GB2148500A - Method for measuring concentration of CaCO3 in slurries - Google Patents
Method for measuring concentration of CaCO3 in slurries Download PDFInfo
- Publication number
- GB2148500A GB2148500A GB08420261A GB8420261A GB2148500A GB 2148500 A GB2148500 A GB 2148500A GB 08420261 A GB08420261 A GB 08420261A GB 8420261 A GB8420261 A GB 8420261A GB 2148500 A GB2148500 A GB 2148500A
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- GB
- United Kingdom
- Prior art keywords
- slurry
- caco3
- concentration
- air
- reactor container
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/46—Removing components of defined structure
- B01D53/48—Sulfur compounds
- B01D53/50—Sulfur oxides
- B01D53/501—Sulfur oxides by treating the gases with a solution or a suspension of an alkali or earth-alkali or ammonium compound
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- Health & Medical Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Biochemistry (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Environmental & Geological Engineering (AREA)
- Biomedical Technology (AREA)
- Molecular Biology (AREA)
- Physics & Mathematics (AREA)
- General Chemical & Material Sciences (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
- Treating Waste Gases (AREA)
Abstract
A method for continuously measuring a concentration of CaCO3 in slurries comprising CaCO3 comprises continuously sampling a given amount of the slurry, feeding the sampled slurry into an agitated continuous reactor container which is isolated from the outside air, keeping the slurry in the reactor container at a temperature of at least 50 DEG C, adding sulfuric acid or hydrochloric acid to adjust the pH to below 4, blowing air into the slurry in the reactor container, withdrawing from the reactor container CO2, produced by the reaction between CaCO3 and the acid, by entrainment with the air, and calculating a concentration of CaCO3 in the slurry from the concentration of CO2 in the withdrawn gas, the amount of the sampled slurry and the flow rate of the blown air.
Description
SPECIFICATION
Method for measuring a concentration of Ca CO3 BACKGROUND OF THE INVENTION
Field of the Invention
This invention relates to a method for continuously measuring a concentration of CaCO3 in slurries comprising CaCO3 such as, for example, an absorption liquid slurry used in flue gas desulfurization systems using a wet lime process.
Description of the Prior Art
The concentration of CaCO3 in an absorption solution used in flue gas desulfurization systems using a wet lime process has been heretofore measured by manual analysis. This manual analysis is disadvantageous in requiring hands and time.
SUMMARY OF THE INVENTION
The present invention is accomplished to overcome the above disadvantages. This object is achieved, according to the present invention, by a method for continuously measuring a concentration of CaCO3 in slurries comprising CaCO3, the method comprising:
continuously sampling a given amount of the slurry;
feeding the sampled slurry into an agitated continuous reactor container which is isolated from the outside air;
keeping the slurry at a temperature of at least 50 C; adding sulfuric acid or hydrochloric acid to adjust the pH to below 4;
blowing air into the slurry in the reactor container;
withdrawing from the reactor container CO2, produced by the reaction between CaCO3 and the acid, by entrainment with the air; and
calculating a concentration of CaCO3 in the slurry by operation of a concentration of CO2 in the mixed gas, the amount of the sampled slurry, and the flow rate of the blown air. The method may further comprise the steps of mixing the withdrawn gas with air, and calculating a concentration of CaCO3 in the slurry by operation of a concentration of CO2 in the mixed gas, the flow rate of the sampled slurry, the flow rate of the blown air, and the flow rate of the air being mixed.
BRIEF DESCRIPTION OF THE DRAWINGS
Figure 1 is a flowchart of an apparatus for measuring a concentration of CaCO3 according to the invention;
Figures 2(a) and 2(b) are graphical representations of the results of the measurement according to one embodiment of the invention; and
Figure 3 is a graphical representation of the relationship between measured value of CaCO3 concentration (mol/vol) determined according to the method of the invention and value determined by known manual analysis.
Figure 4 is a flowchart of a method according to the invention; and
Figure 5 is a graphical representation of the relationship between measured value of CaCO3 concentration (mol/vol) determined according to the method of the invention and value determined by known manual analysis.
DETAILED DESCRIPTION AND EMBODIMENTS OF THE INVENTION
Reference is now made to Fig. 1 which illustrates one embodiment of the invention.
In Fig. 1, sample slurry A comprising CaCO3 is sampled by a fixed displacement pump 1 and is heated through the heater 2 which is controlled by a signal from 1 temperature controller 3 after detection of a temperature of a resident liquid 6 in a reactor container 5 with a detector 4 so that the temperature of the resident liquid 6 is kept at a predetermined temperature, followed by feeding to the reactor container 5. In view of the detection efficiency of CaCO3, the temperature of the resident liquid 6 is preferred to be over 50"C, inclusive, with the upper limit to a boiling point of the liquid.
The pH of the liquid 6 in the reactor container 5 is checked by the use of a pH detector 14 and a delicate pump 12 is controlled by the signal from the pH adjuster 15, by which sulfuric acid (or hydrochloric acid) is introduced into the reactor container 5 and the pH in the system is adjusted to a predetermined level (below 4).
It will be noted that the upper limit of the temperature of the resident liquid 6 is a boiling point of the resident liquid and the pH is preferably controlled to be in the range of from 2 to 4.
During the operation, CO2 is generated according to the following reaction (1) or (2).
CaCO3 + H2SO4oCaSO4 + H20 + C02 t (1) CaCO3 + 2HCleCaCI2 + H20 + CO2 t (2)
In order to smoothly remove the generated CO2, part or all of air B whose flow rate is controlled at a given level by means of a flow controller 11 is blown into the resident liquid through a flow indicator 17 and an air blowing pipe 17 by manupilation of a distributing valve 22. During this operation, the resident liquid 6 is agitated by means of an agitator 7 driven through a sealing material 9 by a motor 10 so that the solid matters contained in the resident liquid 6 in the reactor container 5 do not settle.
An excess of the resident liquid 6 caused by the feed of sample slurry A from the fixed displacement pump 1 is discharged from an overflow pipe 23 into a liquid sealing device 13.
The sealing device 13 is kept at a depth of the liquid which can overcome the inner pressure of the reactor container 5, thus preventing leakage of the C02-containing gas E (withdrawn gas) in the reactor container 5 by entrainment with the overflow. In addition, the sealing device 13 is so designed that the solid matters in the overflow do not settle. The excess of the overflow charged into the liquid sealing device 13 is discharged as waste liquor D.
The mixed gas (withdrawn gas) E consisting of the CO2 generated according to the reaction equation (1) or (2) and the air and evaporated moisture from the air blowing pipe 8 is combined with air which flows through a bypath of the reactor 6 is released as exhaust F. In this connection, part of the exhaust F is subjected to a dehumidifer 24 to remove the moisture therefrom as drain H, then sucked by an air pump 18 and fed to a CO, analyzer 19 in which the concentration of CO2 in the exhaust is measured, followed by discharging as exhaust G. The reason why the air 16 is combined with the mixed gas E is that the gas E is diluted to a level at which the detection with the CO2 analyzer becomes possible. No dilution is necessary when the CO, analyzer 19 has great capability of detection.
The detection signal from the C02 analyzer 19 is fed to is fed to an operator 20 for calculation of a concentration of CaCO3 in the sampled slurry A. To the operator 21 are also inputted flow signal *1 from the air flow meter 11 and flow signal *2 from the fixed displacement pump 1 for the sampling of slurry. These three input signals are logically operated in the operator 20 according to the following equation, thereby determining a concentration of CaCO3 in the sampled slurry A. The concentration of CaCO3 is indicated by a CaCO3 concentration indicator 21.
QxX
Concentration of CaCO3 = (3) [ mol/li (1 0O-X) X 22.4 x F
0: flow rate of air [ Nl/min ] F: flow rate of slurry being sampled [ 1/min ] X: concentration of CO2 [ vol% ] As described before, according to the invention, it is possible to continuously detect a concentration of CaCO3 in slurry.
The present invention is more particularly described by way of example.
Example 1.
A test plant shown in Fig. 1 was used to effect a continuous measurement of a concentration of CaCO3 in a CaCO3-containing slurry under the following conditions.
Concentration of CaCO3 is sample slurry: 0.05, 0.1, 0.2 mol/l
Amount of sampled slurry: 0.12 I/min Flow rate of blown air: 7 Nl/min
Setting of reaction temperature: 50 C Setting of pH for reaction: 4
Preset concentration of CO2: 2 vol%
Total flow rate of air: 20 Nl/min
Reactor container: 1 liter in capacity
The results of the measurement are shown in Figs. 2(a) and 2(b). Fig. 2(b) is a graph of the detected CaCO3 concentration in the slurry sampled at 1-n of Fig. 2(a).
In Fig. 3, the values detected by the method of the invention are indicated as circles in relation to the analytical values obtained by known manual analysis, in which the mark "solid circle" indicates the results using hydrochloric acid and the mark "simple circle" indicates the results using sulfuric acid.
The test was effected using three different concentrations of CaCO3 in slurry, and typical results of the measured value of CO2, manually analytical value of CaCO3, and value of CaCO3 detected according to the invention are shown in the following table 1.
Table 1
Test No. 1 2 3
Concentration of CaCO3 mol/1 0.056 0.104 0.192
by manual analysis
Concentration of CaCO3 mol/l 0.053 0.100 0.195 according to invention
Concentration of CO2 % 0.71 1.32 2.55
Acid used HCI H2SO4 H2SO4
Reference is now made to Fig. 4 which illustrates another embodiment of the invention.
In Fig. 4, there is shown a flowchart of a test plant of measuring a concentration of CaCO3 in which indicated at A is a sample slurry, at B is air, at C is sulfuric acid (or hydrochloric acid), at
D is a waste liquor, at E is a withdrawn gas consisting of air comprising CO2, at F is an exhaust, at G is an exhaust, and at H is drain.Moreover, indicated at 1 is a fixed displacement pump, at
2 is a heater, at 3 is a temperature controller, at 4 is a temperature detector, at 5 is an agitated continuous reactor container which is a closed system or is isolated from the outside air, at 6 is a resident liquid, at 7 is an agitator, at 8 is an air blowing pipe, at 9 is a sealing material, at 10 is a motor, at 11 is a flow controller, at 12 is a delicate pump, at 13 is a liquid sealing device, at 14 is a pH electrode, at 15 is a pH adjuster, at 16 is a dehumidifier, at 17 is an air pump, at
18 a CO, analyzer, at 19 is a CO, concentration setting device, at 20 is a secondary air flow rate controller, at 21 is an operator, at 22 is an indicator, at 23 is an overflow pipe, and at *1, *2 and *3 are signals.
In operation, a given amount of sample slurry A comprising CaCO3 is sampled by the fixed displacement pump 1 and is heated through the heater 4 which is controlled by the signal from the temperature controller 3 after detection of a temperature of the resident liquid 6 in the reactor container 5 with the detector 4 so that the temperature of the resident liquid 6 is kept at a predetermined temperature (50 C), followed by feeding to the reactor container 5. The pH of the liquid 6 in the reactor container 5 is checked by the use of the pH detector 14 and the delicate pump 12 is controlled by the signal from the pH adjuster 15. As a consequence, sulfuric acid (or hydrochloric acid) is introduced into the reactor container 5 and the pH in the system is adjusted to a predetermined level (below 4).It will be noted that the upper limit of the temperature of the resident liquid 6 is a boiling point of the resident liquid and the pH is preferably controlled to be in the range of from 2 to 4.
During the operation, CO2 is generated according to the said reaction (1) or (2).
In order to smoothly remove the generated CO2, air B whose flow rate is controlled at a given level by means of the flow controller 11 is blown through the air blowing pipe 8 into the resident liquid 6. At the same time, the resident liquid 6 is agitated by means of the agitator 7 driven through the sealing material 9 by the motor 10 so that the solid matters contained in the resident liquid 6 in the reactor container 5 do not settle.
An excess of the resident liquid 6 resulting from the feed of sample slurry from the fixed displacement pump 1 is discharged from the overflow pipe 23 into the liquid sealing device 13, in which the liquid level is so controlled as to overcome the inner pressure of the reactor container 5, thus preventing leakage of the C02-containing gas E (withdrawn gas) in the reactor container 5 by entrainment with the overflow. In addition, the sealing device 13 is so designed that the solid matters in the overflow do not settle. The excess of the overflow charged into the liquid sealing device 13 is discharged as waste liquor D.
The withdrawn gas E consisting of the CO2 generated according to the reaction equation (1) or (2), and the air and evaporated moisture from the air blowing pipe 8 is combined with secondary air (air for dilution) whose flow rate is controlled with the secondary air flow controller at a present value controlled by a CO2 concentration signal described hereinafter. Thereafter, the combined mixture is released as exhaust F. In this connection, part of the exhaust F is subjected to the dehumidifer 16 to remove the moisture therefrom as drain H and then sucked by the air pump 17 in the C02 analyzer 18 in which the concentration of C02 in the exhaust is measured, followed by discharging as exhaust G.
One of detection signals from the CO, analyzer 18 is fed to the C02 concentration setter 19 by which the preset flow rate in the secondary air flow controller 20 is so controlled that the detected concentration of CO2 reaches preset concentration of CO2. Another signal from the CO2 concentration setter 18 is fed to the operator 21 for calculation of a concentration of CaCO3 in the sampled slurry A. To the operator 21 are also inputted flow signal *2 from the air flow meter 11, flow signal *1 from the secondary air flow controller 20 and flow signal *3 from the fixed displacement pump 1 for the sampling of slurry.These four input signals are logically operated in the operator 21 according to the following equation, thereby determining a concentration of CaCO3 in the sampled slurry A. The concentration of CaCO3 is indicated by the CaCO3 concentration indicator 22.
x (q4 + Q2) Concentration of CaCO3 = (-----)(------) (4) [mol/1] 100-x 22.4 x F
Q1: flow rate of blown air [ NI/min ] Q2: flow rate of secondary air [ NI/min ] F: flow rate of slurry being sampled [ I/min ] x: concentration of CO2 [vol%]
As described before, according to the invention, it is possible to continuously detect a concentration of CaCO3 in slurry even though the concentration of CaCO3 in slurry widely varies.
Example 2
The present invention is more particularly described by way of example with reference to Figs.
4 and 5. A test plant shown in Fig. 4 was used to effect a test under the following conditions.
Concentration of CaCO3 in sample slurry: 0.01, 0.05, 0.1, 0.2 mol/l
Amount of sampled slurry: 0.12 I/min Total flow rate of air: 7 Nl/min
Setting of reaction temperature: 50 C Setting of pH for reaction: 4
Preset concentration of CO2: 2 vol%
Reactor container: 1 liter in capacity
The results of the measurement shown in Fig. 2 were obtained. In Fig. 5, the values detected by the method of the invention are indicated as circles in relation to the analytical values obtained by known manual analysis, in which the mark "solid circle" indicates the results using hydrochloric acid and the mark "simple circle" indicates the results using sulfuric acid.The test was effected using four different concentrations of CaCO3 in slurry, and typical results of the measured value of CO2, flow rate of secondary air, manually analytical value of CaCO3, and detected value of CaCO3 are shown in the following table 2.
Table 2
Items and Unit Test No. 1 2 3 4
Concentration of CaCO3 mol/l 0.0094 0.053 0.101 0. 196 by manual analysis
Concentration of CaCO3 mol/l 0.009 0.052 0.098 0.193 according to invention
Measured value of CO2 vol% 0.35 1.95 2.02 2.02 concentration
Flow rate of secondary air Nl/min 0.0 0.0 5.8 18.2
As will be appreciated from the foregoing, according to the invention, it becomes possible to accurately measure a concentration of CaCO3 in slurry within a short time and in a continuous manner.
It should be noted that the present invention is not limited to the example described above and various variations and modifications may be possible without departing from the scope and spirit of the present invention.
Claims (6)
1. A method for continuously measuring a concentration of CaCO3 in slurries comprising CaCO3, the method comprising:
continuously sampling a given amount of the slurry;
feeding the sampled slurry into an agitated continuous reactor container which is isolated from the outside air;
keeping the slurry at a temperature of at least 50 C; adding sulfuric acid or hydrochloric acid to adjust the pH to below 4;
blowing air into the slurry in the reactor container;
withdrawing from the reactor container CO2, produced by the reaction between CaCO3 and the acid, by entrainment with the air; and
calculating a concentration of CaCO3 in the slurry by operation of a concentration of CO2 in the mixed gas, the amount of the sampled slurry, and the flow rate of the blown air.
2. A method for continuously measuring a concentration of CaCO3 in slurries comprising CaCO3, the method comprising:
continuously sampling a given amount of the slurry;
feeding the sampled slurry into an agitated continuous reactor container which is isolated from the outside air;
keeping the slurry at a temperature of at least 50 C; adding sulfuric acid or hydrochloric acid to adjust the pH to below 4;
blowing air into the slurry in the reactor container;
withdrawing from the reactor container CO2, produced by the reaction between CaCO3 and the acid, by entrainment with the air;
mixing the withdrawn gas with air for dilution; and
calculating a concentration of CaCO3 in the slurry by operation of a concentration of CO2 in the mixed gas, the amount of the sampled slurry, and the flow rate of the mixed gas.
3. A method for continuously measuring a concentration of CaCO3 in slurries comprising CaCO3, the method comprising:
continuously sampling a given amount of the slurry;
feeding the sampled slurry into an agitated continuous reactor container which is isolated from the outside air;
keeping the slurry in the reactor container at a temperature of at least 50 C; adding sulfuric acid or hydrochloric acid to adjust the pH to below 4;
blowing a known flow rate of air into the slurry;
withdrawing from the reactor container CO2, produced by the reaction between CaCO3 and the acid, by entrainment with the air;;
further mixing the withdrawn gas with air for dilution while controlling a flow rate of the dilution air so that the concentration of CO, in the mixed gas is maintained constant; and
calculating a concentration of CaCO3 in the slurry by operation of the concentration of CO2 in the mixed gas, the flow rate of the blown air, the flow rate of the dilution air and the amount of the sampled slurry.
4. A method for continuously measuring a concentration of CaCO3 in slurries comprising CaCO3, the method comprising:
continuously sampling a given amount of the slurry;
feeding the sampled slurry into an agitated continuous reactor container which is isolated from the outside air;
keeping the slurry in the reactor container at a temperature of at least 50 C; adding sulfuric acid or hydrochloric acid to adjust the pH to below 4;
blowing a known flow rate of air into the slurry;
withdrawing from the reactor container CO2, produced by the reaction between CaCO3 and the acid, by entrainment with the air;
further mixing the withdrawn gas with air for dilution while controlling a flow rate of the dilution air so that the concentration of CO2 in the mixed gas is maintained constant; and
calculating a concentration of CaCO3 in the slurry by operation of the concentration of CO2 in the mixed gas, the flow rate of the mixed gas and the amount of the sampled slurry.
5. The method according to Claim 1 or 2, wherein the temperature of the slurry in the reactor container is in the range of from 50 C to a boiling point of the slurry stayed in the reactor container.
6. The method according to Claim 1 or 2, wherein the pH of the slurry is from 2 to 4.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP58144893A JPS6036955A (en) | 1983-08-10 | 1983-08-10 | Method for measuring concentration of caco3 in slurry |
| JP58144895A JPS6036957A (en) | 1983-08-10 | 1983-08-10 | Method for measuring concentration of caco3 in slurry |
Publications (3)
| Publication Number | Publication Date |
|---|---|
| GB8420261D0 GB8420261D0 (en) | 1984-09-12 |
| GB2148500A true GB2148500A (en) | 1985-05-30 |
| GB2148500B GB2148500B (en) | 1987-02-04 |
Family
ID=26476172
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| GB08420261A Expired GB2148500B (en) | 1983-08-10 | 1984-08-09 | Method for measuring concentration of caco3 in slurries |
Country Status (2)
| Country | Link |
|---|---|
| DE (1) | DE3429951A1 (en) |
| GB (1) | GB2148500B (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CZ298457B6 (en) * | 2006-01-06 | 2007-10-10 | Vysoká škola chemicko - technologická v Praze | Method of determining reactivity of limestone suspensions and additive limestone suspensions for flue gas wet desulphurization |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| AT393462B (en) * | 1990-05-08 | 1991-10-25 | Waagner Biro Ag | METHOD FOR DETERMINING THE REACTIVITY OF A LIMESTONE SUSPENSION CIRCULATELY USED IN A WASHER |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS59150339A (en) * | 1983-02-17 | 1984-08-28 | Mitsubishi Heavy Ind Ltd | Continuous measurement of concentration of carbonate and sulfite in liquid |
-
1984
- 1984-08-09 GB GB08420261A patent/GB2148500B/en not_active Expired
- 1984-08-10 DE DE19843429951 patent/DE3429951A1/en active Granted
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CZ298457B6 (en) * | 2006-01-06 | 2007-10-10 | Vysoká škola chemicko - technologická v Praze | Method of determining reactivity of limestone suspensions and additive limestone suspensions for flue gas wet desulphurization |
Also Published As
| Publication number | Publication date |
|---|---|
| DE3429951C2 (en) | 1987-10-29 |
| GB8420261D0 (en) | 1984-09-12 |
| GB2148500B (en) | 1987-02-04 |
| DE3429951A1 (en) | 1985-02-28 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PE20 | Patent expired after termination of 20 years |
Effective date: 20040808 |