CN102175555B - Method for quickly analyzing phase component of building gypsum - Google Patents

Method for quickly analyzing phase component of building gypsum Download PDF

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CN102175555B
CN102175555B CN 201110033606 CN201110033606A CN102175555B CN 102175555 B CN102175555 B CN 102175555B CN 201110033606 CN201110033606 CN 201110033606 CN 201110033606 A CN201110033606 A CN 201110033606A CN 102175555 B CN102175555 B CN 102175555B
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content
sample
gypsum
constant weight
water
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CN102175555A (en
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谈晓青
陈宁
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Shanghai Building Science Research Institute Co Ltd
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Shanghai Building Science Research Institute Group Co Ltd
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Abstract

The invention belongs to the technique of building material analysis and relates to a method for quickly analyzing a phase component of building gypsum. The defects in the prior art are as follows: the demand on analytical instrument is high, the demand on the test condition is high, the analysis time is long and the operation steps are complex. The method comprises the following three steps: for quickly finishing the phase component analysis for the building gypsum, by utilizing the principle that the building gypsum loses the adhered water at 50 plus/minus 5 DEG C, loses all the crystal water above 180 DEG C and can have hydration reaction with water, the anhydrous gypsum in the building gypsum can combine with water in a 95% ethanol solution so as to form the hemi-hydrated gypsum, and the dihydrate gypsum cannot be generated by combining the hemi-hydrated gypsum with the water, wherein the three steps are as follows: measuring the contents of the adhered water and the anhydrous gypsum, measuring the content and purity of the hemi-hydrated gypsum, and measuring the content of the dihydrate gypsum. The method provided by the invention has the advantages that the analysis device is simple, only one halogen moisture tester is required, the test time is short, and the analysis result has stability and repeatability.

Description

A kind of quick phase composition analytical approach of plaster of Paris
Technical field
The invention belongs to the building materials analytical technology, specifically a kind of quick phase composition analytical approach of plaster of Paris.
Background technology
Plaster of Paris is made through high-temperature calcination by dihydrate gypsum, with β semi-hydrated gypsum CaSO 41/2H 2O is a principal ingredient.In calcination process, tend to produce a certain amount of solubility anhydrite III type CaSO 4The dihydrate gypsum CaSO that does not dewater 42H 2O.
Prior art shows, the performance of plaster of Paris and its semi-hydrated gypsum that contains, solubility anhydrite and the ratio of the dihydrate gypsum three-phase of dehydration is not relevant, relevant with its impurity that contains yet.This just needs accurately to analyze the content of each phase in the plaster of Paris, could control the quality of plaster of Paris.
Have much both at home and abroad, like the aquation method, excite aquation method, alcoholic solution aquation method, vacuum drying or atmosphere pressure desiccation, dehydration-reducing process etc. about the analytical approach of measuring the plaster of Paris phase composition.The shortcoming of prior art is: analytical instrument requires high; Analysis condition is required high; Analysis time is long; Complex operation step; Can not satisfy impact analysis result's greatly accuracy and stability if there is one in these factors.
As the starting material of the various gypsum based gel materials of preparation, the analyzing and testing of plaster of Paris phase composition is absolutely necessary, it can control the quality of Binder Materials in the source; For the manufacturer of extensive calcining plaster of Paris, analysis speed and accuracy are particularly important.Therefore invent that a kind of analysis speed is fast, analysis result accurately the quick phase composition analytical approach of plaster of Paris be very necessary.
Summary of the invention
The purpose of this invention is to provide that a kind of analysis speed is fast, the analysis result quick phase composition analytical approach of plaster of Paris accurately.
The objective of the invention is to realize like this:
1, a kind of quick phase composition analytical approach of plaster of Paris, step is following:
(1) attached water and anhydrite Determination on content;
Accurately take by weighing 5 gram sample weights with moisture determination instrument, be designated as g 1, be accurate to 0.001g; Add 5ml 95% ethanolic solution, sample moistening evenly after, moisture determination instrument is transferred to 50 ℃, dry to constant weight; Sample weight g after the record constant weight 2
Attached water content and anhydrite content are calculated as follows:
Work as g 1>g 2The time: W=(g 1-g 2)/g 1* 100%; X=0;
Work as g 1<g 2The time: W=0; X=15.11 (g 2-g 1)/g 1* 100%.
In the formula: W---attached water content, %;
X---III type anhydrite content, %;
g 1---add the preceding sample mass of 95% ethanolic solution, the unit gram;
g 2---add sample mass after the 95% ethanolic solution oven dry constant weight, the unit gram;
(2) semi-hydrated gypsum content and purity Determination on content;
Accurately take by weighing sample 5g with moisture determination instrument, be accurate to 0.001g, be designated as m 1In capacity distilled water, soak more than the 5h, then moisture determination instrument is transferred to 50 ℃, dry this sample, be designated as m to constant weight 2At last moisture determination instrument is transferred to 200 ℃, heat this sample, be designated as m to constant weight 3
Semi-hydrated gypsum content is calculated as follows:
Work as g 1>g 2The time: Y=5.37 (c+W) * 100%
Work as g 1<g 2The time: Y=5.37 (c-X * 0.265) * 100%
Wherein, c=m 2/ m 1-1;
Purity is calculated as follows: S=e/0.2093 * 100%
E=1-m wherein 3/ m 2
In the formula: Y-semi-hydrated gypsum content, %;
W-attached water content, %;
C-sample immersion increment;
S-purity, %;
E-dihydrate gypsum water of crystallization content;
m 1Sample mass before the-immersion, the unit gram;
m 2Sample mass after the-immersion oven dry constant weight, the unit gram;
m 3Sample appearance is heavy after the-dehydration, the unit gram;
g 1-adding the preceding sample mass of 95% ethanolic solution, unit restrains;
g 2Sample mass after the-adding 95% ethanolic solution oven dry constant weight, the unit gram;
(3) dihydrate gypsum Determination on content;
Accurately take by weighing the 5g sample with moisture determination instrument, be accurate to 0.001g, be designated as p 1Moisture determination instrument is transferred to 200 ℃, and sample weight after the record dehydration constant weight is designated as p 2
Dihydrate gypsum content is calculated as follows:
Work as g 1>g 2The time: Z=4.78 [(d-W)-Y * 0.062] * 100%
Work as g 1<g 2The time: Z=4.78 (d-Y * 0.062) * 100%
Wherein: d=1-p 2/ p 1
In the formula: Z-dihydrate gypsum content, %;
W-attached water content, %;
Y-semi-hydrated gypsum content, %;
D-semi-hydrated gypsum water of crystallization content;
p 1Samples weighed before the-dehydration, the unit gram;
p 2Samples weighed after the-dehydration, the unit gram.
The main points that the present invention implements are:
1, in above-mentioned steps (1), ethanolic solution concentration is 95%, otherwise will influence test findings.
2, in above-mentioned steps (2), sample needs in capacity distilled water, to soak more than the 5h, and the soak time upper limit is not required, and can spend the night after the sample soaked in water.
3, in order to make test findings more accurate, can suitably adjust " stop mode " of halogen moisture determination instrument, promptly consider the utmost point moisture loss in the dry run at a slow speed.
Characteristics of the present invention are:
1, the ultimate principle of utilization plaster of Paris phase composition analytical approach is all accomplished loaded down with trivial details test procedure the short form test operating process through a halogen moisture determination instrument.
2, through to the improvement and the repetition test of plaster of Paris phase composition analytical approach, combine fast, reliable halogen moisture determination instrument, shortened test period greatly, can reach to test the same day and went out the result same day, help control and the improvement of producer to product quality.
3, by halogen moisture determination instrument homogeneous heating stable properties, avoided the interference of human factor to greatest extent, made test findings have more stability and repeatability.Help the extensive popularization of this kind method.
4, the relevance research between promotion plaster of Paris phase composition and the performance promotes the development of this field theoretical research, instructs the application of gypsum base building materials.
The present invention is with the difference of domestic and international prior art:
1, loaded down with trivial details test procedure is all accomplished through a halogen moisture determination instrument, compares with traditional analytical method, has significantly simplified the test operation flow process.
2, combine quick, reliable halogen moisture determination instrument, shortened test period greatly.
3, owing to stablize, avoided the interference of human factor to greatest extent, made test findings have more stability and repeatability by halogen moisture determination instrument homogeneous heating.
The present invention and domestic and international comparing of existing like product, its creativeness be following some:
1, first the halogen moisture determination instrument is used for the analysis of plaster of Paris phase composition.
2, loaded down with trivial details test procedure is all accomplished through a halogen moisture determination instrument, simplified the test operation flow process.
3, plaster of Paris phase composition analytical approach is improved, shortened test period.
4, avoided the interference of human factor to greatest extent, made test findings have better stability and repeatability.
Advantage of the present invention is:
1, analytical equipment is simple, only needs a halogen moisture determination instrument can accomplish loaded down with trivial details Total Test step, simplifies analysis operation.
2, shortened test period greatly, can reach to test the same day and went out the result same day, helped control and the improvement of producer product quality.
3, avoided the interference of human factor to greatest extent, made test findings have more stability and repeatability.
4, test findings helps the relevance research between plaster of Paris phase composition and the performance accurately, promotes the development of this field theoretical research, instructs the application of gypsum base building materials.
Embodiment
Through embodiment the present invention is further specified below.
For the accuracy of analytical approach that the plaster of Paris phase composition is described and good repeatability; Give Shanghai building research institute laboratory, the Huaneng Group pit hole mouth first power plant laboratory and Waigaoqiao of Shaihai power plant laboratory respectively with four samples and make an experiment, three HS-43 halogen moisture determination instruments that testing laboratory all adopts Mei Tele company to produce.A, B, C, D adopt this patent: a kind of quick phase composition analytical approach of plaster of Paris, a, b, c, d adopt alcoholic solution aquation method (constant pressure and dry).A is corresponding with a, by that analogy.Two groups of result datas are listed in the table below, and carry out the variance comparison of statistics.Find out by following table; This patents are adopted in three laboratories: the measured experimental result of a kind of quick phase composition analytical approach of plaster of Paris is relatively more consistent; Variance numerical value all than adopting the little of alcoholic solution aquation method constant pressure and dry, can react the phase composition of plaster of Paris more accurately.
Quick phase composition analysis of plaster of Paris and alcoholic solution aquation method analysis result contrast table
Figure BDA0000046330570000051
The foregoing description is merely preference of the present invention, is not used for limiting the present invention, and is all within principle of the present invention, made any be equal to alternative, revise and change, all within protection scope of the present invention.

Claims (1)

1. the quick phase composition analytical approach of a plaster of Paris, step is following:
(1) attached water and III type anhydrite Determination on content;
Accurately take by weighing 5 gram sample weights with moisture determination instrument, be designated as g 1, be accurate to 0.001g; Add 5ml 95% ethanolic solution, sample moistening evenly after, moisture determination instrument is transferred to 50 ℃, dry to constant weight; Sample weight g after the record constant weight 2
Attached water content and III type anhydrite content are calculated as follows:
Work as g 1>g 2The time: W=(g 1-g 2)/g 1* 100%; X=0;
Work as g 1<g 2The time: W=0; X=15.11 (g 2-g 1)/g 1* 100%.
In the formula: W---attached water content, %;
X---III type anhydrite content, %;
g 1---add the preceding sample mass of 95% ethanolic solution, the unit gram;
g 2---add sample mass after the 95% ethanolic solution oven dry constant weight, the unit gram;
(2) semi-hydrated gypsum content and purity Determination on content;
Accurately take by weighing sample 5g with moisture determination instrument, be accurate to 0.001g, be designated as m 1In capacity distilled water, soak more than the 5h, then moisture determination instrument is transferred to 50 ℃, dry this sample, be designated as m to constant weight 2At last moisture determination instrument is transferred to 200 ℃, heat this sample, be designated as m to constant weight 3
Semi-hydrated gypsum content is calculated as follows:
Work as g 1>g 2The time: Y=5.37 (c+W) * 100%
Work as g 1<g 2The time: Y=5.37 (c-X * 0.265) * 100%
Wherein, c=m 2/ m 1-1;
Purity is calculated as follows: S=e/0.2093 * 100%
E=1-m wherein 3/ m 2
In the formula: Y-semi-hydrated gypsum content, %;
W-attached water content, %;
C---sample immersion increment;
S-purity, %;
E-dihydrate gypsum water of crystallization content;
m 1Sample mass before the-immersion, the unit gram;
m 2Sample mass after the-immersion oven dry constant weight, the unit gram;
m 3Sample appearance is heavy after the-dehydration, the unit gram;
g 1-adding the preceding sample mass of 95% ethanolic solution, unit restrains;
g 2Sample mass after the-adding 95% ethanolic solution oven dry constant weight, the unit gram;
(3) dihydrate gypsum Determination on content;
Accurately take by weighing the 5g sample with moisture determination instrument, be accurate to 0.001g, be designated as p 1Moisture determination instrument is transferred to 200 ℃, and sample weight after the record dehydration constant weight is designated as p 2
Dihydrate gypsum content is calculated as follows:
Work as g 1>g 2The time: Z=4.78 [(d-W)-Y * 0.062] * 100%
Work as g 1<g 2The time: Z=4.78 (d-Y * 0.062) * 100%
Wherein: d=1-p 2/ p 1
In the formula: Z-dihydrate gypsum content, %;
W-attached water content, %;
Y-semi-hydrated gypsum content, %;
D-semi-hydrated gypsum water of crystallization content;
p 1Samples weighed before the-dehydration, the unit gram;
p 2Samples weighed after the-dehydration, the unit gram.
CN 201110033606 2011-01-31 2011-01-31 Method for quickly analyzing phase component of building gypsum Expired - Fee Related CN102175555B (en)

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Publication number Priority date Publication date Assignee Title
CN106323799A (en) * 2015-06-25 2017-01-11 北新集团建材股份有限公司 Method of analyzing crystal water in gypsum plaster boards
CN105606639B (en) * 2015-12-30 2019-09-17 泰山石膏有限公司 The detection method of calcium sulphate crystal transformation temperature in a kind of gypsum raw material
CN105758761B (en) * 2016-03-01 2019-06-11 美巢集团股份公司 The measuring method of type III anhydrous gypsum content in a kind of building gypsum
CN106482992A (en) * 2016-09-19 2017-03-08 洛阳理工学院 A kind of method of gypsum crystallization water content in measure slurry
EP4253341A1 (en) 2022-03-30 2023-10-04 Saint-Gobain Placo Method and system for measuring phase components in calcium sulphate material

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4849175A (en) * 1984-05-16 1989-07-18 Societe Des Ciments Francais Apparatus for automatically determining certain characteristics of cement
CN101514981A (en) * 2008-02-21 2009-08-26 北新集团建材股份有限公司 Method for rapidly analyzing phase composition of building gypsum powder
CN101625300A (en) * 2009-08-18 2010-01-13 河北省电力研究院 Test method of sulphate content of desulfurization gypsum

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4849175A (en) * 1984-05-16 1989-07-18 Societe Des Ciments Francais Apparatus for automatically determining certain characteristics of cement
CN101514981A (en) * 2008-02-21 2009-08-26 北新集团建材股份有限公司 Method for rapidly analyzing phase composition of building gypsum powder
CN101625300A (en) * 2009-08-18 2010-01-13 河北省电力研究院 Test method of sulphate content of desulfurization gypsum

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