CN102590202B - Measuring method of iron - Google Patents
Measuring method of iron Download PDFInfo
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- CN102590202B CN102590202B CN201210036764.7A CN201210036764A CN102590202B CN 102590202 B CN102590202 B CN 102590202B CN 201210036764 A CN201210036764 A CN 201210036764A CN 102590202 B CN102590202 B CN 102590202B
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Abstract
The invention discloses a measuring method of iron. The measuring method comprises the following steps of: preparing multiple Fe<3+> standard solutions with different concentrations; respectively adding a first nitric acid solution and a first potassium thiocyanate solution into the multiple Fe<3+> standard solutions so as to carry out a color reaction; preparing a solution to be tested by taking a ferric phosphate lithium sample, and adding the second nitric acid solution and the second potassium thiocyanate solution into the solution to be tested so as to carry out the color reaction; and carrying out color comparison on the solution to be tested after the color reaction and the Fe<3+> standard solutions after multiple color reactions, thus obtaining iron content in the solution to be tested according to a color comparison result. Compared with the ration measuring method in the prior art, the measuring method provided by the invention utilizes a semi-quantitative colorimetric method to measure the iron content in the solution to be tested, the measured result of the method is exact and reliable, the operation is simple, the application is broad, and the cost is lower.
Description
Technical field
The present invention relates to detection technique field, more particularly, relate to a kind of assay method of iron.
Background technology
In recent years, along with highlighting of the problems such as the day by day exhausted and global warming of resource, the life style of green low-carbon has been subject to advocating.Wherein, the next internal-combustion engines vehicle that partly replaces consumption of fossil fuels of development electric motor car and hybrid electric vehicle is one of main method solving energy crisis and ecological deterioration.Driving power is to affect the critical component that electric motor car is promoted the use of, and nowadays widely used driving power comprises lead-acid battery, ni-mh/NI-G, lithium ion battery etc.In various driving powers, lithium ion battery is high owing to having energy density, and cyclicity is good, and self-discharge rate is low, long service life and the advantage such as environmental pressure is little, has obtained research widely.
The performance of lithium ion battery depends primarily on positive and negative pole material, anode material for lithium-ion batteries comprises polyanion material and the metal oxide containing lithium, wherein, containing features such as the metal oxide of lithium raw material sources are abundant, inexpensive, nontoxic owing to having, environmental friendliness, theoretical capacity are high, thermal stability and good cycle, be widely used in recent years.LiFePO4 is a kind of important metal oxide containing lithium, have discharge capacity large, cheap, non-toxic, do not cause the features such as environmental pollution, be the study hotspot of current field of batteries.
There is the phenomenon of ferric ion stripping in LiFePO4, the too high meeting of iron stripping causes the self discharge of battery to increase the weight of in the time of high temperature, thereby affect the life-span of battery, therefore needs the iron stripping quantity of LiFePO4 correctly to evaluate.Prior art mainly adopts spectrophotometric method to measure iron, measure contained iron content in electrolytic solution by AAS or ICP-AES, platinum crucible used for electrolyte after filtration, by organic material evaporation and with testing after acid-soluble solution, obtains the iron stripping quantity of LiFePO4.But the spectrophotometric method that prior art adopts exists the shortcomings such as instrument and consumptive material costliness, test process be loaded down with trivial details, cost is higher.
Summary of the invention
In view of this, the technical problem to be solved in the present invention is to provide a kind of assay method of iron, and the method is simple to operate, and measurement result is more accurate.
In order to solve above technical matters, the invention provides a kind of assay method of iron, comprise the following steps:
Prepare the Fe of multiple variable concentrations
3+standard solution;
Respectively to described multiple Fe
3+in standard solution, add the first salpeter solution and the first potassium rhodanate solution to carry out chromogenic reaction;
Get LiFePO4 sample preparation product to be tested solution;
In described product to be tested solution, add the second salpeter solution and the second potassium rhodanate solution to carry out chromogenic reaction;
By the Fe after the product to be tested solution after described chromogenic reaction and described multiple chromogenic reaction
3+standard solution carries out colorimetric, obtains the iron content in product to be tested solution according to colorimetric result.
Preferably, also comprise the pre-treatment step of LiFePO4 sample:
LiFePO4 sample is toasted to 3～5h at 110～130 DEG C.
The step of getting LiFePO4 sample preparation product to be tested solution preferably, is specially:
By LiFePO4 sample and electrolytic solution by weight volume ratio be (0.9～1.1) g: (0.9～1.1) ml mixes, and sealing is filtered after preserving 40～60h.
Preferably, the temperature that described sealing is preserved is 50～70 DEG C.
Preferably, the w/v of described LiFePO4 sample and electrolytic solution is 1g: 1ml.
Preferably, the described sealing holding time is 48h.
Preferably, the Fe of described multiple variable concentrations
3+the Fe of standard solution
3+concentration is respectively 2ppm, 4ppm, 8ppm and 10ppm.
Preferably, the mass body volume concentrations of described the first potassium rhodanate solution and the second potassium rhodanate solution is respectively 25%g/ml.
Preferably, the volume ratio of described the first salpeter solution and the first potassium rhodanate solution is 1: 4.
Preferably, the volume ratio of described the second salpeter solution and the second potassium rhodanate solution is 1: 4.
The assay method that the invention provides a kind of iron, comprises the following steps: the Fe for preparing multiple variable concentrations
3+standard solution; Respectively to described multiple Fe
3+in standard solution, add the first salpeter solution and the first potassium rhodanate solution to carry out chromogenic reaction; Get LiFePO4 sample preparation product to be tested solution; In described product to be tested solution, add the second salpeter solution and the second potassium rhodanate solution to carry out chromogenic reaction; By the Fe after the product to be tested solution after described chromogenic reaction and described multiple chromogenic reaction
3+standard solution carries out colorimetric, obtains the iron content in product to be tested solution according to colorimetric result.Compared with the quantitative measuring method of prior art, the present invention utilizes the iron content in semiquantitative colorimetric method for determining product to be tested solution, and the method measurement result accurately and reliably, simple to operate, is widely used, and cost is lower.
Embodiment
Below the technical scheme in the embodiment of the present invention is clearly and completely described, obviously, described embodiment is only the present invention's part embodiment, instead of whole embodiment.Based on the embodiment in the present invention, those of ordinary skill in the art, not making the every other embodiment obtaining under creative work prerequisite, belong to the scope of protection of the invention.
The assay method that the invention discloses a kind of iron, comprises the following steps:
Prepare the Fe of multiple variable concentrations
3+standard solution;
Respectively to described multiple Fe
3+in standard solution, add the first salpeter solution and the first potassium rhodanate solution to carry out chromogenic reaction;
Get LiFePO4 sample preparation product to be tested solution;
In described product to be tested solution, add the second salpeter solution and the second potassium rhodanate solution to carry out chromogenic reaction;
By the Fe after the product to be tested solution after described chromogenic reaction and described multiple chromogenic reaction
3+standard solution carries out colorimetric, obtains the iron content in product to be tested solution according to colorimetric result.
According to the present invention, the Fe of described multiple variable concentrations
3+the Fe of standard solution
3+concentration is respectively 2ppm, 4ppm, 8ppm and 10ppm, can also be 1ppm, 2ppm, 3ppm, 5ppm, 7ppm, 9ppm, 14ppm and 16ppm.The Fe of described standard solution
3+concentration can be prepared according to the stripping quantity of the iron of LiFePO 4 material well known to those skilled in the art, for Fe
3+the concrete numerical value of concentration does not have special requirement.In addition, described Fe
3+standard solution can be according to method well known to those skilled in the art preparation, to this present invention and have no special requirements.Obtain Fe
3+after standard solution, respectively to described multiple Fe
3+in standard solution, add the first salpeter solution and the first potassium rhodanate solution to carry out chromogenic reaction, the step of this chromogenic reaction is preferably: the Fe that pipettes respectively 1000ppm
3+standard strong solution 0.2mL, 0.4mL, 0.8mL, 1.0mL, can also pipette respectively 0.1mL, 0.2mL, 0.3mL, 0.5mL, 0.7mL, 0.9mL, 1.4mL and 1.6mL in 100mL volumetric flask, be settled to scale mark and shake up with electrolytic solution, obtaining the Fe of multiple variable concentrations
3+standard solution; Then pipette respectively the Fe of multiple variable concentrations
3+standard solution enters in color comparison tube, adds 1mL the first salpeter solution and 4mL and the first potassium rhodanate solution, mixes rear leaving standstill.Due to potassium rhodanate and Fe
3+reaction can generate red cotton-shaped complex compound, and therefore, the present invention is taking potassium rhodanate as developer.The mass body volume concentrations of described the first potassium rhodanate solution is preferably 23～28%g/ml, more preferably 25%g/ml.Described the first potassium rhodanate solution is preferably prepared as follows: take 25g potassium rhodanate, add pure water and dissolve, constant volume 100mL, obtains the first potassium rhodanate solution.The molten potassium rhodanate of preparation the first potassium rhodanate that the present invention adopts is preferably commercial product, more preferably potassium rhodanate (analyzing pure).Meanwhile, the first salpeter solution that the present invention adopts is preferably red fuming nitric acid (RFNA) (analyzing pure), to its manufacturer and have no special requirements.
On the other hand, the present invention also comprises the step of preparing product to be tested solution.Before utilizing LiFePO4 sample preparation product to be tested solution, preferably it is carried out to pre-service, be specially: LiFePO4 sample is toasted to 3～5h at 110～130 DEG C, described baking temperature is preferably 120～130 DEG C, more preferably 120 DEG C, described baking time is preferably 4～5 hours, more preferably 4 hours.By the pre-service to described LiFePO4 sample, the Fe in the product to be tested solution that is conducive to prepare
3+content is closer to the stripping quantity of the iron of LiFePO4 in practical lithium-ion.
According to the present invention, described step of getting LiFePO4 sample preparation product to be tested solution is specially: by LiFePO4 sample and electrolytic solution by weight volume ratio be (0.9～1.1) g: (0.9～1.1) ml mixes, and sealing is filtered after preserving 40～60h.Described LiFePO4 sample and electrolytic solution by weight volume ratio are preferably (0.9～1.0) g: (0.9～1.0) ml, more preferably 1g: 1ml; The described sealing holding time is preferably 45～50h, more preferably 48h.The above-mentioned step of preparing product to be tested solution preferably includes normal temperature and measures and pyrometry, and wherein, the temperature that normal temperature is measured is preferably 15～30 DEG C, more preferably 20～25 DEG C; The temperature of described pyrometry is preferably 50～70 DEG C, and more preferably 55～65 DEG C, more preferably 60 DEG C.In addition, the present invention is for described filter method and have no special requirements, and preferably adopts qualitative double-deck Filter paper filtering.The present invention prepares the container of product to be tested solution and has no special requirements for described, is preferably polyethylene bottle, more has and elects the polyethylene bottle with liner as, and the specification of described polyethylene bottle is preferably 100ml.
Prepare after product to be tested solution, in described product to be tested solution, add the second salpeter solution and the second potassium rhodanate solution to carry out chromogenic reaction.Due to potassium rhodanate and Fe
3+reaction can generate red cotton-shaped complex compound, and therefore, the present invention is taking potassium rhodanate as developer.The mass body volume concentrations of described the second potassium rhodanate solution is preferably 23～28%g/ml, more preferably 25%g/ml.Described the second potassium rhodanate solution is preferably prepared as follows: take 25g potassium rhodanate, add pure water and dissolve, constant volume 100mL, obtains the second potassium rhodanate solution.In addition, the present invention is using salpeter solution as oxygenant, and described the second salpeter solution is preferably red fuming nitric acid (RFNA) (analyzing pure), and the concentration of described red fuming nitric acid (RFNA) is preferably commercial red fuming nitric acid (RFNA).Above-mentioned chromogenic reaction is preferably carried out in color comparison tube, and the present invention is for specification of described color comparison tube etc. and have no special requirements, and is preferably 10mL color comparison tube.
At Fe
3+standard solution and product to be tested solution carry out respectively after chromogenic reaction, by the Fe after the product to be tested solution after described chromogenic reaction and described multiple chromogenic reaction
3+standard solution carries out colorimetric, measures the iron content in product to be tested solution according to colorimetric result.Be specially the shade of the standard solution after upper strata red solution and the chromogenic reaction of the product to be tested solution after observation chromogenic reaction, relatively gained solution and any two groups of Fe
3+standard solution is close, proves contained Fe
3+in these two groups of Fe
3+within the scope of concentration of standard solution.
In sum, the present invention utilizes the iron content in semiquantitative colorimetric method for determining product to be tested solution, and the method measurement result accurately and reliably, simple to operate, be widely used, cost is lower, thereby without adopting prior art to adopt conventional instrument and the consumptive material of spectrophotometric method, save cost.
In order to further illustrate technical scheme of the present invention, below in conjunction with embodiment, the preferred embodiment of the invention is described, but should be appreciated that these are described is for further illustrating the features and advantages of the present invention, instead of limiting to the claimed invention.
The chemical reagent that the embodiment of the present invention and comparative example adopt is commercial.
Embodiment 1
Instrument and medicine: the Fe of 10mL color comparison tube, 100mL polyethylene bottle (band liner), potassium rhodanate (analyzing pure), nitric acid (analyzing pure), 1000ppm
3+iron standard solution (top grade is pure)
Determination step:
The configuration of potassium rhodanate solution: take 25g potassium rhodanate, add pure water and dissolve, constant volume 100mL, obtaining mass body volume concentrations is the potassium rhodanate solution of 25%g/ml.
The pre-service of sample: get LiFePO4 and carry out toasting 4h under the high temperature of 120 DEG C.
Normal temperature test iron stripping: take LiFePO 4 material 5.0000g, pipette electrolytic solution 50mL and add, seal preservation 2 days after shaking up, it is filtered with qualitative double-deck filter paper, filtrate is placed in plastic beaker label, obtains the first product to be tested solution.
High temperature test iron stripping: take LiFePO 4 material 5.0000g, pipette electrolytic solution 50mL and add, after shaking up, by its sealing and be placed in 60 DEG C of baking ovens and preserve 2 days, it is filtered with quantitative double-deck filter paper, filtrate is placed in 1 plastic beaker label, obtains the second product to be tested solution.
The Fe of configuration variable concentrations
3+standard solution: the Fe that pipettes respectively 1000ppm
3+standard solution 0.2mL, 0.4mL, 0.8mL and 1.0mL, in volumetric flask, are settled to scale mark and shake up with electrolytic solution, obtain concentration and are respectively 2ppm, 4ppm, 8ppm, the Fe of 10ppm
3+standard solution; Pipette respectively variable concentrations mark liquid again and enter in color comparison tube, add 1mL nitric acid, the potassium rhodanate solution of 4mL 25%g/ml carries out chromogenic reaction, mixes rear leaving standstill.
Colorimetric: pipette the first product to be tested solution 5mL in 10mL color comparison tube with transfer pipet, pipette 1mL nitric acid simultaneously and add in color comparison tube respectively, then add the potassium rhodanate solution of 4mL 25%g/ml, mix rear stratification.Observe and compare the Fe after upper strata red solution and the chromogenic reaction of the first product to be tested solution after chromogenic reaction
3+the depth of standard solution color, obtains: the color of the first product to be tested solution after chromogenic reaction is respectively the Fe of 2ppm and 4ppm with concentration
3+the color of standard solution approaches, therefore, and the Fe of described the first product to be tested solution
3+concentration is between 2ppm and 4ppm.
Colorimetric: pipette the second product to be tested solution 5mL in 10mL color comparison tube with transfer pipet, pipette 1mL nitric acid simultaneously and add in color comparison tube, then add the potassium rhodanate solution of 4mL25%g/ml, mix rear stratification.Observe and compare the Fe after upper strata red solution and the chromogenic reaction of the second product to be tested solution after chromogenic reaction
3+the depth of standard solution color, obtains: the color of the second product to be tested solution after chromogenic reaction is respectively the Fe of 8ppm and 10ppm with concentration
3+the color of standard solution approaches, therefore, and the Fe of described the second product to be tested solution
3+concentration is between 8ppm and 10ppm.
Embodiment 2～4
Adopt respectively the detection method of embodiment 1, the LiFePO4 of respectively different manufacturers being produced carries out the mensuration of iron stripping quantity.
Comparative example 1
Utilize the first product to be tested solution and the second product to be tested solution that spectrophotometric method is prepared embodiment 1 respectively to carry out Fe
3+the mensuration of content, result shows, the Fe of the first product to be tested solution
3+concentration is 3.1ppm, and the concentration of the second product to be tested solution is 9.3ppm.
Can find out from above embodiment and comparative example, the present invention utilizes the iron content in semiquantitative colorimetric method for determining product to be tested solution, and the method measurement result accurately and reliably, simple to operate, is widely used, and cost is lower.
To the above-mentioned explanation of the disclosed embodiments, make professional and technical personnel in the field can realize or use the present invention.To be apparent for those skilled in the art to the multiple amendment of these embodiment, General Principle as defined herein can, in the situation that not departing from the spirit or scope of the present invention, realize in other embodiments.Therefore, the present invention will can not be restricted to these embodiment shown in this article, but will meet the widest scope consistent with principle disclosed herein and features of novelty.
Claims (8)
1. an assay method for iron, comprises the following steps:
Prepare the Fe of multiple variable concentrations
3+standard solution;
Respectively to described multiple Fe
3+in standard solution, add the first salpeter solution and the first potassium rhodanate solution to carry out chromogenic reaction;
LiFePO4 sample is toasted to 3～5h at 110～130 DEG C, by LiFePO4 sample and electrolytic solution after baking by weight volume ratio be (0.9～1.1) g:(0.9～1.1) ml mixes, and filters after sealing preservation 40～60h, prepares product to be tested solution;
In described product to be tested solution, add the second salpeter solution and the second potassium rhodanate solution to carry out chromogenic reaction;
By the Fe after the product to be tested solution after described chromogenic reaction and described multiple chromogenic reaction
3+standard solution carries out colorimetric, obtains the iron content in product to be tested solution according to colorimetric result.
2. assay method according to claim 1, is characterized in that, the temperature that described sealing is preserved is 50～70 DEG C.
3. assay method according to claim 1, is characterized in that, the w/v of described LiFePO4 sample and electrolytic solution is 1g:1ml.
4. assay method according to claim 1, is characterized in that, the described sealing holding time is 48h.
5. assay method according to claim 1, is characterized in that, the Fe of described multiple variable concentrations
3+the Fe of standard solution
3+concentration is respectively 2ppm, 4ppm, 8ppm and 10ppm.
6. assay method according to claim 1, is characterized in that, the mass body volume concentrations of described the first potassium rhodanate solution and the second potassium rhodanate solution is 0.25g/ml.
7. assay method according to claim 1, is characterized in that, the volume ratio of described the first salpeter solution and the first potassium rhodanate solution is 1:4.
8. assay method according to claim 1, is characterized in that, the volume ratio of described the second salpeter solution and the second potassium rhodanate solution is 1:4.
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| CN102967600B (en) * | 2012-11-26 | 2015-12-09 | 宜宾海丝特纤维有限责任公司 | The detection method of sodium hydroxide solution iron content in a kind of viscose rayon |
| CN104034858A (en) * | 2014-06-04 | 2014-09-10 | 同济大学 | Method for simply measuring content of zero-valent iron in iron material |
| CN105021556A (en) * | 2015-07-22 | 2015-11-04 | 浙江瑞邦科技有限公司 | Detection method of iron content in lithium iron phosphate |
| CN109781930A (en) * | 2019-03-20 | 2019-05-21 | 金川集团股份有限公司 | Ferrimetry test paper in a kind of nickel electrowinning system solution |
| CN110865075A (en) * | 2019-12-31 | 2020-03-06 | 南通大学 | Conventional urinary iron detection kit and detection method thereof |
| CN111272684B (en) * | 2020-03-09 | 2023-03-10 | 欣旺达电动汽车电池有限公司 | Fe in electrolyte 2+ Method for measuring concentration |
| CN115184346B (en) * | 2022-07-08 | 2024-06-04 | 天鹏锂能技术(淮安)有限公司 | Battery self-discharge detection method |
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