Analysis of Element Content in Petroleum Coke by X-ray Fluorescence Spectroscopy

X Analysis of element content in petroleum coke by X-ray fluorescence spectroscopy

pick want Based on:《The analysis requirements for elements in raw petroleum coke and calcined petroleum coke specified in SH/T 0934-2016 Determination of Trace Metal Elements in Petroleum Coke by Wavelength Dispersive X-ray Fluorescence Spectroscopy; And the analysis requirements for relevant elements in petroleum coke, calcined petroleum coke, and pre baked anodes specified in "YS/T 63.16-2019 Methods for Testing Carbon Materials for Aluminum - Part 16 Determination of Trace Elements - X-ray Fluorescence Spectroscopy Analysis Method" shall be usedskyrayX-ray fluorescence spectrometerEDX6000CEstablish working conditions and analyze petroleum cokeThe content of Fe, Ca, Si, Na, Ni, V, and S elements. The experimental results indicate that the analysis results are superior to the standard requirements. This method is easy to operate, has fast analysis speed, does not require chemical pretreatment, and is environmentally friendly.

close key word ：X-ray fluorescence spectrometerEDX6000C petroleum coke

skill technique special point ：

EDX6000CSimultaneous and rapid analysis of all elements in petroleum coke, with better repeatability than standard requirements. The method is easy to operate, has fast analysis speed, high accuracy, does not require chemical pretreatment, and is environmentally friendly.

petroleum coke Petroleum coke is a product obtained by distilling crude oil to separate light and heavy oil, and then converting heavy oil through thermal cracking. From the appearance, petroleum coke is a black block (or particle) with irregular shape and varying sizes, with a metallic luster. The particles of coke have a porous structure, and the main element composition is carbon, accounting for more than 80%, with hydrogen content of 1.5% -8%, and the rest being oxygen, nitrogen, sulfur, and metal elements.

Petroleum coke has its physical, chemical, and mechanical properties. Non volatile carbon, volatile compounds, and mineral impuritiesThe chemical properties of coke are determined by factors such as sulfur, metal compounds, water, and ash. The porosity and density in physical properties determine the reactivity and thermophysical properties of coke. The particle composition, processing method, hardness, wear resistance, strength, and other mechanical properties determine its mechanical properties.

Petroleum coke can be used for graphite production, smelting, and chemical engineering depending on its qualityIndustry.

A、Low sulfur, high-quality mature coke is mainly used to manufacture ultra-high power graphite electrodes and certain special carbon products; It is an important material for developing new technologies in electric furnace steelmaking in the steelmaking industry.

B、Medium sulfur, ordinary coke, widely used for aluminum smelting.

C、High sulfur, ordinary coke is used in chemical production, such as manufacturing calcium carbide and carbon Silicon is also used as fuel for metal casting and other applications.

Traditional chemical methods are gradually being adoptedReplaced by X-ray fluorescence spectroscopy. XRThe F-analysis method has the advantages of a wide range of measurable elements and concentrations, as well as being fast, accurate, easy to operate, and environmentally friendly. It has been widely used for analysis and detection in multiple industries. This method uses the tablet method for sample preparation and is analyzed using an X-ray fluorescence spectrometerEDX6000CAnalyze after establishing the element working curve.

1Experimental Section

1.1 Instruments and reagents

X-ray fluorescence spectrometer:EDX6000C

Vibration grinder ： ZHM-1B 型

Prototype press machine ： ZHY-601A type

1.2 Analysis conditions

The analysis conditions for elemental determination are shown in the table1.

1.3. Sample pre-treatment

Place the sample inDry at 110 ± 5 ° C for 2 hours and cool to room temperature. Weigh 12.0000 g of sample and 2.0000 g of stearic acid and mix well. Grind in a tungsten carbide mortar for 20 seconds. When clumping, crush with a spoon. Take about 5g of sample and press it into tablets for analysis.

image2 compression samples

2Results and Discussion

2.1 Standard Samples

This method uses petroleum reference materials from the Institute of Petroleum Science and Technology to create a working curve according to the set analysis conditions.

tableConcentration results of 2 petroleum coke standard samples (μ g/g)

2. 2 Working Curve

According to the conditions of this method, the working curve is established with good linearity, wide linear range of elemental analysis, and wide applicability. Element curve as shown in the figure3.

3.3 Repetitive testing

Select petroleum coke standard sample5COKE1 was used as a validation sample and dynamically tested twice according to the standard requirements. The absolute difference between the two results was calculated and found to be within the allowable range specified in the standard.

table3 Petroleum Coke Standard Samples 5COKEAccuracy test results of method 1 (μ g)/g)

Explanation: Refer to《《YS/T 63.16-2019 Testing methods for carbon materials used in aluminumPart 16Determination of Trace ElementsX Repeat the method of X-ray fluorescence spectroscopy analysissex rThe absolute difference between two results.

3.4 Accuracy Test

Select actual production petroleum coke samples as validation samples and conduct dynamic testingTake the average value twice, and the absolute difference between the two results is within the allowable range specified by the standard. The average value is close to the chemical analysis results.

Conclusion

Based on《SH/T0934-2016 Determination of Trace Metal Elements in Petroleum Coke by Wavelength Dispersive X-ray Fluorescence Spectroscopy "and" YS/T63.16-2019 Determination of Trace Elements in Carbon Materials for Aluminum Part 16 X-ray Fluorescence Spectroscopy Analysis Method "stipulate thatskyrayX-ray fluorescence spectrometerEDX6000CEstablished working conditions and analyzed petroleum coke The content of Fe, Ca, Si, Na, Ni, V, and S elements. The experimental results show that this method has good linearity of the working curve, fast analysis speed, high accuracy, good stability, no need for chemical pretreatment, and no chemical pollution.