CN103398965A - Method for detecting manganese content in graphene oxide and graphene samples - Google Patents

Abstract

The invention relates to a method for detecting manganese content in graphene oxide and graphene samples. The method is characterized by comprising: drawing a standard curve diagram of a relationship between absorbance and manganese content, measuring absorbance of a sample, and searching the corresponding manganese content from the standard curve diagram according to the absorbance of the sample. The method has the following characteristics that: the method is simple and easy to achieve, and detection precision of the manganese content can meet requirements.

Description

Detect the method for manganese content in graphene oxide and Graphene sample

Technical field

The present invention relates to the new energy materials technical field, more specifically say a kind of method that detects manganese content in graphene oxide and Graphene sample.

Background technology

Graphene oxide and Graphene are a kind of materials that newly rises in recent years, have a lot of advantageous characteristic.intensity as Graphene is high, good conductivity etc., graphene oxide or present a kind of novel carbon nanomaterial adsorbent, can remove various heavy metal ion and dyestuff in waste water, developed at present various physics, chemical method prepares grapheme material, wherein widely used is chemical oxidization method, general using oxygenant such as potassium permanganate obtain graphene oxide by graphite oxidation, but also in material, introduced manganese ion simultaneously, rationally control manganese content in graphene oxide and Graphene, can improve the purity of product, and then the performance of raising graphene oxide product, but also do not have a kind of rationally perfect method to detect the content of manganese in graphene oxide and Graphene at present, the main reason that has two aspects: the one, graphite oxide and grapheme material intensity are higher, stable in properties, utilize general strong acid to be difficult to it is cleared up, the 2nd, the graphene oxide material can be sharply weightless in 150～200 ℃ of scopes, while utilizing high temperature sintering or elemental analyser to analyze manganese content, can cause sample disperse and lose, and the manganese of surveying content accuracy is reduced.

Summary of the invention

The invention provides the detection method of manganese content in a kind of graphene oxide and Graphene sample, the method is simple, easily realization, can be for the detection based on graphene oxide and Graphene class material manganese content, it is characterized in that first drawing the canonical plotting of absorbance and manganese relation with contents, then measure the absorbance of sample, absorbance per sample checks in the content of corresponding manganese from absorbance and manganese relation with contents canonical plotting.

Described absorbance and manganese relation with contents canonical plotting making step are as follows:

⑴ pipette respectively the manganese standard solution of 1.00 mL, 3.00 mL, 5.00 mL, 7.00mL, 10.00mL, solution density is 10 μ g/mL, then, add respectively 10mL sulfuric acid and 5g ammonium sulfate, cover surface plate, heating is 40 minutes in electric furnace, and is cooling, with distilled water purge surface plate and sidewall of crucible;

⑵ add respectively the nitric acid of 1.5mL, adds the distilled water of 40mL, is heated to closely boil, and takes off, and adds the 0.3g potassium metaperiodate, and 12min is boiled in heating, and is cooling, moves in the 50mL volumetric flask, and adds distilled water diluting to scale, shakes up;

⑶ move into respectively in the 3cm absorption vessel, with distilled water contrast for referencial use, on spectrophotometer, in wavelength 530nm place, surveys its absorbance, and take absorbance as ordinate, manganese content is horizontal ordinate drawing standard curve map, as shown in Figure 1.

The method of manganese content in described detection graphene oxide and Graphene sample, its step is as follows:

⑴ accurately take sample, is accurate to 0.0001g;

⑵ be positioned over sample in silica crucible, paves, and drips the concentrated sulphuric acid to sample and cover also blackening fully;

⑶ be positioned over silica crucible in electric furnace, is heated to tobacco and disperses;

⑷ take out and to be positioned in muffle furnace in 900 ℃ of calcination 4h, to sample perfect combustion, cooling;

⑸ add 10mL density is sulfuric acid and the 5g ammonium sulfate of 1.84g/mL, covers surface plate, in electric furnace, is heated to residue and dissolves fully, cooling, with distilled water purge surface plate and sidewall of crucible;

⑹ add the nitric acid of 1.5mL, adds the distilled water of 40mL, is heated to closely boil, and takes off, and adds the 0.3g potassium metaperiodate, and 12min is boiled in heating, and is cooling, moves in the 50mL volumetric flask, and adds distilled water diluting to scale, shakes up.

⑺ move in the 3cm absorption vessel, with distilled water contrast for referencial use, on spectrophotometer, in wavelength 530nm place, surveys its absorbance, from absorbance and manganese relation with contents canonical plotting, finds corresponding manganese content.

The invention has the beneficial effects as follows that the method that detects manganese content in graphene oxide and Graphene sample is simple, easily realize, the accuracy of detection of manganese content can meet the demands.

The accompanying drawing explanation:

Accompanying drawing 1 is absorbance of the present invention and manganese relation with contents canonical plotting.

Embodiment:

Below in conjunction with specific embodiment, further describe embodiment of the present invention, so that the public grasps the specific embodiment of the invention method better.

Embodiment 1

⑴ accurately take the 0.5000g graphene oxide, is accurate to 0.0001g;

⑵ be positioned over sample in silica crucible, paves, and drips the concentrated sulphuric acid to sample and cover also blackening fully;

⑶ be positioned over silica crucible in electric furnace, is heated to tobacco and disperses;

⑷ take out and to be positioned in muffle furnace in 900 ℃ of calcination 4h, to sample perfect combustion, cooling;

⑸ add 10mL density is sulfuric acid and the 5g ammonium sulfate of 1.84g/mL, covers surface plate, in electric furnace, is heated to residue and dissolves fully, cooling, with distilled water purge surface plate and sidewall of crucible;

⑹ add the nitric acid of 1.5mL, adds the distilled water of 40mL, is heated to closely boil, and takes off, and adds the 0.3g potassium metaperiodate, and 12min is boiled in heating, and is cooling, moves in the 50mL volumetric flask, and adds distilled water diluting to scale, shakes up.

⑺ move in the 3cm absorption vessel, with distilled water contrast for referencial use, on spectrophotometer, in wavelength 530nm place, surveys its absorbance, from absorbance and manganese relation with contents canonical plotting, finds corresponding manganese content.

Embodiment 2

⑴ accurately take the 0.5000g Graphene, is accurate to 0.0001g;

⑵ be positioned over sample in silica crucible, paves, and drips the concentrated sulphuric acid to sample and cover also blackening fully;

⑶ be positioned over silica crucible in electric furnace, is heated to tobacco and disperses;

⑷ take out and to be positioned in muffle furnace in 900 ℃ of calcination 4h, to sample perfect combustion, cooling;

⑸ add 10mL density is sulfuric acid and the 5g ammonium sulfate of 1.84g/mL, covers surface plate, in electric furnace, is heated to residue and dissolves fully, cooling, with distilled water purge surface plate and sidewall of crucible;

⑹ add the nitric acid of 1.5mL, adds the distilled water of 40mL, is heated to closely boil, and takes off, and adds the 0.3g potassium metaperiodate, and 12min is boiled in heating, and is cooling, moves in the 50mL volumetric flask, and adds distilled water diluting to scale, shakes up.

⑺ move in the 3cm absorption vessel, with distilled water contrast for referencial use, on spectrophotometer, in wavelength 530nm place, surveys its absorbance, from absorbance and manganese relation with contents canonical plotting, finds corresponding manganese content.

The invention has the beneficial effects as follows that the method that detects manganese content in graphene oxide and Graphene sample is simple, easily realize, the accuracy of detection of manganese content can meet the demands.

Claims (4)

1. detect the method for manganese content in graphene oxide and Graphene sample, it is characterized in that first drawing the canonical plotting of absorbance and manganese relation with contents, then measure the absorbance of sample, absorbance per sample checks in the content of corresponding manganese from absorbance and manganese relation with contents canonical plotting.

2. the method for manganese content in detection graphene oxide according to claim 1 and Graphene sample is characterized in that described absorbance and manganese relation with contents canonical plotting making step are as follows:

⑴ pipette respectively the manganese standard solution of 1.00 mL, 3.00 mL, 5.00 mL, 7.00mL, 10.00mL, solution density is 10 μ g/mL, then, add respectively 10mL sulfuric acid and 5g ammonium sulfate, cover surface plate, heating is 40 minutes in electric furnace, and is cooling, with distilled water purge surface plate and sidewall of crucible;

⑵ add respectively the nitric acid of 1.5mL, adds the distilled water of 40mL, is heated to closely boil, and takes off, and adds the 0.3g potassium metaperiodate, and 12min is boiled in heating, and is cooling, moves in the 50mL volumetric flask, and adds distilled water diluting to scale, shakes up;

⑶ move into respectively in the 3cm absorption vessel, with distilled water contrast for referencial use, on spectrophotometer, in wavelength 530nm place, surveys its absorbance, and take absorbance as ordinate, manganese content is horizontal ordinate drawing standard curve map.

3. the method for manganese content in detection graphene oxide according to claim 1 and Graphene sample, is characterized in that the method for manganese content in described detection graphene oxide and Graphene sample, and its step is as follows:

⑴ accurately take sample, is accurate to 0.0001g;

⑵ be positioned over sample in silica crucible, paves, and drips the concentrated sulphuric acid to sample and cover also blackening fully;

⑶ be positioned over silica crucible in electric furnace, is heated to tobacco and disperses;

⑷ take out and to be positioned in muffle furnace in 900 ℃ of calcination 4h, to sample perfect combustion, cooling;

⑸ add 10mL density is sulfuric acid and the 5g ammonium sulfate of 1.84g/mL, covers surface plate, in electric furnace, is heated to residue and dissolves fully, cooling, with distilled water purge surface plate and sidewall of crucible;

⑹ add the nitric acid of 1.5mL, adds the distilled water of 40mL, is heated to closely boil, and takes off, and adds the 0.3g potassium metaperiodate, and 12min is boiled in heating, and is cooling, moves in the 50mL volumetric flask, and adds distilled water diluting to scale, shakes up.

4. ⑺ moves in the 3cm absorption vessel, with distilled water contrast for referencial use, on spectrophotometer, in wavelength 530nm place, surveys its absorbance, from absorbance and manganese relation with contents canonical plotting, finds corresponding manganese content.

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