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A Novel Detection Technique of Hydrazine Hydrate: Modality Change of Hydrogen-Bonding Induced Rapid and Ultrasensitive Colorimetric Assay
Zhenlu Zhao,a Kelong Ai,b Guo Zhang,b Ying Gao,a Xiuyun Yang,* a and Yunhui Li* a
Supporting information
aSchool of Chemical & Enviromental Engineering, Changchun University of Science and Technology, Changchun,
130022, P. R. China.
bState Key Laboratory of Electroanalytical Chemistry, Changchun Institute of Applied Chemistry, Chinese
Academy of Science, Changchun, 130022, P. R. China.
E-mail: liyh@cust.edu.cn; yangxiuyun@cust.edu.cn
Electronic Supplementary Material (ESI) for Chemical CommunicationsThis journal is © The Royal Society of Chemistry 2011
Experimental Section
Chemicals:
Hydrogen tetrachloroaurate (III) trihydrate was purchased from Alfa Aesar. 2,6-pyridinedicarboxylic acid (PDCA)
was obtained from Aldrich. Sodium citrate tribasic dihydrate was purchased from Sigma. All aqueous solutions
were prepared with ultrapure water from a Milli-Q Plus system (Millipore). Hydrazine hydrate was obtained
commercially from the Beijing Chemical Reagent Plant (Beijing, China). All other chemicals are of analytical
grade and used without further purification unless noted.
Preparation of Au nanoparticles
Au nanoparticles (Au NPs) were synthesized by the reduction of HAuCl4 by sodium citrate. Briefly, 50 ml of 1
mM HAuCl4 was heated to reflux with stirring, and then 5 ml of 38.8 mM sodium citrate was rapidly added. The
solution was kept continually boiling for another 30 min to give a wine red solution. The final concentration of Au
NPs was determined to be 10 nM, and the average diameter is 12 nm.
Design of Au nanoparticles-based colorimetric sensing system (ANCSS) and detection of hydrazine hydrate
Firstly, 0.1 M PDCA was prepared by dissolving PDCA in 0.2 M NaOH aqueous solution. Then, 0.1 M PDCA
was adding to as-prepared Au NPs solution with different volume ratios (VAu/VPDCA = 300:x) under stirring.
Finally, the ANCSS was obtained by adjusting pH value of the mixture to 7 using 0.2 M NaOH solution.
Aliquots of the Au NPs solution (300 μl) was added with various concentration solutions of hydrazine hydrate (6
μl), which were obtained by using serial dilution of the stock solution (0.1 M). After the addition of hydrazine
hydrate with different concentration, the response of the ANCSS stimulated by hydrazine hydrate was monitored
by UV-vis spectroscopy within 30 seconds at room temperature.
Characterization:
Transmission electron microscopy (TEM) images were obtained on a JEOL 2010 transmission electron
microscopy operated at an accelerating voltage of 200 kV. UV–vis spectra were recorded on a Cary 50
UV–vis–NIR spectrophotometer (Varian, U.S.A.) Photographs for color changes were taken with a PENTAX
*ISTD digital camera.
Electronic Supplementary Material (ESI) for Chemical CommunicationsThis journal is © The Royal Society of Chemistry 2011
Fingure S1. TEM images of Au NPs (a) and as–modified Au NPs (b) at pH=7.0.
a b
Electronic Supplementary Material (ESI) for Chemical CommunicationsThis journal is © The Royal Society of Chemistry 2011
Fingure S2. UV-vis absorption spectra of the Au NPs, as–modified Au NPs, and as–modified Au NPs after one
week. Inset: the corresponding visual colour of three samples (from left to right: Au NPs, as-modified Au NPs,
as-modified Au NPs after one week).
400 450 500 550 600 650 700 750 800-0.1
0.0
0.1
0.2
0.3
0.4
0.5
0.6
0.7
0.8
Au NPs as-modified Au NPs as-modified Au NPs one week later
Ab
so
rba
nce
Wavelength / nm
Electronic Supplementary Material (ESI) for Chemical CommunicationsThis journal is © The Royal Society of Chemistry 2011
Fingure S3. (a) The response of the ANCSS stimulated by hydrazine hydrate (10 μΜ) at various pH values. (b)
The response of the ANCSS with different ratios of Au and PDCA (VAu/VPDCA) stimulated by hydrazine hydrate
(10 μΜ).
0 10 20 30 40 50 600.00
0.03
0.06
0.09
0.12
0.15
0.18
A 0 51
9 -
A 5
19
Au NPs : PDCA = 300 : X ( V Au NPs
/ V PDCA
)
b
5.5 6.0 6.5 7.0 7.5 8.0 8.5 9.0 9.5
0.05
0.06
0.07
0.08
0.09
0.10
0.11
A 0 51
9 -
A 5
19
PH
a
Electronic Supplementary Material (ESI) for Chemical CommunicationsThis journal is © The Royal Society of Chemistry 2011
Fingure S4. Selectivity of the ANCSS for hydrazine hydrate over other common metallic cations under the
optimized conditions: the concentration of each of the cations and hydrazine hydrate was 10 μM. (a) UV-vis
absorption spectra of the ANCSS upon addition of hydrazine hydrate and common metallic cations under identical
conditions. (b) The corresponding plot of (A0519-A519)/A
0519 intensity of the optimized ANCSS in the presence of
hydrazine hydrate and common metallic cations.
0.00
0.02
0.04
0.06
0.08
0.10
( A
0 519 -
A 5
19 )
/ A 0 5
19
Ni2+ Na+ Co2+Mn2+ Fe3+
Fe2+ Li+ Mg2+ K+Hg2+ Cu2+ Ba2+
Ca2+ Al3+Cd2+ Pb2+ Ag+ N2H4
400 450 500 550 600 650 700 750 800-0.1
0.0
0.1
0.2
0.3
0.4
0.5
0.6
0.7
0.8
0.9A
bs
orb
ance
Wavelength / nm
Ni2+ Na+ Co2+Mn2+ Fe3+
Fe2+ Li+ Mg2+ K+Hg2+ Cu2+ Ba2+
Ca2+ Al3+Cd2+ Pb2+ Ag+
N2H4
0
Electronic Supplementary Material (ESI) for Chemical CommunicationsThis journal is © The Royal Society of Chemistry 2011
Fingure S5. Selectivity of the ANCSS for hydrazine hydrate over other common anions under the optimized
conditions: the concentration of each of the ations and hydrazine hydrate was 10 μM. (a) UV-vis absorption
spectra of the ANCSS upon addition of hydrazine hydrate and common anions under identical conditions. (b) The
corresponding plot of (A0519-A519)/A
0519 intensity of the optimized ANCSS in the presence of hydrazine hydrate
and common ations.
0.00
0.02
0.04
0.06
0.08
0.10
( A
0 519 -
A 5
19 )
/ A 0 5
19
C6H5O73-
C2O42-
EDTA2-
Ac-
SO42-
ClO4-
NO2-
CO32-
SO32-
Br-
Cl-
F-
NO3-
HPO42-
N3-
S2O82-
N2H4
400 450 500 550 600 650 700 750 800-0.1
0.0
0.1
0.2
0.3
0.4
0.5
0.6
0.7
0.8
0.9
Ab
so
rban
ce
Wavelength / nm
C6H5O73-
C2O42-
EDTA2- Ac- SO42-ClO4
-NO2
-CO3
2- SO32- Br- Cl- F-
NO3- HPO4
2- N3- S2O8
2-
N2H4
0
Electronic Supplementary Material (ESI) for Chemical CommunicationsThis journal is © The Royal Society of Chemistry 2011
Fingure S6. Selectivity of the ANCSS for hydrazine hydrate over other common neutral interfering species under
the optimized conditions: the concentration of each of the common neutral interfering species and hydrazine
hydrate was 10 μM. (a) UV-vis absorption spectra of the ANCSS upon addition of hydrazine hydrate and common
neutral interfering species under identical conditions. (b) The corresponding plot of (A0519-A519)/A
0519 intensity of
the optimized ANCSS in the presence of hydrazine hydrate and common neutral interfering species.
0.00
0.02
0.04
0.06
0.08
0.10
( A
0 519 -
A 5
19 )
/ A 0 5
19
CH3NH2
C6H12O6
(NH2)2CO
N (CH2CH2OH) 3
C6H8O6
CH3OH
HCHO
NH3.H2O
NaBH4
NH2OH.HCl
GHS N2H4
400 450 500 550 600 650 700 750 800-0.1
0.0
0.1
0.2
0.3
0.4
0.5
0.6
0.7
0.8
0.9
Ab
so
rban
ce
Wavelength / nm
CH3NH2 C6H12O6 (NH2)2CO N(CH2CH2OH)3 C6H8O6 CH3OH HCHO NH3.H2O NaBH4 NH2OH.HClGHS
N2H4
0
Electronic Supplementary Material (ESI) for Chemical CommunicationsThis journal is © The Royal Society of Chemistry 2011
Fingure S7. Selectivity of the ANCSS for hydrazine hydrate over other common molecules with similar structures
under the optimized conditions: the concentration of each of the common molecules with similar structures and
hydrazine hydrate was 10 μM. UV-vis absorption spectra of the ANCSS upon addition of hydrazine hydrate (a),
methylenediamine dihydrochloride (b), 1,2-ethanediamine (c) and 1,4-benzenediamine (d) under identical
conditions. The results show that Au NPs undergo inter-particle cross-linking to form aggregates stimulated by
those molecules with similar structures. However, when compared with the UV-vis absorption spectra of Au NPs
stimulated by hydrazine hydrate, the peak profile is quite different and another obvious absorption band is
observed upon exposure of ANCSS to those molecules with similar structures, revealing that such ANCSS
provides a remarkable selectivity.
400 450 500 550 600 650 700 750 800-0.1
0.0
0.1
0.2
0.3
0.4
0.5
0.6
0.7(a)
Ab
so
rba
nce
Wavelength / nm
Blank Hydrazine Hydrate
400 450 500 550 600 650 700 750 800-0.1
0.0
0.1
0.2
0.3
0.4
0.5
0.6
0.7(c)
Ab
so
rba
nce
Wavelength / nm
Blank 1,2-ethanediamine
400 450 500 550 600 650 700 750 800-0.1
0.0
0.1
0.2
0.3
0.4
0.5
0.6
0.7
Blank 1,4-benzenediamine
Ab
sorb
anc
e
Wavelength / nm
(d)
Blank Methylenediamine dihydrochloride
400 450 500 550 600 650 700 750 800-0.1
0.0
0.1
0.2
0.3
0.4
0.5
0.6
0.7(b)
Ab
sorb
anc
e
Wavelength / nm
Electronic Supplementary Material (ESI) for Chemical CommunicationsThis journal is © The Royal Society of Chemistry 2011
Fingure S8. Specificity of the ANCSS for hydrazine hydrate over other analytes under the optimized conditions:
the concentration of each of the analytes and hydrazine hydrate was 10 μM and 100 μΜ, respectively. UV-vis
absorption spectra of the ANCSS upon addition of hydrazine hydrate and common metallic cations (a), anions (b),
and neutral interfering species (c) under identical conditions.
400 450 500 550 600 650 700 750 800-0.1
0.0
0.1
0.2
0.3
0.4
0.5
0.6
0.7
0.8
Ab
sorb
ance
Wavelength / nm
Ni2+ Na+ Co2+Mn2+ Fe3+
Fe2+ Li+ Mg2+ K+Hg2+ Cu2+ Ba2+
Ca2+ Al3+Cd2+ Pb2+ Ag+
N2H4
0(a)
400 450 500 550 600 650 700 750 800-0.1
0.0
0.1
0.2
0.3
0.4
0.5
0.6
0.7
0.8
Ab
so
rba
nce
Wavelength / nm
C6H5O73-
C2O42-
EDTA2- Ac- SO42-ClO4
-NO2
-CO3
2- SO32- Br- Cl- F-
NO3- HPO4
2-N3
- S2O82-
N2H4
0(b)
400 450 500 550 600 650 700 750 800-0.1
0.0
0.1
0.2
0.3
0.4
0.5
0.6
0.7
0.8
Ab
sorb
ance
Wavelength / nm
CH3NH2 C6H12O6 (NH2)2CO N(CH2CH2OH)3 C6H8O6 CH3OH HCHO NH3.H2O NaBH4 NH2OH.HClGHS
N2H4
0(c)
Electronic Supplementary Material (ESI) for Chemical CommunicationsThis journal is © The Royal Society of Chemistry 2011
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