(KAJ) Kurdistan Academicians Journal, March 2006 , 4(1) part A (137-145)

A ‫) بةشى‬1( ‫ذ‬1494 -‫بةرط‬, ) ‫ ئازارى‬2706 ‫طؤظارى ئةكاديميانى كوردستان نةوروزى‬

2006
137( ‫لثةرة‬

Atomic Absorption Determination

of Traces of Lead in Ambient Air
and Water after its Preconcentration
Fadhil M. Najib, Khalid M. Omer and Aumed I.Haidar
Department of Chemistry; College of Science; University of Sulaimani, Kurdistan
Region/Iraq

Abstract
The determination of traces of lead from the ambient air and water of Sulaimani city were performed. The
samples of air were withdrawn at a rate of 300ml.min- through homemade impinger systems into 0.5M
perchloric acid for 2 hours as the best absorbent for trapping different forms of lead. Samples of drinking
water were taken from different sources throughout the city. An ion-exchange resin (XAD-16) was used for
the enrichment of collected lead to a detectable level followed by its determination by Flame Atomic
Absorption Spectrometry. Average lead in Sulaimani air and water was found to be 0.4µg/m3 and 28µg/L
which are well below the tolerance levels internationally accepted which were 1.5µg/m3 and 50µg/L
respectively. The results indicated that, the suggested method is suitable for environmental study for the
determination of lead in air and water.
Keywords:- Determination of lead in air and water by Atomic Absorption, air
sampling,an absorbent for lead from air, preconcentration

Introduction Natural waters seldom contain more than 5

Lead is well known as one of the most
toxic metals and noted in the field of
environmental chemistry[1]. The intake of
lead by the body comes from lead in food,
water and air[2]. According to the
stipulation of the center for Disease
Control (USA) and the department of
Health (UK), typically, levels of lead in
blood of children are of the order of 100µ
g/L [3].The sources of air pollution may be
divided into two types, namely mobile and
stationary sources. Mobile sources are
those related to transportation such as
automobiles, trains, airplanes, while
stationary sources include pipelines,
factories, and storage tanks [4]. Lead has
been determined in tap, river and sea water
by different methods in the literature [5-7].
µg/L lead, although higher values have
been reported [8-10]. Lead in water
supply may come from industrial, mine
and smelter discharges or from the
dissolution of old lead plumbing.PVC
pipes also contain lead compounds that can
be leached from them and result in high
lead concentrations in drinking water. The
amount of lead dissolved from the
plumbing system depends on several
factors, including the presence of chloride
and dissolved oxygen, pH, temperature,
water hardness and standing time of the
water, soft, acidic water being the most
highly plumbosolvent.[ 8 ]
In Glasgow (Scotland), where the water
was known to be plumbosolvent, the lead
concentrations is about 100µg/L [9].

Email: fadhilmn@yahoo.com

137
141
(KAJ) Kurdistan Academicians Journal, March 2006 , 4(1) part A
A ‫) بةشى‬1( ‫ ذ‬4 ‫بةرط‬, 2006 ‫ ئازارى‬2706 ‫طؤظارى ئةكاديميانى كوردستان نةوروزى‬
If a concentration of 5µg/L in drinking
water is assumed, the total intake of lead
from this source can be calculated to range
from 3.8µg/day for an infant to 10µg/day
for an adult [8].
Atomic Absorption Spectrometry (AAS)
is one of the most widely used technique
for the determination of trace elements in
water and air, but it has a relatively high
detection limit in the flame mode not
sufficient for direct determination
of this element in these samples. Many
techniques have been used for the
preconcentration of trace elements in water
and air samples, including chelating ion
exchange resin[10],preconcentration by
FIA[11] , and coprecipitation[12].
The aim of this work is to develop a
simple sampling unit and rapid
preconcentration method for the
determination of lead in the environmental
samples of air and water in the city of
Sulaimani.
Experimental
Reagents
All glassas were washed with 2M HNO3
then thoroughly with distilled water.All
reagents used were of analytical grade. A
series solutions of lead ion, for the
calibration curve was prepared by serial
dilution of the AAS standard solution
(GSB G 62071-90) (1000mg/L). 1M of
HClO4 ,HNO3, HCl, H2SO4, CH3COOH
were prepared in the usual way from the
concentrated solutions . A10g quantity of
strong cationic exchange resin in the H+-
form, Amberlite XAD-16, was weighed,
placed in water, left overnight to swel and
was finally packed into a column.
141
Apparatus
A.A.spectrophotometer WFX-120
(BRAIC) was used. All absorption
measurements were performed under the
following operating conditions:
wavelenghth: 217.0nm ; slit setting138
0.2nm; lamp current :4mA; PMT
voltage:5 71 V, burner height: 8mm, flow
rate air/fuel: 5/3 L.min-.
General procedures
a) Sampling of Water
One liter of drinking water from the
sources of sulaimani city were taken. They
were seven wells, seven springs, sarchnar
project and tap water, taken directly and
after turning on the tap water for 20
minutes. The location of places have been
marked on the map of sulaimani showing
in Fig(1) which was obtained from the
Municipality of Sulaimani.
b)Sampling of Air
A home-made system for air sampling
was designed for withdrawing air through
an absorbent and trapping different forms
of lead in an absorbent. A refrigerator
compressor was used to pull air through 2-
3 traps containing the absorbent connected
in series as shown in Fig (2). Sampling of
air was continued for two hours, at a
measured rate. The trapped lead solutions
were transferred to the laboratory,
preconcentrated on the ion exchanger
column. A 500ml quantity of the air
trapped solutions or 500ml of water
samples were preconcentrated by passing it
through a coulumn containing Amberlite
resin XAD-16 and eluted using 10ml of
4M HCl. The enriched solution of lead was
determined by atomic absorption
spectrometer.
(KAJ) Kurdistan Academicians Journal, March 2006 , 4(1) part A
A ‫) بةشى‬1( ‫ ذ‬4 ‫بةرط‬, 2006 ‫ ئازارى‬2706 ‫طؤظارى ئةكاديميانى كوردستان نةوروزى‬

c) Producing lead vapor in a home- constructed in one cubic meter (1 m3),

made chamber
To study a suitable absorbent, a home
made chamber was constructed to provide
a sufficient amount of lead vapor. For this
purpose a chamber of maglone was
in which 5Kg of lead sheet (purchased
locally in Sulaimani market)
was melted and gently boiled inside the
chamber. This made the study of
absorbents and other parameters ea.

Figure 2: series of impingers (bubblers)

:

Study of Interferences:
The cations having close spectral lines
to the selected line of lead and others
Fig. 1: . The Sampling Sites in Sulimani City.

139 including Sn, Mn ,Sb,Cd,Al,Ca,Ni, Fe, Zn

and the anions NO3, SO42-,CO32- and PO43-
were studied for their interferences.This
was done by adding successive amounts
of the interferent until it became five fold
relative to Pb.

141
 0.08
0.06

A.A
y
0.04
(KAJ) Kurdistan Academicians Journal, March 20060.02
, 4(1) part A
A ‫) بةشى‬1( ‫ ذ‬4 ‫بةرط‬, 2006 ‫ ئازارى‬2706 ‫طؤظارى ئةكاديميانى كوردستان نةوروزى‬
0
228 260 300 350 480 600
Results and Discussion flow rate m l/m in
Choice of the Absorbent Figure 3 :choosing the best flow rate for
Different absorbents were tested using air sampling
impinger systems, based either on the
complexation of the analyte with the Absorbents Concentrations
absorbent, or on its solubility in the Fig(4) shows the results of using
medium[3]. Most of common acids were different concentrations of HClO4. It is
tested as absorbents, including ( HNO3, indicated that 0.5M HClO4 is the
CH3COOH, H2SO4,HCl, CH3COONa and optimum. Furthermore, to show the
HClO4) at 0.5M concentration. Air in the absorption capacity of the acid, more
chamber was sampled for two hours at a extensive production of lead vapor in the
medium and nearly constant flow rate. chamber was performed.
Lead in these solutions was measured by
A.A against a calibration curve. 0.4 The
results are shown in table ( 1 ). The table
0.3
A 0.4

indicates that HClO4 is the best absorbent

0.2
0.3

0.2
among the other acids tested. 0.1
0.1
Table 1: Evaluation of absorbents for 0
1 2 3 4 5 6
trapping lead from air ( without preconcentration).
0
concentration mol/L
1 2 3 4 5 6

Effect of flow rate concentration mol/L

Different flow rates of air sampling

Fig4 The role of the concentration of
(200, 260, 300, 350, 480, and 600) ml/min
HClO4 on its absorbing ability of
were tested for the same period of time
lead
(2Hrs.). It was observed from the
experimental data, shown in Fig.(3) that Flow rate stability
the flow rate of 300ml/min was the best, The variation of flow rate during
and was used for the rest
y
of the work. working of the compressor was tested.
0.1 This was done at the minimum and
0.08 140 maximum flow rates. Furthermore the
A 0.06
pump was stopping at the middle of
A.A

y
0.04
0.02
sampling for 15 minutes (for the safety of
0
the pump) and restarting again. The
228 260 300 350 480 600 results shown in Fig (5) indicate that
Absorbents A.Arate m l/m in RSD%
flow

H3PO4 0.0075 3.24

working of the air compressor was
CH3COOH 0.0053 7.6
sufficiently constant for 2 hours and its
HClO4 0.0145 0.07 stability was satisfactory.
Cl 0.006 0.76 700

HNO3 0.0118 3.13 600

H2SO4 0.0111 1.06 500

CH3COONa 0.008 0.9

flow rate ml/min

70 400
60

50 300
40

30 200
flow rate ml/min

20

10 100

141
0
1.0 2.0 3.0 4.0 5.0 6.0 7.0 8.0 9.0
0
minutes
1.00 2.00 3.00 4.00 5.00 6.00 7.00 8.00 9.00
minutes
(KAJ) Kurdistan Academicians Journal, March 2006 , 4(1) part A
A ‫) بةشى‬1( ‫ ذ‬4 ‫بةرط‬, 2006 ‫ ئازارى‬2706 ‫طؤظارى ئةكاديميانى كوردستان نةوروزى‬

preconcentration, and the results are

shown in table ( 2 ). It is obvious that the
preconcentration has improved the
absorbance measurement.

Study of Interferences:
Although atomic absorption is known
to be almost free from interferences, but
this was studied for those metals of close
f low rate ml/min

700

600

500

400

300

200

100

0
1.00 2.00 3.00 4.00 5.00 6.00 7.00 8.00 9.00

spectral lines to 217 line of Pb such as Sb

minut es

Figure 5: The stability of the air and Cu and others including Sn,Fe, Ni, Al,
compressor during the air sampling at the Zn, Ca, Cd. The results showed that non
minimum flow rate, ○ before stopping, of these ions have any interference until
∆ after restarting and at the maximum five fold that of Pb.
flow rate ■ before and after restarting.

Table2: Effect of preconcentration on lead determination

samples A.A before pre- RSD A.A after RSD%

concentration % preconcentration
City center 0.008 22 0.112 1.82
Sarkarez 0.005 14 0.095 3.37
Bakhtyari 0.004 17 0.108 4.6
Twimalik 0.007 3.5 0.135 0.09
Khanakha 0.008 3.9 0.129 3.58
Preconcentration of lead ion
Preconcentration of Lead ion
According to the literature the calibration curve y = 0.0873 x + 0.0683
R2 = 0.9905
concentration of lead in the ambient air is
1
extremely low, in the range of few
0.8
nanograms per cubic meter. In such cases,
enrichment step would be necessary A 0.6
0.4
before analysis. Preconcentration of lead
0.2
was performed in combination with
0
different techniques [13-16]
0 2 4 6 8 10 12
Although Amberlite resin is not very mg / L pb 2 +
selective for exchanging lead, the Figure 6: Calibration curve
selectivity of atomic absorption made the
method reliable since non of the ions Calibration Curve
present in air sample could interfere. The Under the condition given in the
measurements were taken before and after experimental part, the calibration curve

141
(KAJ) Kurdistan Academicians Journal, March 2006 , 4(1) part A
A ‫) بةشى‬1( ‫ ذ‬4 ‫بةرط‬, 2006 ‫ ئازارى‬2706 ‫طؤظارى ئةكاديميانى كوردستان نةوروزى‬

was obtained as shown in Fig(6) with If an average concentration of Pb in air

reasonable linearity (r2=0.991)
Determination of lead in the ambient
air of Sulaimani City
Samples of air were taken in five
different regions in Sulaimani area, from
south, west, east west and the center,
taking into our consideration crowded
places with enormous cars and vehicles.
It was observed, as shown in table
(3)that the amount of lead were under the
standard tolerance limit for lead in air
(1.5g/m3)[1] according to the National
Ambient Air Quality Standards (NAAQS).
Concentration of lead in air depends
on a number of factors, including
proximity to heavy traffic and point
sources. Annual geometric concentrations
measured at more than 100 stations across
Canada declined steadily from 0.74 µg/m3
in 1973 to 0.1µg/m3 in 1989, reflecting the
decrease in the use of lead additives in
petrol.
of 0.2µg/m3 is assumed, the intake of lead
from air can be calculated to range from
0.5µg/day for an infant to 4µg/day for an
adult [8].
From these data we conclude that the
air of Sulaimani city is not polluted by
lead.
Determination of lead in drinking water
Table (4) shows the results of different
sources of drinking water which were
tested, and each location is pointed in the
map Fig (1). The table again indicates that
level of Pb in drinking water of sulaimani
sources are within the tolerance given by
NAAQS.
Conclusion
It is obvious from the experimental
data that both air and water of Sulaimani
are pure as far as pollution by lead is
concerned, because they are within the
permission range according to
(NAAQS)which is (50µg/L).

Table (3): Determination of lead in air at different places Sulaimani city.

Places µg/m3 pb RSD%
City cnter(mzgawti
gawra) 0.37 3.58
Sarkarez 0.1 4.04
Bakhtyari 0.03 1.82
Twimalik 0.08 3.9
Khanakha 0.25 0.09

Table (4) Analysis of drinking water in different sources in Sulaimani city

142
Places
Temperature pH µg/Lpb
Bakhtyari(well)
10.5 7.5 5.1
Azadi1 (well) 9.5 7.8 8.4

141
 (KAJ) Kurdistan Academicians Journal, March 2006 , 4(1) part A
A ‫) بةشى‬1( ‫ ذ‬4 ‫بةرط‬, 2006 ‫ ئازارى‬2706 ‫طؤظارى ئةكاديميانى كوردستان نةوروزى‬

Azadi 2 (well)
10.5 7.6 4.6
Azadi 3(well)
11 7.7 4.5
Ardalan (well) 9.5 7.8 3.3
Kadamkher(well) 10.0 7.9 4.15
Grdi sarchnar(well) 10.2 7.34 4.5

Aziz agha
11 7.4 4.2
(spring)(207)*
Majid bag(spring)(209)
10.5 7.6 4.4
Shex mahmud
10.5 7.4 3.0
(spring)(211s)
Daiki pasha
10.3 7.8 4.0
(spring)(304)
Haji bag(spring)(212)
11 7.8 2.1
Mamayara(spring)(305s)
9.8 7.9 2.0
Mawlana(spring)(407s)
9.7 7.8 3.0

Bachtyari(tap-directly) 9 7.7 28.0

Bachtyari(tap-after 20 min) 9.5 7.7 18.5
Twimalik(tap-directly) 9.0 7.4 14.0
Twimalik(tap-after 20
9.5 7.45 9.0
min)

Sarchnar project 9.0 7.0 3.0

* Sample site positions indicated on the map.

References
1) Manahan S.h.. “ Environmental chemistry”, 6th ed.1994 chapt 7,CRC press
1st ed.1979, chapt 1, academic press.
2) Butler J.D. “ Air pollution chemistry”;143
3) Wang H.j., He F. and Jiang C.Q.; Analyst, 2001, 126, 1164-1167
4) Kebbekus B.B., Mitra S.; “ Environmental Chemical Analysis” 1st ed.1998, 209

141
(KAJ) Kurdistan Academicians Journal, March 2006 , 4(1) part A
A ‫) بةشى‬1( ‫ ذ‬4 ‫بةرط‬, 2006 ‫ ئازارى‬2706 ‫طؤظارى ئةكاديميانى كوردستان نةوروزى‬

5) Rodriguez D., Fernandez P., perec-conde C., Guatierez A. and Camara C.;
Fresenius’s journal of analytical chemistry, 1994,344,6, 442-446
6) Sun H., Yang Li-Li, Zhang D.g., Wang W.X. and Sun J.M.; Fersenius’s journal of
Analytical chemistry; 1997,358,5, 646-651
7) Barrera P.B., Pineiro A.M., Pineiro J.M. and Barrera A.B.; J.Anal.At.Spectrum,
1997,12,3, 301-306
8) Guidelines for drinking water quality, volume 2, WHO, Geneva, 1996
9) Sherlock JC, Quinn MJ; Food additives and Contamination, 1986,3,167-176
10) Anezaki K., Chen X. Ogasawara,T., Nukatsuka I. and Ohzeki k.; Analytical
Science, 1998, 14,523-527
11) Seki T., Hirano Y. and Oguma K.; Analytical Science,2002, 18, 351-354
12) Sato H. and Ueda J.; AnalyticalScience 2001,17,461-463
13) Tahir M.A.; Croatica Chemica Acta CCACCA, 2003,76,(3) 273-277
14) Rodriguez D., Fernandez P., Perez-Conde C., Gutierrez A. and Camara C.;
Fresenius’s journal of Analytical Chemistry 1994, 349,6, 442-446
15) Saracogul S., Divirikil U., Soylak M. and Elci L.; J. Food Drug Anal, 2002,
10.3, 188-194
16) Wuilloud R.G., Acevedo H.A., Vazq uez F.A. and Martinez D.D.; Analytical
letters, 2002,35(10), , 1649-1665.

‫دياريكردنى رِيَذةى قورِقشم لة ئاو وهةواى ناوضةيىى بة ِريَطةى‬

‫بلَيَسة ثاش فرةكردنى ثةيتى‬
144
‫سثيَكتراى مذينى ئةتؤمى ناو‬

141
‫‪(KAJ) Kurdistan Academicians Journal, March 2006 , 4(1) part A‬‬
‫طؤظارى ئةكاديميانى كوردستان نةوروزى ‪ 2706‬ئازارى ‪, 2006‬بةرط ‪ 4‬ذ (‪ )1‬بةشى ‪A‬‬

‫فاضل محةمةد نةجيب ‪ ،‬خاليد محةمةد عومةر ‪ ،‬ئوميَد ئيسماعيل‬

‫حةيدةر‬

‫بةشى كيميا ‪ ،‬كؤليَذى زانست ‪ ،‬زانكؤى سليَمانى ‪ ،‬هةريَمى كوردستان ‪ ،‬عيَراق‬

‫ثوختة‬
‫كةمة برِى(‪ ) trace amount‬قورِقوشم لة ئاو و هةواى ناوضةيىى شارى سليَمانيدا دياريكرا ‪،‬‬
‫نمونةى هةوا بسة يارمةتسى ثةمثي َسكى هةوا مسذ برا بسؤ ناو سسيستةميَكى لة تاقيطسة دروسستكراو (‬
‫‪ ) bubbler‬بسة مسة بةسستى هةلَمذينسى قورِقوشسم و ثيَكهاتووةكانسى ترى لة هةوادا بسة خيَرايسى‬
‫‪ 300‬مسل ‪/‬خولةك بسؤ ناو طيراوةى ‪ 0.5‬مؤلر لة ترشسى ثةر كلؤريسك كسة باشتريسن مذةرة بسؤ‬
‫طرتنسسى قورِقوشسسم و ثيَكهاتوةكانسسى ترى بسسؤ ماوةى دوو كاذي َسسر‪ .‬نمونةى ئاو لة ضةنسسد‬
‫ى (‪ )Ion Exhcnage Resin‬لة جؤرى‬ ‫شويَني َ سكى جياواز لة شار وةرطيرا‪ .‬رِيزنسسى ئايؤن طؤرِك َ‬
‫‪ XAD-16‬بةكارهيَنرا بةمةبةستى فرةكردنى ثةيتى قورِقوشم بؤ ئاستيَكى هةستثيَكراو ثاشان‬
‫دؤزينةوةى رِيَذةكةى بسة تةكنيكسى سسثيَكتراى ( شةبةنطسى) مذينسى ئةتؤمسى ناو بلي َسسة وة‬
‫ئةنجامسسسسة ثراكتيكيةكان دةريانخسسسسست كسسسسة رِيَذةى قورِقوشسسسسم لة هةواو لة ئاودا لة شارى‬
‫سسسليَمانى لة ئاسسستيَكى مةترسسسيداردا نيسسة كسسة بةرزتريسسن رِيَذة لة هةوادا ‪ 0.4µg/m3‬لةكاتيَكدا‬
‫تؤليرانسسسس ليظلى ( بةرزتريسسسن ئاسسسستى رِيَثيَدان ) قورِقشسسسم لة هةوادا بةثىَى سسسستانداردى‬
‫نيَودةولَةتسسى ‪ 1.5µg/m3‬بسسة لم بسسؤ ئاو بةرزتريسسن رِيَذة ‪ 28µg/L‬بوو لة كاتيَكدا تؤليرانسسسى‬
‫قورِقشسسسم لة ئاودا ‪ .50µg/L‬دةرةنجامسسسى كارةكان دةركةوت كسسسة رِي ُسسسطا ثيَشنيازكراوةكسسسة‬
‫ئةطونجيَت بؤ ليَكؤلَينةوةى ذينطةيىى بةمةبةستى خةملندنى قورِقشم لة هةوا و لة ئاودا‪.‬‬

‫تقدير كميات ضئيلة من أيون الرصاص فى الهواء والماء بطريقة‬

‫ألمتصاص الذرى اللهيبى بعد ازدياد التركيز‬
‫فاضل محمد نجيب ‪ ،‬خالد محمد عمر ‪ ،‬اوميد أسماعيل حيدر‬
‫قسم الكمياء‪ ،‬كلية العلوم ‪ ،‬جامعة السليمانية ‪ ،‬أقليم كردستان ‪ ،‬العراق‬
‫ألخلصة‬
‫تمت تقدير ايون الرصاص و مركباتها فى الهواء و الماء فى مدينة السليمانية ‪ .‬سحبت‬
‫نماذج الهواء من قبل مجموعة متوالية من ( ببلر) والذى صنعت مختبريا و بسرعة ‪ 300‬مل‬
‫‪/‬دقيقة الى ‪ 0.5‬مولر من حامض البركلوريك ولمدة ساعتين وذلك لمتصاص الرصاص و‬
‫مركباتها ‪ .‬بينما نماذج الماء اخذت من مصادر مختلفة من مدينة السليمانية ‪ .‬أستخدمت‬
‫راتنج التبادل اليونى من نوع ‪ XAD-16‬لزدياد التركيز الرصاص الى حد التقدير و من ثم تم‬
‫تقديرها بواسطة المطيافية المتصاص الذرى الهيبى‪ .‬و بينت النتائج التجريبية ان كمية‬
‫الرصاص فى الهواء واالماء كانتا في حديهما القصوى ‪ 0.4µg/m3‬و ‪ 28µg/L‬بينما الحد‬
‫المسموح يجب ان لتتعدى ‪ 1.5µg/m3‬و ‪ 50µg/L‬لكل من الماء و الهواء ‪ .‬و من النتائج‬
‫بينت ان الطريقة المقترحة مناسبة تماما لتقدير ايون الرصاص فى النماذج البيئية ‪.‬‬

‫‪Received on 2/6/2004 Accepted on 14/3/2005‬‬

‫وةرطيراوة لة ‪ ،2/6/2004‬ثةسندكراوة لة ‪14/3/2005‬‬

‫‪145‬‬

‫‪141‬‬

‫‪145‬‬