CN101650337A - Method for testing chloride content in smoke gas desulfurization system - Google Patents

Method for testing chloride content in smoke gas desulfurization system Download PDF

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CN101650337A
CN101650337A CN200910075361A CN200910075361A CN101650337A CN 101650337 A CN101650337 A CN 101650337A CN 200910075361 A CN200910075361 A CN 200910075361A CN 200910075361 A CN200910075361 A CN 200910075361A CN 101650337 A CN101650337 A CN 101650337A
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chloride content
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CN101650337B (en
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宋晓红
张欣
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State Grid Corp of China SGCC
Electric Power Research Institute of State Grid Hebei Electric Power Co Ltd
Hebei Electric Power Construction Adjustment Test Institute
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Electric Power Research Institute of State Grid Hebei Electric Power Co Ltd
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Abstract

The invention relates to a method for testing chloride content in a smoke gas desulfurization system, belonging to the technical field of testing the chloride content in a smoke gas desulfurization system. The basic principle of the invention is that as the serum and the product of the desulfurization system has various types and high content of impurities, total ion strength buffer solution needsto be added to improve the anti-interference ability of potentiometric titration in an electrode method and maintain the pH value in measurement within a proper range. By adding total ion strength adjusting buffer solution to the sample to be tested (functions of improving the ion strength, enhancing the anti-interference ability and adjusting the pH value), the invention increases the anti-reference ability in the potentiometric titration method and improves the reliability of the testing result. The invention has the characteristics of stable and reliable method, and greatly improves the reliability of the analysis result compared with the prior art.

Description

The method of testing of chloride content in a kind of flue gas desulphurization system
Technical field
The present invention relates to the determination techniques field of flue gas desulphurization system chloride content.
Background technology
Chloride content in the flue gas desulphurization system is that system is operating must survey project.Determination of chlorine ion content adopts silver nitrate volumetric method or ammonium thiocyanate volumetric method usually.When being used for the mensuration of flue gas desulphurization system slurries and gypsum chlorion, there is following problem respectively in these two kinds of methods: the silver nitrate volumetric method is owing to be subjected to the influence of testing sample color, and its terminal colour changes very not obvious, is easy to generate bigger error at measurment; The ammonium thiocyanate volumetric method is complicated operation not only, and same existence is subjected to the influence of testing sample color easily, titration end-point is difficult for the problem of judgement, for improving the accuracy of measurement result, often need be in titration process, add nitrobenzene, and nitrobenzene is a kind of toxicant that the intense stimulus taste is arranged, very big to tester's actual bodily harm.
Based on above situation, some unit has used potentiometric titration instead, error when potentiometric titration can be eliminated the visual inspection change color fully, but when being actually used in the desulphurization system sample test, since the sample composition complexity, the impurity ion content height is very big to the interference of measurement result, instrument often occurs and misread the phenomenon of titration end-point, bring certain uncertainty to measurement result.
Summary of the invention
The method that the purpose of this invention is to provide a kind of potentiometric determination flue gas desulphurization system chloride content, by in testing sample, adding a kind of total ionic strength adjustment buffer degree buffer solution, improved the stability of potentiometric determination desulphurization system chloride content, the method that is characterized in is reliable and stable, compared with the prior art, improved the reliability of analysis result greatly.
The present invention adopts following technical scheme:
The present invention regulates buffer solution by adding the total ionic strength adjustment buffer degree, and the antijamming capability when having increased the potentiometric titration test has improved reliability of testing result; The compound method that described total ionic strength adjustment buffer degree is regulated buffer solution is: take by weighing 100g potassium nitrate and place the 1000ml beaker, add 50ml acetic acid, add deionized water and be diluted to 500ml, adjusting pH with the sodium hydroxide solution of 40g/L is 5, is diluted to 1L with deionized water at last;
The step of the method for testing of described mensuration desulphurization system chloride content is:
(1) get the gypsum samples of 10-20g drying, add 300ml distilled water, after fully shaking up, filter with quantitative filter paper at a slow speed, and fully wash gypsum samples with distilled water, filtrate is collected constant volume in the 500ml volumetric flask;
(2) get 50-100ml filtrate, place the 250ml beaker, add 10-15ml total ionic strength adjustment buffer degree and regulate buffer solution;
(3) connect potentiometric titrimeter and supporting test electrode.Stirrer is put into beaker, beaker is placed on the magnetic stirrer, make electrode immerse solution, turn on agitator is under middling speed stirs (do not spatter mistake, no bubble produces).Add the silver nitrate standard solution with potentiometric titrimeter and carry out potentiometric titration, the consumption of silver nitrate standard solution when record arrives titration end-point.
(4) do blank assay simultaneously with the distilled water of chloride not.
Chloride content is (with CL -Meter) calculate:
CL -%=3.55(v 2c-v 1c)×500÷(v×s)
Wherein: CL -%: chloride content in the sample, %;
3.55: convert and get in the molal weight of chlorine * 100 ÷, 1000 backs;
V: the filtrate volume of getting during mensuration, ml;
V 2: sample consumes liquor argenti nitratis ophthalmicus volume, ml;
V 1: blank liquor argenti nitratis ophthalmicus volume, the ml of consuming;
C: standard silver nitrate solution concentration, mol/L;
500: filtrate cumulative volume, ml;
S: example weight, g.
Beneficial effect of the present invention is as follows: Determination of chlorine ion content, adopt silver nitrate volumetric method or ammonium thiocyanate volumetric method usually.When being used for the mensuration of flue gas desulphurization system slurries and gypsum chlorion, these two kinds of methods exist the not obvious and test process of indicator change color may produce problems such as harm to the tester respectively.For this reason, preferably select potentiometric titration for use, but this method is when being actually used in the desulphurization system sample test, owing to be subjected to factor affecting such as sample composition complexity, impurity ion content height, instrument often occurs and misread the phenomenon of titration end-point, bring certain uncertainty to measurement result.The ultimate principle of foundation of the present invention be since in desulphurization system slurries and the product impurity component kind many and content is high, need to add total ionic strength adjustment buffer degree buffer solution and improve the antijamming capability of electrode method potentiometric titration, and keep pH when measuring in OK range.The present invention is by adding a kind of total ionic strength adjustment buffer degree buffer solution in testing sample, increased the total ionic strength adjustment buffer degree of solution to be measured and guaranteed that the pH value is at zone of reasonableness, improve the stability of potentiometric determination desulphurization system chloride content, thoroughly eliminated the interference of impurity component.Compared with the prior art method, has improved precision of test result accurately and reliably.
Embodiment
One, testing tool
Analytical balance: precision is more than 0.1mg reaches;
Potentiometric titrimeter and supporting test electrode (compound silver electrode or indicator electrode+contrast electrode);
The conventional instrument in laboratories such as magnetic stirrer.
Two, reagent
1. sodium chloride standard solution (0.0141mol/L): take by weighing 0.8240g benchmark sodium chloride (through 140 ℃ of dry mistakes), soluble in water, move in the 1000ml volumetric flask, be diluted with water to graticule, shake up.This solution contains the 500ug chlorion for every milliliter.
2. silver nitrate standard solution (0.0141mol/L): take by weighing the 2.395g silver nitrate, soluble in water, add the 2ml red fuming nitric acid (RFNA), move in the 1000ml volumetric flask, be diluted with water to graticule, shake up.Be stored in the brown bottle, keep in Dark Place.Demarcate with the sodium chloride standard solution.
Demarcating steps is as follows:
1) draws 10.00ml sodium chloride standard solution, place the 250ml beaker, add 2ml nitric acid, be diluted to 100ml.
2) connect potentiometric titrimeter and supporting test electrode.Stirrer is put into beaker, beaker is placed on the magnetic stirrer, make electrode immerse solution, turn on agitator, under stirring, middling speed (do not spatter mistake, no bubble produces) carry out potentiometric titration with potentiometric titrimeter adding silver nitrate standard solution, when arriving titration end-point, record consumes silver nitrate standard solution volume V (ml).
3) carry out blank assay by same step, record consumes silver nitrate standard solution volume V 0(ml).
Calculate: silver nitrate concentration of standard solution=0.141/ (V-V 0) mol/L
3. the total ionic strength adjustment buffer degree is regulated buffer solution: take by weighing 100g
Figure G2009100753611D00031
Potassium nitrate places the 1000ml beaker, adds 50ml acetic acid, adds deionized water and is diluted to 500ml, and adjusting pH with the sodium hydroxide solution of 40g/L is 5, is diluted to 1L with deionized water at last.
Three, testing procedure and result calculate
(1) get the gypsum samples of 10-20g drying, add 300ml distilled water, after fully shaking up, filter with quantitative filter paper at a slow speed, and fully wash gypsum samples with distilled water, filtrate is collected constant volume in the 500ml volumetric flask;
(2) get 50-100ml filtrate, place the 250ml beaker, add 10-15ml total ionic strength adjustment buffer degree and regulate buffer solution;
(3) connect potentiometric titrimeter and supporting test electrode.Stirrer is put into beaker, beaker is placed on the magnetic stirrer, make electrode immerse solution, turn on agitator is under middling speed stirs (do not spatter mistake, no bubble produces).Add the silver nitrate standard solution with potentiometric titrimeter and carry out potentiometric titration, the consumption of silver nitrate standard solution when record arrives titration end-point.
(4) do blank assay simultaneously with the distilled water of chloride not.
Chloride content is (with CL -Meter) calculate:
CL -%=3.55(v 2c-v 1c)×500÷(v×s)
Wherein: CL -%: chloride content in the sample, %;
3.55: convert and get in the molal weight of chlorine * 100 ÷, 1000 backs;
V: the filtrate volume of getting during mensuration, ml;
V 2: the titration sample consumes liquor argenti nitratis ophthalmicus volume, ml;
V 1: blank liquor argenti nitratis ophthalmicus volume, the ml of consuming of titration;
C: standard silver nitrate solution concentration, mol/L;
500: filtrate cumulative volume, ml;
S: example weight, g.
Adopt the inventive method also to can be used to chloride content in test absorbant slurries and the desulfurization slurry.
Be described further below in conjunction with embodiment, but not as a limitation of the invention.
Embodiment 1:
(1) get the gypsum samples of 10.2010g drying, add 300ml distilled water, after fully shaking up, filter with quantitative filter paper at a slow speed, and fully wash gypsum samples with distilled water, filtrate is collected constant volume in the 500ml volumetric flask;
(2) get 100ml (V) filtrate, place the 250ml beaker, add 10ml total ionic strength adjustment buffer degree and regulate buffer solution;
(3) connect potentiometric titrimeter and supporting test electrode.Stirrer is put into beaker, beaker is placed on the magnetic stirrer, make electrode immerse solution, turn on agitator is under middling speed stirs (do not spatter mistake, no bubble produces).Add 0.0140mol/L (C) silver nitrate standard solution with potentiometric titrimeter and carry out potentiometric titration, the consumption V of silver nitrate standard solution when record arrives titration end-point 2Be 15.10ml.
(4) be blank assay V simultaneously with the distilled water of chloride not 1Be 0ml.
Chloride content is (with CL -Meter) result of calculation is:
CL -%=3.55×0.014×15.10×500÷(100×10.2010)=0.37
Embodiment 2:
(1) get the gypsum samples of 14.0512g drying, add 300ml distilled water, after fully shaking up, filter with quantitative filter paper at a slow speed, and fully wash gypsum samples with distilled water, filtrate is collected constant volume in the 500ml volumetric flask;
(2) get 100ml (V) filtrate, place the 250ml beaker, add 15ml total ionic strength adjustment buffer degree and regulate buffer solution;
(3) connect potentiometric titrimeter and supporting test electrode.Stirrer is put into beaker, beaker is placed on the magnetic stirrer, make electrode immerse solution, turn on agitator is under middling speed stirs (do not spatter mistake, no bubble produces).Add 0.0140mol/L (C) silver nitrate standard solution with potentiometric titrimeter and carry out potentiometric titration, the consumption V of silver nitrate standard solution when record arrives titration end-point 2Be 10.26ml.
(4) be blank assay V simultaneously with the distilled water of chloride not 1Be 0ml.
Chloride content is (with CL -Meter) result of calculation is:
CL -%=3.55×0.014×10.26×500÷(100×14.0512)=0.18
Embodiment 3:
(1) get the gypsum samples of 19.9625g drying, add 300ml distilled water, after fully shaking up, filter with quantitative filter paper at a slow speed, and fully wash gypsum samples with distilled water, filtrate is collected constant volume in the 500ml volumetric flask;
(2) get 50ml (V) filtrate, place the 250ml beaker, add 12ml total ionic strength adjustment buffer degree and regulate buffer solution;
(3) connect potentiometric titrimeter and supporting test electrode.Stirrer is put into beaker, beaker is placed on the magnetic stirrer, make electrode immerse solution, turn on agitator is under middling speed stirs (do not spatter mistake, no bubble produces).Add 0.0140mol/L (C) silver nitrate standard solution with potentiometric titrimeter and carry out potentiometric titration, the consumption V of silver nitrate standard solution when record arrives titration end-point 2Be 5.05ml.
(4) be blank assay V simultaneously with the distilled water of chloride not 1Be 0ml.
Chloride content is (with CL -Meter) result of calculation is:
CL -%=3.55×0.014×5.05×500÷(100×19.9625)=0.063

Claims (1)

1, the method for testing of chloride content in a kind of flue gas desulphurization system is characterized in that regulating buffer solution by adding the total ionic strength adjustment buffer degree, and the antijamming capability when having increased the potentiometric titration test has improved reliability of testing result; The compound method that described total ionic strength adjustment buffer degree is regulated buffer solution is: take by weighing 100g potassium nitrate and place the 1000ml beaker, add 50ml acetic acid, add deionized water and be diluted to 500ml, adjusting pH with the sodium hydroxide solution of 40g/L is 5, is diluted to 1L with deionized water at last;
The step of the method for testing of described mensuration desulphurization system chloride content is:
(1) get the gypsum samples of 10-20g drying, add 300ml distilled water, after fully shaking up, filter with quantitative filter paper at a slow speed, and fully wash gypsum samples with distilled water, filtrate is collected constant volume in the 500ml volumetric flask;
(2) get 50-100ml filtrate, place the 250ml beaker, add 10-15ml total ionic strength adjustment buffer degree and regulate buffer solution;
(3) connect potentiometric titrimeter and supporting test electrode.Stirrer is put into beaker, beaker is placed on the magnetic stirrer, make electrode immerse solution, turn on agitator is under middling speed stirs (do not spatter mistake, no bubble produces).Add the silver nitrate standard solution with potentiometric titrimeter and carry out potentiometric titration, the consumption of silver nitrate standard solution when record arrives titration end-point;
(4) do blank assay simultaneously with the distilled water of chloride not,
Chloride content is (with CL -Meter) calculate:
CL -%=3.55(v 2c-v 1c)×500÷(v×s)
Wherein: CL -%: chloride content in the sample, %;
3.55: convert and get in the molal weight of chlorine * 100 ÷, 1000 backs;
V: the filtrate volume of getting during mensuration, ml;
V 2: sample consumes liquor argenti nitratis ophthalmicus volume, ml;
V 1: blank liquor argenti nitratis ophthalmicus volume, the ml of consuming;
C: standard silver nitrate solution concentration, mol/L;
500: filtrate cumulative volume, ml;
S: example weight, g.
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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103063726A (en) * 2013-01-10 2013-04-24 广州天赐高新材料股份有限公司 Detection method for chlorine ion content in lithium-ion battery electrolyte
CN109603502A (en) * 2018-12-29 2019-04-12 浙江大学 A kind of control system and method for flue gas dechlorination-desulfurization wastewater zero-emission
CN110927329A (en) * 2019-12-16 2020-03-27 国网四川省电力公司电力科学研究院 Atmospheric environment chloride ion deposition rate testing device and method
CN113671111A (en) * 2021-08-26 2021-11-19 金能科技股份有限公司 Method for quantitatively detecting chloride ions in potassium sorbate

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104483370A (en) * 2014-12-19 2015-04-01 国家电网公司 Method for testing concentration of water-soluble fluorine ion in flue gas desulfurization gypsum slurry

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103063726A (en) * 2013-01-10 2013-04-24 广州天赐高新材料股份有限公司 Detection method for chlorine ion content in lithium-ion battery electrolyte
CN103063726B (en) * 2013-01-10 2015-01-07 广州天赐高新材料股份有限公司 Detection method for chlorine ion content in lithium-ion battery electrolyte
CN109603502A (en) * 2018-12-29 2019-04-12 浙江大学 A kind of control system and method for flue gas dechlorination-desulfurization wastewater zero-emission
CN110927329A (en) * 2019-12-16 2020-03-27 国网四川省电力公司电力科学研究院 Atmospheric environment chloride ion deposition rate testing device and method
CN113671111A (en) * 2021-08-26 2021-11-19 金能科技股份有限公司 Method for quantitatively detecting chloride ions in potassium sorbate
CN113671111B (en) * 2021-08-26 2024-04-19 金能化学(齐河)有限公司 Method for quantitatively detecting chloride ions in potassium sorbate

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