Sequential injection system with inline solid phase extraction

Department of Chemistry, Faculty of Science and Technology, Thammasat University

Sequential injection system with in-line solid phase extraction
and soil minicolumn for determination of zinc and copper
in soil leachates
Justyna Paluch, Raquel B.R. Mesquita, Víctor Cerdà, Joanna Kozaka, Marcin Wieczorek, Antóni O.S.S. Rangel

Presented by

Thuan Hoa Nguyen


I ntroduction


Introduction
industrial, urban, agricultural,
gardening, forestry

The effective
of waters
affected
leachates
zinc monitoring
Levels of Copper
and
Zine upby
to soil
1.5 and
5 mg/liter

copper of the potential sources of pollution
 Identification
can be tolerated
without
risk body
to health
CD solution
Healthy

 The liver

 toxic to the cytologic and physiologic

 The kidneys
 The nervous system
 The immune system
3


Introduction

Determination of copper and zinc

Method
1

Flow injection flame atomic absorption
(AAS)

2

Inductively coupled plasma optical
emission (ICP-OES)

3
4

Disadvantage

• Expensive
• Cumbrous

CD solution
Mass spectrometry (ICP-MS)
Neutron activation analysis (NAA)

4


Introduction

objective

To develop sequential injection system with in-line solid
phase extraction and soil minicolumn for determination of
zinc and copperCDin
soil leachates
solution

5

Introduction

Reaction

1-(2-Pyridylazo)-2-naphthol (PAN)

CD solution

Absorbance maximum
at 482 nm

Form complex with di
valence metals

Absorbance maximum
at 560nm

The metal ions (Cu2+, Zn2+) form complex PAN reagent due to the similar binding ability
towards these metal ions.
6


Experiment
7


Experiment

SIA - SPE method for copper and zinc determination

a) Off-line laboratory scale soil core (LSSC)
b) In-line soil mini-column (ILSM)

CD solution

8


Experiment
laboratory scale soil core
The LSSC columns
50

m

L

consisting in acrylic cylinders
(h = 20 cm, d = 8 cm)

CD
solution
Two
types of soil were used:
 Forest soil in Northwest Portugal


Agricultural soil in Northwest Portugal

acidified to pH ≈ 2 before determination
9


Experiment
The In-Line Soil Mini-columns (ILSM)
(h = 3 cm, d = 2 cm)
with surface soil with about 3 g

CD
solution
Two
types of soil were used:
 Forest soil in Northwest Portugal


Agricultural soil in Northwest Portugal

acidified to pH ≈ 2 before determination

10


Experiment

SIA - SPE method for copper and zinc determination

a) Off-line laboratory scale soil core (LSSC)
b) In-line soil mini-column (ILSM)

CD solution

11


SIA - SPE method for copper and zinc determination

Off-line laboratory scale soil core (LSSC)

( Zn2+)
PAN Reagent

Buffer

Waste

CD solution

Detector

Experiment

Standard
mRC

12


Experiment

SIA - SPE method for copper and zinc determination

Off-line laboratory scale soil core (LSSC)

( Zn2+)
PAN Reagent

Buffer

Waste

The Chelex 100 chelating resin

Detector

CD solution

Standard
mRC

13


SIA - SPE method for copper and zinc determination

Off-line laboratory scale soil core (LSSC)

( Zn2+ & Cu2+)
PAN Reagent

Buffer

Waste

CD solution

Detector

Experiment

Standard
mRC

14


RESULTS

and

DISCUSSION

15


RESULTS AND DISCUSSION
Bi parametric determination of zinc and copper
Concentration values
for Zn2+

for Cu2+

Calibration curves
CD solution

for Cu2+

Calibration curves
for Zn2+
for the sum of Zn2+ + Cu2+

16


RESULTS AND DISCUSSION
 Colorimetric reaction
 Sample volume

354 µL - 530 µL  413 µL

 Reagent solution

118, 177, 236 and 295 µL  236 µL

 Optical path length

5 cm

236 µL

413 µL

CD solution

○ Influence of the sample
◊ reagent

17


RESULTS AND DISCUSSION
Analytical parameters of the SI-SPE method for Zn2+ + Cu2+ determination.

CD solution

E
P
S
I
S

I
F
N
O
C

D
E
RM

SI

s
E
-SP
18


RESULTS AND DISCUSSION
Interference assessment
% interference =

absorbance for analyte (interfering ion) – absorbance for analyte
x 100
absorbance for analyte

The developed SI-SPE method can be used for determination
CD solution

of zinc and copper in rain water and soil leachate samples with
No significant interferences.

19


RESULTS AND DISCUSSION
Accuracy assessment

CD solution

 Both analytes can be determined with satisfactory accuracy.

20