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(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samples of air were withdrawn at a rate of 300ml.min- through homemade impinger systems into 0.5M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 µg/L lead, although higher values have
toxic metals and noted in the field of been reported [8-10]. Lead in water
environmental chemistry[1]. The intake of supply may come from industrial, mine
lead by the body comes from lead in food, and smelter discharges or from the
water and air[2]. According to the dissolution of old lead plumbing.PVC
stipulation of the center for Disease pipes also contain lead compounds that can
Control (USA) and the department of be leached from them and result in high
Health (UK), typically, levels of lead in lead concentrations in drinking water. The
blood of children are of the order of 100µ amount of lead dissolved from the
g/L [3].The sources of air pollution may be plumbing system depends on several
divided into two types, namely mobile and factors, including the presence of chloride
stationary sources. Mobile sources are and dissolved oxygen, pH, temperature,
those related to transportation such as water hardness and standing time of the
automobiles, trains, airplanes, while water, soft, acidic water being the most
stationary sources include pipelines, highly plumbosolvent.[ 8 ]
factories, and storage tanks [4]. Lead has In Glasgow (Scotland), where the water
been determined in tap, river and sea water was known to be plumbosolvent, the lead
by different methods in the literature [5-7]. 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

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

141
(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 in which 5Kg of lead sheet (purchased
To study a suitable absorbent, a home locally in Sulaimani market)
made chamber was constructed to provide was melted and gently boiled inside the
a sufficient amount of lead vapor. For this chamber. This made the study of
purpose a chamber of maglone was 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) of 0.2µg/m3 is assumed, the intake of lead
Determination of lead in the ambient from air can be calculated to range from
air of Sulaimani City 0.5µg/day for an infant to 4µg/day for an
Samples of air were taken in five adult [8].
different regions in Sulaimani area, from From these data we conclude that the
south, west, east west and the center, air of Sulaimani city is not polluted by
taking into our consideration crowded lead.
places with enormous cars and vehicles.
It was observed, as shown in table Determination of lead in drinking water
(3)that the amount of lead were under the Table (4) shows the results of different
standard tolerance limit for lead in air sources of drinking water which were
(1.5g/m3)[1] according to the National tested, and each location is pointed in the
Ambient Air Quality Standards (NAAQS). map Fig (1). The table again indicates that
Concentration of lead in air depends level of Pb in drinking water of sulaimani
on a number of factors, including sources are within the tolerance given by
proximity to heavy traffic and point NAAQS.
sources. Annual geometric concentrations
measured at more than 100 stations across Conclusion
Canada declined steadily from 0.74 µg/m3 It is obvious from the experimental
in 1973 to 0.1µg/m3 in 1989, reflecting the data that both air and water of Sulaimani
decrease in the use of lead additives in are pure as far as pollution by lead is
petrol. 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