CN104048963B - The method of testing of sulfate dihydrate calcium content in desulfurated plaster - Google Patents
The method of testing of sulfate dihydrate calcium content in desulfurated plaster Download PDFInfo
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- 239000011505 plaster Substances 0.000 title claims abstract description 66
- PASHVRUKOFIRIK-UHFFFAOYSA-L calcium sulfate dihydrate Chemical compound O.O.[Ca+2].[O-]S([O-])(=O)=O PASHVRUKOFIRIK-UHFFFAOYSA-L 0.000 title claims abstract description 41
- 238000010998 test method Methods 0.000 title claims abstract description 18
- 239000000243 solution Substances 0.000 claims abstract description 28
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 claims abstract description 25
- 239000000463 material Substances 0.000 claims abstract description 22
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 20
- 238000012360 testing method Methods 0.000 claims abstract description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 13
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000007788 liquid Substances 0.000 claims abstract description 8
- 239000011259 mixed solution Substances 0.000 claims abstract description 8
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims abstract description 7
- 238000012216 screening Methods 0.000 claims abstract description 7
- 238000004448 titration Methods 0.000 claims abstract description 7
- 238000012545 processing Methods 0.000 claims abstract description 4
- 238000005070 sampling Methods 0.000 claims abstract description 4
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 61
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 35
- 229910052602 gypsum Inorganic materials 0.000 claims description 32
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 claims description 24
- KWYUFKZDYYNOTN-UHFFFAOYSA-M potassium hydroxide Substances [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 20
- 239000010440 gypsum Substances 0.000 claims description 12
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Chemical compound [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 claims description 11
- 238000006477 desulfuration reaction Methods 0.000 claims description 10
- 230000023556 desulfurization Effects 0.000 claims description 9
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 7
- 229910052925 anhydrite Inorganic materials 0.000 claims description 7
- 239000011575 calcium Substances 0.000 claims description 7
- 229910052791 calcium Inorganic materials 0.000 claims description 7
- 230000001186 cumulative effect Effects 0.000 claims description 4
- 239000002253 acid Substances 0.000 claims description 3
- 239000003513 alkali Substances 0.000 claims description 3
- 235000019256 formaldehyde Nutrition 0.000 claims description 3
- 239000006166 lysate Substances 0.000 claims description 3
- 229910052760 oxygen Inorganic materials 0.000 claims description 3
- 239000002904 solvent Substances 0.000 claims description 3
- 239000006071 cream Substances 0.000 claims 1
- ZZVUWRFHKOJYTH-UHFFFAOYSA-N diphenhydramine Chemical compound C=1C=CC=CC=1C(OCCN(C)C)C1=CC=CC=C1 ZZVUWRFHKOJYTH-UHFFFAOYSA-N 0.000 claims 1
- 239000004575 stone Substances 0.000 claims 1
- 238000009835 boiling Methods 0.000 abstract 1
- 238000001816 cooling Methods 0.000 abstract 1
- 238000000034 method Methods 0.000 description 13
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 6
- GBAOBIBJACZTNA-UHFFFAOYSA-L calcium sulfite Chemical compound [Ca+2].[O-]S([O-])=O GBAOBIBJACZTNA-UHFFFAOYSA-L 0.000 description 6
- 235000010261 calcium sulphite Nutrition 0.000 description 6
- 239000003546 flue gas Substances 0.000 description 6
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 description 4
- KJFMBFZCATUALV-UHFFFAOYSA-N phenolphthalein Chemical compound C1=CC(O)=CC=C1C1(C=2C=CC(O)=CC=2)C2=CC=CC=C2C(=O)O1 KJFMBFZCATUALV-UHFFFAOYSA-N 0.000 description 4
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 3
- 239000005864 Sulphur Substances 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- 238000002425 crystallisation Methods 0.000 description 3
- 230000008025 crystallization Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 238000011410 subtraction method Methods 0.000 description 3
- 239000003109 Disodium ethylene diamine tetraacetate Substances 0.000 description 2
- ZGTMUACCHSMWAC-UHFFFAOYSA-L EDTA disodium salt (anhydrous) Chemical compound [Na+].[Na+].OC(=O)CN(CC([O-])=O)CCN(CC(O)=O)CC([O-])=O ZGTMUACCHSMWAC-UHFFFAOYSA-L 0.000 description 2
- 235000011132 calcium sulphate Nutrition 0.000 description 2
- 230000007812 deficiency Effects 0.000 description 2
- 235000019301 disodium ethylene diamine tetraacetate Nutrition 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000005342 ion exchange Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- DEGAKNSWVGKMLS-UHFFFAOYSA-N calcein Chemical compound O1C(=O)C2=CC=CC=C2C21C1=CC(CN(CC(O)=O)CC(O)=O)=C(O)C=C1OC1=C2C=C(CN(CC(O)=O)CC(=O)O)C(O)=C1 DEGAKNSWVGKMLS-UHFFFAOYSA-N 0.000 description 1
- 239000001175 calcium sulphate Substances 0.000 description 1
- 239000004568 cement Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 230000035800 maturation Effects 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 229960002378 oftasceine Drugs 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 230000009183 running Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000012086 standard solution Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- DIZZDZCUMBBRSG-UHFFFAOYSA-J tetrasodium;2-[[5-[3-[3-[[bis(carboxylatomethyl)amino]methyl]-4-hydroxy-2-methyl-5-propan-2-ylphenyl]-1,1-dioxo-2,1$l^{6}-benzoxathiol-3-yl]-2-hydroxy-6-methyl-3-propan-2-ylphenyl]methyl-(carboxylatomethyl)amino]acetate Chemical compound [Na+].[Na+].[Na+].[Na+].[O-]C(=O)CN(CC([O-])=O)CC1=C(O)C(C(C)C)=CC(C2(C3=CC=CC=C3S(=O)(=O)O2)C=2C(=C(CN(CC([O-])=O)CC([O-])=O)C(O)=C(C(C)C)C=2)C)=C1C DIZZDZCUMBBRSG-UHFFFAOYSA-J 0.000 description 1
- PRZSXZWFJHEZBJ-UHFFFAOYSA-N thymol blue Chemical compound C1=C(O)C(C(C)C)=CC(C2(C3=CC=CC=C3S(=O)(=O)O2)C=2C(=CC(O)=C(C(C)C)C=2)C)=C1C PRZSXZWFJHEZBJ-UHFFFAOYSA-N 0.000 description 1
- 238000013519 translation Methods 0.000 description 1
Abstract
The invention discloses in a kind of desulfurated plaster sulfate dihydrate calcium content method of testing, including（1）Sampling drying；（2）Desulfurated plaster water and hydrochloric acid solution are dissolved, and is heated to boiling, added triethanolamine solution as screening agent after cooling, obtain mixed solution；（3）CMP indicator is added in mixed solution, and adds KOH solution until there is green fluorescence, continuously add excessive KOH solution；（4）Mixed liquor is titrated with EDTA standard liquids, is considered as titration end-point when color is changed into redness by green fluorescence, record volume V of consumed EDTA1；（5）Enter line blank test, blank volume V for consuming EDTA of record0；（6）Data processing：Calculate the amount and content of the material of calcium sulphate dihydrate in desulfurated plaster to be measured.Method of testing of the invention is simple to operate, test speed is fast, test result is accurate, with low cost.
Description
Technical field
The invention belongs to field of environment engineering technology, and in particular to the test of sulfate dihydrate calcium content in a kind of desulfurated plaster
Method, the method is suitable for the Limestone-gypsum Wet Flue Gas Desulfurization Process technique FGD system of thermal power plant to accessory substance desulfurated plaster
Quality is examined and determine.
Background technology
In recent years, FGD（English full name is " Flue Gas Desulphurization ", and Chinese translation is for " flue gas takes off
Sulphur "）System is widely used in coal-fired station of China because of its technology maturation, desulfuration efficiency height.The by-product in FGD systems
Thing desulfurated plaster quality is the important parameter of FGD plant runnings control, and the main component of gypsum is calcium sulphate dihydrate（CaSO4·
2H2O）, calcium sulfite hemihydrate（CaSO3·1/2H2O）, calcium carbonate（CaCO3）With a small amount of other impurities, wherein two water of main component
Typically more than 90%, calcium sulfite hemihydrate is less than 1% to the content of calcium sulfate, and calcium carbonate is less than 3%, and other impurities are mainly fluorinated
Thing, chloride etc..Desulfurated plaster is sentenced by the content of test main component calcium sulphate dihydrate, calcium sulfite hemihydrate and calcium carbonate
Disconnected quality quality, wherein calcium sulfite hemihydrate and calcium carbonate have the method for testing of comparative maturity, and the country there is presently no two
The concrete assay method of H 2 O calcium sulphate, is used mostly ion-exchange, barium sulfate precipitate method or by determining the crystallization water surveying
Calcium sulphate dihydrate.Calcium sulphate dihydrate in being not suitable for fluorine-containing, chlorine, phosphorus and other salts that can be exchanged using ion-exchange
Test, surveys calcium sulphate dihydrate using barium sulfate precipitate method and by determining the crystallization water, and cumbersome, resultant error is larger.
The content of the invention
The technical problem to be solved in the present invention is to overcome the deficiencies in the prior art, there is provided a kind of simple to operate, test speed
Hurry up, test result is accurate, in desulfurated plaster with low cost sulfate dihydrate calcium content method of testing.
To solve above-mentioned technical problem, the technical solution used in the present invention is sulfate dihydrate calcium content in a kind of desulfurated plaster
Method of testing, comprise the following steps：
（1）Sampling drying：Desulfurated plaster to be measured is weighed, and desulfurated plaster is dried；
（2）Acid adding, screening agent：Desulfurated plaster after drying is placed in a container, and successively add in container water and
Hydrochloric acid solution, dissolves desulfurated plaster, and gained lysate is heated to the 30s～60s that seethes with excitement and keep, normal temperature is subsequently cooled to,
Triethanolamine solution is added as screening agent, is fully shaken up, is obtained mixed solution；
（3）Plus indicator, alkali：To step（2）CMP indicator is added in the mixed solution of gained（I.e.（Calcein+first
Base thymol blue+phenolphthalein）Indicator）, then under black background add KOH solution until there is green fluorescence, continue to add
Enter excessive KOH solution, make mixed liquor pH value >=13 of the gained in green fluorescence；
（4）Titration：By step（3）The mixed liquor for obtaining uses EDTA under black background（Disodium ethylene diamine tetraacetate）Standard
Solution is titrated, and is considered as titration end-point when the color of mixed liquor is changed into redness by green fluorescence, what record was consumed
Volume V of EDTA1；
（5）Blank test：It is not added with desulfurated plaster repeat step（2）~（4）, blank volume V for consuming EDTA of record0；
（6）Data processing：As the following formula（1）Calculate the amount of the material of calcium sulphate dihydrate in desulfurated plaster to be measured：
n（CaSO4·2H2O）= n0- n（CaSO3·1/2H2O）- n（CaCO3）= C（EDTA）×（V1- V0）×10-3- m0×W（CaSO3·1/2H2O）/M（CaSO3·1/2H2O）- m0×W（CaCO3）/M（CaCO3）（1）
Formula（1）In：n（CaSO4·2H2O）For the amount of the material of calcium sulphate dihydrate in desulfurated plaster, unit is mol；n0For
The amount of the material of total calcium in desulfurated plaster, unit is mol；n（CaSO3·1/2H2O）For CaSO3·1/2H2The amount of the material of O,
Unit is mol；n（CaCO3）For CaCO3Material amount, unit is mol；C（EDTA）For the concentration of EDTA standard liquids, unit
For mol/L；V1To consume the cumulative volume of EDTA, unit is ml；V0For the blank volume for consuming EDTA, unit is ml；m0For desulfurization
The quality of gypsum, unit are g；W（CaSO3·1/2H2O）For CaSO3·1/2H2Mass fractions of the O in desulfurated plaster；W
（CaCO3）For CaCO3Mass fraction in desulfurated plaster；M（CaSO3·1/2H2O）For CaSO3·1/2H2The molal weight of O,
That is 129g/mol；M（CaCO3）For CaCO3Molal weight, i.e. 100g/mol；
As the following formula（2）Calculate the content of calcium sulphate dihydrate in desulfurated plaster to be measured：
W（CaSO4·2H2O）= n（CaSO4·2H2O）×M（CaSO4·2H2O）/m0×100% （2）
Formula（2）In：W（CaSO4·2H2O）For CaSO4·2H2Mass fractions of the O in desulfurated plaster；n（CaSO4·
2H2O）For the amount of the material of calcium sulphate dihydrate in desulfurated plaster, unit is mol；m0For the quality of desulfurated plaster, unit is g；M
（CaSO4·2H2O）For the molal weight of calcium sulphate dihydrate, i.e. 172g/mol.
In above-mentioned method of testing, it is preferred that the step（1）In, the quality of the desulfurated plaster to be measured be 0.1g～
0.15g。
In above-mentioned method of testing, it is preferred that the step（2）In, the addition volume of the water is 50ml～100ml,
The addition volume of the hydrochloric acid solution is 1ml～2ml, and in the hydrochloric acid solution, the mass fraction of HCl is 20%～25%.
In above-mentioned method of testing, it is preferred that the step（2）In, the addition volume of the triethanolamine solution is 4ml
～6ml, in the triethanolamine solution, the mass fraction of triethanolamine is 30%～40%, and solvent is water.
In above-mentioned method of testing, it is preferred that the step（3）In, the mass fraction of the KOH solution is 15%～
25%。
In above-mentioned method of testing, it is preferred that the step（3）In, the addition of the CMP indicator be 40mg～
60mg。
In above-mentioned method of testing, it is preferred that the step（4）In, the concentration of the EDTA standard liquids is
0.015mol/L～0.025mol/L.
In the present invention, calcium sulfite hemihydrate（CaSO3·1/2H2O）And calcium carbonate（CaCO3）Mass fraction respectively by marking
It is accurate《GB/T21508-2008 coal-fired flue gas desulfurization equipment performance method of testings》The method of testing and 6.13.3.3 of middle 6.13.3.2
Method of testing measure, be prior art.
Compared with prior art, it is an advantage of the current invention that：
Deficiency of the present invention for calcium sulphate dihydrate method of testing in current desulfurated plaster, it is proposed that direct using Subtraction method
The new method of calcium sulphate dihydrate in test desulfurated plaster.The method of the present invention first dissolves desulfurated plaster with hydrochloric acid solution, by adding
Heat makes Ca2+Clear up completely, the content of calcium sulphate dihydrate in desulfurated plaster is then determined using Subtraction method, i.e., using compleximetry
The total calcium in desulfurated plaster is measured, the molal quantity of total calcium deducts the molal quantity of calcium carbonate and calcium sulfite hemihydrate in desulfurated plaster,
So as to draw the molal quantity of calcium sulphate dihydrate, the percent mass of calcium sulphate dihydrate in desulfurated plaster is finally given.Existing de-
The direct test of calcium sulphate dihydrate is not involved with the method for testing of sulphur gypsum, but by testing sulfate ion or three oxygen
Change sulphur or the crystallization water and obtain the content of calcium sulphate dihydrate.
The present invention can greatly reduce the testing time using the content that Subtraction method surveys calcium sulphate dihydrate in desulfurated plaster, operate
Simply, as a result accurately, human and material resources, financial resources are saved, is conducive to the practical operation of thermal power plant staff, to each power plant
Desulfurization monitoring and accident treatment all have a great deal of practical meanings, with good economic benefit and social benefit.
Specific embodiment
Below in conjunction with concrete preferred embodiment, the invention will be further described, but not thereby limiting the invention
Protection domain.
Embodiment 1：
In a kind of desulfurated plaster of the present invention, the method for testing of sulfate dihydrate calcium content, comprises the following steps：
（1）Sampling drying：0.1068g is sampled from Limestone-gypsum Wet Flue Gas Desulfurization Process gypsum to be measured, is dried.
（2）Acid adding, screening agent：By step（1）Desulfurated plaster after drying is poured in the conical flask of 250ml, is initially charged
100ml water, adds the hydrochloric acid solution that 1ml mass fractions are 20%, dissolves desulfurated plaster, shake up；Gained lysate is heated
To seething with excitement and keeping 30s, normal temperature is subsequently cooled to（Usually 20 DEG C～30 DEG C）, add three second that 5ml mass fractions are 35%
Alkanolamine solution（Solvent is water）As screening agent, fully shake up, obtain mixed solution.
（3）Plus indicator, alkali：To step（2）50mg CMP indicator is added in the mixed solution of gained, i.e.,（Calcium is yellowish green
Element+methyl thymol blue+phenolphthalein）Indicator, purchased from St Cement Q Supervision ＆ Testing Center；Then delay under black background
It is slow to add the KOH that mass fraction is 20%（Potassium hydroxide）Solution adds 20% KOH of excessive 5ml until there is green fluorescence
Solution, the mixed liquor pH value in green fluorescence for making gained are 13.
（4）Titration：By step（3）The mixed liquor for obtaining is under black background with the EDTA that concentration is 0.02149mol/L
（Disodium ethylene diamine tetraacetate）Standard liquid is titrated, when the color of mixed liquor in conical flask is changed into redness by green fluorescence
When be considered as titration end-point, record the cumulative volume V of consumed EDTA1For 28.67ml；
（5）Blank test：It is not added with desulfurated plaster repeat step（2）~（4）, blank volume V for consuming EDTA of record0For
0.03ml；
（6）Data processing：As the following formula（1）Calculate the amount of the material of calcium in calcium sulphate dihydrate in gypsum：
n（CaSO4·2H2O）= n0- n（CaSO3·1/2H2O）- n（CaCO3）= C（EDTA）×（V1- V0）×10-3- m0×W（CaSO3·1/2H2O）/M（CaSO3·1/2H2O）- m0×W（CaCO3）/M（CaCO3）（1）
Formula（1）In：n（CaSO4·2H2O）For the amount of the material of calcium sulphate dihydrate in desulfurated plaster, unit is mol；n0For
The amount of the material of total calcium in desulfurated plaster, unit is mol；n（CaSO3·1/2H2O）For CaSO3·1/2H2The amount of the material of O,
Unit is mol；n（CaCO3）For CaCO3Material amount, unit is mol；C（EDTA）For the concentration of EDTA standard liquids, unit
For mol/L；V1To consume the cumulative volume of EDTA, unit is ml；V0For the blank volume for consuming EDTA, unit is ml；m0For desulfurization
The quality of gypsum, unit are g；W（CaSO3·1/2H2O）For CaSO3·1/2H2Mass fractions of the O in desulfurated plaster, at this
0.27% is specially in embodiment；W（CaCO3）For CaCO3Mass fraction in desulfurated plaster, is specially in the present embodiment
2.28%；M（CaSO3·1/2H2O）For CaSO3·1/2H2The molal weight of O, i.e. 129g/mol；M（CaCO3）For CaCO3Rub
You are quality, i.e. 100g/mol.
The amount for drawing the material of calcium sulphate dihydrate in the desulfurated plaster of the present embodiment by substituting into data is（5.889×10-4）mol.
As the following formula（2）Calculate the content of calcium sulphate dihydrate in desulfurated plaster：
W（CaSO4·2H2O）= n（CaSO4·2H2O）×M（CaSO4·2H2O）/m0×100%
Formula（2）In：W（CaSO4·2H2O）For CaSO4·2H2Mass fractions of the O in desulfurated plaster；n（CaSO4·
2H2O）For the amount of the material of calcium sulphate dihydrate in desulfurated plaster, unit is mol；m0For the quality of desulfurated plaster, unit is g；M
（CaSO4·2H2O）For the molal weight of calcium sulphate dihydrate, i.e. 172g/mol.
The mass fraction for drawing calcium sulphate dihydrate in the desulfurated plaster of the present embodiment by substituting into data is 94.84%.
Embodiment 2：
The method of testing of sulfate dihydrate calcium content, its step and 1 basic phase of embodiment in a kind of desulfurated plaster of the present invention
Together, differ only in：In step（1）In, 0.1362g is sampled from another Limestone-gypsum Wet Flue Gas Desulfurization Process gypsum to be tested, should
CaSO in desulfurated plaster3·1/2H2The mass fraction of O is 0.35%, CaCO in the gypsum3Mass fraction be 2.13%；In step
（4）In, V1For 35.78ml；In step（5）In, V0For 0.03ml.
Jing formulas（1）Calculate, show that the amount of the material of calcium sulphate dihydrate in the desulfurated plaster of the present embodiment is（7.356×10-4）Mol, mass fraction are 92.90%.
The above is only the preferred embodiment of the present invention, and protection scope of the present invention is not limited merely to above-mentioned enforcement
Example.All technical schemes belonged under thinking of the present invention belong to protection scope of the present invention.It is noted that for the art
Those of ordinary skill for, improvements and modifications under the premise without departing from the principles of the invention, these improvements and modifications also should
It is considered as protection scope of the present invention.
Claims (1)
1. in a kind of desulfurated plaster sulfate dihydrate calcium content method of testing, comprise the following steps：
（1）Sampling drying：Desulfurated plaster to be measured is weighed, and desulfurated plaster is dried；
（2）Acid adding, screening agent：Desulfurated plaster after drying is placed in a container, and water and hydrochloric acid are successively added in container
Solution, dissolves desulfurated plaster, and gained lysate is heated to the 30s～60s that seethes with excitement and keep, and is subsequently cooled to normal temperature, then plus
Enter triethanolamine solution as screening agent, fully shake up, obtain mixed solution；
（3）Plus indicator, alkali：To step（2）CMP indicator is added in the mixed solution of gained, is then added under black background
Enter KOH solution until there is green fluorescence, continuously add excessive KOH solution, make mixed liquor pH value of the gained in green fluorescence
≥13；
（4）Titration：By step（3）The mixed liquor for obtaining is titrated with EDTA standard liquids under black background, works as mixed liquor
Color be considered as titration end-point when being changed into redness by green fluorescence, record volume V of consumed EDTA1；
（5）Blank test：It is not added with desulfurated plaster repeat step（2）~（4）, blank volume V for consuming EDTA of record0；
（6）Data processing：As the following formula（1）Calculate the amount of the material of calcium sulphate dihydrate in desulfurated plaster to be measured：
n（CaSO4·2H2O）= n0- n（CaSO3·1/2H2O）- n（CaCO3）= C（EDTA）×（V1- V0）×10-3- m0×
W（CaSO3·1/2H2O）/M（CaSO3·1/2H2O）- m0×W（CaCO3）/M（CaCO3）（1）
Formula（1）In：n（CaSO4·2H2O）For the amount of the material of calcium sulphate dihydrate in desulfurated plaster, unit is mol；n0For desulfurization
The amount of the material of total calcium in gypsum, unit is mol；n（CaSO3·1/2H2O）For CaSO3·1/2H2The amount of the material of O, unit
For mol；n（CaCO3）For CaCO3Material amount, unit is mol；C（EDTA）For the concentration of EDTA standard liquids, unit is
mol/L；V1To consume the cumulative volume of EDTA, unit is ml；V0For the blank volume for consuming EDTA, unit is ml；m0For desulfurization stone
The quality of cream, unit are g；W（CaSO3·1/2H2O）For CaSO3·1/2H2Mass fractions of the O in desulfurated plaster；W（CaCO3）
For CaCO3Mass fraction in desulfurated plaster；M（CaSO3·1/2H2O）For CaSO3·1/2H2The molal weight of O, i.e. 129g/
mol；M（CaCO3）For CaCO3Molal weight, i.e. 100g/mol；
As the following formula（2）Calculate the content of calcium sulphate dihydrate in desulfurated plaster to be measured：
W（CaSO4·2H2O）= n（CaSO4·2H2O）×M（CaSO4·2H2O）/m0×100% （2）
Formula（2）In：W（CaSO4·2H2O）For CaSO4·2H2Mass fractions of the O in desulfurated plaster；n（CaSO4·2H2O）For
The amount of the material of calcium sulphate dihydrate in desulfurated plaster, unit is mol；m0For the quality of desulfurated plaster, unit is g；M（CaSO4·
2H2O）For the molal weight of calcium sulphate dihydrate, i.e. 172g/mol；
The step（1）In, the quality of the desulfurated plaster to be measured is 0.1g～0.15g；
The step（2）In, the addition volume of the water is 50ml～100ml, the addition volume of the hydrochloric acid solution be 1ml～
2ml, in the hydrochloric acid solution, the mass fraction of HCl is 20%～25%；
The step（2）In, the addition volume of the triethanolamine solution is 4ml～6ml, three second in the triethanolamine solution
The mass fraction of hydramine is 30%～40%, and solvent is water；
The step（3）In, the addition of the CMP indicator is 40mg～60mg；
The step（4）In, the concentration of the EDTA standard liquids is 0.02149mol/L～0.025mol/L；
The step（3）In, the mass fraction of the KOH solution is 15%～25%.
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