CN104297236A - Method for detecting content of active calcium oxide and non-active calcium oxide in lime - Google Patents
Method for detecting content of active calcium oxide and non-active calcium oxide in lime Download PDFInfo
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- CN104297236A CN104297236A CN201410534731.4A CN201410534731A CN104297236A CN 104297236 A CN104297236 A CN 104297236A CN 201410534731 A CN201410534731 A CN 201410534731A CN 104297236 A CN104297236 A CN 104297236A
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Abstract
The invention discloses a method for detecting the content of active calcium oxide and non-active calcium oxide in lime. The method comprises the steps of crushing lime until the particle diameter is less than or equal to 0.150mm, and drying at 105-110 DEG C for 1.5-2.5 hours; taking 0.5000g of a test sample, and mixing with a blend of 4g of anhydrous sodium carbonate and boric acid, fusing at 880-920 DEG C for 16-24 minutes, putting the fused blocks into 60ml of 8% hydrochloric acid and dissolving at 100-110 DEG C, enabling the volume of a solution to be constant by a 250ml volumetric flask so as to obtain a test solution a; taking 0.5000g of a test sample additionally, adding 5g of saccharose and 45-55ml of water which is boiled firstly and then cooled, vibrating closely for 18-22 minutes, enabling the volume of the solution to be constant by a 250ml volumetric flask so as to obtain a test solution b; removing 50.00ml of the test solution a and the test solution b, and respectively adding 5ml of triethanolamine and 20% potassium hydroxide or sodium hydroxide, so that the pH value of the test solution is greater than or equal to 12.5; then adding 4-5 drops of 1mg/ml magnesium oxide standard solution and 2-3 drops of calconcarboxylic acid, titrating the test solution by an EDTA standard solution until the test solution turns blue from red. The content of the active calcium oxide is calculated according to the following formula as shown in the specification, and the content of the non-active calcium oxide is calculated according to the following formula as shown in the specification, wherein W does not refer to CaO=WTCaO_WfCaO. The method is used for rapidly and accurately detecting the content of the active calcium oxide and non-active calcium oxide in a lime test sample, and is high in popularization and application value.
Description
Technical field
The invention belongs to raw materials for metallurgy oxide content detection technique field, be specifically related to the detection method of active calcium oxide and nonactive calcium oxide content in a kind of lime.
Background technology
The principal ingredient of lime is by CaO, SiO
2, MgO, Fe
2o
3, Al
2o
3, the formation such as P, S and burning decrement.The conventional method measuring above element in lime detects according to " lime stone rauhkalk chemical analysis method " in GB/T 3286 series standard, but the content of calcium oxide comprises the summation of active calcium oxide and nonactive calcium oxide in lime in the lime adopting GB/T 3286 series standard to measure, active calcium oxide and nonactive calcium oxide cannot be separated.What react in metallurgical production is determined by the active calcium oxide in metallurgy lime, and the calcium oxide relation namely generated because of raw burn, burning with nonactive calcium oxide is little.Therefore carry out Accurate Determining to active calcium oxide in lime and nonactive calcium oxide content to be of great practical significance to smelting production.Because difficulty is comparatively large, also do not have effective method can measure the active calcium oxide in lime and nonactive calcium oxide content at present.Therefore, be necessary to research and develop a kind of accuracy high, good stability, analytical cycle is short, testing cost is low, is particularly useful for the detection method of active calcium oxide and nonactive calcium oxide content in lime sample, smelts production to upgrading, the active demand of falling basis, synergy to adapt to modernization.
Summary of the invention
The object of the present invention is to provide the detection method of active calcium oxide and nonactive calcium oxide content in a kind of lime.
The object of the present invention is achieved like this, the detection method of active calcium oxide and nonactive calcium oxide content in described lime, comprises sample pretreatment, peparation and titration measuring and calculating operation, specifically comprise:
A, sample pretreatment: lime sample to be measured is crushed to particle diameter≤0.150mm, in 105 ~ 110 DEG C of drying 1.5 ~ 2.5h.
B, peparation: get a 0.5000g sample and amount to the natrium carbonicum calcinatum of 4g and the blend of boric acid and mix on filter paper, wrap with filter paper in the iron crucible of inserting at the bottom of graphite pads, melting 16 ~ 24min at iron crucible being placed in 880 ~ 920 DEG C, after taking out cooling, frit is placed in the glass container of the hydrochloric acid solution filling 60ml concentration 8%, in 100 ~ 110 DEG C of heating, frit is dissolved after being closed by glass container, until solution is limpid, after being cooled to room temperature, solution is moved in 250ml volumetric flask, be settled to scale with water, shake up test solution a is for subsequent use; Separately get a 0.5000g sample and be placed in sealable glass container, add 5g sucrose, then add the water being cooled to room temperature after 45 ~ 55ml newly boils, by airtight for glass container rear vibration 18 ~ 22min, again solution is moved in 250ml volumetric flask, be settled to scale with water, shake up test solution b is for subsequent use.
C, titration measuring and calculating: respectively pipette 50.00ml test solution a, b, add potassium hydroxide or the sodium hydroxide solution of 5ml triethanolamine and concentration 20% respectively, make pH value >=12.5 of test solution, drip magnesium oxide standard solution and 2 ~ 3 calcon-carboxylic acids of 4 ~ 5 concentration 1mg/mL more respectively, then become blueness with EDTA standard solution titration test solution to it from redness and namely reach terminal.
The calculating of total calcium oxide massfraction is undertaken by following formula:
In formula:
W
tCaO---the massfraction of total calcium oxide in sample, %;
V
1---the total calcium oxide test solution of titration consumes the volume of EDTA standard solution, mL;
V
2---the blank test solution of the total calcium oxide of titration consumes the volume of EDTA standard solution, mL;
T---EDTA standard solution to the titer of calcium oxide, g/mL;
M---sample size, g;
V
3---pipette the volume of total calcium oxide test solution, mL.
The calculating of active calcium oxide massfraction is undertaken by following formula:
In formula:
W
fCaO---the massfraction of active calcium oxide in sample, %;
V
4---titration active calcium oxide test solution consumes the volume of EDTA standard solution, mL;
V
5---the blank test solution of titration active calcium oxide consumes the volume of EDTA standard solution, mL;
T---EDTA standard solution to the titer of calcium oxide, g/mL;
M---sample size, g;
V
6---pipette the volume of active calcium oxide test solution, mL.
The calculating of nonactive calcium oxide massfraction is undertaken by following formula: W
non-CaO=W
tCaO-W
fCaO
In formula:
W
non-CaO---the massfraction of nonactive calcium oxide in sample, %;
W
tCaO---the massfraction of total calcium oxide, %;
W
fCaO---the massfraction of active calcium oxide, %.
Detection method of the present invention has following beneficial effect:
Described method is optimized the particle size range that lime sample during sample pretreatment is pulverized, and effectively prevent excessive or too small caking, the sticky wall problem caused of sample particle diameter, make sample melting, dissolve rapider, reaction more evenly, completely.By optimizing melt temperature and the time of sample, decreasing dissipation during praducing frits, reducing analytical error.Mixed addition and the duration of oscillation of rear distilled water with sucrose by adjustment sample, accelerate the generation promoting lime saccharate, reaction is abundant fast, ensure that the accuracy of analysis.Method for making sample is being carried out on the basis of global optimization, the method of the invention has carried out corresponding adjustment to rate of titration further, detection is analyzed consuming time shorter, efficiency is higher, also indirectly decrease the duration of contact of test solution and air, reduce experimental error, make analysis result more reliable and accurate.
In sum, adopt the method for the invention to detect active calcium oxide in lime sample and nonactive calcium oxide content, testing result has good stability, reappearance and accuracy.In detection speed, it is fast that the method for the invention has analysis speed, and sense cycle is short, the feature that analysis efficiency is high, has not only saved detection time, alleviates the labour intensity of test analysis personnel, also reduces energy consumption, is conducive to enterprise's cost efficiency.In testing process, the method for the invention is simple to operate, easily learns well and understands, to test analysis personnel without excessive demand, has good popularizing application prospect.
Embodiment
The present invention is further illustrated below, but limited the present invention never in any form, and any conversion done based on training centre of the present invention or replacement, all belong to protection scope of the present invention.
The detection method of active calcium oxide and nonactive calcium oxide content in lime of the present invention, comprises sample pretreatment, peparation and titration measuring and calculating operation, specifically comprises:
Described sample pretreatment operation refers to and lime sample to be measured is crushed to particle diameter≤0.150mm, in 105 ~ 110 DEG C of drying 1.5 ~ 2.5h.
Described peparation operation refers to gets a 0.5000g sample and amounts to the natrium carbonicum calcinatum of 4g and the blend of boric acid and mix on filter paper, wrap with filter paper in the iron crucible of inserting at the bottom of graphite pads, melting 16 ~ 24min at iron crucible being placed in 880 ~ 920 DEG C, after taking out cooling, frit is placed in the glass container of the hydrochloric acid solution filling 60ml concentration 8%, in 100 ~ 110 DEG C of heating, frit is dissolved after being closed by glass container, until solution is limpid, after being cooled to room temperature, solution is moved in 250ml volumetric flask, be settled to scale with water, shake up test solution a is for subsequent use; Separately get a 0.5000g sample and be placed in sealable glass container, add 5g sucrose, then add the water being cooled to room temperature after 45 ~ 55ml newly boils, by airtight for glass container rear vibration 18 ~ 22min, again solution is moved in 250ml volumetric flask, be settled to scale with water, shake up test solution b is for subsequent use.
Described titration measuring and calculating operation refers to and respectively pipettes 50.00ml test solution a, b, add potassium hydroxide or the sodium hydroxide solution of 5ml triethanolamine and concentration 20% respectively, make pH value >=12.5 of test solution, drip magnesium oxide standard solution and 2 ~ 3 calcon-carboxylic acids of 4 ~ 5 concentration 1mg/mL more respectively, then become blueness with EDTA standard solution titration test solution to it from redness and namely reach terminal;
The calculating of total calcium oxide massfraction is undertaken by following formula:
In formula:
W
tCaO---the massfraction of total calcium oxide in sample, %;
V
1---the total calcium oxide test solution of titration consumes the volume of EDTA standard solution, mL;
V
2---the blank test solution of the total calcium oxide of titration consumes the volume of EDTA standard solution, mL;
T---EDTA standard solution to the titer of calcium oxide, g/mL;
M---sample size, g;
V
3---pipette the volume of total calcium oxide test solution, mL.
The calculating of active calcium oxide massfraction is undertaken by following formula:
In formula:
W
fCaO---the massfraction of active calcium oxide in sample, %;
V
4---titration active calcium oxide test solution consumes the volume of EDTA standard solution, mL;
V
5---the blank test solution of titration active calcium oxide consumes the volume of EDTA standard solution, mL;
T---EDTA standard solution to the titer of calcium oxide, g/mL;
M---sample size, g;
V
6---pipette the volume of active calcium oxide test solution, mL.
The calculating of nonactive calcium oxide massfraction is undertaken by following formula: W
non-CaO=W
tCaO-W
fCaO
In formula:
W
non-CaO---the massfraction of nonactive calcium oxide in sample, %;
W
tCaO---the massfraction of total calcium oxide, %;
W
fCaO---the massfraction of active calcium oxide, %.
In test solution a, the detection of nonactive calcium oxide content is mainly based on following reaction:
Ca
2++H
2Y
2-→CaY
2-+2H
+
In test solution b, the detection of active oxidation calcium content is mainly based on following reaction:
C
11H
22O
11+CaO+2H
2O→C
11H
22O
11·CaO·2H
2O
Ca
2++H
2Y
2-→CaY
2-+2H
+
In described sample pretreatment operation, lime sample to be measured particle diameter is after crushed 0.125 ~ 0.150mm.
In the natrium carbonicum calcinatum used in described peparation operation and the blend of boric acid, the mass ratio of natrium carbonicum calcinatum and boric acid is 2: 1 or 3: 2.
The filter paper used in described peparation operation is quantitative filter paper.
In the iron crucible at the bottom of graphite pads used in described peparation operation, the thickness of graphite linings is 0.5 ~ 1.0mm.
In described peparation operation, melt temperature is preferably 900 DEG C, and the melting time is preferably 20min.
The glass container used in described peparation operation is beaker.
In described peparation operation, glass container sealing is referred to and to be shielded on glass container with coverture.Such as be shielded on beaker with surface plate.
In described peparation operation, frit solution temperature is preferably 105 DEG C.
The sealable glass container used in described peparation operation is conical flask with cover, is such as with the conical flask of grournd glass lid.
The sealable glass container used in described peparation operation must be dry.
Refer to airtight for glass container tight for the grournd glass capping plug of conical flask in described peparation operation.
The water used in described peparation operation is any one in distilled water or deionized water.
The preferred 50ml of addition of the water of room temperature is cooled to after newly boiling in described peparation operation.
In described peparation operation, room temperature refers to 18 ~ 26 DEG C.
Airtight for glass container rear vibration being referred in described peparation operation is placed on oscillator by airtight for glass container, vibrates with the frequency of 200 ~ 300 beats/min.
In described peparation operation, duration of oscillation is preferably 20min.
The magnesium oxide standard solution used in described titration measuring and calculating operation is prepared as follows: take 1.0000g in advance prior to 850 DEG C of calcinations and the magnesium oxide being cooled to room temperature in exsiccator is placed in beaker, add 20mL water, mixing, cover table ware, add the hydrochloric acid of 20mL concentration 20%, in 105 ~ 110 DEG C of heating for dissolving, cooling, move in 1000mL volumetric flask, be diluted with water to scale, mix.。
Described magnesian purity is 99.9999%.
Described room temperature refers to 18 ~ 26 DEG C.
The calcon-carboxylic acid used in described titration measuring and calculating operation is add the potassium chloride porphyrize mixing gained powder of 50 g dryings by 0.5 g erichrome blue black R or add any one in 10g potassium sulfate porphyrize mixing gained powder by 0.1g calcium carboxylate.
The EDTA standard solution used in described titration measuring and calculating operation is prepared as follows: take 3.73g disodium ethylene diamine tetraacetate and be placed in beaker, add 100mL water, in 105 ~ 110 DEG C of heating for dissolving, be cooled to room temperature, move in 1 000 mL volumetric flasks, be diluted with water to scale, shake up, obtain standard solution; Described EDTA standard solution is demarcated as follows: pipette 20.00 mL calcium oxide standard solution 3 parts, be placed in beaker respectively, add 25 mL water, demarcate by titration step described in operation C, EDTA standard solution is undertaken by following formula the calculating of the titer of calcium oxide:
In formula:
T---EDTA standard solution to the titer of calcium oxide, g/mL;
M---pipette the amount of calcium oxide contained by calcium oxide standard solution, g;
V---titration 3 parts of calcium oxide standard solution consume the average external volume of EDTA standard solution, mL.
Potentiometric titrimeter is used to carry out titration to test solution in described titration measuring and calculating operation.
In described titration measuring and calculating operation, rate of titration is preferably 12 ~ 15ml/min.
embodiment 1
experiment material: elder brother's steel Longshan Mine taken from by lime sample to be measured.
Magnesium oxide standard solution is prepared as follows: take 1.0000g in advance prior to 850 DEG C of calcinations and the magnesium oxide being cooled to room temperature in exsiccator is placed in 250ml beaker, add 20mL water, mixing, cover table ware, add the hydrochloric acid of 20mL concentration 20%, in 108 DEG C of heating for dissolving, cooling, move in 1000mL volumetric flask, be diluted with water to scale, mix.
EDTA standard solution is prepared as follows: take 3.73g disodium ethylene diamine tetraacetate and be placed in 500ml beaker, add 100mL water, in 108 DEG C of heating for dissolving, be cooled to room temperature, move in 1 000 mL volumetric flasks, be diluted with water to scale, shake up, obtain standard solution.
EDTA standard solution is demarcated as follows: pipette 20.00 mL calcium oxide standard solution 3 parts, be placed in beaker respectively, add 25 mL water, demarcate by titration step described in operation C, EDTA standard solution is undertaken by following formula the calculating of the titer of calcium oxide:
=0.040/14.60=0.002740 g/mL
In formula:
T---EDTA standard solution to the titer of calcium oxide, g/mL;
M---pipette the amount of calcium oxide contained by calcium oxide standard solution, g;
V---titration 3 parts of calcium oxide standard solution consume the average external volume of EDTA standard solution, mL.
Experimental facilities: potentiometric titrimeter model 905, manufacturing enterprise is that Switzerland ten thousand leads to.
Experimental technique: lime sample to be measured is crushed to 0.125mm≤particle diameter≤0.150mm, in 108 DEG C of dry 2.0h.
Get a 0.5000g sample and the natrium carbonicum calcinatum amounting to 4g: the blend of boric acid=2:1 mixes on quantitative filter paper, wrapping with quantitative filter paper inserts in the rebasing iron crucible of the thick graphite linings of 0.50mm, melting 20min at iron crucible being placed in 900 DEG C, after taking out cooling, frit is placed in the beaker of the hydrochloric acid solution filling 60ml concentration 8%, cover on beaker with surface plate, in 105 DEG C of heating beakers, frit is dissolved, until solution is limpid, after being cooled to room temperature, solution is moved in 250ml volumetric flask, be settled to scale with distilled water, shake up test solution a is for subsequent use.Then the conical flask that a 0.5000g sample is placed in dry band grournd glass lid is separately got, add 5g sucrose, add the distilled water being cooled to 22 DEG C after 50ml newly boils again, by tight for the grournd glass capping plug of conical flask, be placed on oscillator with the hunting of frequency 20min of 250 beats/min, again solution is moved in 250ml volumetric flask, be settled to scale with distilled water, shake up test solution b is for subsequent use.
Respectively pipette 50.00ml test solution a, b, add the potassium hydroxide solution of 5ml triethanolamine and 20ml concentration 20% respectively, make pH value >=12.5 of test solution, drip magnesium oxide standard solution and 2 calcon-carboxylic acids of 4 concentration 1mg/mL more respectively, described calcon-carboxylic acid adds 10g potassium sulfate porphyrize by 0.1g calcium carboxylate to mix gained powder.Then use EDTA standard solution titration test solution, rate of titration is 14ml/min, until test solution becomes blueness from redness namely reach terminal.
Experimental result:
The calculating of total calcium oxide massfraction is undertaken by following formula:
=(21.80-0.20) × 0.00274 × 250 × 100 ÷ 0.5000 ÷ 50.00=59.18%
In formula:
W
tCaO---the massfraction of total calcium oxide in sample, %;
V
1---the total calcium oxide test solution of titration consumes the volume of EDTA standard solution, 21.80mL;
V
2---the blank test solution of the total calcium oxide of titration consumes the volume of EDTA standard solution, 0.20mL;
T---EDTA standard solution to the titer of calcium oxide, 0.00274g/mL;
M---sample size, 0.5000g;
V
3---pipette the volume of total calcium oxide test solution, 50.00mL.
The calculating of active calcium oxide massfraction is undertaken by following formula:
=(19.25-0.15) × 0.00274 × 250 × 100 ÷ 0.5 ÷ 50=52.33%
In formula:
W
fCaO---the massfraction of active calcium oxide in sample, %;
V
4---titration active calcium oxide test solution consumes the volume of EDTA standard solution, 19.25mL;
V
5---the blank test solution of titration active calcium oxide consumes the volume of EDTA standard solution, 0.15mL;
T---EDTA standard solution to the titer of calcium oxide, 0.00274g/mL;
M---sample size, 0.5000g;
V
6---pipette the volume of active calcium oxide test solution, 50.00mL.
The calculating of nonactive calcium oxide massfraction is undertaken by following formula: W
non-CaO=W
tCaO-W
fCaO==59.18-52.33=6.85%
In formula:
W
non-CaO---the massfraction of nonactive calcium oxide in sample, %;
W
tCaO---the massfraction of total calcium oxide, 59.18%;
W
fCaO---the massfraction of active calcium oxide, 52.33%.
embodiment 2
Experiment material: elder brother's steel Longshan Mine taken from by lime sample to be measured.All the other medicines and reagent are with embodiment 1..
Experimental facilities: with embodiment 1.
Experimental technique: lime sample to be measured is crushed to 0.125mm≤particle diameter≤0.150mm, in 105 DEG C of dry 2.5h.
Get a 0.5000g sample and the natrium carbonicum calcinatum amounting to 4g: the blend of boric acid=3:2 mixes on quantitative filter paper, wrapping with quantitative filter paper inserts in the rebasing iron crucible of the thick graphite linings of 1.0mm, melting 24min at iron crucible being placed in 880 DEG C, after taking out cooling, frit is placed in the beaker of the hydrochloric acid solution filling 60ml concentration 8%, cover on beaker with surface plate, in 100 DEG C of heating beakers, frit is dissolved, until solution is limpid, after being cooled to room temperature, solution is moved in 250ml volumetric flask, be settled to scale with distilled water, shake up test solution a is for subsequent use.Then the conical flask that a 0.5000g sample is placed in dry band grournd glass lid is separately got, add 5g sucrose, add the distilled water being cooled to 26 DEG C after 45ml newly boils again, by tight for the grournd glass capping plug of conical flask, be placed on oscillator with the hunting of frequency 22min of 200 beats/min, again solution is moved in 250ml volumetric flask, be settled to scale with distilled water, shake up test solution b is for subsequent use.
Respectively pipette 50.00ml test solution a, b, add the potassium hydroxide solution of 5ml triethanolamine and 20ml concentration 20% respectively, make pH value >=12.5 of test solution, drip magnesium oxide standard solution and 3 calcon-carboxylic acids of 5 concentration 1mg/mL more respectively, described calcon-carboxylic acid adds 10g potassium sulfate porphyrize by 0.1g calcium carboxylate to mix gained powder.Then use EDTA standard solution titration test solution, rate of titration is 12ml/min, until test solution becomes blueness from redness namely reach terminal.
Experimental result:
The calculating of total calcium oxide massfraction is undertaken by following formula:
=(20.45-0.20) × 0.00274 × 250 × 100 ÷ 0.5000 ÷ 50.00=55.48%
In formula:
W
tCaO---the massfraction of total calcium oxide in sample, %;
V
1---the total calcium oxide test solution of titration consumes the volume of EDTA standard solution, 20.45mL;
V
2---the blank test solution of the total calcium oxide of titration consumes the volume of EDTA standard solution, 0.20mL;
T---EDTA standard solution to the titer of calcium oxide, 0.00274g/mL;
M---sample size, 0.5000g;
V
3---pipette the volume of total calcium oxide test solution, 50.00mL.
The calculating of active calcium oxide massfraction is undertaken by following formula:
=(18.15-0.15) × 0.00274 × 250 × 100 ÷ 0.5 ÷ 50=49.32%
In formula:
W
fCaO---the massfraction of active calcium oxide in sample, %;
V
4---titration active calcium oxide test solution consumes the volume of EDTA standard solution, 18.15mL;
V
5---the blank test solution of titration active calcium oxide consumes the volume of EDTA standard solution, 0.15mL;
T---EDTA standard solution to the titer of calcium oxide, 0.00274g/mL;
M---sample size, 0.5000g;
V
6---pipette the volume of active calcium oxide test solution, 50.00mL.
The calculating of nonactive calcium oxide massfraction is undertaken by following formula: W
non-CaO=W
tCaO-W
fCaO==55.48-49.32=6.16%
In formula:
W
non-CaO---the massfraction of nonactive calcium oxide in sample, %;
W
tCaO---the massfraction of total calcium oxide, 55.48%;
W
fCaO---the massfraction of active calcium oxide, 49.32%.
embodiment 3
Experiment material: elder brother's steel Longshan Mine taken from by lime sample to be measured.All the other medicines and reagent are with embodiment 1..
Experimental facilities: with embodiment 1.
Experimental technique: lime sample to be measured is crushed to 0.125mm≤particle diameter≤0.150mm, in 110 DEG C of dry 1.5h.
Get a 0.5000g sample and the natrium carbonicum calcinatum amounting to 4g: the blend of boric acid=3:2 mixes on quantitative filter paper, wrapping with quantitative filter paper inserts in the rebasing iron crucible of the thick graphite linings of 0.7mm, melting 16min at iron crucible being placed in 920 DEG C, after taking out cooling, frit is placed in the beaker of the hydrochloric acid solution filling 60ml concentration 8%, cover on beaker with surface plate, in 110 DEG C of heating beakers, frit is dissolved, until solution is limpid, after being cooled to room temperature, solution is moved in 250ml volumetric flask, be settled to scale with distilled water, shake up test solution a is for subsequent use.Then the conical flask that a 0.5000g sample is placed in dry band grournd glass lid is separately got, add 5g sucrose, add the distilled water being cooled to 18 DEG C after 55ml newly boils again, by tight for the grournd glass capping plug of conical flask, be placed on oscillator with the hunting of frequency 18min of 300 beats/min, again solution is moved in 250ml volumetric flask, be settled to scale with distilled water, shake up test solution b is for subsequent use.
Respectively pipette 50.00ml test solution a, b, add the potassium hydroxide solution of 5ml triethanolamine and 20ml concentration 20% respectively, make pH value >=12.5 of test solution, drip magnesium oxide standard solution and 3 calcon-carboxylic acids of 4 concentration 1mg/mL more respectively, described calcon-carboxylic acid is the potassium chloride porphyrize mixing gained powder being added 50 g dryings by 0.5 g erichrome blue black R.Then use EDTA standard solution titration test solution, rate of titration is 15ml/min, until test solution becomes blueness from redness namely reach terminal.
Experimental result:
The calculating of total calcium oxide massfraction is undertaken by following formula:
=(19.05-0.15) × 0.00274 × 250 × 100 ÷ 0.5000 ÷ 50.00=51.79%
In formula:
W
tCaO---the massfraction of total calcium oxide in sample, %;
V
1---the total calcium oxide test solution of titration consumes the volume of EDTA standard solution, 19.05mL;
V
2---the blank test solution of the total calcium oxide of titration consumes the volume of EDTA standard solution, 0.15mL;
T---EDTA standard solution to the titer of calcium oxide, 0.00274g/mL;
M---sample size, 0.5000g;
V
3---pipette the volume of total calcium oxide test solution, 50.00mL.
The calculating of active calcium oxide massfraction is undertaken by following formula:
=(17.30-0.10) × 0.00274 × 250 × 100 ÷ 0.5 ÷ 50=47.13%
In formula:
W
fCaO---the massfraction of active calcium oxide in sample, %;
V
4---titration active calcium oxide test solution consumes the volume of EDTA standard solution, 17.30mL;
V
5---the blank test solution of titration active calcium oxide consumes the volume of EDTA standard solution, 0.10mL;
T---EDTA standard solution to the titer of calcium oxide, 0.00274g/mL;
M---sample size, 0.5000g;
V
6---pipette the volume of active calcium oxide test solution, 50.00mL.
The calculating of nonactive calcium oxide massfraction is undertaken by following formula: W
non-CaO=W
tCaO-W
fCaO==51.79-47.13=4.66%
In formula:
W
non-CaO---the massfraction of nonactive calcium oxide in sample, %;
W
tCaO---the massfraction of total calcium oxide, 51.79%;
W
fCaO---the massfraction of active calcium oxide, 47.13%.
embodiment 4
---the precision of detection method of the present invention, accuracy and the recovery
(1) Precision Experiment
Experimental technique: select 4 lime samples, carry out total calcium oxide content and active oxidation determination of calcium content respectively by detection method of the present invention, calculate relative standard deviation, experimental result is in table 1 and table 2.
Total calcium oxide Precision Experiment result of table 1 detection method of the present invention
| Sample | Measured value (%) | Mean value (%) | Relative standard deviation RSD |
| Lime sample 1 | 57.126，57.378，57.423，57.275，57.189 | 57.28 | 0.21 |
| Lime sample 2 | 54.356，54.157，54.478，54.512，54.345 | 54.37 | 0.25 |
| Lime sample 3 | 56.123，56.375，56.505，56．412，56.198 | 56.32 | 0.28 |
| Lime sample 4 | 58.325，58.786，58.565，58.773，58.379 | 58.57 | 0.37 |
The active calcium oxide Precision Experiment result of table 2 detection method of the present invention
| Sample | Measured value (%) | Mean value (%) | Relative standard deviation RSD |
| Lime sample 1 | 53.255，53.701，53.345，53.555，53.423 | 53.46 | 0.33 |
| Lime sample 2 | 48.605，48.109，48.356，48．456，48.110 | 48.33 | 0.45 |
| Lime sample 3 | 50.023，50.375，50.205，50．572，50.195 | 50.27 | 0.42 |
| Lime sample 4 | 53.625，53.386，53.465，53.173，53.179 | 53.37 | 0.36 |
(2) accuracy experiment
Experimental technique: select 2 lime standard models, carry out total calcium oxide content mensuration by detection method of the present invention respectively, each sample parallel measures 5 times, and experimental result is in table 3.
The accuracy experimental result of table 3 detection method of the present invention
| Standard model | Standard value (%) | Measured value (%) | Mean value | Relative standard deviation RSD |
| GBW07214a | 53.34 | 53.525，53.421，53.025，53.190，53.211 | 53.27 | 0.37 |
| GBW07215a | 51.20 | 51.102，51.515，51.249，51.339，51.445 | 51.33 | 0.32 |
(3) recovery experiment
Experimental technique: select a lime sample, adds the calcium of different amount respectively, carries out total calcium oxide content and active oxidation determination of calcium content by detection method of the present invention, each sample parallel analyzes 5 times, average, calculating the recovery is 97 ~ 108%, and experimental result is in table 4 and table 5.
Total calcium oxide content recovery experimental result of table 4 detection method of the present invention
| Sample | Standard value (%) | Addition (%) | Record total amount (%) | The recovery (%) |
| Lime sample | 57.28 | 0.50 | 57.80 | 104 |
| Lime sample | 57.28 | 1.00 | 58.25 | 97 |
| Lime sample | 57.28 | 1.50 | 58.82 | 103 |
| Lime sample | 57.28 | 2.00 | 59.36 | 104 |
The active oxidation calcium content recovery experimental result of table 5 detection method of the present invention
| Sample | Standard value (%) | Addition (%) | Record total amount (%) | The recovery (%) |
| Lime sample | 53.46 | 0.50 | 53.94 | 96 |
| Lime sample | 53.46 | 1.00 | 54.43 | 97 |
| Lime sample | 53.46 | 1.50 | 55.04 | 105 |
| Lime sample | 53.46 | 2.00 | 55.40 | 97 |
From above-mentioned experimental result, the analysis result deviation of detection method of the present invention is little, and precision, accuracy all can meet analyzes requirement, and analysis speed is fast, simple to operate, easily grasps, has higher application value.
Claims (10)
1. the detection method of active calcium oxide and nonactive calcium oxide content in lime, is characterized in that comprising sample pretreatment, peparation and titration measuring and calculating operation, specifically comprises:
A, sample pretreatment: lime sample to be measured is crushed to particle diameter≤0.150mm, in 105 ~ 110 DEG C of drying 1.5 ~ 2.5h;
B, peparation: get a 0.5000g sample and amount to the natrium carbonicum calcinatum of 4g and the blend of boric acid and mix on filter paper, wrap with filter paper in the iron crucible of inserting at the bottom of graphite pads, melting 16 ~ 24min at iron crucible being placed in 880 ~ 920 DEG C, after taking out cooling, frit is placed in the glass container of the hydrochloric acid solution filling 60ml concentration 8%, in 100 ~ 110 DEG C of heating, frit is dissolved after being closed by glass container, until solution is limpid, after being cooled to room temperature, solution is moved in 250ml volumetric flask, be settled to scale with water, shake up test solution a is for subsequent use; Separately get a 0.5000g sample and be placed in sealable glass container, add 5g sucrose, then add the water being cooled to room temperature after 45 ~ 55ml newly boils, by airtight for glass container rear vibration 18 ~ 22min, again solution is moved in 250ml volumetric flask, be settled to scale with water, shake up test solution b is for subsequent use;
C, titration measuring and calculating: respectively pipette 50.00ml test solution a, b, add potassium hydroxide or the sodium hydroxide solution of 5ml triethanolamine and concentration 20% respectively, make pH value >=12.5 of test solution, drip magnesium oxide standard solution and 2 ~ 3 calcon-carboxylic acids of 4 ~ 5 concentration 1mg/mL more respectively, then become blueness with EDTA standard solution titration test solution to it from redness and namely reach terminal;
The calculating of total calcium oxide massfraction is undertaken by following formula:
In formula:
W
tCaO---the massfraction of total calcium oxide in sample, %;
V
1---the total calcium oxide test solution of titration consumes the volume of EDTA standard solution, mL;
V
2---the blank test solution of the total calcium oxide of titration consumes the volume of EDTA standard solution, mL;
T---EDTA standard solution to the titer of calcium oxide, g/mL;
M---sample size, g;
V
3---pipette the volume of total calcium oxide test solution, mL;
The calculating of active calcium oxide massfraction is undertaken by following formula:
In formula:
W
fCaO---the massfraction of active calcium oxide in sample, %;
V
4---titration active calcium oxide test solution consumes the volume of EDTA standard solution, mL;
V
5---the blank test solution of titration active calcium oxide consumes the volume of EDTA standard solution, mL;
T---EDTA standard solution to the titer of calcium oxide, g/mL;
M---sample size, g;
V
6---pipette the volume of active calcium oxide test solution, mL;
The calculating of nonactive calcium oxide massfraction is undertaken by following formula: W
non-CaO=W
tCaO-W
fCaO
In formula:
W
non-CaO---the massfraction of nonactive calcium oxide in sample, %;
W
tCaO---the massfraction of total calcium oxide, %;
W
fCaO---the massfraction of active calcium oxide, %.
2. detection method according to claim 1, is characterized in that the lime sample to be measured particle diameter after crushed described in operation A is 0.125 ~ 0.150mm.
3. detection method according to claim 1, is characterized in that the mass ratio of natrium carbonicum calcinatum and boric acid in the blend of natrium carbonicum calcinatum described in process B and boric acid is 2: 1 or 3:2.
4. detection method according to claim 1, it is characterized in that the melt temperature described in process B is 900 DEG C, the melting time is 20min.
5. detection method according to claim 1, is characterized in that the frit solution temperature described in process B is 100 ~ 110 DEG C.
6. detection method according to claim 1, is characterized in that the duration of oscillation described in process B is 20min.
7. detection method according to claim 1, it is characterized in that the magnesium oxide standard solution described in operation C is prepared as follows: take 1.0000g in advance prior to 850 DEG C of calcinations and the magnesium oxide being cooled to room temperature in exsiccator is placed in beaker, add 20mL water, mixing, covers table ware, add the hydrochloric acid of 20mL concentration 20%, in 105 ~ 110 DEG C of heating for dissolving, cooling, moves in 1000mL volumetric flask, be diluted with water to scale, mix.
8. detection method according to claim 1, is characterized in that the calcon-carboxylic acid described in operation C is add the potassium chloride porphyrize mixing gained powder of 50 g dryings by 0.5 g erichrome blue black R or add any one in 10g potassium sulfate porphyrize mixing gained powder by 0.1g calcium carboxylate.
9. detection method according to claim 1, it is characterized in that the EDTA standard solution described in operation C is prepared as follows: take 3.73g disodium ethylene diamine tetraacetate and be placed in beaker, add 100mL water, in 105 ~ 110 DEG C of heating for dissolving, be cooled to room temperature, move in 1 000 mL volumetric flasks, be diluted with water to scale, shake up, obtain standard solution; Described EDTA standard solution is demarcated as follows: pipette 20.00 mL calcium oxide standard solution 3 parts, be placed in beaker respectively, add 25 mL water, demarcate by titration step described in operation C, EDTA standard solution is undertaken by following formula the calculating of the titer of calcium oxide:
In formula:
T---EDTA standard solution to the titer of calcium oxide, g/mL;
M---pipette the amount of calcium oxide contained by calcium oxide standard solution, g;
V---titration 3 parts of calcium oxide standard solution consume the average external volume of EDTA standard solution, mL.
10. detection method according to claim 1, is characterized in that the rate of titration described in operation C is 12 ~ 15ml/min.
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