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Analysis method for measuring manganese, silicon and potassium in graphene oxide

An analysis method, the technology of manganese in ene, is applied in the field of quantitative analysis of impurity elements in graphene oxide, and achieves the effects of fast measurement, wide application range and easy promotion

Active Publication Date: 2018-09-11
AVIC BEIJING INST OF AERONAUTICAL MATERIALS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there is no report on the quantitative analysis of element content in graphene oxide by using inductively coupled plasma emission spectrometry at home and abroad.

Method used

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  • Analysis method for measuring manganese, silicon and potassium in graphene oxide
  • Analysis method for measuring manganese, silicon and potassium in graphene oxide
  • Analysis method for measuring manganese, silicon and potassium in graphene oxide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0084] Graphene oxide prepared by the Hummers method is used as a sample to measure manganese, silicon and potassium content in graphene oxide, and an inductively coupled plasma spectrometer is used. The working conditions and analysis lines of the instrument are as follows: analysis lines: Mn 257.610nm, Si251.611nm, K 766.468nm;

[0085] 2. Table 1 Instrument working conditions

[0086] project

parameters

project

parameters

High frequency, MHz

40.68

Incident power, kW

0.9

Entrance slit, μm

20

Sheath gas flow, L / min

0.2

Auxiliary air flow L / min

0.3

Sample lifting volume, mL / min

1.2

Integration time, s

2

Integral method

one point

Reflected power, W

＜10

-

-

[0087] (1), the reagents used in the determination process are as follows:

[0088] (1.1), hydrochloric acid: ρ1.19g / mL, prepared by high-purity or sub-boiling distillation;

[0089] (1.2), nitric acid...

Embodiment 2

[0140] Graphene oxide prepared by the Hummers method was used as a sample to measure the contents of manganese, silicon and potassium in the graphene oxide. The working conditions of the instrument and the analysis line were as in Example 1.

[0141] (1), the reagent used in the assay process is consistent with Example 1;

[0142] (2), sampling and sample preparation are consistent with embodiment 1;

[0143] (3), sample dissolution test is consistent with embodiment 1;

[0144] (4), coexistence element interference test is consistent with embodiment 1;

[0145] (5), working curve linearity test

[0146] Pipette 8.00mg of Mn, 0.50mg of Si, and 0.20mg of K into a 100mL volumetric flask, add 10mL of hydrochloric acid and 5 drops of hydrofluoric acid, dilute to the mark with water, and shake well. This mixed standard solution contains 8.00% Mn, 0.50% Si, 0.20% K, which is the highest point in the standard curve.

[0147] Pipette 6.00mg of Mn, 0.30mg of Si, and 0.10mg of K int...

Embodiment 3

[0165] Graphene oxide prepared by the Hummers method was used as a sample to measure the contents of manganese, silicon and potassium in the graphene oxide. The working conditions of the instrument and the analysis line were as in Example 1.

[0166] (1), the reagent used in the assay process is consistent with Example 1;

[0167] (2), sampling and sample preparation are consistent with embodiment 1;

[0168] (3), sample dissolution test is consistent with embodiment 1;

[0169] (4), coexistence element interference test is consistent with embodiment 1;

[0170] (5), working curve linearity test

[0171] Pipette 8.00mg of Mn, 0.50mg of Si, and 0.20mg of K into a 100mL volumetric flask, add 10mL of hydrochloric acid and 5 drops of hydrofluoric acid, dilute to the mark with water, and shake well. This mixed standard solution contains 8.00% Mn, 0.50% Si, 0.20% K, which is the highest point in the standard curve.

[0172] Pipette 6.00mg of Mn, 0.30mg of Si, and 0.10mg of K int...

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Abstract

The invention belongs to the field of technologies for quantitatively analyzing impurity elements of graphene oxide, and relates to an analysis method for measuring manganese, silicon and potassium ingraphene oxide. According to the analysis method, a sample is heated in an electric furnace in a stepped temperature rising mode; then the sample is burned in a muffle furnace, and finally the oxidesare dissolved by an acid. An inductive coupling plasma spectrometer is adopted for measurement. Through a dissolution condition test, a coexist element interference test, and a work curve linear test, an optimal analysis line is determined, the measurement accuracy is improved; the measurement range is wide, the detection range of manganese is 0.10% to 10.0%, the detection range of silicon is 0.05% to 1.00%, and the detection range of potassium is 0.01% to 0.20%. The analysis method has the advantages of good repeatability, high recovery rate, and high precision. By analyzing a standard sample and analysis results of different instruments, the provided analysis method has the advantages of high accuracy and stability, and totally meets the requirements of trace element analysis. The measurement method is direct and rapid, the operation is simple and convenient, and a large amount of labor and materials is saved.

Description

technical field [0001] The invention belongs to the quantitative analysis technology of graphene oxide impurity elements, and relates to an analysis method for determining manganese, silicon and potassium elements in graphene oxide. Background technique [0002] Graphene, a one-atom-thick two-dimensional layer of carbon atoms, is considered the building block from which other allotropes of carbon are built. Compared with graphene, the presence of a large number of oxygen-containing functional groups in graphene oxide makes it have excellent hydrophilicity and high chemical coordination, and is easy to combine with other materials to form new nanocomposites. Manganese, silicon and potassium elements exist in graphene oxide as impurity elements, and their presence will cause graphene oxide to reunite, lose its unique two-dimensional structure, seriously affect product quality, and bring huge hidden dangers to material applications. Therefore, the establishment of an accurate ...

Claims

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Application Information

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IPC IPC(8): G01N21/73G01N1/44G01N1/28G01N1/34
CPCG01N1/28G01N1/34G01N1/44G01N21/73
Inventor 汪磊耿晓颖杨春晟蒙益林高帅
Owner AVIC BEIJING INST OF AERONAUTICAL MATERIALS
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