CN106770262A - A kind of method of graphene oxide powder manganese content detection - Google Patents
A kind of method of graphene oxide powder manganese content detection Download PDFInfo
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- CN106770262A CN106770262A CN201710095879.6A CN201710095879A CN106770262A CN 106770262 A CN106770262 A CN 106770262A CN 201710095879 A CN201710095879 A CN 201710095879A CN 106770262 A CN106770262 A CN 106770262A
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- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
- G01N21/78—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
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Abstract
The invention belongs to new material detection technique field, more particularly to a kind of method of graphene oxide manganese content detection, it is characterised by that first graphene oxide powder being carbonized, then pre-processed and filtered, finally developed the color, its manganese content is detected by using ultra-violet and visible spectrophotometer.The beneficial effects of the invention are as follows can quickly determine manganese content in graphene oxide, research staff and user is set to have gained some understanding manganese content, while used as a Testing index of graphene oxide, method is simple, and operation is easy.
Description
Technical field
The invention belongs to new material detection technique field, more particularly to the side that a kind of graphene oxide powder manganese content is detected
Method.
Background technology
Graphene (Graphene, also known as mono-layer graphite or two-dimentional graphite) is the Two-dimensional Carbon atomic crystal of monoatomic thickness,
It is considered as the basic structural unit of fullerene, CNT and graphite.People are in theory to the research existing 60 of Graphene
For many years, Graphene is also widely used for describing the property of various carbon-based materials.Graphene is a kind of new material, and it is originated and grinds
Study carefully personnel and obtain Nobel chemistry Prize in 2010.Graphene is applied in lithium ion battery negative material, can significantly be carried
The capacitance and high rate charge-discharge performance of negative material high.Cause the great interest of scientific worker.
Graphene is widely applied so that people to being increased on the quality requirement of graphene product, while improve
To the quality requirement of graphene oxide powder, and tenor is one of its most important index, for being aoxidized with potassium permanganate
Agent, using being easy to containing manganese ion in graphene oxide prepared by the method for graphite oxide, to control the metal manganese ion
Content, need to detect to its manganese content.
The content of the invention
The present invention is directed to above-mentioned problem, there is provided a kind of method of graphene oxide powder manganese content detection.
In order to achieve the above object, the technical solution adopted by the present invention is,
, be carbonized for graphene oxide powder first by a kind of method of graphene oxide powder manganese content detection, is then carried out
Pretreatment and filtering, are finally developed the color, and its manganese content is detected by using ultra-violet and visible spectrophotometer；Specifically include with
Lower step：
A, Specification Curve of Increasing：On spectrophotometer, absorption curve is determined in the range of the nm of wavelength 525.5 ~ 545.5, survey it
Absorbance, subtracts the absorbance in company with the blank sample solution of sample, accurately draws absorbance-manganese content standard curve；
B, graphene oxide powder carbonization：The g graphene oxide powders of powder 0.2 ~ 1 are weighed in silica crucible, is tiled；It is added dropwise
The mL of sulfuric acid 3 ~ 6 is in powder；Silica crucible is positioned on electric hot plate, 120 DEG C ~ 140 DEG C 0.5 ~ 2h of calcination is heated to, then
180 DEG C ~ 230 DEG C 1 ~ 3h of calcination are warming up to, 240 DEG C ~ 270 DEG C to acid solution are warming up to again and are evaporated；Silica crucible is removed, it is cold
But to room temperature；
C, colour developing pretreatment：8 ~ 15 mL sulfuric acid and 4 g ~ 6g ammonium sulfate are added in silica crucible, crucible cover is covered, in heating plate
190 DEG C ~ 240 DEG C are heated to ammonium sulfate and are completely dissolved；It is cooled to room temperature；Add 1 ~ 3mL nitric acid, be then slowly added to 30mL ~
The distilled water of 60mL, is heated to nearly boiling（And add 6-8 explosion-proof pearl）, remove silica crucible and be cooled to room temperature；
D, filtering：Graphene oxide residue filter is fallen with filter paper, in 190 DEG C in heating plate ~ 240 DEG C heating, by moisture evaporation
To 15mL ~ 30mL or so, remove；
E, colour developing：0.2 g ~ 0.5g potassium metaperiodates are added immediately, and 5 ~ 13 min are boiled in heating, treat in colour stable, short time not
Change（Heating can not be crossed, it may occur that the phenomenon of color fade, cause the inaccuracy of result）, remove and be cooled to room temperature,
Move in 50mL volumetric flasks, constant volume shakes up；
F, by solution move into 1 cm cuvettes in, carry out detection reading in the drawn mark song of spectrophotometer, draw it
Manganese content.
Preferably, the standard curve is drawn by following methods：The manganese standard liquid of different content is prepared, it is pre- through colour developing
After treatment and color development treatment, determined in the range of 525.5 ~ 545.5 nm and survey its absorbance, accurately draw absorbance-manganese content mark
Directrix curve.
Compared with prior art, advantages and positive effects of the present invention are,
1st, the present invention tests various criterion concentration absorbance using ultraviolet-visible spectrophotometer, according to concentration known manganese mark
Liquid hold-up and the corresponding relation of absorbance, set up manganese content-absorbance curve, only need to test in solution to be measured in actual test
Absorbance, you can its manganese content is calculated by standard curve.
2nd, the present invention is less demanding to instrument and equipment, the characteristics of with detection faster, in overcoming existing method of testing
Complex steps, cycle shortcoming long, without Large expensive instrument, and reduce testing cost.
Specific embodiment
In order to be more clearly understood that the above objects, features and advantages of the present invention, with reference to embodiment to this hair
It is bright to be described further.It should be noted that in the case where not conflicting, the feature in embodiments herein and embodiment can
To be mutually combined.
Many details are elaborated in the following description in order to fully understand the present invention, but, the present invention may be used also
To be implemented using other modes described here are different from, therefore, the present invention is not limited to the specific of specification described below
The limitation of embodiment.
The invention provides a kind of method of graphene oxide powder manganese content detection, graphene oxide powder is entered first
Row carbonization, is then pre-processed and is filtered, and is finally developed the color, and its manganese is detected by using ultra-violet and visible spectrophotometer
Content.
Embodiment 1
1）Specification Curve of Increasing：Specification Curve of Increasing.1.00,3.00,5.00,7.00,10.00 mL manganese standard liquids are pipetted, point
Be not placed in one group of 200 silica crucible of mL, operated by determination step after adding 10 mL sulfuric acid and 5g ammonium sulfate, manganese content according to
It is secondary to be：0.2nd, 0.6,1.0,1.4,2.0 μ g/mL, move into 1cm cuvettes, make reference with distilled water, in spectrophotometer
On, its absorbance is surveyed in the range of the nm of wavelength 525.5 ~ 545.5, the absorbance in company with the blank sample solution of sample is subtracted, it is accurate
Really draw standard curve C=21.66A+0.233（r=0.995）.（Linearly dependent coefficient >=0.990）
The titer processing data of table 1
2）Graphene oxide powder is carbonized：Powder 0.5g graphene oxide powders are weighed in silica crucible, is tiled.Sulfuric acid is added dropwise
4 mL are in powder.Silica crucible is positioned on electric hot plate, 140 DEG C of calcination 1h are heated to, 210 DEG C of calcinations are then warming up to
1.5h, is warming up to 250 DEG C and is evaporated to acid solution again.Silica crucible is removed, room temperature is cooled to.
3）Colour developing pretreatment：10mL sulfuric acid and 5g ammonium sulfate are added in silica crucible, crucible cover is covered, in heating plate 210
DEG C being heated to ammonium sulfate is completely dissolved.It is cooled to room temperature.The nitric acid of 1.5mL is added, the distilled water of 50mL is then slowly added to, plus
Heat is boiled near（6-8 explosion-proof pearl）, remove silica crucible and be cooled to room temperature.
4）Filtering：Graphene oxide residue filter is fallen with filter paper, is heated in 210 DEG C in heating plate, by moisture evaporation extremely
20mL or so, removes.
5）Colour developing：0.3g potassium metaperiodates are added immediately, 10 min are boiled in heating, treat do not occur in colour stable, short time
Change（Heating can not be crossed, it may occur that the phenomenon of color fade, cause the inaccuracy of result）, remove and be cooled to room temperature, move to
In 50mL volumetric flasks, constant volume shakes up.
6）By in solution 1 cm cuvettes of immigration, detection reading is carried out in the drawn mark song of spectrophotometer, obtained
Go out its manganese content.
The manganese content test data of table 2
As seen from the above table, six groups of deviations of parallel laboratory test are 0.000682%, less than tolerance 0.0015%, therefore the difference of each data
Within the scope of tolerance.
Embodiment 2
1）Specification Curve of Increasing：Specification Curve of Increasing.1.00,3.00,5.00,7.00,10.00 mL manganese standard liquids are pipetted, point
Be not placed in one group of 200 silica crucible of mL, operated by determination step after adding 10 mL sulfuric acid and 5g ammonium sulfate, manganese content according to
It is secondary to be：0.2nd, 0.6,1.0,1.4,2.0 μ g/mL, move into 1cm cuvettes, make reference with distilled water, in spectrophotometer
On, its absorbance is surveyed in the range of the nm of wavelength 525.5 ~ 545.5, the absorbance in company with the blank sample solution of sample is subtracted, it is accurate
Really draw standard curve C=21.66A+0.233（r=0.995）.（Linearly dependent coefficient >=0.990）
The titer processing data of table 3
2）Graphene oxide powder is carbonized：Powder 0.5g graphene oxide powders are weighed in silica crucible, is tiled.Sulfuric acid is added dropwise
5 mL are in powder.Silica crucible is positioned on electric hot plate, 130 DEG C of calcination 2h are heated to, 220 DEG C of calcinations are then warming up to
1h, is warming up to 260 DEG C and is evaporated to acid solution again.Silica crucible is removed, room temperature is cooled to.
3）Colour developing pretreatment：10mL sulfuric acid and 5g ammonium sulfate are added in silica crucible, crucible cover is covered, in heating plate 220
DEG C being heated to ammonium sulfate is completely dissolved.It is cooled to room temperature.The nitric acid of 1.5mL is added, the distilled water of 50mL is then slowly added to, plus
Heat is boiled near（6-8 explosion-proof pearl）, remove silica crucible and be cooled to room temperature.
4）Filtering：Graphene oxide residue filter is fallen with filter paper, is heated in 220 DEG C in heating plate, by moisture evaporation extremely
30mL or so, removes.
5）Colour developing：0.3g potassium metaperiodates are added immediately, 12 min are boiled in heating, treat do not occur in colour stable, short time
Change（Heating can not be crossed, it may occur that the phenomenon of color fade, cause the inaccuracy of result）, remove and be cooled to room temperature, move to
In 50mL volumetric flasks, constant volume shakes up.
6）By in solution 1 cm cuvettes of immigration, detection reading is carried out in the drawn mark song of spectrophotometer, obtained
Go out its manganese content.
The manganese content test data of table 4
As seen from the above table, three groups of maximum differences of parallel laboratory test are 0.000728%, less than tolerance 0.0015%.
Embodiment 3
1）Specification Curve of Increasing：Specification Curve of Increasing.1.00,3.00,5.00,7.00,10.00 mL manganese standard liquids are pipetted, point
Be not placed in one group of 200 silica crucible of mL, operated by determination step after adding 10 mL sulfuric acid and 5g ammonium sulfate, manganese content according to
It is secondary to be：0.2nd, 0.6,1.0,1.4,2.0 μ g/mL, move into 1cm cuvettes, make reference with distilled water, in spectrophotometer
On, its absorbance is surveyed in the range of the nm of wavelength 525.5 ~ 545.5, the absorbance in company with the blank sample solution of sample is subtracted, it is accurate
Really draw standard curve C=29.99A+0.087（r=0.992）.（Linearly dependent coefficient >=0.990）
The titer processing data of table 5
2）Graphene oxide powder is carbonized：Powder 0.5g graphene oxide powders are weighed in silica crucible, is tiled.Sulfuric acid is added dropwise
4 mL are in powder.Silica crucible is positioned on electric hot plate, 130 DEG C of calcination 2h are heated to, 230 DEG C of calcinations are then warming up to
1h, is warming up to 250 DEG C and is evaporated to acid solution again.Silica crucible is removed, room temperature is cooled to.
3）Colour developing pretreatment：10mL sulfuric acid and 5g ammonium sulfate are added in silica crucible, crucible cover is covered, in heating plate 230
DEG C being heated to ammonium sulfate is completely dissolved.It is cooled to room temperature.The nitric acid of 1.5mL is added, the distilled water of 40mL is then slowly added to, plus
Heat is boiled near（6-8 explosion-proof pearl）, remove silica crucible and be cooled to room temperature.
4）Filtering：Graphene oxide residue filter is fallen with filter paper, is heated in 230 DEG C in heating plate, by moisture evaporation extremely
30mL or so, removes.
5）Colour developing：0.3g potassium metaperiodates are added immediately, 8 min are boiled in heating, treat not become in colour stable, short time
Change（Heating can not be crossed, it may occur that the phenomenon of color fade, cause the inaccuracy of result）, remove and be cooled to room temperature, move to
In 50mL volumetric flasks, constant volume shakes up.
6）By in solution 1 cm cuvettes of immigration, detection reading is carried out in the drawn mark song of spectrophotometer, obtained
Go out its manganese content.
The manganese content test data of table 6
As seen from the above table, three groups of maximum differences of parallel laboratory test are 0.000302%, less than tolerance 0.0015%.
The beneficial effects of the invention are as follows can quickly determine manganese content in graphene oxide, make research staff and user couple
Manganese content is had gained some understanding, while used as a Testing index of graphene oxide, method is simple, and operation is easy.
The above, is only presently preferred embodiments of the present invention, is not the limitation for making other forms to the present invention, is appointed
What those skilled in the art changed possibly also with the technology contents of the disclosure above or be modified as equivalent variations etc.
Effect embodiment is applied to other fields, but every without departing from technical solution of the present invention content, according to technical spirit of the invention
Any simple modification, equivalent variations and the remodeling made to above example, still fall within the protection domain of technical solution of the present invention.
Claims (2)
1. a kind of method that graphene oxide powder manganese content is detected, it is characterised in that first carry out graphene oxide powder
Carbonization, is then pre-processed and is filtered, and is finally developed the color, and detects that its manganese contains by using ultra-violet and visible spectrophotometer
Amount；Specifically include following steps：
Specification Curve of Increasing：On spectrophotometer, absorption curve is determined in the range of the nm of wavelength 525.5 ~ 545.5, survey its suction
Luminosity, subtracts the absorbance in company with the blank sample solution of sample, accurately draws absorbance-manganese content standard curve；
Graphene oxide powder is carbonized：The g graphene oxide powders of powder 0.2 ~ 1 are weighed in silica crucible, is tiled；Sulphur is added dropwise
3 ~ 6 mL are in powder for acid；Silica crucible is positioned on electric hot plate, 120 DEG C ~ 140 DEG C 0.5 ~ 2h of calcination are heated to, then risen
Temperature is warming up to 240 DEG C ~ 270 DEG C to acid solution and is evaporated again to 180 DEG C ~ 230 DEG C 1 ~ 3h of calcination；Silica crucible is removed, is cooled down
To room temperature；
Colour developing pretreatment：8 ~ 15 mL sulfuric acid and 4 g ~ 6g ammonium sulfate are added in silica crucible, crucible cover is covered, in heating plate 190
DEG C ~ 240 DEG C be heated to ammonium sulfate and be completely dissolved；It is cooled to room temperature；The nitric acid of 1 ~ 3mL is added, 30mL ~ 60mL is then slowly added to
Distilled water, be heated to nearly boiling, remove silica crucible and be cooled to room temperature；
Filtering：Graphene oxide residue filter is fallen with filter paper, is heated in 190 DEG C in heating plate ~ 240 DEG C, by moisture evaporation extremely
15mL ~ 30mL or so, removes；
Colour developing：0.2 g ~ 0.5g potassium metaperiodates are added immediately, 5 ~ 13 min are boiled in heating, treat not sent out in colour stable, short time
Changing, removes and is cooled to room temperature, moves in 50mL volumetric flasks, and constant volume shakes up；
By in solution 1 cm cuvettes of immigration, detection reading is carried out in the drawn mark song of spectrophotometer, draw its manganese
Content.
2. a kind of graphene oxide powder manganese content determination method according to claims 1, it is characterised in that institute
Standard curve is stated to be drawn by following methods：Prepare different content manganese standard liquid, through colour developing pretreatment and color development treatment after,
Its absorbance is determined in the range of 525.5 ~ 545.5 nm, absorbance-manganese content standard curve is accurately drawn.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109283319A (en) * | 2018-11-09 | 2019-01-29 | 榆林市科学技术信息研究所 | A kind of device for analyzing ore amount of storage and the ore investigation method based on the device |
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| CN109283319A (en) * | 2018-11-09 | 2019-01-29 | 榆林市科学技术信息研究所 | A kind of device for analyzing ore amount of storage and the ore investigation method based on the device |
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