Ca(OH)2 in the CaO sample is detected first, and the accuracy of the contents of all ingredients in the ash calcium powder is further improved.
Description
Technical field
The present invention relates to sierozem power technical field, particularly relate to the detection method of a kind of sierozem power composition.
Background technology
Sierozem power is by with CaCO3For the natural fat lime stone of main component, after high-temperature calcination, become quick lime
(CaO) after, then through selected, partial digested, the most again by high speed selecting crude drugs with winnower beater grinder pulverize, its apparent pure white carefully
Greasy；Sierozem power is Ca (OH)2, CaO and a small amount of CaCO3Mixture, be the intensely processed products of Calx.Sierozem power is usually in building
Using widely as having in water proof putty in material, it is as the active matter of building coating simultaneously, is possible not only to improve coating
Scrub performance, and reduce the cost of raw material of coating.
Sierozem power is a kind of alkaline mixture, meets water and releases substantial amounts of heat, and reaction generates Ca (OH)2, Ca (OH)2Inhale
Receive CO in air2Generate CaCO3, this is the principle of water proof putty.But in process of production, there is presently no a kind of method to come really
Determine the method for each composition in mixture, and bring bigger hidden danger to product.At present from the point of view of document, big multi-method is to use
Chemistry titration method determines the active matter Ca (OH) in the middle of mixture2Content, about CaCO3And the mensuration side of CaO
Method, and chemistry titration method is accurate not, and error is bigger.
Tianjin good fortune is carried out Wu Jun of White building materials company limited et al. and has been delivered Ca in sierozem power (OH)2The mensuration side of content
Method；The Yuan Wei of Beijing University of Chemical Technology uses chemical analysis method to determine Ca (OH)2And CaCO3Mixture.These methods are all mentioned
Component analysis in mixture, but people be there is presently no for the mensuration of each in industrial products sierozem power composition and pass through instrument
Analyze and determine.Therefore, need offer badly and a kind of measure the detection method of each composition in sierozem power.
Summary of the invention
Present invention solves the technical problem that the detection method being to provide a kind of sierozem power composition, the detection method of the application
The content of each component in sierozem power can be measured accurately.
In view of this, this application provides the detection method of a kind of sierozem power composition, comprise the following steps:
Use thermogravimetry to analyze CaO sample, obtain Ca (OH) in CaO sample2Content；
Sierozem power sample is placed in thermogravimetric analyzer, sierozem power sample is warming up to 900 DEG C from room temperature 20 DEG C～25 DEG C
～1100 DEG C, according to described sierozem power sample weightlessness in the range of said temperature and Ca (OH) in CaO sample2Content, press
Calculate according to following formula, obtain Ca (OH)2, CaO and CaCO3Content；
X%*a%+Y%=4.096*WWeightless 1；
X%+Y%=1-2.275*WWeightless 2；
Wherein, the content of CaO during X is sierozem power；
Y is Ca (OH) in sierozem power2Content；
A% is Ca (OH) in CaO sample2Content；
WWeightless 1Quality and Ca (OH) for sierozem power sample2The difference of the quality of the sample after decomposition；
WWeightless 2For Ca (OH)2The quality of the sample after decomposition and CaCO3The difference of the quality of the sample after decomposition.
Preferably, described intensification process particularly as follows:
By sierozem power sample when room temperature 20 DEG C～25 DEG C is warming up to 400～600 DEG C with the heating rate of 5～10 DEG C/min
Constant temperature, makes reacted sample constant weight, then constant temperature when being warming up to 600～900 DEG C with the heating rate of 5～10 DEG C, makes the most anti-
Sample constant weight after should.
Preferably, described intensification process particularly as follows:
By sierozem power sample constant temperature when room temperature 20 DEG C～25 DEG C is warming up to 500 DEG C with the heating rate of 5 DEG C/min, make anti-
Sample constant weight after should, then constant temperature when being warming up to 800 DEG C with the heating rate of 5 DEG C, make the most reacted sample constant weight.
Preferably, Ca (OH) in described CaO sample2Content be to be changed into Ca after the part CaO moisture absorption in CaO sample
(OH)2Amount.
Preferably, Ca (OH) in CaO sample is obtained2Content process particularly as follows:
CaO sample is placed in thermogravimetric analyzer, CaO sample is warming up to 400 DEG C～600 from room temperature 20 DEG C～25 DEG C
DEG C, according to described CaO sample weightlessness in the range of said temperature, calculate according to the following formula, obtain Ca (OH) in CaO sample2's
Content；
WCa(OH)2=4.096*WWeightless 3；
A%=(4.096*WWeightless 3/WCaO) * 100%；
Wherein, WWeightless 3Quality and Ca (OH) for CaO sample2The difference of the quality of the sample after decomposition；
WCaOQuality for CaO sample；
A% is Ca (OH) in CaO sample2Content.
This application provides the detection method of a kind of sierozem power composition, comprise the following steps: use thermogravimetry analysis
CaO sample, obtains Ca (OH) in CaO sample2Content；Sierozem power sample is placed in thermogravimetric analyzer, by sierozem power sample
From room temperature to 900 DEG C～1100 DEG C, according to described sierozem power sample weightlessness in the range of said temperature with in CaO sample
Ca(OH)2Content, calculate according to calculating formula, obtain Ca (OH)2, CaO and CaCO3Content.The application uses thermogravimetric to divide
Analysis method obtains the content of each component in sierozem power, simultaneously during sierozem power compound mensuration, it is contemplated that in sierozem power
CaO self moisture absorption is changed into Ca (OH)2, and affect CaO Yu Ca in sierozem power (OH)2The problem of content accuracy, first surveys
Determine Ca (OH) in CaO sample2Content, further increase the accuracy of each constituent content in sierozem power.
Accompanying drawing explanation
Fig. 1 is the TGA curve chart of CaO sample；
Fig. 2 is the TGA curve chart of sierozem power sample in embodiment 1；
Fig. 3 is the TGA curve chart of sierozem power sample in embodiment 2；
Fig. 4 is the TGA curve chart of sierozem power sample in embodiment 3；
Fig. 5 is the TGA curve chart of sierozem power sample in embodiment 4；
Fig. 6 is the TGA curve chart of sierozem power sample in embodiment 5；
Fig. 7 is the TGA curve chart of sierozem power sample in embodiment 6.
Detailed description of the invention
In order to be further appreciated by the present invention, below in conjunction with embodiment, the preferred embodiment of the invention is described, but
Should be appreciated that these describe simply as to further illustrate the features and advantages of the present invention rather than to the claims in the present invention
Limit.
The embodiment of the invention discloses the detection method of a kind of sierozem power composition, comprise the following steps:
Use thermogravimetry to analyze CaO sample, obtain Ca (OH) in CaO sample2Content；
Sierozem power sample is placed in thermogravimetric analyzer, by sierozem power sample from room temperature to 900 DEG C～1100 DEG C, root
According to described sierozem power sample weightlessness in the range of said temperature and Ca (OH) in CaO sample2Content, count according to the following formula
Calculate, obtain Ca (OH)2, CaO and CaCO3Content；
X%*a%+Y%=4.096*WWeightless 1；
X%+Y%=1-2.275*WWeightless 2；
Wherein, the content of CaO during X is sierozem power；
Y is Ca (OH) in sierozem power2Content；
A% is Ca (OH) in CaO sample2Content；
WWeightless 1Quality and Ca (OH) for sierozem power sample2The difference of the quality of the sample after decomposition；
WWeightless 2For Ca (OH)2The quality of the sample after decomposition and CaCO3The difference of the quality of the sample after decomposition.
This application provides the detection method of a kind of sierozem power composition, use the detection method of the application accurately to obtain
CaO, Ca (OH) in sierozem power2With CaCO3Content.
Owing to calcium oxide has strong moisture absorption performance, therefore the quality source of the calcium oxide in sierozem power should be two
Part, a part is the carbonate-free lime of the non-moisture absorption, and another part is to become calcium hydroxide after the calcium oxide moisture absorption, and these two parts are constituted
The gross mass of calcium oxide.Therefore, the application has how many calcium oxide moisture absorption to become hydrogen-oxygen in needing the calcium oxide first determined
Change calcium.The application have employed in thermogravimetry mensuration calcium oxide has how many calcium oxide to change for calcium hydroxide, specifically utilizes
The decomposition temperature scope of calcium hydroxide is 400～600 DEG C, utilizes thermogravimetric analyzer to measure the weightlessness of sample, further according to reaction equation,
Being calculated the amount of calcium hydroxide, the amount of this calcium hydroxide is by the calcium hydroxide being changed into after the partial oxidation calcium moisture absorption, thus
I.e. can determine that the content of calcium hydroxide in calcium oxide；The reaction equation that said process relates to is as follows:
CaO+H2O=Ca (OH)2；Ca(OH)2=CaO+H2O；
The calculating formula of above-mentioned calculating process is as follows:
WCa(OH)2=4.096 × WWeightless 3；
A%=(4.096 × WWeightless 3/WCaO) × 100%；
Wherein, WWeightless 3Quality and Ca (OH) for CaO sample2The difference of the quality of the sample after decomposition；
WCaOQuality for CaO sample；
A% is Ca (OH) in CaO sample2Content.
Ca (OH) in described CaO sample2Content be similarly in sierozem power Ca (OH) in CaO2Content, therefore with CaO sample
Ca (OH) in product2Content based on, carry out CaO, Ca (OH) in sierozem power2With CaCO3The detection of content, particularly as follows:
By sierozem power sample constant temperature when room temperature is warming up to 400～600 DEG C with the heating rate of 5～10 DEG C/min, make anti-
Sample constant weight after should, then constant temperature when being warming up to 600～900 DEG C with the heating rate of 5～10 DEG C, make the most reacted sample
Constant weight.
Further, by sierozem power sample constant temperature when room temperature is warming up to 500 DEG C with the heating rate of 5 DEG C/min, make anti-
Sample constant weight after should, then constant temperature when being warming up to 800 DEG C with the heating rate of 5 DEG C, make the most reacted sample constant weight.
Above-mentioned thermogravimetric analysis detection process is with Ca (OH)2Decomposition temperature scope be 400～600 DEG C, CaCO3Decomposition
Temperature range is carried out based on being 600～900 DEG C.Described calcium hydroxide is decomposed into calcium oxide and water in 400～600 DEG C,
Calcium carbonate is decomposed into calcium carbonate and carbon dioxide in 600～900 DEG C, and water and carbon dioxide are in case of heating with gas
The form of body is overflowed, and thus, obtains the sierozem power sample weightlessness in each stage, uses thermogravimetry to respectively obtain the water of weightlessness
With the amount of carbon dioxide, thus it is calculated calcium hydroxide and calcium carbonate according to the decomposition reaction formula of calcium hydroxide Yu calcium carbonate
Content, but, the content of above-mentioned calcium hydroxide be include the partial oxidation calcium moisture absorption after the calcium hydroxide that is changed into, therefore, profit
In the calcium oxide sample obtained with above-mentioned thermogravimetry, the content of calcium hydroxide, by formula calculated below, obtains in sierozem power
Calcium oxide and the content of calcium hydroxide.
X%*a%+Y%=4.096*WWeightless 1；
X%+Y%=1-2.275*WWeightless 2；
Wherein, the content of CaO during X is sierozem power；
Y is Ca (OH) in sierozem power2Content；
A% is Ca (OH) in CaO sample2Content；
WWeightless 1Quality and Ca (OH) for sierozem power sample2The difference of the quality of the sample after decomposition；
WWeightless 2For Ca (OH)2The quality of the sample after decomposition and CaCO3The difference of the quality of the sample after decomposition.
By simultaneous above-mentioned two equation, obtain the content of calcium hydroxide and calcium oxide, and then obtain containing of calcium carbonate
Amount, the calcium hydroxide in the application sierozem power is as follows with the reaction equation of High Temperature Dissociation of Calcium Carbonate:
Ca(OH)2=CaO+H2O；CaCO3=CaO+CO2。
The thermogravimetry that herein described thermogravimetry is well known to those skilled in the art, does not has spy to this application
Other restriction.
Concrete, in sierozem power, calcium hydroxide, calcium carbonate are as follows with the calculating process of calcium oxide:
(1)Ca(OH)2Cubage formula is: WCa(OH)2%=(74.096/18.088) × WWater is weightless=4.096 × WWater is weightless；
Wherein, WWater is weightless-sample is weight loss when 500 DEG C, and instrument is given.
74.096,18.088---are respectively Ca (OH)2And H2The molecular weight of O；
(2)CaCO3Cubage formula is: WCaCO3%=(100.09/44) × WCO2 is weightless=2.275 × WCO2 is weightless
WCO2 is weightless-sample is weight loss when 800 DEG C, and instrument is given.
100.09,44---are respectively Ca (OH)2And CO2Molecular weight.
Carry out the thermogravimetric analysis of simple CaO sample simultaneously, determine wherein there are how many Ca (OH)2, according to decompose equation with
And Thermogravimetric Data draws: simple CaO sample fluid loss is 10.32%, then can get Ca (OH) in simple CaO sample2Percentage
Number is 42.27%；
Assume CaO, Ca in sample (OH)2And CaCO3Content is respectively x, y, z；Then equation group (1), (2) meter can be set up
Calculate each content of material
42.27% × x%+y%=4.096 × WWater is weightless(1)；
X%+y%=1-WCaCO3%=1-2.275 × WCO2 is weightless(2)；
Simultaneous aforesaid equation, then obtain the content of calcium oxide in sierozem power, calcium hydroxide and calcium carbonate.
This application provides the detection method of a kind of sierozem power composition, during detection, the application utilizes hydroxide
Calcium and calcium carbonate decompose the weightlessness of generation, calcium oxide, calcium carbonate and hydroxide in calculated sierozem power at different temperatures
The content of calcium, the method is simple, and accuracy is higher.
In order to be further appreciated by the present invention, below in conjunction with the detection method of the sierozem power composition that the present invention is provided by embodiment
Being described in detail, protection scope of the present invention is not limited by the following examples.
Embodiment 1
Use thermogravimetric analyzer CaO sample is measured, start instrument temperature programming function, make sample from room temperature with
5 DEG C/min heating rate constant temperature when 500 DEG C makes sample constant weight, determines Ca (OH) in CaO sample by instrument software2Mistake
Weight, TGA curve is as shown in Figure 1；
Use thermogravimetric analyzer that sierozem power sample is measured, start the temperature programming function of instrument, make sample from room
Temperature makes sample constant weight with 5 DEG C/min heating rate constant temperature when 500 DEG C, then proceedes to make sample exist with 5 DEG C/min heating rate
At 800 DEG C, constant temperature is to constant weight.Determined the weightlessness of each temperature by instrument software, the TGA curve of the present embodiment as in figure 2 it is shown,
Calculating process is illustrated in detail:
(1) CaO mono-product thermogravimetric analysis, owing to Dan Pinzhong contains Ca (OH)2, calculate according to computing formula, the mistake of Dan Pinzhong
The water yield provided for 10.32% (as shown in Figure 1) from thermogravimetric result, according to Ca (OH)2Decomposition reaction formula, then Ca (OH) in single product2Contain
Amount is: 10.32% × 4.096=42.27%.
(2) CaO, Ca (OH) during sample is assumed in sample thermogravimetric analysis2With CaCO3Content is respectively as follows: x%, y%, z%；
Owing in the mono-product of CaO, 42.27% is Ca (OH)2, therefore the weightlessness of biased sample meets following formula:
42.27% × x%+y%=4.096 × WSample weight loss-water (1)
X%+y%=1-2.275 × WSample weight loss-carbon dioxide (2)
Solving equations, obtains x%=16.4%, y%=41.81, z%=41.79；
The present embodiment CaO, Ca (OH)2With CaCO3Stoichiometric be 1:2:2, from above-mentioned result of calculation, this enforcement
The assay method accuracy of example is higher.
Embodiment 2
CaO, Ca in sierozem power (OH) in the present embodiment2With CaCO3Stoichiometric be 1:2:1, each composition in sierozem power
Mensuration process same as in Example 1, TGA curve is as it is shown on figure 3, the present embodiment CaO, Ca (OH)2With CaCO3Stoichiometric
As shown in table 1 with actual result tables of data.
Embodiment 3
CaO, Ca in sierozem power (OH) in the present embodiment2With CaCO3Stoichiometric be 2:1:1, each composition in sierozem power
Mensuration process same as in Example 1, TGA curve as shown in Figure 4, the present embodiment CaO, Ca (OH)2With CaCO3Stoichiometric
As shown in table 1 with actual result tables of data.
Embodiment 4
CaO, Ca in sierozem power (OH) in the present embodiment2With CaCO3Stoichiometric be 1:1:1, each composition in sierozem power
Mensuration process same as in Example 1, TGA curve is as it is shown in figure 5, the present embodiment CaO, Ca (OH)2With CaCO3Stoichiometric
As shown in table 1 with actual result tables of data.
Embodiment 5
CaO, Ca in sierozem power (OH) in the present embodiment2With CaCO3Stoichiometric be 2:2:1, each composition in sierozem power
Mensuration process same as in Example 1, TGA curve as shown in Figure 6, the present embodiment CaO, Ca (OH)2With CaCO3Stoichiometric
As shown in table 1 with actual result tables of data.
Embodiment 6
CaO, Ca in sierozem power (OH) in the present embodiment2With CaCO3Stoichiometric be 1:1:2, each composition in sierozem power
Mensuration process same as in Example 1, TGA curve is as it is shown in fig. 7, the present embodiment CaO, Ca (OH)2With CaCO3Stoichiometric
As shown in table 1 with actual result tables of data.
The stoichiometric of each component and results of calculation data synopsis in table 1 sierozem power
The explanation of above example is only intended to help to understand method and the core concept thereof of the present invention.It is right to it should be pointed out that,
For those skilled in the art, under the premise without departing from the principles of the invention, it is also possible to the present invention is carried out
Some improvement and modification, these improve and modify in the protection domain also falling into the claims in the present invention.
Described above to the disclosed embodiments, makes professional and technical personnel in the field be capable of or uses the present invention.
Multiple amendment to these embodiments will be apparent from for those skilled in the art, as defined herein
General Principle can realize without departing from the spirit or scope of the present invention in other embodiments.Therefore, the present invention
It is not intended to be limited to the embodiments shown herein, and is to fit to and principles disclosed herein and features of novelty phase one
The widest scope caused.
Claims (5)
1. a detection method for sierozem power composition, comprises the following steps:
Use thermogravimetry to analyze CaO sample, obtain Ca (OH) in CaO sample2Content；
Sierozem power sample is placed in thermogravimetric analyzer, by sierozem power sample from room temperature 20 DEG C～25 DEG C be warming up to 900 DEG C～
1100 DEG C, according to described sierozem power sample weightlessness in the range of said temperature and Ca (OH) in CaO sample2Content, according to
Following formula calculates, and obtains Ca (OH)2, CaO and CaCO3Content；
X%*a%+Y%=4.096*WWeightless 1；
X%+Y%=1-2.275*WWeightless 2；
Wherein, the content of CaO during X is sierozem power；
Y is Ca (OH) in sierozem power2Content；
A% is Ca (OH) in CaO sample2Content；
WWeightless 1Quality and Ca (OH) for sierozem power sample2The difference of the quality of the sample after decomposition；
WWeightless 2For Ca (OH)2The quality of the sample after decomposition and CaCO3The difference of the quality of the sample after decomposition.
Detection method the most according to claim 1, it is characterised in that the process of described intensification particularly as follows:
By sierozem power sample perseverance when room temperature 20 DEG C～25 DEG C is warming up to 400～600 DEG C with the heating rate of 5～10 DEG C/min
Temperature, makes reacted sample constant weight, then constant temperature when being warming up to 600～900 DEG C with the heating rate of 5～10 DEG C, makes secondary response again
After sample constant weight.
Detection method the most according to claim 2, it is characterised in that the process of described intensification particularly as follows:
By sierozem power sample constant temperature when room temperature 20 DEG C～25 DEG C is warming up to 500 DEG C with the heating rate of 5 DEG C/min, after making reaction
Sample constant weight, then constant temperature when being warming up to 800 DEG C with the heating rate of 5 DEG C, make the most reacted sample constant weight.
Detection method the most according to claim 1, it is characterised in that Ca (OH) in described CaO sample2Content be CaO sample
Ca (OH) it is changed into after the part CaO moisture absorption in product2Amount.
Detection method the most according to claim 1, it is characterised in that obtain Ca (OH) in CaO sample2The process of content
Particularly as follows:
CaO sample is placed in thermogravimetric analyzer, CaO sample is warming up to 400 DEG C～600 DEG C from room temperature 20 DEG C～25 DEG C, root
According to described CaO sample weightlessness in the range of said temperature, calculate according to the following formula, obtain Ca (OH) in CaO sample2Content；
WCa(OH)2=4.096*WWeightless 3；
A%=(4.096*WWeightless 3/WCaO) * 100%；
Wherein, WWeightless 3Quality and Ca (OH) for CaO sample2The difference of the quality of the sample after decomposition；
WCaOQuality for CaO sample；
A% is Ca (OH) in CaO sample2Content.
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| CN111595721A (en) * | 2020-06-24 | 2020-08-28 | 广东联塑科技实业有限公司 | Method for measuring PVC (polyvinyl chloride) content and calcium content in polyvinyl chloride product |
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| CN112945793A (en) * | 2021-03-30 | 2021-06-11 | 福建中烟工业有限责任公司 | Method and device for detecting content of liquid content in carrier gel |
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