Instrument introduction
The remarkable features of Petrochemical oil analysis of Tianrui Instrument ICP2060T inductively coupled plasma emission spectrometer:
1.
The semiconductor refrigeration sample introduction device improves the stability and sensitivity of the injection, and the test is more accurate and reliable.
2.
The special torch for gasoline ensures long-term stability of the plasma and reduces the background of the substrate.
3.
Increase oxygen assisted injection to maintain plasma stability and prevent carbon deposits.
4.
Self-developed RF solid-state RF generator automatic matching method, suitable for samples such as organic and high matrix
Take in the sample.
5.
The height of the plasma observation is automatically adjusted to accurately locate the best observation position.
6.
Very high resolution, can accurately separate P213.618nm, Cu213.598nm and P214.911nm,
Experimental part
1.1
Instruments and reagents
Tianrui Instrument
ICP2060T
Inductively coupled plasma emission spectrometer
CONOSTANS-21
Mixed standard oil
, 300 ppm
,
100g
CONOSTAN Co
Standard solution,
5000ppm
,
50g
CONOSTANICP
Special thinner, one gallon.
Pipette,
0-5ml
Prand, Germany
One ten thousandth electronic balance,
BS224S
Sartorius
1.2
Instrument working conditions
High frequency generator:
27.12MHz
, the center channel is
0.6mm
Quartz torch, high frequency power
1100W
, the reflection power is about
50W
Plasma gas flow
15L/min
Auxiliary gas flow
1.0L/min
Carrier gas flow
0.4L/min
Oxygen flow rate
30ml/min
, spray chamber temperature
-10
°C, peristaltic pump speed
3ml/min
, phosphorus analysis line
213.620nm
, silicon analysis line
251.611nm
, iron analysis line
538.204nm
, manganese analysis line
257.610nm
Lead analysis line
220.353nm
Cobalt analysis line
228.616nm
.
1.3
experiment method
After the instrument is automatically ignited and the parameters are set according to the working conditions of the instrument, the diluent directly enters the mist chamber through the atomizer and enters the plasma. After the instrument is stabilized, the blank solution, the standard solution and the diluted sample solution are measured once, and the instrument is based on the working curve. The content of each element in the final sample can be directly derived.
2.
Results and discussion
2.1
Optimal analysis line selection
in
ICP
Many molecular bands appear in the spectrum due to the spectrum
,
Produced a very deep spectral background
,
Therefore, the influence of metal element analysis is affected. The three most commonly used analytical lines of silicon are selected. After the test, the sensitivity of the line is comprehensively considered, the background of the spectrum and the interference are observed, and the analysis line of phosphorus is selected.
213.620nm
, silicon analysis line
251.611nm
, iron analysis line
538.204nm
, manganese analysis line
257.610nm
Lead analysis line
220.353nm
. The detection limit and linear range of the calculation method are shown in the table.
1
The linear relationship of the elements was determined experimentally, and the blank solution of each element was
10
Repeated determination
,
Measured value
3
The standard deviation of the multiple is divided by the slope of the curve as the method detection limit. By table
1
It can be seen that the fitting coefficient of the element working curve is higher than
0.999
, indicating that the linear relationship is good in the linear range of the working curve. Since the operating parameters of the instrument are optimized, the test conditions of the elements are optimized to improve the accuracy of the test results.
table
1ICP
Determination of linearity and detection limit of elements in gasoline samples
2.3
Sample analysis according to test method for determination of gasoline standard samples
10
Times
,
Calculate the results of repeated data determination
2
table
2
Gasoline sample analysis results
2.4
Recovery experiment
The organic standard is added to the gasoline sample and the standard recovery test is carried out according to the test method.
,
See the table
3
table
3
It can be seen that the recovery of phosphorus, silicon, iron, manganese and lead in gasoline by the method is good, indicating that the method has high accuracy and the test result is stable.
3.
in conclusion
use
ICP-AES
The direct determination of the multi-element relative digestion method in gasoline has higher accuracy and better reproducibility, and the test speed is fast, which greatly improves the work efficiency, and also saves a lot of manpower and material cost, and at the same time relative to the import.
ICP
For higher configuration and cost, Tianrui Instrument
ICP2060T
With low cost, high speed and high accuracy, it can directly measure phosphorus, silicon, iron, manganese and lead in gasoline samples, which can fully meet the testing requirements of customers in the petrochemical industry.
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