CN102628850A - Method for quickly calibrating concentration of potassium dichromate standard titration solution - Google Patents
Method for quickly calibrating concentration of potassium dichromate standard titration solution Download PDFInfo
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- CN102628850A CN102628850A CN2012100926824A CN201210092682A CN102628850A CN 102628850 A CN102628850 A CN 102628850A CN 2012100926824 A CN2012100926824 A CN 2012100926824A CN 201210092682 A CN201210092682 A CN 201210092682A CN 102628850 A CN102628850 A CN 102628850A
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Abstract
The invention provides a method for quickly calibrating the concentration of potassium dichromate standard titration solution. The method is characterized by comprising the following steps: preparing standard solution with the concentration equal to that of potassium dichromate standard solution to be calibrated by using standard potassium dichromate and calculating the concentration C1; removing ferrous ion solution, titrating by using standard solution prepared by a standard reagent of the standard potassium dichromate and recording the consumed volume V1; removing ferrous ion solution with the same quantity, titrating by using the potassium dichromate standard solution to be calibrated and recording the volume V2 consumed by the standard solution; and calculating the concentration C2 of the potassium dichromate standard solution to be calibrated by a formula. According to the method, the concentration of the ferrous ion standard solution is not calculated; the concentration of the potassium dichromate standard titration solution is calculated without the concentration of the ferrous ion standard solution; and a blank test is not required. Calibration is performed synchronously; an indicator, blank and the like in the original calibration, and the undetermined superimposed and amplification effect during calculation are reduced; and calibration is accurate, simple and easy to master and calculation is simple and convenient.
Description
Technical field
The present invention relates to a kind of method of demarcating potassium dichromate standard titration solution concentration.
Background technology
The potassium dichromate standard titration solution is a kind of standard titration solution commonly used in the chemical analysis titration, is usually used in the titration of redox reaction, in result's calculating, need accurately know its standard value.Its compound method is according to two kinds of methods are arranged among the GB/T601-2002; A kind of is directly to prepare with base weight potassium chromate standard reagent; Calculating concentration need not demarcated, and this is seldom feasible for potassium dichromate standard titration solution consumption, but very big for the consumption of potassium dichromate standard titration solution in the daily production analysis in a lot of laboratories; The cost that is all spent with the preparation of base weight potassium chromate standard reagent is bigger, all is to prepare laggard rower with the potassium dichromate AR to decide.The demarcation of potassium dichromate standard titration solution and calculating are after demarcating with sodium thiosulfate standard solution among the GB/T601-2002; Concentration with sodium thiosulfate standard solution calculates; But sodium thiosulfate standard solution is demarcated with the solution of a certain amount of base weight potassium chromate reagent after must preparing again and placing for two weeks; The uncertainty of sodium thiosulfate standard solution and calculating round-off error etc. will pass to the potassium dichromate standard titration solution in this process; Cause the uncertain multiple stack of potassium dichromate concentration, make its uncertain increasing.And agents useful for same is many in hypo solution and the potassium bichromate solution titration process, and stepwise titration is operated unskilled people and is difficult for titration success, and troublesome poeration.Also have a kind of situation, in daily production, replace sodium thiosulfate standard solution to come titration to dissolve appearance with the standard of analytical reagent potassium dichromate preparation with the ferrous sulphate standard solution, the same GB of step is said.There is the uncertain multiple stack of potassium dichromate concentration so equally, makes its uncertain increasing.
Summary of the invention
Technical matters to be solved by this invention provides a kind of method of demarcating and calculating potassium dichromate standard titration solution concentration, to overcome existing in prior technology the titration of ferrous ion standard solution and concentration is calculated the superpose defective of the potassium dichromate standard titration solution concentration distortion that brings of the error that is produced.
For solving the problems of the technologies described above; The present invention provides a kind of method of demarcating and calculating potassium dichromate standard titration solution concentration, and the present invention need not calculate the concentration of ferrous ion standard solution, need not calculate the concentration of potassium dichromate standard titration solution with the concentration of ferrous ion standard solution again; Need not carry out blank test; Demarcate and to carry out synchronously, uncertain stack and amplification in having reduced in the former demarcation indicator, blank etc. and having calculated, and calculate easy.It is characterized in that, may further comprise the steps:
Step 1, with base weight potassium chromate preparation standard solution with the suitable concentration of potassium dichromate concentration of standard solution to be calibrated, calculate its concentration C
1
Step 2, pipette a ferrous ions soln, with the standard solution titration of base weight potassium chromate standard reagent preparation, the volume V of record standard solution consumption
1
Step 3, pipette with the said ferrous ions soln of step 2 same amount a, with potassium dichromate standard solution while titration to be calibrated, the volume V of record standard solution consumption
2
Step 4, according to the principle that ferrous ion amount that standard solution consumed equates, use
Formula
(1), calculates the concentration C of potassium dichromate standard titration solution to be calibrated
2
More improved, in the said step 2, adopt once above titration respectively, each time consumes the volume extreme difference of volumetric soiutions can not be greater than 0.05mL, and the mean value of getting the volume that each time consume volumetric soiutions is as V
1Value substitution formula (1), improve V more
1Fiduciary level.
More improved equally, in the said step 3, adopt once above titration respectively, each time consumes the volume extreme difference of volumetric soiutions can not be greater than 0.05mL, and the mean value of getting the volume that each time consume volumetric soiutions is as V
2Value substitution formula (1), improve V more
2Fiduciary level.
Preferably, said step 2,3 described ferrous ions soln concentration and potassium dichromate concentration of standard solution C to be calibrated
1Quite.Said ferrous ions soln is a l ferrous ammonium sulfate solution.
Beneficial effect of the present invention is:
(1) only need prepare with base weight potassium chromate standard reagent the standard titration solution of a certain amount of accurate concentration, ferrous ions soln can roughly be prepared, and these solution can use repeatedly, and particularly as long as ferrous iron solution is evenly, but basic indefinite duration.
(2) demarcate and to carry out synchronously, uncertain stack and amplification in having reduced in the former demarcation indicator, blank etc. and having calculated.
(3) used method is skilled and wield reaction in the daily titration in most laboratories in the demarcation, and simple to operation, agents useful for same is few, and blank can be ignored, and speed, the accuracy of demarcation improve greatly.
Below in conjunction with embodiment technical scheme of the present invention is further specified.
Embodiment
About concentration of the potassium bichromate solution of (1) demarcating according to need; Take by weighing a certain amount of (being accurate to 0.01mg) base weight potassium chromate standard reagent after treatment; The standard solution of preparation and the close concentration of potassium bichromate solution of demarcating, as required amount what, can be respectively with the volumetric flask 200mL～5000mL of different capabilities; Prepare the base weight potassium chromate solution of different volumes, calculate the exact value c of its concentration
(benchmark)
(2) l ferrous ammonium sulfate solution of preparation and the close concentration of potassium dichromate standard titration solution is a certain amount of, and what also measure as required, can prepare the l ferrous ammonium sulfate solution of different volumes, does not need very accurately constant volume and accurate concentration.
(3) pipette two parts of standard solution titrations of l ferrous ammonium sulfate solution simultaneously with the preparation of base weight potassium chromate standard reagent; Add 15mL sulfuric acid-phosphoric acid acid mixture (15+15+70), be diluted with water to 100mL, add 4～5 diphenylamine sulfonic acid sodium salt indicator solutions (2g/L); The potassium dichromate standard titration solution of preparing with the base weight potassium chromate respectively; It is terminal point that titration to test solution is stable aubergine, the volume that record consumes, and V averages
(benchmark), pipette and two parts of preceding same amount l ferrous ammonium sulfate solution with method, with potassium dichromate standard solution titration to be calibrated, with the method titration, the volume that record consumes, V averages
(waiting to mark), the iron ammonium sulfate amount that consumes according to them equates, uses formula
Calculate the concentration of potassium dichromate standard titration solution to be calibrated.
Specific embodiment:
Example 1: calibrated and calculated concentration is about the potassium dichromate standard titration solution concentration of 0.025mol/mL
(1) take by weighing 1.2258g potassium dichromate (standard reagent, 120 ℃ ± 5 ℃ are dried to constant), water-soluble, move in the 1000mL volumetric flask, be diluted with water to scale, mixing, the concentration of this potassium dichromate standard titration solution is c (1/6K
2Cr
2O
7)=0.02500mol/L.
(2) take by weighing 10g iron ammonium sulfate [(NH
4)
2Fe (SO
4)
26H
2O, formula weight 392.13], be dissolved in the 1000mL sulfuric acid (5+95) mixing.
(3) obtain four parts of 25.00mL iron ammonium sulfate volumetric soiutions; Add 15mL sulfuric acid-phosphoric acid acid mixture (15+15+70); Be diluted with water to 100mL; Add 4～5 diphenylamine sulfonic acid sodium salt indicator solutions (2g/L); Two parts of potassium dichromate standard titration solutions that use base weight potassium chromate compound concentration as 0.02500mol/L respectively; It is terminal point that titration to test solution is stable aubergine; The potassium dichromate standard titration solution volume that twice titration consumes is respectively 24.88mL and 24.85mL; Mean value is 24.86mL, in addition uses potassium dichromate standard titration solution to be calibrated titration respectively with method for two parts, and the potassium dichromate standard titration solution volume that twice titration consumes is respectively 24.95mL and 24.93mL; Mean value is 24.94mL, the concentration of potassium dichromate standard titration solution then to be calibrated
Example 2: calibrated and calculated concentration is about the potassium dichromate standard titration solution concentration of 0.05mol/mL
(1) take by weighing 12.258g potassium dichromate (standard reagent, 120 ℃ ± 5 ℃ are dried to constant), water-soluble, move in the 5000mL volumetric flask, be diluted with water to scale, mixing, the concentration of this potassium dichromate standard titration solution is c (1/6K
2Cr
2O
7)=0.05000mol/L.
(2) take by weighing 100g iron ammonium sulfate [(NH
4)
2Fe (SO
4)
26H
2O, formula weight 392.13], be dissolved in the 5000mL sulfuric acid (5+95) mixing.
(3) obtain four parts of 20.00mL iron ammonium sulfate volumetric soiutions; Add 15mL sulfuric acid-phosphoric acid acid mixture (15+15+70); Be diluted with water to 100mL; Add 4～5 diphenylamine sulfonic acid sodium salt indicator solutions (2g/L); Two parts of potassium dichromate standard titration solutions that use base weight potassium chromate compound concentration as 0.05000mol/L respectively; It is terminal point that titration to test solution is stable aubergine; The potassium dichromate standard titration solution volume that twice titration consumes is respectively 20.01mL and 20.05mL; Mean value is 20.03mL, in addition uses potassium dichromate standard titration solution to be calibrated titration respectively with method for two parts, and the potassium dichromate standard titration solution volume that twice titration consumes is respectively 19.95mL and 19.93mL; Mean value is 19.94mL, the concentration of potassium dichromate standard titration solution then to be calibrated
Example 3: calibrated and calculated concentration is about the potassium dichromate standard titration solution concentration of 0.1mol/mL
(1) take by weighing 2.4516g potassium dichromate (standard reagent, 120 ℃ ± 5 ℃ are dried to constant), water-soluble, move in the 500mL volumetric flask, be diluted with water to scale, mixing, the concentration of this potassium dichromate standard titration solution is c (1/6K
2Cr
2O
7)=0.1000mol/L.
(2) take by weighing 20g iron ammonium sulfate [(NH
4)
2Fe (SO
4)
26H
2O, formula weight 392.13], be dissolved in the 500mL sulfuric acid (5+95) mixing.
(3) obtain four parts of 25.00mL iron ammonium sulfate volumetric soiutions; Add 15mL sulfuric acid-phosphoric acid acid mixture (15+15+70); Be diluted with water to 100mL; Add 4～5 diphenylamine sulfonic acid sodium salt indicator solutions (2g/L); Two parts of potassium dichromate standard titration solutions that use base weight potassium chromate compound concentration as 0.1000mol/L respectively; It is terminal point that titration to test solution is stable aubergine; The potassium dichromate standard titration solution volume that twice titration consumes is respectively 25.05mL and 25.03mL; Mean value is 25.04mL, in addition uses potassium dichromate standard titration solution to be calibrated titration respectively with method for two parts, and the potassium dichromate standard titration solution volume that twice titration consumes is respectively 24.88mL and 24.92mL; Mean value is 24.90mL, the concentration of potassium dichromate standard titration solution then to be calibrated
It should be noted last that; Above embodiment is only unrestricted in order to technical scheme of the present invention to be described; Although with reference to preferred embodiment the present invention is specified, those of ordinary skill in the art should be appreciated that and can make amendment or be equal to replacement technical scheme of the present invention; And not breaking away from the spirit and the scope of technical scheme of the present invention, it all should be encompassed in the middle of the claim scope of the present invention.
Claims (5)
1. method of demarcating fast potassium dichromate standard titration solution concentration is characterized in that may further comprise the steps:
Step 1, with base weight potassium chromate preparation standard solution with the suitable concentration of potassium dichromate concentration of standard solution to be calibrated, calculate its concentration C
1
Step 2, pipette ferrous ions soln, with the standard solution titration of base weight potassium chromate standard reagent preparation, the volume V of record standard solution consumption
1
Step 3, pipette the said ferrous ions soln with step 2 equivalent, with potassium dichromate standard solution to be calibrated titration simultaneously, the volume V of record standard solution consumption
2
Step 4, according to the principle that ferrous ion amount that standard solution consumed equates, use formula
Calculate the concentration C of potassium dichromate standard titration solution to be calibrated
2
2. the method for quick demarcation potassium dichromate standard titration solution concentration according to claim 1 is characterized in that, in the said step 2, adopts once above titration respectively, and the mean value of volume of getting each time consumption volumetric soiutions is as V
1Value.
3. the method for quick demarcation potassium dichromate standard titration solution concentration according to claim 2 is characterized in that, in the said step 3, adopts once above titration respectively, and the mean value of volume of getting each time consumption volumetric soiutions is as V
2Value.
4. according to the method for the described quick demarcation potassium dichromate standard titration solution concentration of one of claim 1-3, it is characterized in that said step 2,3 described ferrous ions soln concentration and potassium dichromate concentration of standard solution C to be calibrated
1Quite.
5. the method for quick demarcation potassium dichromate standard titration solution concentration according to claim 4 is characterized in that said ferrous ions soln is a l ferrous ammonium sulfate solution.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103487550A (en) * | 2013-09-23 | 2014-01-01 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for determining content of nitric acid in titanium plate pickling solution |
| CN106093019A (en) * | 2016-05-31 | 2016-11-09 | 贵州大学 | A kind of method analyzing content of organics in sodium aluminate solution |
| CN109580871A (en) * | 2018-11-26 | 2019-04-05 | 九江萍钢钢铁有限公司 | A kind of method of potassium bichromate standard solution calibration |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103487550A (en) * | 2013-09-23 | 2014-01-01 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for determining content of nitric acid in titanium plate pickling solution |
| CN106093019A (en) * | 2016-05-31 | 2016-11-09 | 贵州大学 | A kind of method analyzing content of organics in sodium aluminate solution |
| CN109580871A (en) * | 2018-11-26 | 2019-04-05 | 九江萍钢钢铁有限公司 | A kind of method of potassium bichromate standard solution calibration |
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