Determination of heavy metals in soil by ICP-2060T

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ICP-2060T

Determination of heavy metals in soil


Abstract: The sample is digested by heating acid to

ICP-2060T

Determination of copper, zinc, nickel, lead, cadmium, chromium. The method is applied to the determination of copper, zinc, nickel, lead, cadmium, chromium and arsenic in soil samples, and the pretreatment process is simple, the equipment is simple, and the cost is low. The experimental results show that when the method is applied to the determination of heavy metals in soil, the determination results are accurate and reliable, and the repeatability is good.

1

Foreword

As the main carrier of agricultural production and an important part of the ecological environment, soil quality is closely related to people's life. With the development of the economy, a large amount of untreated waste containing heavy metals is discharged into the environment, making The farmland soil environment and crops have been polluted and destroyed to varying degrees, which in turn endangers human health and even life through the food chain. Therefore, the problem of heavy metal pollution in soil has become an increasingly serious ecological problem. Analytical determination of heavy metals in soil, before sample

Processing is the key. In this paper, the hot plate heating method is used for pretreatment of soil samples.

ICP-AES

The content of copper, zinc, nickel, lead, cadmium and chromium is determined, the method is simple, safe, low cost, and the test result has high accuracy and precision.

2

Experimental part

2.1

Main instruments and reagents

2.1.1

instrument

ICP-2060T

Inductively coupled plasma atomic emission spectrometer, Jiangsu Tianrui Instrument Co., Ltd.;

BS224S

Electronic balance, Sartorius Scientific Instruments (Beijing) Co., Ltd.;

EPED-40T

Laboratory-grade ultra-pure water machine, Nanjing Yipu Yida Technology Development Co., Ltd.;

EG35A

Type electronic temperature control heating plate, Beijing Laibo Tyco Instrument Co., Ltd.; pipetting gun (

10-100uL

,

100-1000uL

) Two, Prand, Germany.

The polytetrafluoroethylene beaker and the plastic volumetric flask used are all made of nitric acid (

1+1

Soak overnight, rinse directly with ultrapure water before use, and dry naturally before use.

2.1.2

Reagent

The experimental water is ultrapure water; the experimental acid is excellent grade pure acid: hydrochloric acid, nitric acid, hydrofluoric acid, perchloric acid

Soil standards are provided by the State Environmental Protection Administration Standards Institute

Standard material: standard solution of copper, zinc, nickel, lead, cadmium, chromium (

1000mg/L

) provided by the National Nonferrous Metals Analysis and Testing Center.

2.2

experimental method

2.2.1

Preparation of sample test solution

Accurate weighing

0.2

-

0.3g

(accurate to

0.0001g

Sample

50mL

In a Teflon beaker, wet with water and then add

10mL

Hydrochloric acid, heated at a low temperature on a hot plate in a fume hood, causing the sample to be initially decomposed and to be evaporated to about

3 mL

When you take it, take a little cold and then join

5 mL

Nitric acid,

5 mL

Hydrofluoric acid,

3 mL

Perchloric acid, after heating, heating on a hot plate at medium temperature

1

After about an hour, then open the lid and continue to heat the silicon. In order to achieve a good flying silicon effect, the beaker should be shaken frequently. When heated to a thick white smoke of perchloric acid, it is capped to decompose the black organic carbide. After the black organic matter on the inner wall of the beaker disappears, the lid is opened, the white smoke is driven away, and the contents are viscous, and the content can be supplemented depending on the digestion.

3 mL

Nitric acid,

3 mL

Hydrofluoric acid,

1 mL

Perchloric acid, repeat the above digestion process. When the white smoke is exhausted again and the contents are viscous, remove the cooling, rinse the inner wall and lid with water, and add

1 mL

(

1+1

The nitric acid solution warms the residue. Then transfer the whole amount to

50 mL

In the volumetric flask, after cooling, make up to the line and shake it for testing. At least one parallel sample is guaranteed for each sample, and a blank solution is prepared by using water as a sample, and at least one sample is prepared in each batch.

2

More than one blank solution.

2.2.2

Calibration curve

Accurate preparation

0

,

0.2

,

0.5

,

1.0

,

2.0

,

3.0mg/L

Standard solution of copper, zinc, nickel, lead, cadmium, chromium, stable in the instrument

30min

The standard solution is measured and the calibration curve is drawn.

2.2.3

Sample determination

According to the table

1

Set instrument parameters:

table

1 ICP-AES working conditions

element

Cu Zn Ni Pb Cr Cd

Repeat test times

/

Times

3 3 3 3 3 3

Integration time

/s 3 3 3 3 3 3

Integration method

Gaussian curve

Gaussian curve

Gaussian curve

Gaussian curve

Gaussian curve

Gaussian curve

Analysis wavelength

/nm 324.752 213.857 231.604 220.353 267.716 228.802

power

/w 1000 1000 1000 1000 1000 1000

Plasma gas flow

L/h 650 650 650 650 650 650

Carrier gas flow

L/h 20 20 20 20 20 20

Injection volume

Ml/min 1.5 1.5 1.5 1.5 1.5 1.5

use

ICP-2060T

The emission intensity of the element in the sample is measured, and the element concentration is calculated by a calibration curve.

3

Results and discussion

3.1

Sample weight affects test results

Figure

1

For the same soil sample, the relationship between different weighing weight and test results, as can be seen from the figure, when the sample weight is greater than

0.2g

When the test results are stable. In order to reduce the influence of the matrix effect while ensuring the accuracy and precision of the method, the weighing weight of the method sample is

0.25g

about.

Figure

1 Total sample and test results


3.2

Method detection limit and linear range

The linear range, method sensitivity, instrument detection limit and method detection limit of each heavy metal element working curve were determined through several experiments.

By table

2

It can be seen that the fitting coefficients of the working curves of the heavy metal elements are 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, see table

1

To maximize the sensitivity of element excitation. The detection limit of the instrument and the detection limit of the method are all low, further indicating that the experimental conditions of the method are reliable (Table

2

).

table

2

ICP-2060T

Determination of linearity, sensitivity, and detection limit of heavy metals in soil

element

Cu Zn Ni Pb Cr Cd

Linear range

/ug/mL 0

-

3 0

-

3 0

-

3 0

-

3 0

-

3 0

-

3

Instrument detection limit

/ug/mL 0.0029 0.0193 0.0073 0.0218 0.0031 0.0116

Method detection limit

/ug/mL 0.0031 0.0265 0.0085 0.0299 0.5706 0.0233

Working curve fitting coefficient

0.9997 0.9997 0.9998 0.9995 0.9997 0.9996
3.3

Precision and accuracy of the method

Parallel treatment of soil reference materials

6

Parts, determine the content of heavy metals, and calculate the relative standard deviation of the results (

RSD%

) to evaluate the precision of the method.


table

3

ICP-2060T

Determination of the results of the determination of the standard by the heavy metal method of soil (

n=6

)

element

standard value

/mg/kg

measured value

Mg/kg RSD%

Recovery rate

Cu 21 20.1 2.5 95.7 Zn 680 689.2 2.2 101.4 Ni 20.4 19.2 1.7 94.1 Pb 98 102.3 2.0 104.4 Cr 62 59.3 2.8 95.6 Cd 4.3 4.6 4.2 106.9

By table

3

It can be seen that the method is used to determine soil samples.

6

The recovery rate of heavy metals is in the range of

94.1

-

106.9

Relative standard deviation

RSD%

) are smaller than

5%

It shows that the precision of the method is high, the measurement result is stable, and the experimental conditions in the analysis process are easily controlled.

4

in conclusion

The experimental results show that the method can be used in soil samples when the composition of the soil sample matrix is ​​complex.

6

The heavy metal elements are simultaneously digested, and the effect is ideal.

Optimized by the ideal pre-processing method and instrument state

ICP-AES

When measuring the content of copper, zinc, nickel, lead, cadmium and chromium in soil samples, it has high sensitivity, precision and accuracy. The determination results are accurate and reliable. The experimental conditions in the analysis process are easy to control and can meet the soil analysis. Claim.

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