CN103439329B - The assay method of ferric oxide content in a kind of coal combustion adjuvant - Google Patents
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Abstract
The invention discloses the assay method of ferric oxide content in a kind of coal combustion adjuvant. The present invention is dissolved sample to be tested through mixture of sulfuric phosphoric acid, potassium fluoride hydrotropy is smoldered to bottleneck, take off coolingly, add hydrochloric acid, drip Reduction with Stannous Chloride to light yellow, heating, take off and be cooled to 50～60 DEG C, drip sodium tungstate, be reduced to blue look with titanium trichloride solution, be oxidizing to blue decoloration with potassium bichromate solution, drip diphenylamine sulfonic acid sodium salt, being titrated to stable purple with potassium bichromate standard liquid is terminal, obtains sample to be tested titration milliliter number; Demarcate titer with the standard substance of known ferric oxide content, obtain the content of di-iron trioxide in sample according to the titration milliliter number of titer and sample. The present invention does not need to use specific analytical instrument, have easy to operate, quick, analysis cost is low, its measurement result has good stability, reappearance and accuracy, can meet the mensuration of ferric oxide content in daily blast furnace injection coal catalytic combustion burning-rate accelerator.
Description
Technical field
The invention belongs to chemical analysis technology field, relate to a kind of assay method of ferric oxide content, be specifically related toThe assay method of ferric oxide content in a kind of blast furnace injection coal catalytic combustion burning-rate accelerator.
Background technology
Improve significantly Coal Injection Amount into BF and be and reduce pig iron production cost, alleviate environmental pollution and Optimization Technology structureImportant technical, the combustibility of coal dust is the restricted link that Coal Injection Rate at BF improves. In order to improve the combustion of coal dust selfBurn performance, in pulverized coal injection in blast furnace, mix appropriate combustion adjuvant, can improve the combustion rate of pulverized coal injection in blast furnace. And, largeThe industrial furnace of amount uses confirmation on the spot, adds after combustion adjuvant, and not only the CO concentration in smoke evacuation obviously reduces, and can also make flue gas blackDegree declines 12 grades, can effectively reduce the coal-fired pollution to environment. Combustion characteristics according to coal dust under blast furnace blowing condition, systemStandby perfect combustion catalizer is very significant for the catalytic combustion of pulverized coal injection in blast furnace. And each constituent content in combustion adjuvantHow many combustion efficiencies that directly affect coal dust, this analyzes the content of each element in combustion adjuvant accurately with regard to requiring, but orderFront domestic national standard and the professional standard of also not formulating combustion adjuvant chemical analysis method.
The mensuration of ferric oxide content in blast furnace injection coal catalytic combustion burning-rate accelerator, does not also have the analysis of standard at presentMethod. The analysis of conventional ferric oxide content generally adopts atomic absorption method, but the method must rely on specific analytical instrument,Analysis cost is high, is difficult to adapt to the use of small scale experiments chamber, in production application, is very restricted. Three oxidations twoThe phenanthrolene photometry in addition of the analytic routines of iron content, but the method also relies on specific analytical instrument, not only analyzesCost is high, and complex operation step, and analysis time, length was also difficult to meet need of production.
Summary of the invention
For solving the problems such as ferric oxide content difficulty is larger in blast furnace injection coal catalytic combustion burning-rate accelerator of measuring, thisInvention provide one not need to use specific analytical instrument, and easy to operate, quick, analysis cost is low, measurement result hasThe assay method of ferric oxide content in the coal combustion adjuvant of good stability, reappearance and accuracy.
The present invention realizes by following steps:
A, in coal combustion adjuvant sample to be tested, by 40～60mL/gSampleAdd mixture of sulfuric phosphoric acid, obtain test liquid;
B, in steps A gained test liquid, by 10～16mL/gSampleAdd 25% potassium fluoride solution, shake container makes sampleDisperse, be placed on electric hot plate and dissolve, and evaporation smolder to bottleneck, take off and be cooled to room temperature, obtain test liquid;
C, in step B gained test liquid, by 20～40mL/gSampleAdd volume ratio HCl:H2The hydrochloric acid of O=1:1, with fewWater gaging purge bottleneck, dropping 6% stannous chloride solution is reduced to light yellow, obtains test liquid;
D, in step C gained test liquid, by 80～100mL/gSampleAdd distilled water, be placed on and micro-ly on electric hot plate boil 1 pointClock, takes off and is cooled to 50～60 DEG C, obtains test liquid;
E, in step D gained test liquid, drip 10 25% sodium tungstate solutions, drip titanium trichloride solution be reduced to orchidLook, drips potassium bichromate solution and is oxidizing to blue decoloration, drips 5 diphenylamine sulfonic acid sodium solutions, uses potassium bichromate standard liquidBeing titrated to stable purple is terminal, obtains titration milliliter and counts VExamination；
The calculating of ferric oxide content W in F, sample:
W=T×VExamination
The average titer of T-di-iron trioxide standard substance,
VExaminationThe titration milliliter number of-sample.
The present invention has the following advantages:
(1), the present invention is without using specific analytical instrument, and reagent dosage is few, analysis cost is low, in general little realityTesting chamber just can implement.
(2) the present invention is easy to operate, and analysis speed is fast, within general 25 minutes, just can analyze a sample, greatly shorten inspectionThe survey cycle, improve detection efficiency, alleviate testing staff's labour intensity.
(3) measurement result of the present invention has good stability, reappearance and accuracy.
(4) the present invention is with high accuracy, analyzes reliable, practically, can meet daily blast furnace injection coal catalytic combustion and helpIn combustion agent, the mensuration of ferric oxide content needs.
Detailed description of the invention
The present invention is further illustrated below, but never in any form the present invention is limited, based on the present inventionAny conversion or replacement that training centre is done, all belong to protection scope of the present invention.
The present invention includes following steps:
A, in coal combustion adjuvant sample to be tested, by 40～60mL/gSampleAdd mixture of sulfuric phosphoric acid, obtain test liquid;
B, in steps A gained test liquid, by 10～16mL/gSampleAdd 25% potassium fluoride solution, shake container makes sampleDisperse, be placed on electric hot plate and dissolve, and evaporation smolder to bottleneck, take off and be cooled to room temperature, obtain test liquid;
C, in step B gained test liquid, by 20～40mL/gSampleAdd volume ratio HCl:H2The hydrochloric acid of O=1:1, with fewWater gaging purge bottleneck, dropping 6% stannous chloride solution is reduced to light yellow, obtains test liquid;
D, in step C gained test liquid, by 80～100mL/gSampleAdd distilled water, be placed on and micro-ly on electric hot plate boil 1 pointClock, takes off and is cooled to 50～60 DEG C, obtains test liquid;
E, in step D gained test liquid, drip 10 25% sodium tungstate solutions, drip titanium trichloride solution be reduced to orchidLook, drips potassium bichromate solution and is oxidizing to blue decoloration, drips 5 diphenylamine sulfonic acid sodium solutions, uses potassium bichromate standard liquidBeing titrated to stable purple is terminal, obtains titration milliliter and counts VExamination；
The calculating of ferric oxide content W in F, sample:
W=T×VExamination
The average titer of T-di-iron trioxide standard substance,
VExaminationThe titration milliliter number of-sample.
The average titer T of described di-iron trioxide standard substance obtains through the following steps:
A, with the standard substance of multiple known ferric oxide contents, adopt the mode of A to E step, obtain each standardThe titration milliliter that material is corresponding is counted Vn；
B, the following formula of basis obtain multiple titer Tn：
Tn=Wn÷Vn
WnThe percentage composition of-each di-iron trioxide standard substance,
VnThe titration milliliter number that-corresponding each standard substance obtains;
C, the following formula of basis obtain average titer T:
T=(T1+T2+…+Tn)/n
The number of n-standard substance used.
Described mixture of sulfuric phosphoric acid is volume ratio H2SO4:H3PO4The mixed acid of=1:1.
Container in described step B is conical flask.
It is to be placed on the electric hot plate that is heated to 300～350 DEG C that test liquid in described step B is placed on dissolving on electric hot plateDissolve.
25% potassium fluoride solution in described step B is to take 25g potassium fluoride to be dissolved in 100mL distilled water and to obtain.
6% stannous chloride solution in described step C is that 6g stannous chloride is dissolved in to the hydrochloric acid that 20mL density is 1.19g/mLIn, to 100mL, and add a small amount of metallic tin grain to obtain with distilled water diluting.
25% sodium tungstate solution in described step e is to take 25g sodium tungstate to be dissolved in 50mL distilled water, adds 5mL densityFor the phosphoric acid of 1.69g/mL, rare to 100mL with distilled water, shake up and obtain.
Titanium trichloride solution in described step e is to get 15～20% titanium trichloride liquid volume ratio HCl:H2O=5:9520 times of hydrochloric acid dilutions, add the protection of one deck white oil and obtain.
Diphenylamine sulfonic acid sodium solution in described step e is to take 0.3g diphenylamine sulfonic acid sodium salt to be dissolved in 20mL distilled water,Rare to 100mL with distilled water, shake up and obtain.
Potassium bichromate solution in described step e is to get three times of potassium bichromate standard liquid dilutions to obtain.
Described potassium bichromate standard liquid is prepared by following steps:
(1), commercially available analytically pure 1.0g potassium bichromate is placed in to 500mL beaker;
(2), press 100mL/gPotassium bichromateAmount, in step (1) beaker, add distilled water, dissolve completely;
(3), solution in step (2) is moved in 1000mL volumetric flask, be diluted with water to 1000mL, shake up, obtain approximatelyThe potassium bichromate standard liquid of 1.0mg/mL.
Described hydrochloric acid, sulfuric acid, phosphoric acid, potassium fluoride, stannous chloride, sodium tungstate, titanium trichloride, potassium bichromate and/or hexicholAmine sodium sulfonate is commercial analysis net product.
Described vessel and instrument are vessel and the instrument of common use for laboratory.
Embodiment 1
The reagent that the present invention is used and preparation thereof:
1, potassium fluoride (25%): take 25g potassium fluoride and be dissolved in 100mL distilled water, move in plastic bottle and preserve;
2, stannous chloride (6%): 6g stannous chloride is dissolved in the hydrochloric acid that 20mL density is 1.19g/mL, rare with distilled waterRelease to 100mL, and add a small amount of metallic tin grain;
3, sodium tungstate (25%): take 25g sodium tungstate and be dissolved in 50mL distilled water, as muddiness increases filtration, add 5mL closeDegree is the phosphoric acid of 1.69g/mL, rare to 100mL with distilled water, shakes up;
4, titanium trichloride solution: get 15～20% titanium trichloride liquid volume ratio HCl:H2The hydrochloric acid dilution 20 of O=5:95Doubly, add the protection of one deck white oil;
5, diphenylamine sulfonic acid sodium salt indicator (0.3%): take 0.3g diphenylamine sulfonic acid sodium salt and be dissolved in 20mL distilled water, with steamingHeat up in a steamer water rare to 100mL, shake up;
6, potassium bichromate solution: get three times of potassium bichromate standard liquid dilutions;
7, the preparation of potassium bichromate standard liquid:
7A, commercially available analytically pure 1.0g potassium bichromate is placed in to 500mL beaker;
7B, press 100mL/gPotassium bichromateAmount, in the beaker of step 7A, add distilled water, dissolve completely;
7C, solution in step 7B is moved in 1000mL volumetric flask, be diluted with water to 1000mL, shake up, obtain approximatelyThe potassium bichromate standard liquid of 1.0mg/mL;
Described hydrochloric acid, sulfuric acid, phosphoric acid are commercial analysis net product;
Described vessel and instrument are vessel and the instrument of common use for laboratory.
Embodiment 2
1, the titration of sample
1A, in 0.5000g coal combustion adjuvant sample to be tested, by 40mL/gSampleAmount, add volume ratio H2SO4:H3PO4=The mixture of sulfuric phosphoric acid of 1:1, obtains test liquid;
1B, in the test liquid of step 1A gained, by 10mL/gSampleAmount, add 25% potassium fluoride solution, shake conical flaskMake sample disperse, be placed on the electric hot plate that is heated to 300～350 DEG C and dissolve, and evaporation smolder to bottleneck, take off and be cooled to chamberTemperature, obtains test liquid;
1C, in the test liquid of step 1B gained, by 20mL/gSampleAmount, add volume ratio HCl:H2O=1:1 hydrochloric acid,With a small amount of water purge bottleneck, dropping 6% stannous chloride solution is reduced to light yellow, obtains test liquid;
1D, in the test liquid of step 1C gained, by 80mL/gSampleAmount, add distilled water, be placed on electric hot plate micro-Boil 1 minute, take off, be cooled to 50～60 DEG C, obtain test liquid;
1E, in the sample of step 1D gained, drip 10 25% sodium tungstate solutions, drip titanium trichloride solution be reduced toBlue look, drips potassium bichromate solution and is oxidizing to blue decoloration, drips 5 diphenylamine sulfonic acid sodium solutions, molten by potassium bichromate standardIt is terminal that liquid is titrated to stable purple, obtains sample to be tested titration milliliter and counts VExamination=12.05mL。
2, determining of titer
2A, with the known ferric oxide content (W of 3 each 0.5000g1%=1.39%、W2%=2.35%、W3%=3.08%)Standard substance, adopts 1A to 1E step, obtains respectively three titration milliliter number (V1=7.05mL、V2=11.90mL、V3=15.60mL）；
2B, according to di-iron trioxide standard substance content in step 2A and corresponding titration milliliter number, as followsObtain 3 titer (T1=0.1972、T2=0.1975、T3=0.1974）：
Tn=Wn÷Vn
T1=1.39÷7.05=0.1972
T2=2.35÷11.90=0.1975
T3=3.08÷15.60=0.1974
2C, according to the titer of step 2B gained, obtain as follows average titer T=0.1974:
T=(T1+T2+T3)/3
=(0.1972+0.1975+0.1974)/3=0.1974
3, the calculating of ferric oxide content in sample
According to the average titer of the sample titration milliliter number of step 1E gained and step 2C gained, obtain as followsThe content W=2.38 (%) of di-iron trioxide in sample to be tested:
W=T×VExamination
=0.1974×12.05=2.38。
Embodiment 3
1, the titration of sample
1A, in 1.5000g coal combustion adjuvant sample to be tested, by 60mL/gSampleAmount, add volume ratio H2SO4:H3PO4=The mixture of sulfuric phosphoric acid of 1:1, obtains test liquid;
1B, in the test liquid of step 1A gained, by 16mL/gSampleAmount, add 25% potassium fluoride solution, shake conical flaskMake sample disperse, be placed on the electric hot plate that is heated to 300～350 DEG C and dissolve, and evaporation smolder to bottleneck, take off and be cooled to chamberTemperature, obtains test liquid;
1C, in the test liquid of step 1B gained, by 40mL/gSampleAmount, add volume ratio HCl:H2The salt of O=1:1Acid, with a small amount of water purge bottleneck, dropping 6% stannous chloride solution is reduced to light yellow, obtains test liquid;
1D, in the test liquid of step 1C gained, by 100mL/gSampleAmount, add distilled water, be placed on electric hot plate micro-Boil 1 minute, take off, be cooled to 50～60 DEG C, obtain test liquid;
1E, in the sample of step 1D gained, drip 10 25% sodium tungstate solutions, drip titanium trichloride solution be reduced toBlue look, drips potassium bichromate solution and is oxidizing to blue decoloration, drips 5 diphenylamine sulfonic acid sodium solutions, molten by potassium bichromate standardIt is terminal that liquid is titrated to stable purple, obtains sample to be tested titration milliliter and counts VExamination=36.20mL。
2, determining of titer
2A, with the known ferric oxide content (W of 5 each 1.500g1%=1.52%、W2%=2.17%、W3%=2.52%、W4%=2.79%、W5Standard substance %=3.14%), adopts 1A to 1E step, obtains respectively titration milliliter number (V1=23.15mL、V2=33.00mL、V3=38.35mL、V4=42.35mL、V5=47.75mL）；
2B, according to di-iron trioxide standard substance content in step 2A and corresponding titration milliliter number, as followsObtain titer (T1=0.06566、T2=0.06576、T3=0.06571、T4=0.06588、T5=0.06576）：
Tn=Wn÷Vn
T1=1.52÷23.15=0.06566
T2=2.17÷33.00=0.06576
T3=2.52÷38.35=0.06571
T4=2.79÷42.35=0.06588
T5=3.14÷47.75=0.06576
2C, according to the titer of step 2B gained, obtain as follows average titer T=0.06575:
T=(T1+T2+T3+T4+T5)/5
=(0.06566+0.06576+0.06571+0.06588+0.06576)/5
=0.06575
3, the calculating of ferric oxide content in sample
According to the average titer of the sample titration milliliter number of step 1E gained and step 2C gained, obtain as followsThe content W=2.38 (%) of di-iron trioxide in sample:
W=T×VExamination
=0.06575×36.20=2.38。
Embodiment 4
1, the titration of sample
1A, in 1.0000g coal combustion adjuvant sample to be tested, by 50mL/gSampleAmount, add volume ratio H2SO4:H3PO4=The mixture of sulfuric phosphoric acid of 1:1, obtains test liquid;
1B, in the test liquid of step 1A gained, by 14mL/gSampleAmount, add 25% potassium fluoride solution, shake conical flaskMake sample disperse, be placed on the electric hot plate that is heated to 300～350 DEG C and dissolve, and evaporation smolder to bottleneck, take off and be cooled to chamberTemperature, obtains test liquid;
1C, in the test liquid of step 1B gained, by 30mL/gSampleAmount, add volume ratio HCl:H2The salt of O=1:1Acid, with a small amount of water purge bottleneck, dropping 6% stannous chloride solution is reduced to light yellow, obtains test liquid;
1D, in the test liquid of step 1C gained, by 90mL/gSampleAmount, add distilled water, be placed on electric hot plate micro-Boil 1 minute, take off, be cooled to 50～60 DEG C, obtain test liquid;
1E, in the sample of step 1D gained, drip 10 25% sodium tungstate solutions, drip titanium trichloride solution be reduced toBlue look, drips potassium bichromate solution and is oxidizing to blue decoloration, drips 5 diphenylamine sulfonic acid sodium solutions, molten by potassium bichromate standardIt is terminal that liquid is titrated to stable purple, obtains sample to be tested titration milliliter and counts VExamination=24.10mL。
2, determining of titer
2A, with 3 known ferric oxide content (W1%=1.39%、W2%=2.35%、W3Standard substance %=3.08%), adoptsBy 1A to 1E step, obtain respectively three titration milliliter number (V1=14.10mL、V2=23.75mL、V3=31.20mL）；
2B, according to di-iron trioxide standard substance content in step 2A and corresponding titration milliliter number, as followsObtain 3 titer (T1=0.09858、T2=0.09895、T3=0.09872）：
Tn=Wn÷Vn
T1=1.39÷14.10=0.09858
T2=2.35÷23.75=0.09895
T3=3.08÷31.20=0.09872
2C, according to the titer of step 2B gained, obtain as follows average titer T=0.09875:
T=(T1+T2+T3)/3
=(0.09858+0.09895+0.09872)/3
=0.09875
3, the calculating of ferric oxide content in sample
Count V according to the sample to be tested titration milliliter of step 1E gainedExaminationWith the average titer T of step 2C gained, below pressingFormula obtains the content W=2.38 (%) of di-iron trioxide in sample:
W=T×VExamination
=0.09875×24.10=2.38。
Claims (6)
1. an assay method for ferric oxide content in coal combustion adjuvant, is characterized in that comprising the following steps:
A, in coal combustion adjuvant sample to be tested, by 40 ~ 60mL/gSampleAdd mixture of sulfuric phosphoric acid, obtain test liquid, mixture of sulfuric phosphoric acid is volumeCompare H2SO4:H3PO4The mixed acid of=1:1;
B, in steps A gained test liquid, by 10 ~ 16mL/gSampleAdd 25% potassium fluoride solution, shake container disperses sample,Be placed on the electric hot plate that is heated to 300 ~ 350 DEG C and dissolve, and evaporation smolder to bottleneck, take off and be cooled to room temperature, obtain test liquid;
C, in step B gained test liquid, by 20 ~ 40mL/gSampleAdd volume ratio HCl:H2The hydrochloric acid of O=1:1, blows with a small amount of waterWash bottle mouth, dropping 6% stannous chloride solution is reduced to light yellow, obtains test liquid;
D, in step C gained test liquid, by 80 ~ 100mL/gSampleAdd distilled water, be placed on micro-boiling 1 minute on electric hot plate, getUnder be cooled to 50 ~ 60 DEG C, obtain test liquid;
E, in step D gained test liquid, drip 10 25% sodium tungstate solutions, drip titanium trichloride solution be reduced to blue look, dripAdd potassium bichromate solution and be oxidizing to blue decoloration, drip 5 diphenylamine sulfonic acid sodium solutions, be titrated to potassium bichromate standard liquidStable purple is terminal, obtains titration milliliter and counts VExamination; Described titanium trichloride solution is to get 15 ~ 20% titanium trichloride liquid bodiesThe long-pending HCl:H that compares220 times of O=5:95 hydrochloric acid dilutions, add the protection of one deck white oil and obtain; Potassium bichromate solution is to get potassium bichromateStandard liquid dilutes three times and obtains; Potassium bichromate standard liquid is made by following steps:
(1) pure commercially available analysis 1.0g potassium bichromate is placed in to 500mL beaker;
(2) press the amount of 100mL/g potassium bichromate, in step (1) beaker, add distilled water, dissolve completely;
(3) solution in step (2) is moved in 1000mL volumetric flask, be diluted with water to 1000mL, shake up, obtain about 1.0mg/mLPotassium bichromate standard liquid;
The calculating of ferric oxide content W in F, sample:
W=T×VExamination
The average titer of T-di-iron trioxide standard substance,
VExaminationThe titration milliliter number of-sample.
2. assay method according to claim 1, is characterized in that the average titer T of described di-iron trioxide standard substanceTo obtain through the following steps:
A, with the standard substance of multiple known ferric oxide contents, adopt the mode of A to E step, obtain each standard substanceCorresponding titration milliliter is counted Vn；
B, the following formula of basis obtain multiple titer Tn：
Tn=Wn÷Vn
WnThe percentage composition of-each di-iron trioxide standard substance,
VnThe titration milliliter number that-corresponding each standard substance obtains;
C, the following formula of basis obtain average titer T:
T=(T1+T2+…+Tn)/n
The number of n-standard substance used.
3. assay method according to claim 1, is characterized in that 25% potassium fluoride solution in described step B is to take25g potassium fluoride is dissolved in 100mL distilled water and obtains.
4. assay method according to claim 1, is characterized in that 6% stannous chloride solution in described step C is by 6gStannous chloride is dissolved in the hydrochloric acid that 20mL density is 1.19g/mL, to 100mL, and adds a small amount of metallic tin grain with distilled water dilutingObtain.
5. assay method according to claim 1, is characterized in that 25% sodium tungstate solution in described step e is to take25g sodium tungstate is dissolved in 50mL distilled water, and adding 5mL density is the phosphoric acid of 1.69g/mL, rare to 100mL with distilled water, shakes upObtain.
6. assay method according to claim 1, is characterized in that the diphenylamine sulfonic acid sodium solution in described step e is to claimGet 0.3g diphenylamine sulfonic acid sodium salt and be dissolved in 20mL distilled water, rare to 100mL with distilled water, shake up and obtain.
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