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 International Journal of Electronics, Electrical and Computational System
IJEECS
ISSN 2348-117X
Volume 6, Issue 4
April 2017

Design and Development of Nano pH Sensor and Interfacing

with Arduino
Shivam Vajpayee1, Baban Kumar2, Ritula Thakur1, Manish Kumar2
1
Department of EE, National Institute of Technical Teachers Training and Research, Chandigarh, India
2
Agrionics, CSIR-Central Scientific Instruments Organization, Chandigarh, India

ABSTRACT
Day by day the demand of pH sensor is increasing especially in the industry and in precision agriculture field. The
main purpose of this research is to enhance the developing rate of agriculture products and precise measurement.
Many sensor and actuators have been developed for this purpose in which some are commercialized and some still
remained. Now days nanotubes are famous as their increasing demand, Carbon nano tube is predictable to be one of
the majority promising field in prospect biomedical. The benefits of nanotube over the normal sensor are more
accurate, higher resolution, higher sensitivity and micrometer size. pH measurement is basically the concentration of
H+ ion present in sample. This research paper includes the aspect of nanomaterial and interfacing of nano sensor
with microcontroller. The main purposes of interfacing are to make the hardware valuable over the field level and
industrial level as well. Many technologies and sensors have been developed already but still research work is going
on. The main aspect of this research paper is to develop the real time monitoring of the data or pH value and display
it out of the field. it is well known fact that pH value of soil or the water is very important information in the
precision agriculture field.
KEYWORDS: pH value, Nanomaterial, Zinc and Antimony, Arduino.

I.INTRODUCTION
Over the past few decades, as larger and quicker farm equipment have delivered the ability to manage
ever-increasing farm, farmers have for the a good number part persistent to treat huge fields as uniform
elements. Attitudes have been altered in the past quite a lot of years, though, and a new scheme of farming
called precision agriculture is rapidly emerging. Based on what are called "site-specific" methods,
precision agriculture involve studying and managing variations within fields that can affect crop yield [1].
Nanoparticle is the material having high surface to volume ratio. A safe, low cost and reproducible
approach for the synthesis of antimony nanostructures with most of them having morphology and having
well defined faces in the range of 60-190 nm. A non- toxic and safe method has developed for the
synthesis of Sb nanoparticle from Sb metal powder and deionized water. The reported strategy other than
being sans organics is practical, quick and free of contamination [2].
Antimony is a semimetal and is broadly used as a fire retardant in synthetic industry, as enclosure of
electric devices and as a catalytic mediator in unrefined synthesis. It is also reported to have enhanced
thermoelectric effect in nano dimension comparing with their bulk counterparts. But the requirement of
simple and reliable protocols for the preparation of nanomaterial in common and antimony in particular
with restricted morphology.
ZnO is unique inorganic material that has been attracted and extensive research due to its characteristic
features and new applications in broad areas of science and technology. It has multiple properties like
semiconducting, piezoelectric catalysis and power metallurgy. In addition ZnO optical properties play a
very important role in optoelectronics and catalytic. The solution shows strong visible light absorption at
260 nm, characteristics of silver nano particles. A new technique for manufacturing antimony pH
microelectrodes is described. Several investigators have turned to metallic pH responsive electrodes in an
attempt to conquer some of the troubles of making glass pH microelectrodes. Of all the potential for small
to micro metallic pH microelectrodes, only antimony and tungsten electrodes have been used, due to many
reasons-relative low melting point, ease of production and availability in unpolluted form [3]

II.THEORY OF pH
pH is one of the the majority usually measured chemical properties. Technically, pH is a calculate of
hydrogen ion activity in a sample. pH is also called soil response which describes the acidity or alkalinity

66 Shivam Vajpayee, Baban Kumar, Ritula Thakur, Manish Kumar

 International Journal of Electronics, Electrical and Computational System
IJEECS
ISSN 2348-117X
Volume 6, Issue 4
April 2017

of the sample. Unfortunately, soil pH is an elusive, often misunderstand concept. This is due, in part, to the
fact that pH calculates something. No person has ever seen a ―hydrogen ion‖, even with the most powerful
microscope. [4]. New way of atomic structure is based on the nuclear theory. It‘s called a law because, as
previously noted, no person has seen an atom to confirm the details of its structure. The atomic
presumption holds that an atom is collected of a dense, central core called a nucleus contain positively
charged protons bounded by less dense negatively charged particles called electrons. The electrons are
scattered in a very large space around the nucleus in orbits like to the planets in our solar system. Those
electrons in the external orbits of a little elements are freely held and are called ―free electrons‖.[5]
Hydrogen (chemical symbol H) is a very easy atom consisting single of one proton and one electron. The
lone electron in its orbit is loosely held and open to drift about. Hydrogen ions are produced when an atom
of hydrogen loses its electron, leaving the hydrogen atom in an ionic state with a net positive charge. It is
cleared in fig 1

Fig.1 Free Electrons

The pH of a solution is distinct as –log (H+), where (H+) is the lively concentration of hydrogen
ions in the solution. Ion activity refers to chemical potential, or the ―freedom‖ of ions to interact
with other ions in solution. Active hydrogen ions are ―free‖ in a intelligence that they may interact
with other ions or molecules in a solution. In aqueous (water-based) solutions, there is good proof
to suggest that hydrogen ions does not exist as H+ but freely connect as hydronium ions.[6]

III.MATERIAL AND METHODOLOGY

Nanoparticles are the simplest form of structures with sizes in the nm range. In rule any collection
of atoms bonded jointly with a structural radius of < 100 nm can be measured a nano particle.
These can include, e.g., fullerenes, metal clusters (agglomerates of metal atoms), huge molecules,
such as proteins, and even hydrogen-bonded assemblies of water molecules, which survive in
water at ambient temperatures [7].
(1) Materials Used
Table 1.1 shows the chemicals used for formation of electrode and the synthesis of the antimony and the
zinc nano particles.
Table 1. Lists of Materials / Chemicals Used
Chemicals Symbol Source/Company Molecular Weight
Zinc Nitrate Zn(NO3)2 Molychem 189.36
Zinc Acetate Zn(O₂CCH₃)₂ Sigma Aldrich 183.48
Sodium Hydroxide NaOH Merck 40
Acetone C3H6O SISCO 58.08
Antimony Powder Sb Molychem Ltd. 121.75
Antimony Chloride SbCl3 Molychem 228.11
Methanol CH3OH Merck 32.04
Ethanol C2H5OH ChangsituYangyuan Chemical 46.08
China
Hydrochloric Acid Hcl (35%) Merk Specialist pvt. Ltd. 36.46
Sulfuric Acid H2SO4 (97%) Merk India Ltd. 98.07

67 Shivam Vajpayee, Baban Kumar, Ritula Thakur, Manish Kumar

 International Journal of Electronics, Electrical and Computational System
IJEECS
ISSN 2348-117X
Volume 6, Issue 4
April 2017

(2)Fabrication of Antimony Electrode:A safe and facile method was developed for the fabrication of
electrodes form Sb metal powder as soil sensing pH electrode. Synthesis of antimony nanoparticles and
deposition technique was also introduced. Synthesis of nano particle was done using hydrothermal
technique method while the deposition technique which we have used is dipping technique. Overall this
whole method of fabrication, synthesis and deposition of Sb nanoparticles on antimony electrodes is a very
easy, safe and cheap process. For the fabrication of antimony electrodes we have been used direct heating
method. The Sb powder was direct heated and as a result antimony electrode was fabricated[8].
In typical synthesis, simple water and antimony powder with PVP is used as a capping agent and heated in
Teflon vessel at 210/20c in an autoclave for the synthesis of Sb nanoparticleS[9].
After fabrication of Sb electrode and synthesis of Sb nanoparticles deposited Sb nanoparticles on antimony
electrode through dipping method which was a very easy safe method[10].
For this fabrication we took a conical shaped 15 ml borosil glass tube and filled it with gm with Sb
powder. Then the glass tube was placed in heating furnace at 650oc for 4 hours for direct heating. When
the antimony powder was completely molten, we switched off the heating furnace and kept it for cooling
for 12 hours. After 12 hours it was in solid form then the glass tube was broken and electrode was taken
out which was in conical shape. The electrode was shiny silver in colour and the upper yellow layer was on
oxide layer. This layer should be separated from the electrode as it is considered to be an impurity layer.
Then the copper wire was soldered above the surface of electrode for further electrical connections and
after the deposition of antimony.
(3)Synthesis Protocols
In this domain synthesis step of electrodes is explained, actually in every synthesis protocol there are a
flow diagram in which synthesis process are explained step by step.
(a) Synthesis Of Zno Nanoparticles For Refrence Electrode
ZnO is an intrinsic n-type semiconductor material that has been hexagonal configuration with lattice
parameter of a=b=0.3250 nanometer and c=0.5207 nm. Also, it has broad group gap of 3.37eV gives this
fabric an upper hand compare to others. Due to these individual criteria, the ZnO has an edge for
application of semiconductor including clear electronics, ultraviolet (UV) light emitters, piezoelectric
device, and substance gas sensor, transistors, solar cells, catalysts and spin electronics. Among all
methods, precipitation and sol-gel technique provides suitable control of nucleation, ageing and growth of
particles in solution. The direct precipitation is also one of the simple and cost effective methods for
volume production of materials. In this way, particle development owes to interact between dissimilar
aqueous solution and therefore very small particles are formed. Tiny size particles with lower solubility
product dissolve and re-precipitate on the surface of larger particles in solution, accordingly agglomeration
takes place in solution as the particles together to minimize surface energy. A simple and cost effective
direct precipitation method was used to synthesize ZnO nano particles using starch as a precipitating
agent[11].

Experimental Flow Chart

Fig.2 Chemical Reactions to Synthesize Zinc Oxide Nanostructure

68 Shivam Vajpayee, Baban Kumar, Ritula Thakur, Manish Kumar

 International Journal of Electronics, Electrical and Computational System
IJEECS
ISSN 2348-117X
Volume 6, Issue 4
April 2017

Zinc nitrate (Zn (NO3)2.6H2O) and soluble starch (C6H10O5) were purchased from Fisher scientific,
Germany and used without further purification. Distilled water was use to prepare precursor solution. ZnO
nanoparticles were synthesized by hydrothermal process using starch and zinc nitrate as precursors. In a
classic synthesis, 1.3 gm soluble starch dissolve in 200 ml Dilute water after that located in the stove for
16-20 mins, when starch is totally dissolve in water, 7.5grame zinc nitrate (Zn(NO3)2.6H2O) added it was
kept below constant stirring for 1 hour. In the same way 1.7 gm NaOH was also ready in 150 ml of
distilled water. The NaOH solution supplementary drop wise in the zinc nitrate and starch sample with
vigorous stirring. The chemical reactions occurred in this process is shown in fig.1.2. The final
precipitating solution was centrifuged at 6000 revolution per minute for 8 min and washed with acetone to
remove any impurities or possible absorbed ions [12].
(b) Synthesis of Sb Nanoparticles For Working Electrode: Antimony powder, AR grade (Ranbaxy, > 3
μm) was used as a foundation of metal/precursor and purified by ultra sonication in water. In a classic
preparation process,three mg of antimony residue was added to 30 ml of clean water in a glass vial. The
reaction combination was sonicated for about twenty min in a glass vial, transfer into a stainless steel
Teflon lined metallic bomb and sealed under usual conditions. The closed autoclave was then located
inside furnace and the mixture was heated slowly (2°C/min) to 210 °C and maintain at this temperature for
12 h. After cooling, the resultant suspension was centrifuged to retrieve the product, washed and then
finally vacuum dried for few hours[13].
(4) Electrodeposition of Zno Nanoparticles On Zinc Electrode
Electro-deposition of nano particles was performed in three electrode system contained in a single
compartment cell. The working substrates used in the experiment are platinum wire, Zinc electrode, and
silver electrode. They were cleaned ultrasonically in detergent, deionized water and ethanol former to the
layer deposition. The zinc electrode is used as the working electrode, silver/silver chloride electrode
(Ag/AgCl) serving as reference electrode, and the Pt wire working as the count electrode, which was used
to preserve a constant Zn ion concentration during the electrodeposition.The ZnO nanorod films were
cathodic electrodeposited from baths containing4mM of zinc acetate (ZnC4H6O4) dissolved in the 30 ml
deionized water as supporting electrolyte. The bath temperature was maintained at 75 ◦Cby using a
thermostat. The ZnO layers were electrodeposited under potentiostatic condition of 0.9V for 30 minutes
[14].

Fig.3 CH Instruments Electrochemical Analyzer and Voltammetry Setup for Zn Electrode

(5) Electrodeposition of Sb Nanoparticles On Sb Electrode

Bulk electrolysis test was carried out in a three-electrode cell by the CHI 660C electrochemical analyzer
(CH device). The complete setup for electro deposition of antimony electrode is shown in the Fig.4. The
working electrode was antimony, counter electrode was platinum wire and the reference electrode was
Ag/AgCl. Before each electrochemical measurement, the electrodes were hand-polished with
metallographic SiC smooth paper. Subsequently, the electrodes were refined with alumina grinding paste
and then cleaned ultrasonically in the alcohols and deionizer water, respectively. Before starting the
deposition prepare the antimony stock solution was prepared using the Sb(lll) chloride. Bath containing
0.05 gm SbCl2 was added in the 15 ml deionised the solution was sonicated for 10 min when the sonication
was completed, 2.5 ml HCl was drop wise added in the solution, add the deionised water to make the
solution 30 ml. The Sb films were electrodeposited under potentiostatic condition of -1.2 V for 15 sec.

69 Shivam Vajpayee, Baban Kumar, Ritula Thakur, Manish Kumar

 International Journal of Electronics, Electrical and Computational System
IJEECS
ISSN 2348-117X
Volume 6, Issue 4
April 2017

Fig.4 CH Instruments Electrochemical Analyzer and Voltammetry Setup for Sb Electrode

Soil pH is defined by equation pH = -log10H+ in which the activity of H+ ion in the soil suspentation and H+
is expressed as grams ions per liter. The effective concentration of H + ion includes all sources such as
those dissociated from soil particles and dissociation of soluble acid. pH is determined by the measurement
of electro chemical potential that existed between different solution. These electro-chemical methods are
accomplished by treasuring the voltage developed between electrodes that are in contact with different
reaction media.[15] The system depicts the development of a pH meter for soil to control the amount of
added fertilizer for irrigation purpose. For development of soil pH sensor a number of modules described
below have been be implemented:
 The zinc and antimony nanoparticles have been synthesized.
 Characterization of the synthesized zinc and antimony nanoparticles.
 A Soil pH sensing electrode has been fabricated using the antimony metal powder.
 The sensing electrode (antimony) has been coated with the antimony nanoparticle using the
electrochemical deposition method for increasing its sensing efficiency.
 The reference electrode (zinc) has been coated with the zinc nanoparticle using the electrochemical
deposition method.
 Conical shaped pH sensing electrode has been be joined to a reference electrode by an interfacing
insulator.
 Electrodes have been connected to a digital multimeter.
 Now the instrument was directly be pierced into the water.
 Potential generated between the electrodes is directly related with pH value of water.
 Connect these electrodes to the arduino and display the data to LCD.
Fig. 5shows the flowchart of the methodology for carrying out the work
START

Synthesis and characterization of ZnO/Sb

Fabrication of Antimony Electrode

Connecting Electrode to the

Calibration of Electrode Conductimeter

Connecting the Electrodes to multimeter and arduino

Record the Output

STOP

Fig. 5 Flowchart of Soil pH Sensor

70 Shivam Vajpayee, Baban Kumar, Ritula Thakur, Manish Kumar
 International Journal of Electronics, Electrical and Computational System
IJEECS
ISSN 2348-117X
Volume 6, Issue 4
April 2017

So above diagram shows the connectivity to the electrode with microcontroller.

IV.MICROCONTROLLER
In this research work arduino has been used as microcontroller since its has also included A/D converter.
Arduino is a tiny microcontroller panel with a USB plug to attach to computer. It has number of
association sockets that can be wired up to outer electronics, such as relays, light sensors, motor etc. They
can either be motorized through the USB connection from a 12V battery. They can be restricted from the c
programmed by the computer and then cut off and allowed to work independently. The Uno is a
microcontroller panel based on the AT mega328P. It has 14 digital input/output pins (of which 6 can be
used as PWM outputs), six analog inputs, a 16 MHz quartz crystal, a USB connection, a power jack, an
ICSP legend and a reset button. It contains everything needed to sustain the microcontroller; simply
connect it to a processor with a USB cable or power it with a AC-to-DC adapter or battery to get started. It
is shown in fig in .6[16].

Fig 6 Arduino Uno Board

V.RESULT AND DISCUSSION

(1)Electrodeposition Graph Of Zinc Electrode
Electrode position of zinc electrode was carried out using the bulk electrolysis techniques. Zinc
proceeded by a three dimensional instantaneous nucleation and growth process. The zinc deposited formed
by bulk electrolysis consisted of hexagonal grains with a size of 4-5 µm. In Bulk Electrolysis (BE), a
constant potential is applied and the incorporated charges are recorded as a function of time. The following
Fig.7 shows the potential waveform applied as a function of time and the sampling scheme.

Fig.7 Electrodeposition of Zinc Electrode

(2)Electrodeposition Graph Of Antimony Electrode
Fig.8 shows the graph between time and deposited charge on the sensing electrode. Initial potential
voltage for the antimony deposition is -1.2 v and deposition time was 15 sec. The electro deposition was
perform with the help of CHI instruments, with three electrode configuration, refrence electrode Ag/AgCl,
working electrode Sb and the counter electrode wire[17].

71 Shivam Vajpayee, Baban Kumar, Ritula Thakur, Manish Kumar

 International Journal of Electronics, Electrical and Computational System
IJEECS
ISSN 2348-117X
Volume 6, Issue 4
April 2017

Fig.8 Electrodeposition of Antimony Electrode

(3) Repeatability Test Of Antimony And Zinc Metal Electrode

For testing of repeatability ten times value in mill volt are taken, after this average value is considered for
further studies. Every sample milli volt values are taken after some time[18].
Table 2 Repetability Test of Metal Electrodes
S.No. pH 4 pH 6 pH 7 pH 9 pH 10 pH 12
Voltage Voltage Voltage Voltage Voltage Voltage
(mv) (mv) (mv) (mv) (mv) (mv)
1 774 679 579 445 400 200
2 772 683 580 440 400 200
3 776 680 583 450 402 200
4 780 682 582 450 398 200
5 768 681 581 450 400 200
6 770 682 583 452 399 198
7 778 680 579 448 401 202
8 774 682 581 452 400 200

9 775 683 581 448 400 200

10 773 678 581 450 400 200

Avg. 774 681 581 450 400 200

Valu
e

(4)Repetability Test Of Antimony And Zinc Nano Electrode

In the same way like as above nano electrode repeatability test has been accomplished,
Table 3 Repetability Test of Nano Electrode
S.No. pH 4 pH 6 pH 7 pH 9 pH 10 pH 12
Voltage Voltage Voltage Voltage Voltage Voltage
(mv) (mv) (mv) (mv) (mv) (mv)
1 820 750 655 540 490 341
2 821 760 654 540 488 342
3 822 750 655 540 498 340
4 819 760 656 540 492 340
5 818 755 655 540 492 337
6 819 760 656 542 492 343
7 818 755 655 538 490 337
8 821 760 654 540 494 339
9 822 750 655 542 492 341
10 820 750 655 538 492 340
Avg.Value 820 755 655 540 492 340

72 Shivam Vajpayee, Baban Kumar, Ritula Thakur, Manish Kumar

 International Journal of Electronics, Electrical and Computational System
IJEECS
ISSN 2348-117X
Volume 6, Issue 4
April 2017

(4) Response Time Experiments Of Antimony And Zinc Nanoelectrode Sensor

pH measurements were completed in chain using standard buffers and soil samples, to ascertain the
response time of the sensor to changes in pH. The effect of pH (given different pH ranges) on response
time of the sensor when immersed into standard buffered solutions was relatively consistent, response time
increasing with increasing Ph [19].
The antimony electrode is rugged enough to use in low soil to solution mixtures. However, as response
time is the critical property in the evaluation of the pH sensors, undoubtedly the antimony electrode
appears most suitable for adaptation and use as a continuous, ‗on-the-go‘ field pH sensor. This conclusion
was reached because the antimony electrode was shown to have a considerably faster response time.
Correlation linear equation is
Y = -100x + 1550 ( x1= 11, x2 = 12, y1= 450, y2 =350 ), r2 = 0.939 (correlation factor)

Fig 9 pH Versus Voltage graph for Nano Electrode

5 Response Time Experiments Of Antimony And Zinc Metal Electrode Sensor:

Fig10 PH Versus Voltage Graph for Metal Electrode

Y= -100x+1300, ( X1 = 7, X2 = 6, Y1= 600, Y2 = 700)

Correlation coefficient, r2= 0.9192
6 Measurement Of Ph Value Using Arduino
Since pH scale is nonlinear, so a range has been selected for measuring the pH value.
Table 4. Voltage Range for Arduino
S. No Voltage Range (mv) pH Value
1 774-820 4
2 681-753 6
3 581-655 7
4 450-540 9
5 400-492 10
6 200-340 12

73 Shivam Vajpayee, Baban Kumar, Ritula Thakur, Manish Kumar

 International Journal of Electronics, Electrical and Computational System
IJEECS
ISSN 2348-117X
Volume 6, Issue 4
April 2017

From the above table it is cleared if any value lies between voltage range then correspondence data will be
displayed, for an example range 753-774 will display 5 pH value.

7 Images Of Data Display In Lcd With Arduino At Different pH Sample

The Antimony and zinc electrodes are used, interfacing between electrodes and arduino can easily be seen
in all images, LCD 16*2 has been used in practical. Solution are made to add NaCl and NaOH with water
respectively for acid and base[20]

Fig 11.Data Display at 4 pH Sample

It is cleared in above image that the solution is acid since it has 4 pH value, Here the sensor is antimony
and zinc as a refrence electrode.

Fig 12 Data Display at 5 pH Sample

In above picture acid solution at pH value 5 is shown, interfacing are clearly shown in picture. Next
diagram pH value 6 has been shown.

Fig 13. Data Display at 6 pH Sample

In this same manner remaining sample i.e. upto 12 pH value has been measure

74 Shivam Vajpayee, Baban Kumar, Ritula Thakur, Manish Kumar

 International Journal of Electronics, Electrical and Computational System
IJEECS
ISSN 2348-117X
Volume 6, Issue 4
April 2017

ACKNOWLEDGEMENT
The Authors are grateful to director CSIO for his kind support, guidance and the permission to carry out
above research work.

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