Determination of phosphorus, silicon, iron, manganese and lead in gasoline by direct injection method

Probe orientation needle 265*2980 needle head diameter is 6.0 end probe needle
Test - lowercase jpg
Kaixin micro test


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

element

phosphorus(

P

)

silicon(

Si

)

iron(

Fe

)

manganese(

Mn

)

lead(

Pb

)

Working curve fitting coefficient

0.9998

0.9999

0.9999

0.9999

0.9999

Method detection limit

/

(

Mg/L

)

0.079

0.014

0.004

0.001

0.066

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

element

measured value

/

(

Mg/L

)

RSD/%

phosphorus(

P

)

0.949

3.63

silicon(

Si

)

0.929

1.99

iron(

Fe

)

0.904

0.77

manganese(

Mn

)

0.933

1.68

lead(

Pb

)

0.941

1.97

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

element

Scaling amount

measured value

/

(

Mg/L

)

Recovery rate

/%

phosphorus(

P

)

0.93

0.949

102.0

silicon(

Si

)

0.93

0.929

99.9

iron(

Fe

)

0.93

0.904

97.2

manganese(

Mn

)

0.93

0.933

100.3

lead(

Pb

)

0.93

0.941

101.2

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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