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Flow Rate Effect of Syringe Pump on Quartz Crystal

Microbalance Sensor Resonance Frequency Stability


Ridha N. Ikhsani, Setyawan P. Sakti
Department of Physics, Brawijaya University
Malang, Indonesia
ridha.fisika@gmail.com, sakti@ub.ac.id

Abstract— Most Quartz Crystal Microbalance biosensor the sensor surface from the beginning of buffer or sample
system works in liquid phase utilizing flow injection system using solution injection, or change of liquid flow rate. Change of
a continuous peristaltic pump with electronic control. In the liquid high on top of the sensor also gives rise to pressure
development of QCM sensor as a disposable system, sample change. Small spike signal is observed in the sensor signal
injection using a syringe pump will be a candidate option as it output [7], [8]. The frequency change caused by the
can be operated manually. In this work, a flow rate effect of the hydrostatic pressure can be originated from many factors. One
microsyringe pump on the frequency stability of quartz crystal can be from the stress to the sensor caused by the pressure
microbalance resonance during injection is investigated. Flow change [9], [10]. This small signal spike, however, not affects
rate in a closed pipe causes a pressure change of the liquid on top
the whole sensor signal respond and mostly neglected.
of the sensor. Therefore, it can affect the resonance frequency of
the sensor. In this work, a microliter syringe pump with a Understanding the flow rate effect to the sensor response is
maximum volume of 100P PL is used. Sensor response is observed importance for the development of the QCM sensor for
in two pumping directions, which is injection and ejection of practical application. For a simple operation, the utilization of
liquid. At beginning 50PL water was injected on top of the sensor a flow injection system should be minimized. Manual liquid
surface. This volume fills the chamber of the sensor cell of 30PL. injection to the sensor surface or a small-volume liquid
After it steady frequency in contact with water; the water is dropping on top of the sensor surface will minimize the
ejected for 20PL and then injected back for 15PL. The sequence complexity of a flow injection system. Sample dropping
was repeated several times by changing injection and ejection method without pumping has been reported [11]. Small spike
speed. At a flow rate of less than 0.17PL/second the frequency signal was also observed after the sample injection using a
change of the sensor resonance frequency during injection into microliter manual pump. However, in a worst condition, the
the chamber change by 1-2 Hz. At liquid ejection, the frequency spike of the frequency responds caused by liquid pipetting on
of the sensor is still. top of the sensor surface can be significant [12]. Optimizing
Keywords— Flow rate; QCM; Microliter Syringe pump the sensor structure, cell reaction chamber, and pipetting or
I. INTRODUCTION injection method is needed to make QCM sensor applicable
for a practical, rapid diagnostic system without complex
Quartz Crystal Microbalance (QCM) sensor is one of the preparation.
mass-sensitive sensors, which can operate in a gas phase as
well as in liquid phase. The QCM sensor response is measured Manual pipetting or injection may vary in speed.
based on its frequency change, impedance change or decay According to the fundamental law of liquid flow in a close
length caused by signal perturbation. For each approach channel, the higher flow rate is a result of higher different
required an appropriate electronic system to get the sensor pressure from two ends of the channel. Variation of flow rate
signal from a mass change on the sensor surface [1]. indicates a variation in the pressure different. This pressure
different may affect the QCM sensor respond. Liquid sample
Since the first introduction of the QCM sensor by injection at the sensor surface leads to a short instability of the
Sauerbrey in 1957, QCM sensors have been used in many sensor response. In this work, we investigate the effect of flow
applications, including the measurement of thin layers, rate injection using a syringe pump to mimics manual
chemical analysis, gas sensor, humidity, and biosensors [2]. injection using a microliter pump for further development of a
Most of the QCM biosensors work in liquid phase [3], [4]. In practical QCM system for rapid diagnostic with minimum
this case, one of the sensor surfaces is in contact with buffer electronic requirements.
solution, and the other side is in contact with air to avoid an
excessive damping effect. Liquid viscosity affects the II. SYSTEM DESIGN AND METHOD
performance of the sensor as its append an additional damping In this experiment, a QCM sensor is made from a
load to the sensor [5]. In addition, hydrostatic pressure also commercial piezoelectric resonator with HC-49/U size. The
affects to the QCM sensor frequency [6]. resonator disc has an outer diameter of 8.7 mm and a
Based on the basic physics principle, liquid flow in a fundamental frequency of 10 MHz. The resonator has an
close channel is caused by a pressure different between two electrode diameter of 5mm made from silver with 100nm
ends of the channel. Therefore, there is a pressure change on thick. The sensor was purchased from PT Great Microtama

978-1-5090-1128-5/16/$31.00 ©2016 IEEE 107


Electronics Indonesia. Figure 1 shows the photograph of the through manual input using a keypad. Figure 4 shows the
sensor used in the experiment. The specification as described block diagram of the system. Figure 5 shows the whole
by the manufacturer is listed in Table 1. For this purpose, both system.
sides of the sensor surface were coated with polystyrene.

Mechanical
transmission 8.5 cm

Stepper

7 cm
Motor

11 cm
Syringe Teflon
Fig. 1. QCM sensor in the form of HC49/U Side part
Pump
TABLE I. RESONATOR SPECIFICATION 26 cm

Parameter Value Fig. 3. Schematic of the syringe injection pump construction


Frequency 10.0 MHz (Fund. AT-Cut)
Frequency Tolerance @ 25 degC ±10 ppm
Frequency Stability ±30 ppm Input PIC18F4550 Stepper Rotational
Equivalent Series Resistance 30 : keypad Convert to Motor to linier
Load Capacitance 12 pF (μL) ASCII translator
Drive Level 100PW
Microliter
syringe
The sensor is mounted in the cell as shown in Figure 2.
The cell is made from acrylic. The main part of the
construction is a liquid channel for injection, reaction chamber Fig. 4. Syringe injection system blocks diagram
on top of the sensor surface, and liquid tank to keep the excess
water from the sensor chamber during injection. This liquid
tank is also intended for a pipetting place for further
application.

Fig. 2. Reaction cell and QCM sensor in the experiment

The volume of the cell chamber on top of the sensor


surface to be filled with water is 30PL. A silicone ring is used
as a spacer and damper to minimize mechanical stress to the
sensor during installation in the cell. The sensor is driven
using oscillator at its series resonance frequency. Frequency
measurement is done using in-house developed frequency Fig. 5. Equipment set used in the experiment
counter with a resolution of 1 Hz [13].
The experiment was done by the following sequences. At
Syringe injection system was developed using a glass first, the sensor was installed in the reaction cell. The
syringe with a maximum volume of 100PL. The maximum resonance frequency of the sensor was recorded. A 50PL water
stroke length of the syringe is 8.5cm. The injection system was injected into the sensor chamber. Part of the injected
was developed in-house using a stepper motor and linear water flows to the liquid tank. After a new resonance
translator as in Figure 3. The injection speed of the system is frequency of the sensor in contact with water is reached, water
controlled using PIC18F4550 microcontroller. injection and ejection were done. During the process, one
Flow rate of the syringe injection system has been surface of the sensor is still in contact with water, and the
calibrated using a volumetric method. Flow rate is controlled chamber volume remains full of water. Along the sequence,

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the resonance frequency of the QCM sensor during the process it reverts to the initial frequency with 1 Hz different. No
is recorded. frequency change is observed during the ejection process (see
Figure 7). These results show a significant different comparing
III. RESULT AND DISCUSSION to the sensor frequency responds observed during the sample
Before water injection, the sensor is in contact with air in injection done by other works [12].
the cell chamber. A stable resonance frequency is observed. At flow rate 0.22PL /second, the frequency change of the
Injection of 50PL water into the sensor chamber was started. sensor during water injection is slightly higher than the
By the injection, the sensor surface of the reaction chamber is frequency change caused by injection of 0.17PL /second. AT
filled with water slowly. At the same time, the sensor surface 0.22PL/seconds the frequency change during the injection is
is also gradually come into contact with water. The result is a
3Hz. The frequency change is only 1-2 Hz at an injection
decrease in the frequency of the sensor. The decreasing
speed of 0.17PL/seconds. The different can be caused by
frequency occurs until the entire surface of the sensor in
different pressure change of both flow rate. The Higher flow
contact with water. In this state, the reaction chamber is fully
rate is caused by higher pressure differences. This effect is
filled with water.
similar to the effect of the increase in gas pressure in the
After 10 minutes, an amount of 15PL water is injected into frequency sensor [10].
the sensor chamber. This injection caused an increase of water
In the ejection process, the injection pump does not
level in the liquid tank of the reaction cell. In this event, the
generate pressure. In the ejection, pressure is mainly caused by
syringe pump generates a step pressure against the injection
the water level relative to the sensor surface. As the water
side to allow the water flows. In the same time, the QCM
level change in the liquid tank of the sensor less than 10mm,
sensor detects changes in water pressure. In some cases, it
no significant pressure change occurs on the sensor surface.
causes a change in the instantaneous frequency of the sensor
Whilst the contribution of the external pressure from the
as described before and can be seen in other works [7], [8],
atmosphere is still, t sensitivity of the sensor is not adequate to
[9], [10], and [12]. The same effect will occur when water is
detect the change. As a result, no frequency change is
ejected from the cell chamber.
observed.
Figure 6 shows the resonance frequency of the sensor
during the injection and ejection sequence of 15PL water at a
speed of 0.17PL per second for 90 seconds. At the first
injection sequence, there is no frequency spike observed. It
means that pressure change caused by the injection speed of
17PL/second does not affect the sensor resonance frequency.
However, we can observe a decreasing frequency of 2-3 Hz
during the injection. After the injection process stopped, the
resonance frequency of the sensor reverts to its original
frequency but changing by one Hz. The same respond is also
observed in the other injection sequence.
In the ejection process, the sensor behaves differently.
There is no frequency change during the ejection of the water
(see Figure 6). The sensor resonance frequency is still. There Fig. 7. Sensor resonance frequency caused by 20PL water injection and
ejection.
is no frequency change observed during the ejection sequence.
IV. CONCLUSION
The effect of water flow rate injected and ejected using a
syringe pump on QCM sensor was investigated. No frequency
change is observed during the ejection of the water. The small
frequency change is observed during the injection of water
into the sensor chamber. Higher injection speed results in a
higher-frequency change. Flow rate of less than 0.17PL
/second affects the resonance frequency of the sensor by 1-2
Hz. Those effects are a worst-case condition in this
experiment. Better frequency stability during the liquid sample
addition to the sensor surface is obtained by ejecting the liquid
from the sample chamber of the sensor cell.
ACKNOWLEDGMENT
Fig. 6. Sensor resonance frequency caused by 15PL water injection and
ejection. This work is supported by Ministry of Research,
Technology and Higher Education of the Republic of
At a higher injection speed, 20PL for 90 seconds (0.22PL Indonesia through the Hibah Kerjasama Luar Negeri dan
/second), the behavior is similar. During the injection, the Publikasi (HKLN) scheme project.
resonance frequency of the sensor decreases gradually. Then,

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