CN103063804A - Analysis method for rapid determination of redundant alkali amount of brine - Google Patents

Analysis method for rapid determination of redundant alkali amount of brine Download PDF

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CN103063804A
CN103063804A CN2012105839945A CN201210583994A CN103063804A CN 103063804 A CN103063804 A CN 103063804A CN 2012105839945 A CN2012105839945 A CN 2012105839945A CN 201210583994 A CN201210583994 A CN 201210583994A CN 103063804 A CN103063804 A CN 103063804A
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titration
analysis method
brine
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salt solution
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管国兴
谢兴胜
陈留平
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China Salt Jintan Co Ltd
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China Salt Jintan Co Ltd
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Abstract

The invention relates to an analysis method for rapid determination of a redundant alkali amount of brine. The analysis method comprises the following steps of weighing VmL of a brine sample, adding a phenolphthalein indicator into the brine sample, carrying out hydrochloric acid titration until a titration end point, wherein a color becomes a reddish color at the titration end point, recording a titration volume of V1, adding a bromocresol green-methyl red mixed indicator into the brine solution, carrying out titration until the color becomes a reddish color, recording a titration volume of V2, and carrying out detection result calculation according to the formulas of NaOH(g/L)=(V1-V2)*CHCl*40.078/V and Na2CO3(g/L)=V2*CHCl*105.998/V. The analysis method adopts a one-step method so that a color changes at a titration end point and thus the analysis method is conducive to determination and reduces workload and system errors.

Description

Cross the analytical approach of alkali number in the Fast Measurement salt solution
Technical field
The present invention relates to cross in a kind of Fast Measurement salt solution the analytical approach of alkali number.
Technical background
Present many enterprises adopt standard GB/T/T4348.1-2000 " mensuration of sodium carbonate in the industrial NaOH " to detect and cross alkali number in the bittern, principle is to adopt two-step approach, add first barium chloride, generate barium carbonate, add the phenolphthalein agent of giving instruction and detect first NaOH, second step is got same sample solution, adds the indicator of bromcresol green-methyl red, detects the result that total alkali content was released alkali number on the contrary.
And Salt Industry mostly also is to adopt two-step approach, and the first step is to add potentiometric titration: Na equally 2CO 3+ BaCl 2=2NaCl+BaCO 3, NaOH+HCl=NaCl+H 2O; And second step adopts methyl orange titration, Na 2CO 3+ 2HCl=2NaCl+H 2O+CO 2↑, NaOH+HCl=NaCl+H 2It is orange that O, second step adopt the drawback of methyl orange titration to be that the color of methyl orange is become by yellow, and the variation of two kinds of colors is not clearly, and causes terminal point to be difficult to judge, all is the mode of getting two increments that adopts simultaneously when detecting, and work efficiency is not high.
Summary of the invention
The technical problem to be solved in the present invention is that two-step approach that existing Salt Industry adopts is measured and crossed alkali number in the salt solution and be difficult for judging terminal point, inefficiency.
The analytical approach step of crossing alkali number in the Fast Measurement salt solution provided by the invention comprises: measure a duplicate samples salt solution V milliliter, add phenolphthalein indicator, hydrochloric acid is titrated to color and is blush, record titration volume is V1, the mixed indicator that in this solution, adds again the green and methyl red of bromine first powder, titration end-point is titrated to blush by green, is recorded as volume V2; Testing result is calculated: NaOH(g/L)=(V1-V2) * C HCl* 40.078/V, Na 2CO 3(g/L)=V2*C HCl* 105.998/V.
As preferably, measure a duplicate samples salt solution V milliliter after, add first 25 milliliters of deionized waters, add again phenolphthalein indicator.
As preferably, the mass percent concentration ratio of the mixed indicator of the green and methyl red of bromine first powder is 1:1-2:1.
Classical method is to adopt methyl orange and this paper utilizes bromcresol green and methyl red mixed indicator, and the color change interval of methyl orange is: 3.1-4.4; And the color change interval of the mixed indicator of bromcresol green and methyl red is: pH5.0 is following to be kermesinus, pH5.1 is celadon, pH5.2 is above to be green, because our first step is to adopt phenolphthalein to make indicator, so volumetric soiutions is to equal 10 to PH, from above-mentioned color change interval, when continuing in this solution, to add mixed indicator since PH greater than 5.2, so green can appear in solution, pH value can be just less than 5 when being titrated to the terminal point blush.
During PH=5, this moment, the H+ ion activity was 10 -5, H+ ion activity 3.98*10 when pH value equals 4.4 -5, both differ 2.98*10 -5, that is to say that using these two kinds of indicator method errors is 2.98/10000ths, this can be ignored fully for conventional volumetry, and therefore, in this sense, two kinds of indicator can replace, and can consider the impact of analysis result.
The single stage method that this paper adopts both can make the terminal point variable color more be beneficial to outside the judgement, can reduce workload and systematic error again.
Embodiment
The invention will be further described below by specific embodiment, but be not limited to this.
Embodiment 1 classical two-step approach is surveyed excess base in the edible salt water
Measure 25 milliliters of duplicate samples salt solution, add barium chloride solution to producing without white precipitate, add phenolphthalein indicator (0.5% phenolphthalein ethanolic solution: get 0.5g phenolphthalein, with the dissolving of 95% ethanol, and be diluted to 100mL), hydrochloric acid is titrated to color and is blush;
Measure in addition 25 milliliters of sample salt solution, add methyl orange indicator (0.1% aqueous solution), hydrochloric acid is titrated to color and is orange.
Embodiment 2 single stage method of the present invention are surveyed excess base in the edible salt water
Measure 25 milliliters of duplicate samples salt solution, add 25 milliliters of deionized waters, add phenolphthalein indicator, hydrochloric acid is titrated to color and is blush, record titration volume is V1, add the mixed indicator (mass percent concentration ratio is 1:1) of the green and methyl red of bromine first powder in this solution, titration end-point is titrated to blush by green, is recorded as volume V2 again; Testing result is calculated: NaOH(g/L)=(V1-V2) * C HCl* 40.078/V, Na 2CO 3(g/L)=V2*C HCl* 105.998/V.
Embodiment 3 identical brine sample adopt respectively embodiment 1, the actual testing result of 2 methods
Figure BDA00002677950100031
Because crossing the testing result of alkali number in our salt solution is to belong to microanalysis, therefore, above-mentioned error can be ignored substantially.
The single stage method that this paper adopts both can make the terminal point variable color more be beneficial to judgement, can reduce workload and systematic error again, and carried out two kinds of method contrasts in reality detects, and confirmed the consistance of its testing result.

Claims (3)

1. cross the analytical approach of alkali number in the Fast Measurement salt solution, step comprises: measure a duplicate samples salt solution V milliliter, add phenolphthalein indicator, hydrochloric acid is titrated to color and is blush, record titration volume is V1, add the mixed indicator of the green and methyl red of bromine first powder in this solution, titration end-point is titrated to blush by green, is recorded as volume V2 again; Testing result is calculated: NaOH(g/L)=(V1-V2) * C HCl* 40.078/V, Na 2CO 3(g/L)=V2*C HCl* 105.998/V.
2. cross the analytical approach of alkali number in the Fast Measurement salt solution claimed in claim 1, it is characterized in that measuring a duplicate samples salt solution V milliliter after, add first 25 milliliters of deionized waters, add again phenolphthalein indicator.
3. cross the analytical approach of alkali number in the Fast Measurement salt solution claimed in claim 1, it is characterized in that the mass percent concentration ratio of the mixed indicator of the green and methyl red of bromine first powder is 1:1-2:1.
CN2012105839945A 2012-12-28 2012-12-28 Analysis method for rapid determination of redundant alkali amount of brine Pending CN103063804A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106053716A (en) * 2016-06-21 2016-10-26 中色奥博特铜铝业有限公司 Detection method of sodium hydroxide and sodium carbonate contents in surface degreasing fluid
CN107271604A (en) * 2017-07-14 2017-10-20 江苏脉科技有限公司 Cross alkali number in-line analyzer
CN109828082A (en) * 2019-02-25 2019-05-31 山东京博石油化工有限公司 A kind of quantitative detecting method of desulfurization alcoholic lye neutral and alkali ingredient
CN111257313A (en) * 2020-03-03 2020-06-09 江苏一脉科技有限公司 High-precision alkali passing amount online analysis system and method

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101183078A (en) * 2007-12-17 2008-05-21 中国铝业股份有限公司 Method for determining sodium hydrate content in aliphatic alcohol of extraction evaporation mother liquor
JP2011149900A (en) * 2010-01-25 2011-08-04 Dowa Holdings Co Ltd Method for analysing impurity in cyanoaurate

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101183078A (en) * 2007-12-17 2008-05-21 中国铝业股份有限公司 Method for determining sodium hydrate content in aliphatic alcohol of extraction evaporation mother liquor
JP2011149900A (en) * 2010-01-25 2011-08-04 Dowa Holdings Co Ltd Method for analysing impurity in cyanoaurate

Non-Patent Citations (1)

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Title
谢兴胜等: "快速测定盐水中过碱量的分析方法", 《盐业与化工》, vol. 41, no. 12, 15 December 2012 (2012-12-15), pages 24 - 25 *

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106053716A (en) * 2016-06-21 2016-10-26 中色奥博特铜铝业有限公司 Detection method of sodium hydroxide and sodium carbonate contents in surface degreasing fluid
CN107271604A (en) * 2017-07-14 2017-10-20 江苏脉科技有限公司 Cross alkali number in-line analyzer
CN109828082A (en) * 2019-02-25 2019-05-31 山东京博石油化工有限公司 A kind of quantitative detecting method of desulfurization alcoholic lye neutral and alkali ingredient
CN111257313A (en) * 2020-03-03 2020-06-09 江苏一脉科技有限公司 High-precision alkali passing amount online analysis system and method

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Application publication date: 20130424