CN101509909A - Sulphates content testing method in flue gas desulfurization system - Google Patents
Sulphates content testing method in flue gas desulfurization system Download PDFInfo
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Abstract
The invention provides a test method of the sulphate content in a flue gas desulfurization system, relating to the technical field of a test method of the sulphate content in a desulphurization system. The test method is characterized in that two samples to be tested are taken simultaneously, wherein one sample is used for determining the sulphite content, and the other sample is used for determining the total content of the sulphite and sulphate; and the sulphate content is calculated by the difference between the total content of the sulphite and sulphate and the sulphite content. The test method has the positive effects that the method is accurate, thus greatly improving the accuracy and the reliability of analysis results of the sulphate in the desulphurization system, and providing reliable analysis results for the operation of the desulphurization system. As the sulphite content in the desulphurization system is an indispensable project to be tested in the conventional analysis, thus not increasing the workload when determining the sulphate content. As the test can be completed only by using an analytical instrument in a conventional laboratory, and a determining project and a determining instrument do not need to be increased, the test method is a very practical analysis method.
Description
Technical field
The present invention relates to the assay method technical field of sulphates content in the flue gas desulphurization system.
Background technology
In flue-gas desulfurizing engineering, the size of sulphates content not only influences the quality of desulfurization product, also will influence the operation of whole desulphurization system.In wet method fume desulfurizing system, if the sulphite too high levels then causes the absorption tower slurries to be clamminess and the difficulty of dewatering easily, make slurries adhesion, fouling on system, equipment easily, cause equipment resistance to increase even system jams.Therefore, need in time to grasp the sulphates content in absorption tower slurries and the desulfurization product, so that the operational factor of Adjustment System oxidation fan improves the sulfite oxidation rate, the sulphates content of accurately measuring in absorption tower slurries and the desulfurization product just seems particularly important.Because desulphurization system is shorter working time in China, still needleless is to the method for testing of sulphates content in the desulphurization system at present.Adopt the unit of semi-dry desulphurization, nearly all the sulphates content in the desulfurization product is not measured; Adopt the unit of wet desulphurization, majority is not measured the sulphates content in the slurries, to desulfurization product---and the mensuration of sulphates content is the sulfate gravimetric method that has adopted among the GB/T5484-2000 " chemical analysis of gypsum method " in the desulfurated plaster.But in fact, the scope of application of GB/T5484-2000 " chemical analysis of gypsum method " is the plaster of paris and muriacite, for desulfurated plaster (belonging to chemical gypsum) and not exclusively suitable.Owing to may contain a certain amount of sulphite in the desulfurated plaster, and in " water and effluent monitoring analytical approach " (China Environmental Science Press, the 4th edition) in the 162nd page of sulfate-gravimetric determination, spell out " comprise in the sample sulphite can make result higher ".Therefore, for the determining sulphate that contains under the sulphite situation, should take into full account the influence of sulphite, and manage its elimination.And for desulphurization system, (wet desulphurization slurries and semi-dry desulphurization ash Central Asia sulphates content may be higher owing to contain a certain amount of sulphite through regular meeting; Desulfurization product Central Asia sulphates content also may be higher during the wet desulfurization system misoperation), when measuring its sulphates content, must eliminate the influence of sulphite.
About the analytical approach of sulfate in the desulphurization system, still there is not domestic or international standard at present.Most units adopt methods such as gravimetric method or barium chromate photometry directly to measure, but do not consider the influence of sulphite to measuring.
Summary of the invention
The method of testing that the purpose of this invention is to provide sulphates content in a kind of flue gas desulphurization system, be characterized in that method accurately and reliably, compared with the prior art, improved the accurate reliability of analysis result greatly, reliable analysis result can be provided for the operation of desulphurization system.
Main technical schemes of the present invention is: the method for testing of sulphates content in a kind of flue gas desulphurization system, it is characterized in that getting simultaneously two parts of testing samples, and a copy of it is used to measure sulphite content; Another part is used to measure sulphite and sulfate total amount; At last, the difference by both calculates sulphates content.
Described mensuration sulphite content is preferable with iodimetric titration, and its testing procedure is:
(1) takes by weighing sample (solid sample is answered dry and can be all by standard sieve, and slurries can directly be measured weight or volume);
(2) sample is put into iodine flask, add entry, add iodine standard solution again, fully shake mixing, add hydrochloric acid, fully shake iodine flask sample is fully dissolved;
(3) with the iodine of sodium thiosulfate standard solution overtitration, when near terminal point, solution becomes when faint yellow, adds starch solution, is titration end-point when disappearing when solution is blue;
(4) carry out blank assay simultaneously, repeat above-mentioned steps (2), (3), iodine standard solution addition and sample will be consistent, and record consumes the hypo solution volume.
Sulphite cubage method is: the size of sulphite content, represent with content of sulfur dioxide, and can calculate SO by following formula
2=0.03203 (v
2c
2-v
1c
1) * 100 ÷ s,
Wherein: SO
2Expression content of sulfur dioxide %; V
1The consumption ml of expression sodium thiosulfate standard solution; c
1The concentration mol/L of expression sodium thiosulfate standard solution; V
2The consumption ml of expression iodine standard solution; c
2The concentration mol/L of expression iodine standard solution; S represents example weight g; 0.03203: behind the molecular weight ÷ 2 of sulphuric dioxide, again unit is scaled g by mg; c
2=v
0c
1/ v
2V
0The volume ml of the hypo solution that the expression blank assay consumes.
Measure other standard methods such as the also available hydrochloric acid Pararosaniline of method photometry of sulphite content.
The preferred approach of described mensuration sulphite and sulfate total amount is: be sulfate with the sulphite complete oxidation earlier, use the gravimetric determination sulphates content again, the gravimetric method testing procedure is:
(1) takes by weighing sample (solid sample is answered dry and can be all by standard sieve, and slurries can directly be measured weight or volume);
(2) sample is put into beaker, add superoxol and acetic acid-sodium acetate buffer solution, after fully stirring and evenly mixing makes calcium sulfite oxidation, dissolving, use filter paper filtering, washing is collected in filtrate and cleansing solution in the beaker for several times;
(3) in filtrate, add hydrochloric acid;
(4) one side heated and boiled solution is Yi Bian under agitation slowly drip barium chloride solution; Precipitation is slowly grown, continue to boil solution and clarify until solution;
(5) solution is remained near leaving standstill under the temperature of seething with excitement, can add an amount of warm water as required;
(6) use filter paper filtering, cyclic washing is till the no chlorion of check;
(7) will precipitate and filter paper moves in the porcelain crucible of pre-burn in the lump, slowly heat ashing after, in muffle furnace,, in exsiccator, after the cooling, weigh in 800 ℃ of calcinations; Calcination repeatedly is until constant weight.
Described solid sample to be measured is chosen or when preparing, and make the testing sample can be all by the 250um standard sieve, if still can not guarantee the homogeneity of taking a sample, and then will be all by the 150um standard sieve.
Described buffer solution pH is 3.8～4.2 for good.
Described iodine standard solution is that 0.1mol/L is preferable, and addition is determined by preliminary experiment.
The computing method of sulphates content are in the sample: sulphates content is represented with sulfur trioxide content; SO
3=(0.343m
2-0.0125m
3) * 100 ÷ s
2,
SO wherein
3: expression sulfur trioxide content %; m
2: expression precipitation weight g; m
3: by the content of sulfur dioxide % that calculates after the sulphite mensuration; s
2: expression example weight g; 0.0125: the conversion coefficient the when percentage composition of sulphuric dioxide is converted to sulfuric anhydride (sulfuric anhydride molecular weight ÷ sulfur dioxide molecule amount) ÷ 100; 0.343: barium sulphate is converted to the conversion coefficient (sulfuric anhydride molecular weight ÷ barium sulphate molecular weight) of sulfuric anhydride.
The also available elder generation of method that measures sulphite and sulfate total amount with the sulphite complete oxidation after, use methods such as barium chromate spectrphotometric method for measuring sulfate total amount again.
Good effect of the present invention is: compared with the prior art method, has improved the accurate reliability of analysis result accurately and reliably greatly, and reliable analysis result can be provided for the operation of desulphurization system.Because desulphurization system Central Asia sulphates content is must survey project in the conventional analysis, therefore, do not increase workload carrying out sulphates content when measuring.Owing to adopt the Routine Test Lab analytical instrument can finish test, need not increase mensuration project and determining instrument, be a kind of very practical analytical approach.
Be described further below in conjunction with embodiment, but not as a limitation of the invention.
Embodiment
One, testing tool
Standard sieve: 250um and 150um; Analytical balance: precision is more than 0.1mg reaches;
Muffle furnace: the muffle heating furnace, carry out resistance heated in the burner hearth periphery.Answer the serviceability temperature controller, accurately control furnace temperature, and regularly carry out verification; Filter paper: ashless quantitative filter paper at a slow speed.
Two, reagent
1. (1+1) hydrochloric acid solution: the concentrated hydrochloric acid of 1 part of volume mixes with the water of 1 part of volume;
2. barium chloride solution (50g/l): weighing 60g barium chloride is soluble in water, is diluted with water to 11;
3. superoxol (1+9): superoxol dilute with water with 30%;
4.pH be 4 buffer solution: take by weighing the 75g sodium acetate and be dissolved in 500ml (1+2) acetic acid;
5.0.1mol/L sodium thiosulfate standard solution: directly prepare with standard mole reagent, be stored in the brown bottle;
6.0.1mol/L iodine standard solution (1/2I
2): take by weighing 12.7g iodine in the 500ml beaker, add the 40g potassium iodide, add the suitable quantity of water dissolving after, be transferred in the brown volumetric flask of 1000ml, need not demarcate.
7.1% starch solution: take by weighing the 1g soluble starch with low amounts of water furnishing pasty state, use again firm boil water towards rare to 100ml.
Three, testing procedure
1. sample chooses and prepares
Solid sample: for guaranteeing the homogeneity of institute's sample thief, at first to carry out the sample fragmentation, make the testing sample can be all by the 250um standard sieve, if still can not guarantee the homogeneity of taking a sample, then will be all by the 150um standard sieve.If sample is too wet, when being difficult for carrying out fragmentation, then at first will be in air air dry or in drying box in predrying below 45 ℃.Get by the sample behind the standard sieve, in drying box,, be used as testing sample in 45 ℃ times dry 2 hours.
Fluid sample: the weight or volume that can directly measure sample.
Analysis result, solid sample are used with respect to the mass percent of dried sample and are represented; Slurry samples is represented with mass percent or mass concentration.
2. sulfate and sulphite total amount test
(1) takes by weighing the 0.2-0.3g sample, be accurate to 0.1mg;
(2) sample is put into the 300ml beaker, adding 10ml (1+9) superoxol and 10ml pH are 4 acetic acid---sodium acetate buffer solution, add water and make overall solution volume at 150ml.After fully stirring and evenly mixing makes calcium sulfite oxidation, dissolving,, with the warm water washing for several times, filtrate and cleansing solution are collected in the 500ml beaker with quantitative filter paper filtration at a slow speed;
(3) in filtrate, add 2ml (1+1) hydrochloric acid, add water and make cumulative volume at 300ml;
(4) one side heated and boiled solution is Yi Bian under agitation slowly drip barium chloride solution (50g/l) 25ml (about 10 minutes of dropping time); Precipitation is slowly grown, continue to boil the solution number and minute clarify until solution;
(5) solution is remained near leaving standstill 3 hours under the temperature of seething with excitement, will keep overall solution volume during this period about 300ml, can add an amount of warm water as required;
(6) with quantitative filter paper filtration at a slow speed, use the warm water cyclic washing, till the no chlorion of check;
(7) will precipitate and filter paper moves in the porcelain crucible of pre-burn in the lump, slowly heat ashing after, in muffle furnace,, in exsiccator, after the cooling, weigh in 800 ℃ of calcinations 30 minutes; Repeat calcination, until constant weight.
3. sulphite content measuring
(1) takes by weighing the 1-2g sample, be accurate to 0.1mg;
(2) sample is put into the 300ml iodine flask, added about 50ml water, add again and a certain amount ofly (can determine by preliminary experiment, usually 25ml get final product) iodine standard solution, fully shake mixing, adding (1+1) hydrochloric acid 20ml, add a cover, fully shake iodine flask sample is fully dissolved;
(3) with the iodine of 0.1mol/L sodium thiosulfate standard solution overtitration, when near terminal point, solution becomes when faint yellow, adds the 1ml starch solution, is titration end-point when disappearing when solution is blue.
(4) carry out blank assay simultaneously, repeating step (2), (3), iodine standard solution addition and sample will be consistent, and record consumes the hypo solution volume.
Four, the result calculates
1. sulphite cubage
The size of sulphite content, represent with content of sulfur dioxide:
Content of sulfur dioxide can be calculated by following formula
SO
2＝0.03203(v
2c
2-v
1c
1)×100÷s (1)
Wherein:
SO
2Expression content of sulfur dioxide (%);
V
1The consumption (ml) of expression sodium thiosulfate standard solution;
c
1The concentration (mol/L) of expression sodium thiosulfate standard solution;
V
2The consumption (ml) of expression iodine standard solution;
c
2The concentration (mol/L) of expression iodine standard solution;
S represents example weight (g);
0.03203: behind the molecular weight ÷ 2 of sulphuric dioxide, again unit is scaled g by mg.
c
2＝v
0c
1/v
2
V
0The volume (ml) of the hypo solution that the expression blank assay consumes.
2. sulphates content calculates
Sulphates content how much, represents with sulfur trioxide content.
SO
3＝(0.343m
2-0.0125m
3)×100÷s
2 (2)
Wherein
SO
3: expression sulfur trioxide content (%);
m
2: expression precipitation weight (g);
m
3: by the content of sulfur dioxide (%) that calculates after the sulphite mensuration;
s
2: expression example weight (g).
0.0125: the percentage composition of sulphuric dioxide is converted to the conversion coefficient of sulfuric anhydride (sulfuric anhydride molecular weight ÷ sulfur dioxide molecule amount) ÷ 100
0.343: barium sulphate is converted to the conversion coefficient (sulfuric anhydride molecular weight ÷ barium sulphate molecular weight) of sulfuric anhydride.
For example:
1, the mensuration of sulphates content in the solid sample
1.1 the mensuration of sulfate and sulphite total amount
(1) takes by weighing the 0.2058g testing sample;
(2) sample is put into the 300ml beaker, adding 10ml (1+9) superoxol and 10ml pH is 4 acetic acid---the buffer solution of sodium acetate adds water and makes overall solution volume at 150ml.After fully stirring and evenly mixing makes calcium sulfite oxidation, dissolving,, with the warm water washing for several times, filtrate and cleansing solution are collected in the 500ml beaker with quantitative filter paper filtration at a slow speed;
(3) in filtrate, add 2ml (1+1) hydrochloric acid, add water and make cumulative volume at 300ml;
(4) one side heated and boiled solution is Yi Bian under agitation slowly drip barium chloride solution (50g/l) 25ml (about 10 minutes of dropping time); Precipitation is slowly grown, continue to boil the solution number and minute clarify until solution;
(5) solution is remained near leaving standstill 3 hours under the temperature of seething with excitement, will keep overall solution volume during this period about 300ml, can add an amount of warm water as required;
(6) with quantitative filter paper filtration at a slow speed, use the warm water cyclic washing, till the no chlorion of check;
(7) will precipitate and filter paper moves in the porcelain crucible of pre-burn in the lump, slowly heat ashing after, in muffle furnace,, in exsiccator, after the cooling, weigh in 800 ℃ of calcinations 30 minutes; Calcination repeatedly is until constant weight.Last actual weighing results is 0.4244g.
1.2 sulphite assay
(1) takes by weighing the 1.0290g testing sample;
(2) sample is put into the 300ml iodine flask, added about 50ml water, add the iodine standard solution (the actual 0.1038mol/L of being of mark liquid concentration) of 25ml again, fully shake mixing, add (1+1) hydrochloric acid 20ml, add a cover, fully shake iodine flask and sample was fully dissolved in 15 minutes;
(3) with the iodine of 0.1mol/L sodium thiosulfate standard solution overtitration, when solution becomes when faint yellow, add the 1ml starch solution, consume sodium thiosulfate 11.45ml when disappearing when solution is blue;
(4) carry out blank assay simultaneously and consume sodium thiosulfate 25.95ml.
1.3 calculate, test result is
According to formula (2), draw SO
2=4.5l
In the substitution formula (1), calculate SO
3=43.32
2. the mensuration of sulphates content in the slurry samples
2.1 the mensuration of sulfate and sulphite total amount
(1) takes by weighing the 0.2310g testing sample;
(2) sample is put into the 300ml beaker, adding 10ml (1+9) superoxol and 10ml pH are 4 acetic acid---sodium acetate buffer solution, add water and make overall solution volume at 150ml.After fully stirring and evenly mixing makes calcium sulfite oxidation, dissolving,, with the warm water washing for several times, filtrate and cleansing solution are collected in the 500ml beaker with quantitative filter paper filtration at a slow speed;
(3) in filtrate, add 2ml (1+1) hydrochloric acid, add water and make cumulative volume at 300ml;
(4) one side heated and boiled solution is Yi Bian under agitation slowly drip barium chloride solution (50g/l) 25ml (about 10 minutes of dropping time); Precipitation is slowly grown, continue to boil the solution number and minute clarify until solution;
(5) solution is remained near leaving standstill 3 hours under the temperature of seething with excitement, will keep overall solution volume during this period about 300ml, can add an amount of warm water as required;
(6) with quantitative filter paper filtration at a slow speed, use the warm water cyclic washing, till the no chlorion of check;
(7) will precipitate and filter paper moves in the porcelain crucible of pre-burn in the lump, slowly heat ashing (noting not producing flame) after, in muffle furnace,, in exsiccator, after the cooling, weigh in 800 ℃ of calcinations 30 minutes; Calcination repeatedly is until constant weight.Last actual weighing results is 0.4105g.
2.2 sulphite assay
(1) takes by weighing the 1.2000g testing sample;
(2) sample is put into the 300ml iodine flask, added about 50ml water, add the iodine standard solution (the actual 0.1038mol/L of being of mark liquid concentration) of 25ml again, fully shake mixing, add (1+1) hydrochloric acid 20ml, add a cover, fully shake iodine flask and sample was fully dissolved in 15 minutes;
(3) with the iodine of 0.1mol/L sodium thiosulfate standard solution overtitration, when solution becomes when faint yellow, add the 1ml starch solution, consume sodium thiosulfate 9.85ml when disappearing when solution is blue;
(4) carry out blank assay simultaneously and consume sodium thiosulfate 25.95ml.
1.3 calculate, test result is
According to formula (2), draw SO
2=4.30
In the substitution formula (1), calculate SO
3=37.68
With the method for method of the present invention and traditional gravimetric determination sulphates content the sulphates content in the potpourri of " country-level standard substance gypsum GBWO3100 and chemical pure calcium sulfite hemihydrate " (mass percent that adds calcium sulfite is 2---between 20%) is measured, the sulfur trioxide content standard value is 32.55% among the known gypsum GBWO3100, and the contrast of test result is as follows:
Be followed successively by 31.90,32.25,32.46,32.56,32.67 with method measurement result provided by the invention, the mean value of measurement result is 32.37, standard deviation 0.27, relative standard deviation 0.83%;
Do not add hydrogen peroxide and carry out oxidation, directly add the back result with traditional gravimetric determination of acid and be respectively 33.03,34.46,35.66,35.75,36.00, the mean value of measurement result is 34.98, standard deviation 1.11, relative standard deviation 3.41%.
By as can be known above, the present invention has improved the accuracy of test result greatly, especially under sulphite content condition with higher.
Claims (4)
1, the method for testing of sulphates content in a kind of flue gas desulphurization system is characterized in that getting simultaneously two parts of testing samples, and a copy of it is used to measure sulphite content; Another part is used to measure sulphite and sulfate total amount; Difference by both calculates sulphates content.
The test and the computing method of sulphite content were when 2, sulphates content was measured in the flue gas desulphurization system according to claim 1: iodimetric titration is adopted in test, and the testing procedure of iodimetric titration is:
(1) takes by weighing sample;
(2) sample is put into iodine flask, add entry, add iodine standard solution again, fully shake mixing, add hydrochloric acid, fully shake iodine flask sample is fully dissolved;
(3) with the iodine of sodium thiosulfate standard solution overtitration, when near terminal point, solution becomes when faint yellow, adds starch solution, is titration end-point when disappearing when solution is blue;
(4) carry out blank assay simultaneously, repeat above-mentioned steps (2), (3), iodine standard solution addition and sample will be consistent, and record consumes the hypo solution volume;
Computing method are: the size of sulphite content, represent with content of sulfur dioxide: and content of sulfur dioxide, can calculate by following formula: SO
2=0.03203 (v
2c
2-v
1c
1) * 100 ÷ s, wherein: SO
2Expression content of sulfur dioxide %; V
1The consumption ml of expression sodium thiosulfate standard solution; c
1The concentration mol/L of expression sodium thiosulfate standard solution; V
2The consumption ml of expression iodine standard solution; c
2The concentration mol/L of expression iodine standard solution; S represents example weight g; 0.03203: behind the molecular weight ÷ 2 of sulphuric dioxide, again unit is scaled g by mg; c
2=v
0c
1/ v
2: V
0The volume ml of the hypo solution that the expression blank assay consumes.
3, the test of sulphates content and computing method are in the flue gas desulphurization system according to claim 1 and 2: the mensuration of sulphite and sulfate total amount adopts earlier the sulphite complete oxidation, measure the method for sulfate total amount again, the assay method exploitation gravimetric method of sulfate total amount; Determination step during gravimetric determination sulfate total amount is:
(1) takes by weighing sample;
(2) sample is put into beaker, add superoxol and acetic acid-sodium acetate buffer solution, after fully stirring and evenly mixing makes calcium sulfite oxidation, dissolving, use filter paper filtering, washing is collected in filtrate and cleansing solution in the beaker for several times;
(3) in filtrate, add hydrochloric acid;
(4) one side heated and boiled solution is Yi Bian under agitation slowly drip barium chloride solution; Precipitation is slowly grown, continue to boil solution and clarify until solution;
(5) solution is remained near leaving standstill under the temperature of seething with excitement, can add an amount of warm water as required;
(6) use filter paper filtering, cyclic washing is till the no chlorion of check;
(7) will precipitate and filter paper moves in the porcelain crucible of pre-burn in the lump, slowly heat ashing after, in muffle furnace,, in exsiccator, after the cooling, weigh in 800 ℃ of calcinations; Calcination repeatedly is until constant weight;
The computing method of sulphates content are when measuring sulphite and sulfate total amount: sulphates content is represented with sulfur trioxide content; SO
3=(0.343m
2-0.0125m
3) * 100 ÷ s
2, SO wherein
3: expression sulfur trioxide content %; m
2: expression precipitation weight g; m
3: by the content of sulfur dioxide % that calculates after the sulphite mensuration; s
2: expression example weight g; 0.0125: the percentage composition of sulphuric dioxide is converted to the conversion coefficient of sulfuric anhydride, i.e. (sulfuric anhydride molecular weight ÷ sulfur dioxide molecule amount) ÷ 100; 0.343: barium sulphate is converted to the conversion coefficient of sulfuric anhydride, i.e. sulfuric anhydride molecular weight ÷ barium sulphate molecular weight.
4, the method for testing of sulphates content in the flue gas desulphurization system according to claim 3 is characterized in that described buffer solution pH is 3.8～4.2.
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| CN112240912B (en) * | 2019-07-17 | 2022-08-12 | 上海梅山钢铁股份有限公司 | Method for determining content of calcium nitrite in sintering desulfurization and denitrification ash |
| CN111208032A (en) * | 2020-02-26 | 2020-05-29 | 江苏省沙钢钢铁研究院有限公司 | Method for measuring and analyzing content of calcium sulfite and calcium sulfide |
| CN113533624A (en) * | 2021-05-25 | 2021-10-22 | 华电电力科学研究院有限公司 | Online sampling and sulfite measuring system for desulfurized slurry and working method thereof |
| CN113390753A (en) * | 2021-06-15 | 2021-09-14 | 广西电网有限责任公司电力科学研究院 | Method for testing content of combustible in limestone wet desulphurization slurry solid |
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