CN103398965B - Detect the method for Fe content in graphene oxide and Graphene sample - Google Patents
Detect the method for Fe content in graphene oxide and Graphene sample Download PDFInfo
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Abstract
Detect the method for Fe content in graphene oxide and Graphene sample, it is characterized in that the canonical plotting first drawing absorbance and Fe content relation, then the absorbance of sample is measured, absorbance per sample checks in the content of corresponding manganese from absorbance and Fe content affinity criterions curve map, the invention has the beneficial effects as follows that the method detecting Fe content in graphene oxide and Graphene sample is simple, easy realization, the accuracy of detection of Fe content can meet the demands.
Description
Technical field
The present invention relates to novel energy resource material technology field, is more particularly a kind of method detecting Fe content in graphene oxide and Graphene sample.
Background technology
Graphene oxide and Graphene are a kind of materials of new rise in recent years, have a lot of advantageous characteristic.Intensity as Graphene is high, good conductivity etc., graphene oxide or current a kind of novel carbon nanomaterial adsorbent, various heavy metal ion and dyestuff in waste water can be removed, have now been developed various physics, chemical method prepares grapheme material, wherein widely used is chemical oxidization method, graphite oxidation is obtained graphene oxide by general oxygenant such as potassium permanganate, but also in material, introduce manganese ion simultaneously, Fe content in conservative control graphene oxide and Graphene, the purity of product can be improved, and then improve the performance of graphene oxide product, but also there is no a kind of rationally perfect method to detect the content of manganese in graphene oxide and Graphene at present, mainly deposit reason both ways: one is that graphite oxide and grapheme material intensity are higher, stable in properties, general strong acid is utilized to be difficult to be cleared up, two is that graphene oxide composite material can be sharply weightless within the scope of 150 ~ 200 DEG C, sample can be caused to disperse and lose, surveyed Fe content accuracy is reduced when utilizing high temperature sintering or elemental analyser to analyze Fe content.
Summary of the invention
The invention provides the detection method of Fe content in a kind of graphene oxide and Graphene sample, the method simply, easily realizes, may be used for the detection based on Fe content in graphene oxide and Graphene class material, it is characterized in that the canonical plotting first drawing absorbance and Fe content relation, then measure the absorbance of sample, absorbance per sample checks in the content of corresponding manganese from absorbance and Fe content affinity criterions curve map.
Described absorbance and Fe content affinity criterions curve map making step as follows:
(1) pipette the manganese standard solution of 1.00 mL, 3.00 mL, 5.00 mL, 7.00mL, 10.00mL respectively, solution density is 10 μ g/mL, then, add 10mL sulfuric acid and 5g ammonium sulfate respectively, cover surface plate, heat 40 minutes in electric furnace, cooling, with distilled water purge surface plate and sidewall of crucible;
(2) add the nitric acid of 1.5mL respectively, add the distilled water of 40mL, be heated to closely boil, take off, add 0.3g potassium metaperiodate, 12min is boiled in heating, and cooling, moves in 50mL volumetric flask, and add distilled water diluting to scale, shake up;
(3) move in 3cm absorption vessel respectively, with distilled water contrast for referencial use, on spectrophotometer, in wavelength 530nm place, surveying its absorbance, take absorbance as ordinate, and Fe content is horizontal ordinate drawing standard curve map, as shown in Figure 1.
The method of Fe content in described detection graphene oxide and Graphene sample, its step is as follows:
(1) accurately take sample, be accurate to 0.0001g;
(2) sample is positioned in silica crucible, paves, drip the concentrated sulphuric acid to sample and cover completely and blackening;
(3) silica crucible is positioned in electric furnace, is heated to tobacco and disperses;
(4) taking out to be positioned in muffle furnace in 900 DEG C of calcination 4h, burns completely to sample, cooling;
(5) add sulfuric acid and 5g ammonium sulfate that 10mL density is 1.84g/mL, cover surface plate, be heated to residue and dissolve completely in electric furnace, cooling, with distilled water purge surface plate and sidewall of crucible;
(6) add the nitric acid of 1.5mL, add the distilled water of 40mL, be heated to closely boil, take off, add 0.3g potassium metaperiodate, 12min is boiled in heating, and cooling, moves in 50mL volumetric flask, and add distilled water diluting to scale, shake up.
(7) move in 3cm absorption vessel, with distilled water contrast for referencial use, on spectrophotometer, in wavelength 530nm place, survey its absorbance, find corresponding Fe content from absorbance to Fe content affinity criterions curve map.
The invention has the beneficial effects as follows that the method detecting Fe content in graphene oxide and Graphene sample is simple, easily realize, the accuracy of detection of Fe content can meet the demands.
accompanying drawing illustrates:
Accompanying drawing 1 is absorbance of the present invention and Fe content affinity criterions curve map.
embodiment:
Embodiment of the present invention are further described, so that the public grasps specific embodiment of the invention method better below in conjunction with specific embodiment.
embodiment 1
(1) accurately take 0.5000g graphene oxide, be accurate to 0.0001g;
(2) sample is positioned in silica crucible, paves, drip the concentrated sulphuric acid to sample and cover completely and blackening;
(3) silica crucible is positioned in electric furnace, is heated to tobacco and disperses;
(4) taking out to be positioned in muffle furnace in 900 DEG C of calcination 4h, burns completely to sample, cooling;
(5) add sulfuric acid and 5g ammonium sulfate that 10mL density is 1.84g/mL, cover surface plate, be heated to residue and dissolve completely in electric furnace, cooling, with distilled water purge surface plate and sidewall of crucible;
(6) add the nitric acid of 1.5mL, add the distilled water of 40mL, be heated to closely boil, take off, add 0.3g potassium metaperiodate, 12min is boiled in heating, and cooling, moves in 50mL volumetric flask, and add distilled water diluting to scale, shake up.
(7) move in 3cm absorption vessel, with distilled water contrast for referencial use, on spectrophotometer, in wavelength 530nm place, survey its absorbance, find corresponding Fe content from absorbance to Fe content affinity criterions curve map.
embodiment 2
(1) accurately take 0.5000g Graphene, be accurate to 0.0001g;
(2) sample is positioned in silica crucible, paves, drip the concentrated sulphuric acid to sample and cover completely and blackening;
(3) silica crucible is positioned in electric furnace, is heated to tobacco and disperses;
(4) taking out to be positioned in muffle furnace in 900 DEG C of calcination 4h, burns completely to sample, cooling;
(5) add sulfuric acid and 5g ammonium sulfate that 10mL density is 1.84g/mL, cover surface plate, be heated to residue and dissolve completely in electric furnace, cooling, with distilled water purge surface plate and sidewall of crucible;
(6) add the nitric acid of 1.5mL, add the distilled water of 40mL, be heated to closely boil, take off, add 0.3g potassium metaperiodate, 12min is boiled in heating, and cooling, moves in 50mL volumetric flask, and add distilled water diluting to scale, shake up.
(7) move in 3cm absorption vessel, with distilled water contrast for referencial use, on spectrophotometer, in wavelength 530nm place, survey its absorbance, find corresponding Fe content from absorbance to Fe content affinity criterions curve map.
The invention has the beneficial effects as follows that the method detecting Fe content in graphene oxide and Graphene sample is simple, easily realize, the accuracy of detection of Fe content can meet the demands.
Claims (1)
1. detect the method for Fe content in graphene oxide and Graphene sample, it is characterized in that the canonical plotting first drawing absorbance and Fe content relation, then measure the absorbance of sample, absorbance per sample checks in the content of corresponding manganese from absorbance and Fe content affinity criterions curve map;
The step of described absorbance and Fe content affinity criterions curve map is as follows:
(1) pipette the manganese standard solution of 1.00 mL, 3.00 mL, 5.00 mL, 7.00mL, 10.00mL respectively, solution density is 10 μ g/mL, then, add 10mL sulfuric acid and 5g ammonium sulfate respectively, cover surface plate, heat 40 minutes in electric furnace, cooling, with distilled water purge surface plate and sidewall of crucible;
(2) add the nitric acid of 1.5mL respectively, add the distilled water of 40mL, be heated to closely boil, take off, add 0.3g potassium metaperiodate, 12min is boiled in heating, and cooling, moves in 50mL volumetric flask, and add distilled water diluting to scale, shake up;
(3) move in 3cm absorption vessel respectively, with distilled water contrast for referencial use, on spectrophotometer, in wavelength 530nm place, surveying its absorbance, take absorbance as ordinate, and Fe content is horizontal ordinate drawing standard curve map;
The described step checking in the content of corresponding manganese from absorbance and Fe content affinity criterions curve map is as follows:
(1) accurately take sample, be accurate to 0.0001g;
(2) sample is positioned in silica crucible, paves, drip the concentrated sulphuric acid to sample and cover completely and blackening;
(3) silica crucible is positioned in electric furnace, is heated to tobacco and disperses;
(4) taking out to be positioned in muffle furnace in 900 DEG C of calcination 4h, burns completely to sample, cooling;
(5) add sulfuric acid and 5g ammonium sulfate that 10mL density is 1.84g/mL, cover surface plate, be heated to residue and dissolve completely in electric furnace, cooling, with distilled water purge surface plate and sidewall of crucible;
(6) add the nitric acid of 1.5mL, add the distilled water of 40mL, be heated to closely boil, take off, add 0.3g potassium metaperiodate, 12min is boiled in heating, and cooling, moves in 50mL volumetric flask, and add distilled water diluting to scale, shake up;
(7) move in 3cm absorption vessel, with distilled water contrast for referencial use, on spectrophotometer, in wavelength 530nm place, survey its absorbance, find corresponding Fe content from absorbance to Fe content affinity criterions curve map.
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| CN104677846A (en) * | 2015-02-28 | 2015-06-03 | 济宁利特纳米技术有限责任公司 | Quantitative analysis method for graphene dispersion liquid |
| CN106770262A (en) * | 2017-02-22 | 2017-05-31 | 济宁利特纳米技术有限责任公司 | A kind of method of graphene oxide powder manganese content detection |
| CN107036988A (en) * | 2017-05-18 | 2017-08-11 | 山东玉皇新能源科技有限公司 | It is a kind of to detect the method that graphene Gold Samples belong to constituent content |
| CN107102096B (en) * | 2017-06-12 | 2019-12-13 | 常州第六元素材料科技股份有限公司 | Method for detecting ash content of graphene oxide |
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| JPS5612549A (en) * | 1979-07-13 | 1981-02-06 | Kawasaki Steel Corp | Method for determining manganese content in iron and steel |
| JPH0252240A (en) * | 1988-08-15 | 1990-02-21 | Nippon Steel Corp | Solution circulation type automatic absorption analysis |
| CN101078688A (en) * | 2007-05-31 | 2007-11-28 | 中国铝业股份有限公司 | Method for determining phosphor and manganese of ferro-phosphorus |
| US20110299085A1 (en) * | 2010-06-04 | 2011-12-08 | Solum, Inc. | Rapid Tissue Analysis Technique |
| CN102313705A (en) * | 2010-12-07 | 2012-01-11 | 中国一拖集团有限公司 | Method for determining manganese content in hair |
| CN102243153B (en) * | 2011-05-03 | 2013-03-27 | 武钢集团昆明钢铁股份有限公司 | Method for measuring contents of manganese, copper and oxides in directly reduced iron |
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| CN102735515A (en) * | 2012-07-23 | 2012-10-17 | 武钢集团昆明钢铁股份有限公司 | Method for measuring contents of Fe, Mn, Cu, Tin and Mg in titanium sponge, titanium and titanium alloy |
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Address after: 272000 A5 building, Chongwen road research and production base, Jining hi tech Industrial Development Zone, Shandong, China Patentee after: Shandong lett Nano Technology Co., Ltd. Address before: 272000 A5 building, Chongwen road research and production base, Jining hi tech Industrial Development Zone, Shandong, China Patentee before: Jining Leader Nano Technology Co., Ltd. |