CN108827943A - The method of multiple element in the digestion procedure and detection carbon material of carbon material - Google Patents
The method of multiple element in the digestion procedure and detection carbon material of carbon material Download PDFInfo
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- CN108827943A CN108827943A CN201810338644.XA CN201810338644A CN108827943A CN 108827943 A CN108827943 A CN 108827943A CN 201810338644 A CN201810338644 A CN 201810338644A CN 108827943 A CN108827943 A CN 108827943A
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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
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
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Abstract
The present invention provides the methods of multiple element in the digestion procedure of carbon material and detection carbon material.Above-mentioned digestion procedure includes：Carbon material and acid solution are mixed, and obtained mixed solution is heated to clear, obtains carbon material digestion solution, wherein the acid solution contains sulfuric acid, perchloric acid and nitric acid.Inventors have found that carbon material can be adequately dissolved in above-mentioned acid solution in a heated condition, the carbon material digestion solution of clear is obtained, to guarantee the accuracy during subsequent detection, and the preparation method is easy to operate, convenient to carry out.
Description
Technical field
The present invention relates to technical field of analytical chemistry, specifically, being related in the digestion procedure and detection carbon material of carbon material
The method of multiple element.
Background technique
Aluminium, iron, manganese, copper, zinc, cobalt, potassium, sodium, calcium, magnesium, molybdenum, titanium are usually contained in the carbon material that different field uses at present
The grade nonmetalloids such as various metals and elemental silicon, phosphorus (such as impurity, it can be the other metallic elements and Fei Jin in addition to carbon
Belong to element), the method for measuring and analyzing content of the above-mentioned other elements in addition to carbon mainly using to sample by ashing processing after,
It is 3% nitric acid constant volume that mass fraction is recycled after melting using lithium tetraborate, using the principle of atomic emission spectrum, carries out instrument
Analysis detection, and this method is many and diverse and deviation is larger.
Therefore, the detection method of each element still needs to be studied in carbon material.
Summary of the invention
The present invention is directed to solve at least some of the technical problems in related technologies.For this purpose, of the invention
One purpose is the digestion procedure and carbon for the carbon material for proposing that a kind of operating method is simple, detection time is short or accuracy is high
The detection method of each element in material.
In one aspect of the invention, the present invention provides a kind of digestion procedures of carbon material.Implementation according to the present invention
Example, the above method include：Carbon material and acid solution are mixed, and obtained mixed solution is heated to clear, is obtained
Carbon material digestion solution, wherein the acid solution contains sulfuric acid, perchloric acid and nitric acid.Inventors have found that carbon materials in a heated condition
Material can be adequately dissolved in above-mentioned acid solution, the pretreatment such as do not need to be filtered carbon material, clear can be obtained
Carbon material digestion solution, it is simple to operate, time-consuming short, and auxiliary appliance used is less, it is convenient to carry out and subsequent by carbon material
Result error is small when digestion solution is for constituent content mensure, and accuracy and precision are high.
According to an embodiment of the invention, the carbon material include in graphene, carbon nanotube, petroleum coke and carbon block at least
It is a kind of.
According to an embodiment of the invention, further including by the carbon before mixing the carbon material and the acid solution
Material is ground to the step of in powder morphology.
According to an embodiment of the invention, the concentration of sulfuric acid is 0.0575~0.575g/mL, perchloric acid in the acid solution
Concentration be 0.0425~0.425g/mL and the concentration of nitric acid is 0.0504~0.504g/mL.
According to an embodiment of the invention, the mixed solution is placed in the heating device that initial temperature is not less than 80 degrees Celsius
On heated.
According to an embodiment of the invention, the initial temperature is more than or equal to 80 degrees Celsius and is less than or equal to 150 degrees Celsius.
According to an embodiment of the invention, the heating rate heated to the mixed solution is less than or equal to 5 DEG C/minute
Clock.
In one aspect of the invention, the present invention provides a kind of methods of multiple element in detection carbon material.According to this
The embodiment of invention, this method include：Carbon material digestion solution is prepared using mentioned-above method, and using high purity water to described
Carbon material digestion solution carries out constant volume；It is returned to zero according to blank sample to inductively-coupled plasma spectrometer, then utilizes electricity
Sense coupled plasma spectrometer measures the intensity value of above-mentioned each element at the corresponding optimal wavelength of each element respectively；According to upper
The intensity value and standard curve measured is stated, determines the content of above-mentioned each element.Not only detection method is simple as a result, easily operated,
And detection accuracy is high, can be with the content of each element in Accurate Determining carbon material, and this method has mentioned-above carbon
All feature and advantage of the digestion procedure of material, this is no longer going to repeat them.
According to an embodiment of the invention, each element be selected from aluminium, iron, manganese, copper, zinc, cobalt, potassium, sodium, calcium, magnesium, molybdenum, titanium,
At least one of silicon and phosphorus.
According to an embodiment of the invention, the standard curve is obtained by following steps：Mixing standard liquid and acid solution are mixed
It closes, and obtained mixed solution is subjected to gradient dilution, obtain a series of standard solution to be measured of various concentrations, wherein described
Acid solution is consistent with the acid solution for being used to prepare carbon material digestion solution；Using inductively-coupled plasma spectrometer respectively described
The intensity value that each element is measured at the corresponding optimal wavelength of each element is with the mass percentage of each element respectively
Abscissa, the intensity value of each element are ordinate, and drafting obtains standard curve.
The present invention at least can get following technical effect：
1, measuring method use scope of the present invention is wide, including all carbon such as graphene, carbon nanotube and petroleum coke, carbon block
The measurement and analysis of multiple element content in cellulosic material.
2, the method for the invention such as does not need to be filtered carbon material sample at the pretreatment, can be directly added into corresponding reagent
Constant volume detects afterwards.
3, method of the invention is easy to operate, the preparation time of carbon material digestion solution is short, detects multiple element in carbon material
Result error it is small, high reliablity.
4, auxiliary appliance used in the present invention is less, and carbon materials can be completed in balance, conical flask, heating plate, wash bottle and volumetric flask
The resolution of material.
Detailed description of the invention
Fig. 1 is the flow diagram that multiple element in carbon material is detected in one embodiment of the invention.
Specific embodiment
The embodiment of the present invention is described below in detail.The embodiments described below is exemplary, and is only used for explaining this hair
It is bright, and be not considered as limiting the invention.Particular technique or condition are not specified in embodiment, according to text in the art
It offers described technology or conditions or is carried out according to product description.Reagents or instruments used without specified manufacturer,
For can be with conventional products that are commercially available.
In one aspect of the invention, the present invention provides a kind of digestion procedures of carbon material.Implementation according to the present invention
Example, the above method include：Carbon material and acid solution are mixed, and obtained mixed solution is heated to clear, is obtained
Carbon material digestion solution, wherein acid solution contains sulfuric acid, perchloric acid and nitric acid.Inventors have found that in a heated condition, carbon material
It can adequately be dissolved in above-mentioned acid solution, the pretreatment such as not need to be filtered carbon material, clear can be obtained
Carbon material digestion solution, it is simple to operate, time-consuming short, and auxiliary appliance used is less, it is convenient to carry out, and measurement result deviation
Small, accuracy and precision are high.
According to an embodiment of the invention, the specific type of carbon material is there is no limit requiring, can in this field it is any
The carbon material (material containing carbon, and based on carbon) known.In an embodiment of the present invention, carbon material includes graphite
At least one of alkene, carbon nanotube, petroleum coke and carbon block.The digestion procedure of above-mentioned carbon material can be adapted for various as a result,
Carbon material expands its scope of application.
According to an embodiment of the invention, in order to preferably be dissolved in carbon material in acid solution, by the carbon material and institute
Before stating acid solution mixing, the carbon material can be ground in powder morphology in advance.Specific lapping mode can be machine
The partial size of tool ball milling, mortar grinder etc., powder is not particularly limited, as long as guaranteeing that sample is uniform.Thus, it is possible to improve
Rate of dissolution of the carbon material in acid solution shortens technique duration.
According to an embodiment of the invention, carbon material is being immersed acid in order to improve the accuracy of subsequent detection constituent content
Before solution, carbon material can be dried, remove moisture therein.Thus, it is possible to improve the accuracy of testing result.
According to an embodiment of the invention, in order to improve rate of dissolution and solubility of the carbon material in acid solution, acid solution
Contain sulfuric acid, perchloric acid and nitric acid.Thus, it is possible to carbon material solubility in acid solution is greatly improved, so that finally obtain
Carbon material test sample more clear improves the accuracy of multielement content in subsequent detection carbon material, and can be effective
It reduces and mixed solution is heated to clear the time it takes.
According to an embodiment of the invention, in acid solution various acid specific concentration there is no limit require, this field skill
Art personnel can be according to the actual demands flexible design such as different carbon materials.In an embodiment of the present invention, in order to enable carbon material
It is completely dissolved, so that the mixed solution more clear obtained, in acid solution, the concentration of sulfuric acid is 0.0575~0.575g/
ML, the concentration of perchloric acid is 0.0425~0.425g/mL and the concentration of nitric acid is 0.0504~0.504g/mL.As a result, compared to
It is molten in acid can to greatly improve carbon material by the acid solution of the acid concentration proportion preparation in the range for acid solution under other proportions
Rate of dissolution in liquid shortens dissolution time, wherein the concentration of any one or more acid is excessive or too small, can all slow down carbon materials
Expect the rate of dissolution in acid solution, when especially sulfuric acid concentration is excessively high, rate of dissolution of the carbon material in acid solution slows down
It is particularly evident.
According to an embodiment of the invention, prepare the method for the acid solution of above-mentioned concentration also there is no limit requiring, this field skill
Art personnel can flexible choice preparation method according to actual needs.In some embodiments of the invention, it can prepare in advance pre-
Determine the sulfuric acid solution, perchloric acid solution and nitric acid solution of concentration, then mixes prepared solution according to certain volume ratio.Tool
Body, the method for preparing above-mentioned acid solution includes：With the sulfuric acid solution of 1.61g/mL, 1.19g/mL perchloric acid solution and
The nitric acid solution of 1.41g/mL is raw material acid, and by raw material acids such as the sulfuric acid solutions, perchloric acid solution, nitric acid solution of above-mentioned concentration
It is by volume (1.5-15.0)：(1.0-10.0)：The ratio of (0.3-3.0) mixes, so can obtain be comprising concentration
The perchloric acid and concentration that the sulfuric acid of 0.0575~0.575g/mL, concentration are 0.0425~0.425g/mL is 0.0504~
The acid solution of the nitric acid of 0.504g/mL.Preparation method is simple as a result, and fast, required ancillary equipment is simple.Certainly, this field skill
Art personnel also can choose the raw material acid of other concentration, molten come the acid for obtaining required concentration by adjusting its volume proportion
Liquid, in this regard, the not restricted requirement of the application.
According to an embodiment of the invention, as previously mentioned, the mixed solution obtained after carbon material and acid solution are mixed need to add
Heat is to clear, just carbon material digestion solution can be obtained, i.e. guarantee carbon material is all dissolved into acid solution, in order to guarantee carbon materials
Material has preferable rate of dissolution in acid solution, according to an embodiment of the invention, mixed solution can be placed in initial temperature not
It is heated on heating device lower than 80 degrees Celsius.Thus, it is possible to rate of dissolution of the carbon material in acid solution is quickly improved,
Shorten dissolution time, and then shortening prepares the time of carbon material digestion solution, improves efficiency.Preferred embodiment in accordance with the present invention,
Initial temperature is more than or equal to 80 degrees Celsius and is less than or equal to 150 degrees Celsius, such as 80 DEG C, 100 DEG C, 120 DEG C or 150 DEG C.By
This, can quickly improve rate of dissolution of the carbon material in acid solution；If initial temperature is too low, carbon material be completely dissolved the time compared with
It is long；If initial temperature is excessively high, reacts too violent, be as a result not easily controlled, reaction solution is easy to splash and hurt sb.'s feelings, and due to carbon material and
The initial temperature of the mixed solution of acid solution differs larger close to room temperature, with the initial temperature of heating device, is unfavorable for carbon material
Powder it is evenly dispersed, or even reunite.
According to an embodiment of the invention, the heating rate heated to mixed solution is not higher than 5 DEG C/min.As a result,
Both it can guarantee that carbon material was cleared up with faster speed, efficiency is higher, and reacting will not excessively acutely as a result easily controllable, reaction
Liquid will not splash, and safety is preferable, while energy consumption is lower.
According to an embodiment of the invention, the specific type of heating device, there is no limit requiring, those skilled in the art can be with
Flexible choice according to actual needs.In an embodiment of the present invention, heating device can be electric boiling plate.Thus, it is possible to control
Electric boiling plate is slowly heated to required initial temperature by room temperature, and control electric boiling plate is also convenient for during subsequent heat
Heating rate.
According to an embodiment of the invention, for the ease of the content of multielement in subsequent detection carbon material, it can be to carbon material
Powder is dissolved completely in acid solution, that is, after being heated to clear, by solvent sample (i.e. carbon material digestion solution) from heating
It is removed on device, it is appropriate cooling, suitable high purity water is added, continues cool to room temperature, thereby, it is possible to ensure operational safety,
And high purity water and sample can be uniformly mixed, and then all be moved to solution after cooling in the volumetric flask of certain capacity, constant volume,
It shakes up and carbon material test sample is made.
In one aspect of the invention, the present invention provides a kind of methods of multiple element in detection carbon material.According to this
The embodiment of invention, referring to Fig.1, this method includes：
S100：Carbon material digestion solution is prepared using mentioned-above method, and the carbon material is cleared up using high purity water
Liquid carries out constant volume.
According to an embodiment of the invention, carbon material digestion solution herein is consistent with mentioned-above carbon material digestion solution,
This is no longer excessively repeated.According to an embodiment of the invention, it can be complete to carbon material for carrying out constant volume to the carbon material digestion solution
Fully dissolved is in acid solution, that is, after being heated to clear, solvent sample is removed from heating device, appropriate cooling, adds
Enter suitable high purity water, continue cool to room temperature, then all moves to solution after cooling in the volumetric flask of certain capacity, it is fixed
Hold.
S200：It is returned to zero according to blank sample to inductively-coupled plasma spectrometer, then utilizes inductive coupling etc.
Emission spectrometer measures the intensity value of above-mentioned each element at the corresponding optimal wavelength of each element respectively.
According to an embodiment of the invention, in order to ensure the accuracy of testing result, before the intensity value of measurement each element,
It is returned to zero according to blank sample.Wherein, need to illustrate when, blank sample refers in addition to without containing carbon material, other compositions
With carbon material digestion solution ingredient consistent and preparation step also with the consistent sample of the preparation step of carbon material digestion solution.Specifically,
With blank sample, returned to zero at the corresponding optimal wavelength of each element respectively using inductively-coupled plasma spectrometer.By
This, can be improved the accuracy of testing result.
It, can be with according to an embodiment of the invention, the specific type of the multiple element in above-mentioned carbon material is not particularly limited
The impurity element for preparing for carbon material, transporting, being introduced in process, specifically, can be for metallic element and in addition to carbon
Nonmetalloid, such as above-mentioned each element can be in aluminium, iron, manganese, copper, zinc, cobalt, potassium, sodium, calcium, magnesium, molybdenum, titanium, silicon and phosphorus
At least one.
S300：According to the above-mentioned intensity value and standard curve measured, the content of above-mentioned each element is determined.
According to an embodiment of the invention, the production method of standard curve there is no limit require, those skilled in the art according to
Actual demand selection.In an embodiment of the present invention, standard curve is obtained by following steps：Standard liquid will be mixed and acid is molten
Liquid mixing, and obtained mixed solution is subjected to gradient dilution, a series of standard solution to be measured of various concentrations is obtained, wherein
Acid solution is consistent with the acid solution for being used to prepare carbon material digestion solution；Using inductively-coupled plasma spectrometer respectively in each member
The intensity value that each element is measured at the corresponding optimal wavelength of element, respectively using the mass percentage of each element as abscissa, each member
The intensity value of element is ordinate, and drafting obtains standard curve.Standard curve making is accurate as a result, helps to improve final detection
The reliability of each element content in carbon material.In addition, being also required to carry out blank with blank sample before carrying out production standard curve
Zeroing, the precision of standard curve is improved with this.
According to an embodiment of the invention, mixing standard liquid refers to standard solution known to wherein each element content, member therein
There is no limit requirement, those skilled in the art can carry out flexible design according to the element in required detection carbon material for plain type,
For example, if the content of four kinds of metallic elements such as titanium in carbon material, aluminium, copper, nickel need to be detected, mix can be contained only in standard liquid titanium,
Four kinds of aluminium, copper, nickel elements；If need to only detect a kind of content of element (such as nickel) in carbon material, then can in mixing standard liquid
To contain only nickel element.In some embodiments of the invention, can according between each element influence each other relationship by it is several,
Ten several elements not interfered substantially mutually are mixed to get mixing standard liquid, and the relationship of influencing each other between each element can be according to this
The specification of field common knowledge and equipment, prompt etc. obtain.
According to an embodiment of the invention, when preparation standard solution to be measured, the gradient value of gradient dilution and different is carried out
Concentration value also there is no limit requiring, those skilled in the art can flexible choice according to actual needs, for example, five can be chosen
Or six or seven different concentration values, gradient magnitude those skilled in the art can be preferably linear better with flexible setting
Standard curve, and definitely the concentration range of curve is preferably able to the concentration of covering testing result.The standard curve meeting made as a result,
More precisely, test result accuracy is more preferable.
Inventors have found that above-mentioned detection method is not only simple, and it is easily operated, and detection accuracy is high, can accurately survey
Determine the content of each element in carbon material.
Embodiment
Embodiment described below follows the steps below：
The step of preparing carbon material test sample：
1) preparation of acid solution：By volume, by concentration be the sulfuric acid of 1.61g/mL, 1.19g/mL perchloric acid,
The nitric acid of 1.41g/mL is (1.5-15.0) by volume：(1.0-10.0)：(0.3-3.0) is mixed, and acid solution is obtained, and is made
To compare, any two kinds in the above-mentioned three kinds of acid of the selection of comparative example 1~3 are mixed, and mixed proportion is constant；
2) it is weighed using a ten thousandth balance and is ground into powdered carbon material sample to be measured, be placed in mortar and be ground to
Required carbon material powder；
3) it is accurately weighed using a ten thousandth balance through air dried ground sample 0.1000g-1.0000g, is put in cone
In shape bottle, pave；
4) electric boiling plate is slowly increased to 80 DEG C to 150 DEG C by room temperature；
5) the appropriate acid solution prepared is added in conical flask, carbon material powder is uniformly impregnated with；
6) by the lid upper surface ware of the conical flask for the carbon material powder being impregnated with equipped with acid solution, and start to rise in 80 DEG C
Temperature becomes clear in about 60 minutes, such as undissolved complete, is placed on and continues to boil a few minutes on electric boiling plate, obtains carbon materials
Expect digestion solution；
7) conical flask that carbon material digestion solution is filled in step 6) is removed from electric boiling plate, it is cooling, high purity water is added,
Continue cool to room temperature；
8) sample solution for obtaining step 7) moves into 100ml volumetric flask, and conical flask is cleaned, and washing lotion moves into volumetric flask
In, constant volume shakes up the test sample that carbon material is made；
The step of detecting each element content in carbon material：
9) standard curve is made：
Mixing standard liquid, (State center for standard matter buys each independent standard liquid of element to be measured, and the concentration of independent standard liquid is
1000mg/L can as needed mix several or ten several independent standard liquids of substantially non-interfering element) and acid solution mix
It closes, and obtained mixed solution is subjected to gradient dilution in 100mL volumetric flask, obtain the to be measured molten of six various concentrations
Liquid, wherein acid solution is consistent with the acid solution for being used to prepare carbon material digestion solution；
It is returned to zero according to blank sample；
Each element is measured at the corresponding optimal wavelength of each element respectively using inductively-coupled plasma spectrometer (ICP)
Intensity value, respectively using the mass percentage of each element as abscissa, the intensity value of each element is ordinate, and drafting is marked
Directrix curve.
10) divide and take the test sample solution obtained in 25.00ml step 8) in 100ml volumetric flask, obtain test fluid, it will
Test fluid is returned to zero at ICP each element optimal wavelength with blank sample, measures the intensity of each element, from working curve (or standard
Curve) on find the content of corresponding each element.
Comparative example 1
It is carried out according to above-mentioned steps, difference is：Volume is added in the conical flask added with the carbon material powder of 0.1000g
Than being 2：1 sulfuric acid and the acid solution of nitric acid.
Comparative example 2
It is carried out according to above-mentioned steps, difference is：Volume is added in the conical flask added with the carbon material powder of 0.1000g
Than being 1：1 sulfuric acid and the acid solution of perchloric acid.
Comparative example 3
It is carried out according to above-mentioned steps, difference is：Volume is added in the conical flask added with the carbon material powder of 0.1000g
Than being 1：1 perchloric acid and the acid solution of nitric acid.
Embodiment 1
It is carried out according to above-mentioned steps, difference is：Volume is added in the conical flask added with the carbon material powder of 0.1000g
Than being 5：1：1 sulfuric acid and perchloric acid and the acid solution of nitric acid.
The mixed solution of carbon material powder and acid solution concussion in comparative example 1-3 and embodiment 1 is mixed, and by conical flask
It is placed in 80 DEG C and begins to warm up heating, similarity condition processing compares final clarity (each embodiment operates five times), clarity
It is successively 1 > comparative example of embodiment, 3 > comparative example, 2 > comparative example 1, it can be seen that carbon material powder is molten in the acid that three kinds of acid-mixeds are closed
Solubility in liquid is greater than solubility of the carbon material powder in the acid solution that wherein any two kinds of acid is mixed to get, 0.1000g
Insoluble solid matter mass statistics is shown in Table 1 after carbon material powder processing.
Table 1
Embodiment 2
It is carried out according to above-mentioned steps, difference is：Sulphur is added in the conical flask added with the carbon material powder of 0.5000g
Acid, perchloric acid and nitric acid volume ratio are respectively 15：1：1 acid solution, total volume 15mL.
Embodiment 3
It is carried out according to above-mentioned steps, difference is：Sulphur is added in the conical flask added with the carbon material powder of 0.5000g
Acid, perchloric acid and nitric acid volume ratio difference 10：5：1 acid solution, total volume 15mL.
Embodiment 4
It is carried out according to above-mentioned steps, difference is：Sulphur is added in the conical flask added with the carbon material powder of 0.5000g
Acid, perchloric acid and nitric acid volume difference 5：2：1 acid solution, total volume 15mL.
Embodiment 5
It is carried out according to above-mentioned steps, difference is：Sulphur is added in the conical flask added with the carbon material powder of 0.5000g
Acid, perchloric acid and nitric acid volume ratio difference 1：1：1 acid solution, total volume 15mL.
The mixed solution of carbon material powder and acid solution concussion in embodiment 2-5 is mixed, and conical flask is placed in 120 DEG C
Begin to warm up heating；Same heating temperature processing compares treatment effect (each embodiment operates five times), in embodiment 2-5
0.5000g carbon material powder can be heated to clear, but duration used is not identical, a length of 2 > of embodiment when used
3 > embodiment of embodiment, 4 > embodiment 5, it follows that three kinds of sour volume proportions closer to when, rate of dissolution is faster.Specifically
As a result 2 be see the table below.
Table 2
Embodiment 6
It is carried out according to above-mentioned steps, difference is：Sulphur is added in the conical flask added with the carbon material powder of 0.3000g
Acid, perchloric acid and nitric acid volume ratio are 2:1:1 acid solution, and begin to warm up in 80 degree and heat up after a certain period of time.
Embodiment 7
It is carried out according to above-mentioned steps, difference is：Sulphur is added in the conical flask added with the carbon material powder of 0.3000g
Acid, perchloric acid and nitric acid volume ratio are 2:1:1 acid solution, and begin to warm up in 100 degree and heat up after a certain period of time.
Embodiment 8
It is carried out according to above-mentioned steps, difference is：Sulphur is added in the conical flask added with the carbon material powder of 0.3000g
Acid, perchloric acid and nitric acid volume ratio are 2:1:1 acid solution, and begin to warm up in 120 degree and heat up after a certain period of time.
Embodiment 9
It is carried out according to above-mentioned steps, difference is：Sulphur is added in the conical flask added with the carbon material powder of 0.3000g
Acid, perchloric acid and nitric acid volume ratio are 2:1:1 acid solution, and begin to warm up in 150 degree and heat up after a certain period of time.
The mixed solution of carbon material powder and acid solution concussion in embodiment 6-9 is mixed, and conical flask is set into above-mentioned side
Heat temperature raising at a temperature of in case, equally comparison treatment effect, although the scheme of aforementioned four embodiment is by 0.3000g carbon materials
Feed powder end is heated to clear, but the time used is not identical, a length of 6 > embodiment of embodiment, 7 > embodiment 8 when used
> embodiment 9, it follows that the initial temperature that mixed solution is heated is higher, carbon material powder is completely dissolved institute's used time
Length is shorter.Concrete outcome see the table below 3.
Table 3
Embodiment 10
The volume ratio of sulfuric acid, perchloric acid and nitric acid is 2 in acid solution:1:1；(, 80 DEG C of initial heating temperature；Carbon materials
Expect to handle under the conditions of powder quality is 0.1000-1.0000g with batch carbon material powder, detect multiple element content therein,
Analysis data see the table below 4 (units:mg/Kg).
Table 4
Note：First average value, the first standard deviation and the first relative deviation are flat to the 5th testing result for the first time
Mean value, standard deviation and relative deviation；Second average value, the second standard deviation and the second relative deviation are the 6th time to the tenth time
Average value, standard deviation and the relative deviation of testing result；Twice average value, standard twice deviation, relative deviation is twice
Once to average value, standard deviation and the relative deviation of the tenth testing result.
In the description of this specification, reference term " one embodiment ", " some embodiments ", " example ", " specifically show
The description of example " or " some examples " etc. means specific features, structure, material or spy described in conjunction with this embodiment or example
Point is included at least one embodiment or example of the invention.In the present specification, schematic expression of the above terms are not
It must be directed to identical embodiment or example.Moreover, particular features, structures, materials, or characteristics described can be in office
It can be combined in any suitable manner in one or more embodiment or examples.In addition, without conflicting with each other, the skill of this field
Art personnel can tie the feature of different embodiments or examples described in this specification and different embodiments or examples
It closes and combines.
Although the embodiments of the present invention has been shown and described above, it is to be understood that above-described embodiment is example
Property, it is not considered as limiting the invention, those skilled in the art within the scope of the invention can be to above-mentioned
Embodiment is changed, modifies, replacement and variant.
Claims (10)
1. a kind of digestion procedure of carbon material, which is characterized in that including：
Carbon material and acid solution are mixed, and obtained mixed solution is heated to clear, obtains carbon material digestion solution,
Wherein, the acid solution contains sulfuric acid, perchloric acid and nitric acid.
2. the method according to claim 1, wherein the carbon material includes graphene, carbon nanotube, petroleum coke
At least one of with carbon block.
3. the method according to claim 1, wherein before the carbon material and the acid solution are mixed,
Further include the steps that for the carbon material being ground in powder morphology.
4. the method according to claim 1, wherein in the acid solution, the concentration of sulfuric acid is 0.0575~
0.575g/mL, the concentration of perchloric acid is 0.0425~0.425g/mL and the concentration of nitric acid is 0.0504~0.504g/mL.
5. being taken the photograph the method according to claim 1, wherein the mixed solution is placed in initial temperature not less than 80
It is heated on the heating device of family name's degree.
6. according to the method described in claim 5, it is characterized in that, the initial temperature be more than or equal to 80 degrees Celsius and be less than etc.
In 150 degrees Celsius.
7. the method according to claim 1, wherein the heating rate heated to the mixed solution is less than
Equal to 5 DEG C/min.
8. a kind of method of multiple element in detection carbon material, which is characterized in that including：
Carbon material digestion solution is prepared using the method for any of claims 1-7, and using high purity water to the carbon materials
Expect that digestion solution carries out constant volume；
It is returned to zero according to blank sample to inductively-coupled plasma spectrometer, then utilizes the inductively coupled plasma body
Spectrometer measures the intensity value of above-mentioned each element at the corresponding optimal wavelength of each element respectively；
According to the above-mentioned intensity value and standard curve measured, the content of above-mentioned each element is determined.
9. according to the method described in claim 8, it is characterized in that, each element be selected from aluminium, iron, manganese, copper, zinc, cobalt, potassium,
At least one of sodium, calcium, magnesium, molybdenum, titanium, silicon and phosphorus.
10. method according to claim 8 or claim 9, which is characterized in that the standard curve is obtained by following steps：
Standard liquid will be mixed and acid solution mixes, and obtained mixed solution is subjected to gradient dilution, it is dense to obtain a series of differences
The standard of degree solution to be measured, wherein the acid solution is consistent with the acid solution for being used to prepare carbon material digestion solution；
The each element is measured at the corresponding optimal wavelength of each element respectively using inductively-coupled plasma spectrometer
Intensity value, respectively using the mass percentage of each element as abscissa, the intensity value of each element is ordinate, is drawn
Standard curve is made.
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