CN110530911A - The method for measuring the silicate mineral in portland slag cement and slag content - Google Patents
The method for measuring the silicate mineral in portland slag cement and slag content Download PDFInfo
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- CN110530911A CN110530911A CN201910934834.2A CN201910934834A CN110530911A CN 110530911 A CN110530911 A CN 110530911A CN 201910934834 A CN201910934834 A CN 201910934834A CN 110530911 A CN110530911 A CN 110530911A
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
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Abstract
The invention discloses a kind of methods of silicate mineral and slag content in measurement portland slag cement.Ground granulated blast furnace slag is milled into slag powder sample；It weighs ZnO standard substance and solvent to be added, batch mixer mix grinding, dries to obtain the mixed-powder that is uniformly mixed with zinc oxide of slag；The diffraction data for acquiring slag powder sample calculates calibration constants in conjunction with zinc oxide and slag powder sample room relative amount, obtains the known or whole unknown crystal structure phase structure files in slag part；The partial size for controlling portland slag cement acquires the diffraction data of portland slag cement, determines the mineral structure file of contained mineral, and quantitative analysis obtains the relative amount of each mineral and slag.The method of the present invention passes through the ZMV value for being mixed to get unknown material phase of unknown material phase and internal standard compound, establishes the known or whole unknown crystal structured files in part of unknown material phase, and then analyzes and can determine that the actual content of crystalline state, amorphous state in the sample.
Description
Technical field
The invention belongs to test and analyze technical field, and in particular to the XRD- of slag content in a kind of portland slag cement
The known or whole unknown crystal structure quantitative analysis methods in part.
Background technique
Common portland cement (Common Portland Cement) refers to Portland clinker, suitable gypsum
And hydraulic cementing materials made of defined mixing material.
The main bonding component of common portland cement is clinker, and performance depends primarily on the mineral composition and mine of clinker
Object structure.Clinker mainly includes four big mineral: tricalcium silicate (C3S), dicalcium silicate (C2S), tricalcium aluminate (C3A), iron aluminic acid
Four calcium solid solution (C4AF), it is even higher that total amount of these four mineral in common portland cement clinker accounts for 95%.Wherein,
For C3S content usually 50% or so, it not only influences early strength, but also influences the later strength of cement, is to influence cement
The determinant of intensity；The content of C2S is generally 20% or so, influences less on early strength, is to determine later strength
Principal element；The content of C3A is generally 10% hereinafter, the influence to cement early strength is maximum；The content of C4AF generally exists
10% or so, it is considered that C4AF does not have biggish effect to the intensity of cement, but has the test of scholar to prove C4AF not only
Development that is sizable, and facilitating later strength is served to the early strength of cement.In summary, common Portland water
The property of mud depends primarily on the content and composition of its 4 kinds main clinker minerals.
Portland slag cement refer to Portland clinker, gypsum, slag powders according to a certain percentage combined grinding and
At common portland cement, all kinds of specific proportion requirements of portland slag cement are shown in Table 1:
Table 1
Different cement types is suitable for different engineerings and position, this has been common recognition in the industry.It is excessive to add mixing material,
It will cause clinker minerals content deficiency in cement, lead to the decline of the decline of performance, especially mechanics, endurance quality, improve
Construction engineering quality security risk.For this purpose, relevant national standard mixes the clinker content of common portland cement and adding
The type for closing material is all made that stringent regulation.
But all there is certain deficiency in existing test method:
(1) GB 175-2007 has used the concept of constituent content when classifying to cement products, but in subsequent product skill
Art has no concrete regulation in requiring, and requiring nothing more than the producer should be at least monthly by GB/T 12960-2007 " the quantitative survey of cement component
It is fixed " cement component is checked.Clinker, mixing material (flyash, mine needed for the standard requirements producer provides manufacture of cement
Slag and lime stone etc.), the raw material such as gypsum and corresponding proportion, and then clinker in cement, mixed is calculated by the method for chemical analysis
Close the content of material, gypsum.This method more depends on the credibility of enterprise, only a kind of theoretical calculation method, actual
It cannot even reflect the effective content of clinker mineral in process of supervision, the true of clinker and all kinds of mixing materials forms that there are no from what is said or talked about
It rises.
(2) traditional X-ray diffraction method (Standardization Act) has pre-treatment sample preparation complicated, it is difficult to offset overlap peak to fixed
The influence of result is measured, while the content of crystalline state mineral can only be measured, the content of amorphous state slag can not be measured.
(3) the Rietveld method based on X-ray diffraction, it is quantitative accurate, related raw material is provided without enterprise, but there are preceding places
Reason is complicated, requires to add internal standard compound every time before test, and there are the uneven risks of internal standard mixing.Obtained result be crystalline state and
Amorphous relative amount can not determine the actual content of slag in amorphous state.
Traditional Rietveld method calculates the ZMV value of all crystalline state object phases according to structural parameters, but for unknown knot
The ZMV value of structure is then helpless, and it is even more impossible to calculate the relative amount of unknown material phase.
Summary of the invention
In view of the problems of the existing technology, the purpose of the present invention is to provide one kind to be based on portland slag cement chats
The known or whole unknown crystal structure quantitative analysis methods in the part XRD- of slag content.The present invention slag it is unknown or part
Analysis detection is carried out in the case where knowing amorphous phase, silicate mineral and slag content can be obtained.
The technical solution that the present invention is taken to achieve the goals above are as follows:
1.1, the foundation of the known or whole unknown crystal structure phases in slag part:
1.1.1, the granulated blast-furnace slag (abbreviation slag) by vitreum content 95% or more, grinding to 5~15 μm of systems
At slag powder sample；
1.1.2, slag 4~6g of powder sample is weighed, the ZnO mark for occupying slag powder sample quality 12%~18% is weighed
Quasi- substance, using ZnO standard substance as internal standard compound, the ZnO standard substance that number is NIST SRM674 is can be used in specific implementation,
8~12ml of organic solvent is added, above-mentioned three is stirred evenly, batch mixer mix grinding, drying obtains slag and mixes with zinc oxide
Even mixed-powder, granularity control is between 5~10 μm after mix grinding；
1.1.3, using the diffraction data of X-ray diffractometer acquisition slag powder sample, combined and mixed according to diffraction data
Relative amount in powder between zinc oxide and slag powder sample calculates calibration constants (ZMV) (calibration constants ZMV of slag
In, Z refers to that chemical formula number, M refer to that chemical formula molecular weight, V refer to unit cell volume in structure cell), it determines the structural solid of slag, that is, determines mine
The amorphous phase situation of slag powder sample obtains the known or whole unknown crystal structure phase structure files in slag part；
In specific implementation, according to parameters such as the space group of slag, cell parameters, according to slag and internal standard compound zinc oxide it
Between relative amount, calculate the ZMV of slag, and obtain the structural solid file of slag.
1.2, portland slag cement slag content quantifies:
1.2.1, by the size controlling of portland slag cement between 5~15 μm；
1.2.2, portland slag cement is fitted into X-ray diffraction specimen holder using back dress method, uses X-ray diffractometer
The diffraction data for acquiring portland slag cement, can be reduced artificial sample preparation to error caused by diffraction patterns in this way；
1.2.3, according to diffraction data determine portland slag cement contained in mineral mineral structure file, i.e. mineral
Object phase, obtain qualitative results；
1.2.4, known to the slag part obtained according to mineral structure file combination step 1.1 or whole unknown crystal structure
Phase structure file carries out quantitative analysis, obtains the relative amount of each mineral and slag in portland slag cement.
Quantitative analysis is carried out using Rietveld refine software in the specific implementation of the step 1.2.4, detailed process is:
(1) according to the reasonable diffraction light sources line style of apparatus selection (Emission Profile) of acquisition data；
(2) it according to sample characteristic (according to crystallization degree), selects back end (Background)；
(3) according to actual instrumentation condition, it is arranged instrument parameter (Instrument)；
(4) according to equipment actual conditions and sample X-ray absorption feature, sample amendment option (Correction) is selected；
(5) structured file (portion that the known mineral structure file and the 1.1st part determined including qualitative analysis obtains is called in
Divide known or whole unknown crystal structure structured files)；
(6) it is fitted；
(7) it if it is necessary, carrying out necessary preferred orientation amendment, is fitted again；
(8) fitting obtains the relative amount of each mineral and slag in portland slag cement.
In the step 1.1.2, the mass ratio of slag powder sample and ZnO standard substance are as follows: (82~88): (18~
12)。
The solid-liquid ratio of the slag powder sample and organic solvent is 1g:2ml.
The organic solvent is that dehydrated alcohol, isopropanol, methanol and hexamethylene etc. do not occur with portland cement, slag
The organic solvent of chemical reaction.
In the step 1.2.2, X-ray diffractometer acquires the condition of X ray diffracting spectrum are as follows: voltage and current 30Kv/
10mA；Lynxeye detector array is open 4.8 °；Divergent slit (DS)=0.6mm (0.3 °)；Front and back rope draws slit=2.5 °；
8mm shading knife；3mm antiscatter slits；Sample stage revolving speed 15rpm.
The method of the present invention is mixed to get by unknown material phase and internal standard compound (ZnO's), and the ZMV value of unknown material phase is built simultaneously
The known or whole unknown crystal structured files in the part of vertical unknown material phase.Then in the X-ray diffraction Rietveld of actual sample
This document is used in software, can determine that the actual content of crystalline state, amorphous state in the sample.No mark may be implemented with the method for the present invention
Sample quantitative phase analysis and obtain same accuracy.
The beneficial effects of the present invention are:
(1) measuring method of clinker mineral and mixing material content in portland slag cement is established, it is effective according to clinker
Content judges the blending amount of mixture material of cement, in method more scientific, more specific aim, is more advantageous to and guarantees cement products safety；
(2) it is controlled for the production of cement production enterprise, one kind is provided and quickly and effectively examines control means, guarantees product
Stability.
Detailed description of the invention
Fig. 1 is Xiangshan Bay cement-slag diffracting spectrum and qualitative results figure；
Fig. 2 is Leqing conch-slag diffracting spectrum and qualitative results figure；
Fig. 3 is tongue-slag diffracting spectrum and qualitative results figure；
Fig. 4 is Mo Cheng-slag diffracting spectrum and qualitative results figure；
Fig. 5 is Zhoushan silver horse-slag diffracting spectrum and qualitative results figure；
Fig. 6 is Shangyu Ji Shan-slag diffracting spectrum and qualitative results figure；
Fig. 7 is Qinglongshan-slag diffracting spectrum and qualitative results figure；
Fig. 8 is Taizhou superiors-slag diffracting spectrum and qualitative results figure；
Fig. 9 is Hu Shan-slag diffracting spectrum and qualitative results figure；
Figure 10 is Zhuji all directions-slag diffracting spectrum and qualitative results figure；
Figure 11 is slag amorphous phase average diffraction map figure；
Figure 12 is slag indexing peak-seeking fitted figure；
Figure 13 is to prepare portland slag cement diffracting spectrum and qualitative results figure；
Figure 14 is refine quantitative result figure of the invention.
Specific embodiment
To better understand the essence of the present invention, below by specific embodiment to technical solution of the present invention carry out into
The elaboration of one step.
The embodiment of the present invention the following steps are included:
(1) foundation of the known or whole unknown crystal structure phases in slag part:
To establish known to the canonical dissection of slag or whole unknown crystal structure phase, need to collect the common slag in cement plant
It is for statistical analysis.
Slag samples used in 10 cement plants (1 sample of every factory) is acquired thus, and concrete condition is shown in Table 2:
2 slag of table statistics
Above-mentioned slag is dried, is ground, makes the control of its average grain diameter at 7 μm or so.According to following experiment parameters and
The acquisition of condition progress slag X ray diffracting data: voltage and current 30Kv/10mA；Lynxeye detector array, opening
4.8°；Divergent slit (DS)=0.6mm (0.3 °)；Front and back rope draws slit=2.5 °；8mm shading knife；3mm antiscatter slits；Sample
Sample platform revolving speed 15rpm.Scanning mode, step-scan；Scanning speed, 1s/ step；Step-length, 0.02 °.Using Brooker, company is provided
Diffrac.EVA software carry out qualitative analysis, the diffracting spectrum and qualitative results of each slag samples be as Figure 1-10 shows.
Above-mentioned slag diffracting spectrum all have the characteristics that one it is common: diffracting spectrum 2 θ of diffraction peak be 22 °~38 °
Range between, there are a huge Amorphous Scattering peaks, and peak value highest point is generally within 2 θ of diffraction peak of diffracting spectrum
Between 30.2 °~31.4 ° of narrow range.
From the peak number amount of above-mentioned diffracting spectrum as it can be seen that removing two cement plants of above-mentioned No. 1 Xiangshan Bay cement and No. 7 Qinglongshans
Outside, the sample in remaining cement plant is substantially pure slag, and it is long that only several samples contain the crystalline state that a small amount of cooling procedure is precipitated
The mineral such as stone, quartz, but generally based on the amorphous phase substance of slag.
The scattering peak of the amorphous phase of each slag of the sample in remaining cement plant is averaged, available slag is put down
Equal diffracting spectrum, as shown in figure 11: the diffracted intensity maximum value of slag amorphous phase scattering peak and is adopted in 2 θ=30.5 ° or so
The diffractive features of most of slag samples of collection are all relatively.The diffraction data for the husky steel slag that No. 9 cement plants Hu Shan provide
The closest and basic nodeless mesh substance with average diffraction data.
Then, specific implementation carries out building for the known or whole unknown crystal structure phases of slag canonical dissection using husky steel slag
It is vertical.
1. the indexing of slag diffraction data:
In the Diffrac.TOPAS software that husky steel slag diffraction data importing Brooker company is provided, back end, instrument are determined
Device parameter.Peak-seeking chooses the preferable diffraction maximum of preceding 20 diffraction, and fitting spectrogram is as shown in figure 12: to the peak of the diffraction maximum of fitting
Shape carries out indexing, obtains the indexing parameter of diffraction maximum, indexing parameter is brought into the indices of crystallographic plane structure of slag, uses
Pohle (Pawley) refine method obtains space group belonging to slag " crystal " and cell parameter result are as follows: space group is
Ia-3d, cell parameter 2nm.
2. the determination of the known or whole unknown crystal structure phases in slag part:
The diffraction data of pure slag is called in TOPAS software, instrument parameter, light source file, back end are set in software
Series and amendment option.The hkl phase for establishing slag assumes that the space group of slag is Ia-3d according to indexing result, tentatively sets
A=2nm in its fixed cell parameter, and its range is limited, operation fitting.By indices of crystallographic plane phase, (indices of crystallographic plane are mutually according to crystalline substance afterwards
Facial index structure establish a kind of phase/parameter) intensity fix.
Mine is calculated with the diffraction data of known slag and internal standard compound zinc oxide relative amount substance substitution slag diffraction data
The ZMV value of slag, and then determine the known or whole unknown crystal structure structured files in the part of slag.
Specifically:
1.1.1, slag powder-like is made to 10 μm in the granulated blast-furnace slag by vitreum content 95% or more, grinding
Product；
1.1.2, slag powder sample 5g is weighed, the ZnO standard substance for occupying slag powder sample quality 15% is weighed, is had
Body implements that the ZnO standard substance that number is NIST SRM 674 can be used, and organic solvent 10ml is added, and above-mentioned three is stirred equal
Even, batch mixer mix grinding, drying obtains the mixed-powder that slag is uniformly mixed with zinc oxide, and granularity control is between 7 μm after mix grinding；
1.1.3, the diffraction data of slag powder sample is acquired using X-ray diffractometer,
According to the relative amount in diffraction data combination mixed-powder between zinc oxide and slag powder sample, slag is calculated
Calibration constants (ZMV), determine the structural solid of slag, that is, determine the amorphous phase situation of slag powder sample, obtain slag portion
Divide known or whole unknown crystal structure phase structure files.
Obtain its ZM value=0.076, V value=7967.713, space group Ia-3d, a=1.997nm.
By known to above-mentioned slag part or whole unknown crystal structure structured file saves, to be made with quantitative analysis later
With.
(2) it is configured to portland slag cement in the slag incorporation clinker of fixed proportion, wherein slag and clinker
Proportion are as follows: 21g:79g.
The clinker is solid by tricalcium silicate (C3S), dicalcium silicate (C2S), tricalcium aluminate (C3A), tetra calcium aluminoferrite
Solution (C4AF) is constituted, mass ratio are as follows: 63.4:28.7:2.5:10.8:3.7.
(3) by prepared portland slag cement, the mix grinding certain time in agate grinding pot, specific mix grinding program is such as
Under: the portland slag cement that 10g is mixed is fitted into the agate jar that volume is 50ml, and 20ml dehydrated alcohol is added,
Ball grinder is placed in mix grinding 10-15min on planetary ball mill, it is ensured that the average grain diameter of sample, and must not mistake at 10 μm or so
Degree grinding.
(4) sample after mix grinding is dried.
(5) sample is fitted into X-ray diffraction specimen holder after will be dry, and sample making course reduces the preferred orientation of sample to the greatest extent
It generates.The sample made is put into the collection that sample X ray diffracting data is carried out in X-ray diffractometer afterwards.
(6) diffractometer condition setting is as follows: voltage and current 30Kv/10mA；Lynxeye detector array is open 4.8 °；
Divergent slit (DS)=0.6mm (0.3 °)；Front and back rope draws slit=2.5 °；8mm shading knife；3mm antiscatter slits；Sample stage turns
Fast 15rpm.Scanning mode, step-scan；Scanning speed, 1s/ step；Step-length, 0.02 °.
(7) the Diffrac.EVA software provided using Brooker company is mutually qualitative to slag cements progress object is prepared, as a result
It is as shown in figure 13:
Table 3 is prepared cement sample qualitative results and is summarized
(8) the Diffrac.TOPAS software provided using Brooker company to the diffraction data of portland slag cement into
The known or whole unknown crystal structures in the part row Rietveld- quantify refine:
1. light source selected works select CuK α；2. back end file selects 4 grades of multinomials and 1/x function；3. actual instrumentation parameter is defeated
Enter in software；4. selecting suitable amendment option；6. according to qualitative results by C3S-M1, C3S-M3, C2S, C3A, C4AF, Fang Mei
Stone, the known or whole unknown crystal structure structured files in slag part are called in TOPAS software, and it is quasi- to carry out Rietveld refine
It closes；7. and carry out necessary preferred orientation amendment, the Mineral Quantitative result for obtaining portland slag cement sample is as shown in figure 14.
The known or whole unknown crystal structure refinement quantitative results in the part 4 Rietveld- of table
Wherein, Hatrurite M3, Hatrurite M1, C2S beta, C2S beta (JOST),
Brownmillerite, C3A Cubic, the main composition that Periclase, Clinker-amor are clinker, Slag is institute
The known or whole unknown crystal structure phases in the slag part of foundation.
It is found that quantitatively obtaining clinker content by the known or whole unknown crystal structure refinements in the part Reitveld- and being
77.7%, slag content 22.2%.The error of slag content calculated value and actual value is+1.2%.
Claims (5)
1. it is a kind of measurement portland slag cement in silicate mineral and slag content method, which is characterized in that including with
Lower step:
1.1, the foundation of the known or whole unknown crystal structure phases in slag part:
1.1.1, slag powder sample is made to 5~15 μm in the granulated blast-furnace slag by vitreum content 95% or more, grinding；
1.1.2, slag 4~6g of powder sample is weighed, the ZnO reference substance for occupying slag powder sample quality 12%~18% is weighed
Matter is added 8~12ml of organic solvent, above-mentioned three is stirred evenly, batch mixer mix grinding, and drying obtains slag and mixes with zinc oxide
Uniform mixed-powder, granularity control is between 5~10 μm after mix grinding；
1.1.3, using the diffraction data of X-ray diffractometer acquisition slag powder sample, according to diffraction data combination mixed-powder
Relative amount between middle zinc oxide and slag powder sample calculates the calibration constants (ZMV) of slag, determines that the structure of slag is real
Body determines the amorphous phase situation of slag powder sample, obtain the known or whole unknown crystal structure phase structure texts in slag part
Part；
1.2, portland slag cement slag content quantifies:
1.2.1, by the size controlling of portland slag cement between 5~15 μm；
1.2.2, portland slag cement is fitted into X-ray diffraction specimen holder using back dress method, is acquired using X-ray diffractometer
The diffraction data of portland slag cement；
1.2.3, according to diffraction data determine portland slag cement contained in mineral mineral structure file；
1.2.4, known to the slag part obtained according to mineral structure file combination step 1.1 or whole unknown crystal structure is mutually tied
Structure file carries out quantitative analysis, obtains the relative amount of each mineral and slag in portland slag cement.
2. the side of silicate mineral and slag content in a kind of measurement portland slag cement according to claim 1
Method, it is characterised in that: in the step 1.1.2, the mass ratio of slag powder sample and ZnO standard substance are as follows: (82~88):
(18~12).
3. the side of silicate mineral and slag content in a kind of measurement portland slag cement according to claim 1
Method, it is characterised in that: the solid-liquid ratio of the slag powder sample and organic solvent is 1g:2ml.
4. the side of silicate mineral and slag content in a kind of measurement portland slag cement according to claim 1
Method, it is characterised in that: the organic solvent be dehydrated alcohol, isopropanol, methanol and hexamethylene etc. not with portland cement, mine
The organic solvent that slag chemically reacts.
5. the side of silicate mineral and slag content in a kind of measurement portland slag cement according to claim 1
Method, it is characterised in that: in the step 1.2.2, X-ray diffractometer acquires the condition of X ray diffracting spectrum are as follows: voltage and current is
30Kv/10mA；Lynxeye detector array is open 4.8 °；Divergent slit (DS)=0.6mm (0.3 °)；Front and back rope drawing slit=
2.5°；8mm shading knife；3mm antiscatter slits；Sample stage revolving speed 15rpm.
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| CN114441588A (en) * | 2020-11-05 | 2022-05-06 | 中国建筑材料科学研究总院有限公司 | Method and device for measuring granulated blast furnace slag content in cement |
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| 许闽等: ""使用PONKCS法确定水泥中的方镁石含量"", 《新型建筑材料》 * |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114441588A (en) * | 2020-11-05 | 2022-05-06 | 中国建筑材料科学研究总院有限公司 | Method and device for measuring granulated blast furnace slag content in cement |
| CN112985946A (en) * | 2021-03-10 | 2021-06-18 | 南京海关工业产品检测中心 | Detection method for judging oxidation degree of copper concentrate containing bornite |
| CN112985946B (en) * | 2021-03-10 | 2022-03-08 | 南京海关工业产品检测中心 | Detection method for judging oxidation degree of copper concentrate containing bornite |
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