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Quantitative Analysis of Formaldehyde Using

UV‐VIS Spectrophotometer Pattern Recognition
and Artificial Neural Networks

Article in Analytical Letters · January 2007

DOI: 10.1080/00032710600867606

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 QUANTITATIVE ANALYSIS OF FORMALDEHYDE
USING UV-VIS SPECTROMETER PATTERN
RECOGNITION AND ARTIFICIAL
NEURAL NETWORK

Han Chern Loh a,*, Kok Wai Chong b, Musa Ahmad b

a
Universiti Tunku Abdul Rahman (UTAR), Faculty of Engineering and Science
(FES), Jalan Genting Kelang, Setapak, 53300 Kuala Lumpur, Malaysia.
b
School of Chemical Sciences & Food Technology, Faculty of Science &
Technology, National University of Malaysia (UKM), 43600 Bangi, Selangor,
Malaysia.
*
Corresponding author: (Tel) +60123124877, (Fax) +60341079803, (Email)
hcloh@mail.utar.edu.my
_____________________________________________________________________
Abstract

This study is focused on quantitative analysis of formaldehyde in aqueous solution by

using Fluoral-P reagent. The characterisation of the reaction including the effect of
reagent concentrations, pH, response time, dynamic range, reproducibility,
photostability and selectivity by using UV-Vis spectrophotometer. The RSD value
was found between 1.79% and 2.12%. The dynamic range of the complex gives a
linear stimulation between 0.00 – 3.60 ppm for the concentration of formaldehyde.
The reproducibility of this study is high with 1.79 % and 2.12 % for 20 ppm and 40
ppm of formaldehyde respectively. The interference from acetaldehyde
(formaldehyde: acetaldehyde = 1:100) is lower than 2.10 %. In addition, application
of ANN on quantitative analysis for formaldehyde has also been done in this study to
optimise the dynamic range of formaldehyde that involved in the formation of
Fluoral-P-formaldehyde complex. A three layers feed-forward network and the back
propagation algorithm operated training process was used in this study. For
quantitative analysis of formaldehyde, ANN networking with 23 hidden neurons and
40,000 cycle number with 0.001% learning rate produce the best training result with
SSE value 0.5847.

Keywords: Formaldehyde, Fluoral-P, Spectrometric, Artificial neural network,

Back propagation
_____________________________________________________________________

1. Introduction

The drastic increase of formaldehyde production and usage nowadays has

exposed society to this harmful chemical reagent. Since the past three decades,
formaldehyde already known as mutant, carcinogen, and very toxic to eyes,
membrane as well as respiration system of human being [1]. Formaldehyde has been
classified as one of the major pollutants due to its toxicity. It tends to form nitric acid
and PAN (peroxide acetyl nitrate) through photochemistry reaction [2].
 There were many reagents used for formaldehyde determination. These
including 5,5-dimetil-1,3-sikloheksadion (Dimedone) [3], N-metil-4-hidrazino-7-
nitrobenzofurazan (MNBDH) [4], Fluoral-P [5] and 2,4-dinitrofenilhidrazina (DNPH)
[1]. However Fluoral-P was used in this study as this reagent has the highest
selectivity [5] if compared to others.

Formaldehyde reacts with Fluoral-P and produces 3,5-diacetyl-1,4-

dihydroluthydine (Equation 1). This compound is yellow greenish in colour, which
absorbs light at wavelength of 412 nm [6].

O H H O
CH3 CH 3
O
C
C
+ 2 C C H3C C C CH3
H H O NH 2
C C
H H3C N CH3

H
Formaldehid Fluoral-P 3,5-diacetyl-1,4-dihydroluthydine

(Equation 1)

ANNs are computational models that share some of the properties of the brain.
They are parallel information-processing structures that attempt to emulate certain
performance characteristics of the biological neural system. These networks consist of
many simples “units” working in parallel with no central control and learning takes
place by modifying the weights between connections. They process information by
their dynamic state response to external inputs [7]. The basic components of an ANNs
are “neurons”, weights and learning rules [8]. Thus, ANNs are also described as data
processing systems that simulate the human brain by building on information through
“learning” [9].

The application of ANNs embraces of many fields like medical [10-12],

industry [13], chemistry [14], physic [15], music [16], agriculture [17], management
[18], archaeology [19] and engineering [20]. A variety of algorithms can be used for
ANNs training purpose. These algorithms including radial basis function (RBF) [21],
probabilistic neural network (PNN) [22], recursive prediction error (RPE) [23-24],
Kohonen network [25-26] and back propagation (BP) algorithm [27-36]. However BP
was applied in this study due to this algorithm is the simplest comparatively [27-29].
The objectives of using ANN in this study are to extend the working range of
formaldehyde analysis and predict the formaldehyde concentration. This analysis is a
preliminary study for the development of formaldehyde sensor in the future.

2. Experimental

2.1 Reagents and Apparatus

All reagents used in this study were of analytical-reagent grade. Acetic acid
and acetyl acetone were purchased from J. T. Baker whilst ammonium acetate,
potassium chloride, hydrochloric, potassium hydrogen phthalate, potassium
dihydrogen phosphate, sodium oxide, Borax and sodium bicarbonate were purchased
from Fluka. Formaldehyde was obtained from AnalaR. All chemicals were used
without further purification. Deionised water obtained from Maxima Ultra Pure Water
Elga (Elga Stat Maxima UF model) was used throughout the experiment for solution
preparation. All spectrophotometric measurements were made with Varian Cary 50
UV-Vis Spectrophotometer (Varian Australia Pty. Ltd., Victoria, Australia) using
quartz cell.

2.2 Preparation of Fluoral-P and Buffer Solutions

Fluoral-P reagent was prepared by dissolving 7.7 g ammonium acetate with deionised
water in 250 mL volumetric flask. This solution was then added with 1.5 mL of 1.0 M
acetic acid and 1.0 mL of 1.0 M acetyl acetone. The mixture was added with
deionised water until the line and was shaken. Buffer solutions were prepared as
shown in Table 1 [37].

2.3 Procedures

The effect of reagent concentration on the absorption intensity of the complex

was studied by using different initial concentration of Fluoral-P. The absorption
measurements of the complex were then taken using the same concentration of
formaldehyde solution. The dynamic range of response to formaldehyde concentration
was determined by introducing different concentrations of formaldehyde and the
absorption signal measurement was carried out using UV-Vis spectrometer. The
reproducibility study was carried out by using a new batch reagent after each
measurement. The interference from acetaldehyde was studied by introducing
different amounts of acetaldehyde to the formaldehyde solution so that the mole ratio
of formaldehyde to acetaldehyde in the solution was varied (1:10, 1:20, 1:30, 1:40,
1:50, 1:60, 1:70, 1:80, 1:90 and 1:100).

2.4 Data treatment and analysis

The ANN training and data treatment were realised using a Matlab program.
In this study, a three layers feed-forward ANN with a BP training algorithm was
employed for data treatment. The input layer consists of 23 neurons, which
represented the absorption intensities measured at 7 different wavelengths from each
spectrum. The network was trained up to 40,000 cycles and the progress of sum-
squared error (SSE) between the calculated and the measured output was recorded. In
order to check its forecast capability and precision, a new set of input data was
introduced. The best network chosen was based on several tests using the trained
network that incorporated the inspection for data training fitting errors and prediction
test of errors.

3. Results and discussion

The spectrophotometric spectra for the solutions of Flural-P, formaldehyde and

the Fluoral-P-formaldehyde complex are shown in Fig. 1. The maximum absorption,
maks, for Fluoral-P reagent alone was at wavelength of 291 nm whilst formaldehyde
did not show any peak between the wavelength of 200 and 800 nm. After
formaldehyde solution was added to 2 ppm of Fluoral-P reagent, the colour was
changed from light yellow to yellowish green where Fluoral-P-formaldehyde was
formed.

The absorption was measured at wavelength of 411 nm for the complex. This
wavelength is very similar with the previous work of 412 nm [5]. The optimum
response of the complex was obtained at pH 7 (Fig. 2). Hence this pH was used
throughout this study. The photostability of this complex is more than 8 hours. The
study of response time was carried out by using three different concentrations of
formaldehyde, i. e. 20, 40 and 60 ppm (Fig. 3). The high reaction rate was obtained
for the first 20 minutes. After 20 minutes, the reaction rate had become lower and
constant.

The effect of the reagent concentration on the complex was studied by using
different initial concentrations of the reagent. Fig. 4 shows the effect of reagent
concentration of Fluoral-P used during complexation. As the concentration of Fluoral-
P is increased, the measured absorbance is also increased. This is due to the more
Fluoral-P-formaldehyde complex has been formed when more reagent is available.
The curvature at higher concentration is expected due to the reagent has been fully
reacts with formaldehyde. The same curvatures have been reported by Loh and co-
worker [27-28,38] as well as Musa and Narayanaswamy works [39]. Reagent
concentration of 1.24 x 10-5 M was chosen for the following study in this study.

The dynamic range of Fluoral-P-formaldehyde complex determined is shown

in Fig. 5. The plot of formaldehyde concentration against absorption was linear for
formaldehyde concentration in the range of 0.60 – 3.60 ppm formaldehyde. The linear
range is rather narrow. However this problem can be overcome by applying artificial
neural network (ANN) like what have been reported in the previous works [27-30,
38].

Two different concentrations of formaldehyde, i. e. 20 and 40 ppm were

chosen for reproducibility study (Fig. 6). The results give relative standard deviation
(RSD) values of 1.79 % and 2.12 % for 20 ppm and 40 ppm of formaldehyde
respectively. The low RSD values obtained in this study indicates that this method has
a good potential to be adopted as analytical method for formaldehyde determination
because it is highly reproducible. The interference from acetaldehyde towards
complex has been carried out by using ten different mole ratio of formaldehyde:
acetaldehyde i.e. 1: 0, 1:10, 1:20, 1:30, 1:40, 1:50, 1:60, 1:70, 1:80, 1:90 and 1:100
(Fig. 7). Interfering effect for all ratios are lower than 2.10 %. The interfering
percentage is calculated with the equation below:
I −I
Interference Percentage = o i x 100%
Io
where Io is intensity without interference whilst Ii is intensity with interference.
Hence, no obvious interference is caused by acetaldehyde if compared with this
formaldehyde detection method.

Fig. 8 showed the three-dimensional absorption spectra of the Fluoral-P-

formaldehyde complex, measured at different formaldehyde concentrations. The
absorption reading of different formaldehyde concentrations at this wavelength is
shown in Fig. 5 with the non-linear characteristics lie beneath in the collected data
with the linear relationship range from 0.60 – 3.60 ppm formaldehyde. Therefore the
beneficial linear range is rather narrow. Here, ANN is suitable to be used for non-
linear modelling purposes in order to extend the calibration response [23-24, 27-28].

In this study, 7 wavelengths points (238, 254, 262, 277, 316, 411 and 460 nm)
from each spectrum were selected to represent the input data for the ANN. These
points were selected due to the general outline of the original spectra were represented
and the variations in the sensor response were significant. The same training method
has been used and reported [27-30] to avoid several problems during network
training. These problems are long training period and large matrices entailed for the
network connection [27-28, 38].

A total of 22 spectra (0.6, 1.2, 2.4, 3.0, 4.2, 4.8, 6.0, 6.6, 7.8, 8.4, 9.6, 10.2,
11.4, 12.0, 13.2, 13.8, 15.0, 15.6, 16.8, 17.4, 18.4 and 19.2 ppm) were used for ANN
training. The optimisation of network was performed by changing the number of
hidden neurons and cycle number (Table 1). The SSE was measured at the end of
each training and being recorded. Table 3 shows the SSE values of network after
undergone different cycle number and hidden neurons. Network with 23 hidden
neurons and 40000 cycle number was chosen for this study due to the network gave
the lowest average calibration error value.

All of these networks were presented with eleven calibration spectra (1.8, 3.6,
5.4, 7.2, 9.0, 10.8, 12.6, 14.4, 16.2, 18.6 and 19.8 ppm) in order to improve the
process in choosing the best architecture of network and to establish their prediction
capability. Table 2 displays the predicted values of all formaldehyde concentrations
with the measured formaldehyde concentrations with the network training. The useful
dynamic range is now extended to a wider range of 0 – 19.8 ppm with average
calibration error and SSE are 0.1771 and 0.5847 respectively.

4. Conclusion

The studies carried out in this work indicate that formaldehyde determination
by using Fluoral-P as reagent is optimum at pH 7 and the 1.24 x 10-5 M reagent
concentration. A good reproducibility (2.12 %) of measurement was obtained. This
study can be developed further as into formaldehyde sensor fabrication. The network,
trained using BP algorithm was highly accurate in predicting the response of this
sensor, with average prediction error of 0.5847 g/L. The ultimate effect of
implementing ANN on formaldehyde detection was broadening the useful response
range from limited linear response (0.60 – 3.60 ppm) to extensive calibration response
(0.00 – 3.60 ppm).

Acknowledgements

Scholarship of National Science Fellowship (NSF) towards Han Chern Loh

from the Ministry of Science, Technology and Innovation (MOSTI), Malaysia is
greatly acknowledged.
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Table 1: Preparation of Buffer Solutions

PH Value Method of Preparation

1 100 mL 0.2M KCl + 268 mL 0.2M HCl
3 100 mL 0.1M sodium hydrogen phthalate + 44.6 mL 0.1M HCl
5 100 mL 0.1M sodium hydrogen phthalate + 45.2 mL 0.1M NaOH
7 100 mL 0.1M sodium dihydrogenate phosphate + 58.2 mL 0.1M NaOH
9 100 mL 0.025M Borax + 9.2 mL 0.1M HCl
11 100 mL 0.05M sodium bicarbonate + 45.4 mL 0.1M NaOH
13 100 mL 0.2M KCl + 264 mL 0.2M NaOH

Table 2: Predictions of the network with 23 hidden neurons

Measured Formaldehyde Predicted Formaldehyde

Concentration (ppm) Concentration (ppm) Error

1.8000 1.8184 0.0184

3.6000 3.6399 0.0399
5.4000 5.4153 0.0153
7.2000 6.9539 0.2461
9.0000 9.2226 0.2226
10.8000 10.8309 0.0309
12.6000 11.7830 0.8170
14.4000 14.2678 0.1322
16.2000 16.2355 0.0355
18.6000 18.4093 0.1907
19.8000 19.6664 0.1336
Average Calibration Error 0.1771

SSE 0.5847

Table 3: SSE values of network after undergone different cycle number and hidden
neuron

Cycle Number Hidden Neuron Average Calibration Erroe SSE

40000 23 0.1771 0.5847
41000 23 0.2092 0.5153
37000 26 0.2203 0.5374
42000 26 0.2626 0.4640
44000 26 0.2214 0.5064
Abs

Wavelength

Fig. 1: Spectra for Fluoral-P-formaldehyde complex (a), Fluoral-P (b), and

formaldehyde (c)

1.6

1.5

1.4
Abs

1.3

1.2

1.1

1
0 2 4 6 8 10 12 14
pH

Fig. 2 : Effect of pH towards Fluoral-P-formaldehyde complex with 1.24 x 10-3 mM

of Fluoral-P and 10 ppm of formaldehyde at wavelength of 411 nm
 Abs

Time (min)

Fig. 3: Response time for reaction between Fluoral-P and formaldehyde at

formaldehyde concentration of 20ppm (a), 40 ppm (b) and 60ppm (c) with 1.24 x 10-3
mM of Fluoral-P at wavelength of 411 nm

0.5

0.4

0.3
Abs

0.2

0.1

0
0 0.1 0.2 0.3
Fluoral-P Concentration (mM)

Fig. 4: Reagent effect towards absorption of Fluoral-P-formaldehyde complex

between 1.24 x 10-2 mM – 1.48 x 10 mM.
 0.6

0.5

0.4
Abs

0.3

0.2

0.1

0
0 2 4 6 8 10 12 14 16 18 20
Formadehyde concentration (ppm)

Fig. 5: Absorption of Fluoral-P-formaldehyde complex at different formaldehyde

concentration (0.00 – 19.8 ppm) at wavelength of 411 nm

0.30

0.25

0.20
Abs

0.15

0.10

0.05

0.00
1 2 3 4 5 6 7 8 9 10
Measurement
20ppm 40ppm

Fig. 6: Reproducibility analysis for Fluoral-P-formaldehyde complex

 Abs

Ratio formaldehyde: acetaldehyde

Fig. 7: Interference effect of acetaldehyde at different ratio of formaldehid and

acetaldehyde

1.0

0.8

0.6
Abs
0.4

0.2

0
19.0
230 9.50
360 Formaldehyde
Wavelength 500 4.75 concentration
0 (ppm)

Fig. 8: Three-dimensional absorption spectra of the Fluoral-P-formaldehyde complex

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