Evaluation of the concentration of chemical elements in suspended particulate matter inside a small bronze and iron foundry industry, using a streaker sampler and EDXRF

Research article

Received: 18 February 2013 Accepted: 25 June 2013 Published online in Wiley Online Library: 10 September 2013

(wileyonlinelibrary.com) DOI 10.1002/xrs.2509

Evaluation of the concentration of chemicalelements in suspended particulate matterinside a small bronze and iron foundryindustry, using a streaker sampler and EDXRFPaulo Rogério Massoni,a Eduardo de Almeida,a

José Eduardo Delfini Cançadob and Virgílio Franco do Nascimento Filhoa*

The aim of this study was to determine and evaluate the temporal profiles of the concentration of chemical elements in thesuspended particulate matter present inside a small bronze and an iron foundry industry. To collect the samples, we used astreaker sampler that separates particles with aerodynamic diameters smaller than 10μm (PM10) in two fractions: fine(particles with aerodynamic diameters less than 2.5μm; PM2.5) and coarse (between 2.5μm and less than 10μm; PM10–2.5).The collection of samples was taken every 20min during a total time of 8 and 5h of molding and casting of bronze and iron,respectively. The samples collected in the form of strips on a filter (fine fraction) and an impactor (coarse fraction) wereanalyzed by the energy dispersive X-ray fluorescence technique. In the excitation, an X-ray tube with Mo target and Zr filterwas used, operated at 30mA/30 kV. For detecting the characteristic of X-rays, a semiconductor Si(Li) detector was used,coupled to a multi-channel spectrometer, with a 300 s excitation/detection time. The results of the temporal profiles of chem-ical element concentrations in coarse and fine fractions were discussed and compared with the maximum levels set by the Bra-zilian and international environmental agencies. Copyright © 2013 John Wiley & Sons, Ltd.

* Correspondence to: Virgílio Franco do Nascimento Filho, Laboratório deInstrumentação Nuclear (LIN) – Centro de Energia Nuclear na Agricultura(CENA), Universidade de São Paulo (USP), avenida Centenário, no. 303, CEP13.400-970, Piracicaba, São Paulo State, Brazil. E-mail: [email protected]

a Laboratório de Instrumentação Nuclear (LIN) – Centro de Energia Nuclear naAgricultura (CENA), Universidade de São Paulo (USP), avenida Centenário,no. 303, CEP 13.400-970, Piracicaba, São Paulo State, Brazil

b Laboratório de Poluição Atmosférica Experimental (LPAE) – Faculdade deMedicina (FM), Universidade de São Paulo (USP), avenida Dr. Arnaldo, no.455, CEP 01246-903, São Paulo, São Paulo State, Brazil

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Introduction

In the small foundry industries, workers spend most of theirdaily work without the use of appropriate respiratoryprotective equipment and supervision concerning workingconditions (Figure 1). In these places, potentially toxicelements such as Cr, Mn, Ni, Zn, and Pb, in high concentra-tions can cause damage to health by affecting the neuro-logical and immunological systems, and some of theseelements can also be extremely dangerous due to theircarcinogenic properties.[1–4]

Thus, it is necessary to monitor the quantity and qualityof suspended particulate matter (SPM), which can containhigh concentrations of these elements and thus have a hightoxicity[5]. Workers are subjected to inhalation of particleswith diameters smaller than 10 μm (PM10) in fine or respira-ble fractions (aerodynamic diameters smaller than 2.5 μm;PM2.5) and coarse (diameters between 2.5 μm and less than10 μm; PM10–2.5), affecting the tracheobronchial and alveolarregions, respectively.[2]

Therefore, the objective of this study was to determine thequality and quantity of chemicals present in fine and coarseSPM fractions and to identify the critical moments of toxicity inthis industrial activity. For this type of study, the energydispersive X-ray fluorescence (EDXRF) technique `was employedbecause it is non-destructive and multi-element, together withthe use of a rotary collector that has been used in environmentalpollution studies,[3,5–11] and has great potential for application instudies of pollution in industrial environments.

X-Ray Spectrom. 2013, 42, 493–501

Materials and methods

Sampling location, streaker sampler, and sample collection

The industry of bronze casting and iron is small (15 employees),with a monthly production of 15 t of each metal and is locatedin Piracicaba city, São Paulo State, Southeast Brazil. The mostoften used bronze is SAE 40, ASTM 83 600, or copper alloyBZ 85.5.5–5 (USA) CB 20, with the following composition:Cu = 84–86%, Sn = 4.3-6.0%, Pb = 4.6%, Zn = 4.6%, Fe = 0.25%(maximum), Ni = 0.80% (maximum), and trace Mn and Al = 0.05%.The ingot iron has the following composition: Si = 2.16%,Mn = 0.078%, P = 0.07%, S = 0.014%, C = 4.06% and theremainder is Fe.

The collection of samples in the smelting and casting bronze(700 kg) was carried out for 8 h (08:30 h to 16:30 h) and iron(600 kg) for 5 h (12:40 h to 17:40 h) by using a streaker aerosol

Copyright © 2013 John Wiley & Sons, Ltd.

Figure 1. Workers filling the molds with molten material (bronze), wherea high concentration of toxic elements is probably obvious in the fumesand where most of them are without nose guards.

Air inlet

1

2 4 3

Figure 2. Installation diagram of (1) streaker aerosol sampler coupled to(2) gauge volume, (3) flowmeter, and (4) vacuum pump that sucks tocollect the suspended particulate matter.

P. R. Massoni et al.

494

sampler, manufactured by PIXE International Corp (Tallahassee,Florida).[12], model S2P, programmed to collect samples every20min. This sampler, connected to a vacuum pump, flow meter,and volume meter (Figure 2) was positioned 15m from the site offusion of raw material and molding at a height of 3m above theground (Figure 3).

streaker sampler

air volume meter (m3)

Figure 3. Aerosol streaker sampler installed within the sampling site, showinpling site.

wileyonlinelibrary.com/journal/xrs Copyright © 2013 Jo

At the entrance of the sampler is a pre-impactor that traps theparticles with aerodynamic diameters equal to or greater than10μm. Then the particles of coarse fraction (PM10-2.5) are depos-ited by impact in a Kapton membrane (SF - 1 K) coated with a thinlayer of an adhesive fluid (4% paraffin in toluene) placed on aplastic disk (the impactor), while the fine fraction (PM2.5) followsthe center hole of the collector and it is filtered by a polycarbonatemembrane, manufactured by Nuclepore (GE Healthcare Life Sciences,Piscataway, NJ 08854 USA) (SF-1N4, polycarbonate track-etchedmembrane) with 0.4μm in pore size. Both membranes are 82mmin diameter. Thus, the coarse particles are deposited by impact,forming rectangular strips of 3×0.4mm, whereas the fine particlesdeposited by filtering forming an 8×2mm strips (Figures 4 and 5).

Sample irradiation

After the collection of airborne particulate matter in the industry,the filter and the impactor are disengaged from the streakerinside and placed, one at a time, in an acrylic holder mountedin the detector head (Figure 6) to perform quantitative analysisby EDXRF technique.

For excitation, a 17.44 keV monoenergetic beam from an X-raytube with Mo target and Zr filter was used, operated at 30mA/30 kV. For the characteristic X-ray detection, a Si(Li) high resolu-tion semiconductor detector was used, coupled to a conventionalmulti-channel analyzer, with 300 s counting time per sample.

Because of the small area of deposition of particles in the filterand impactor (Figure 5), it was necessary to collimate the X-raybeam from the tube, with consequent reduction in the intensityof the initial beam. For this purpose, a silver-coated brass collima-tor (72mm long, 10mm in diameter at the entrance slit, andrectangular 5 × 0.5mm at the exit) was built[7,13] instead of usinga costly mono or polycapillary focusing X-ray optics.[6,11]

With this geometry of excitation/detection, it was possible tomeasure the intensity of characteristic X-rays of the elementscontained in the samples for later determination of the concen-tration of elements present in the atmosphere of the casting ateach 20min time interval. The interpretation of X-ray spectrawas carried out using the AXIL software,[14] developed at theUniversity of Antwerp, Belgium. As an illustration, Figure 7 showsthe X-ray spectra from fine – PM2.5 and coarse – PM10-2.5 fractionsamples collected from 15:50 h to 16:10 h, during the moldingbronze. There are high peaks of Pb and Zn in both the PM2.5

and PM10-2.5.

flow meter (liters/min)

vacuumpump

g the sucked-air volume meter, flow meter, and vacuum pump at the sam-

hn Wiley & Sons, Ltd. X-Ray Spectrom. 2013, 42, 493–501

Figure 4. Schematic of the streaker sampler, showing the impactor and filter receiving the coarse (PM10–2.5) and fine (PM2.5) suspended atmosphericparticulate matters.

Figure 5. Impactor for collection of coarse particles (SF-1 K, left) and filter for the fine (SF-1N4, right) particles.

Figure 6. Streaker sampler disassembled (left), showing the filter tocollect fine particulate and the Lucite support for sample analysis byenergy dispersive X-ray fluorescence (in front), and the filter in the Luciteholder on the top of Si(Li) X-ray detector (right), positioned in front of thebrass collimator (adapted at the exit of X-ray tube with Mo target).

Chemical composition of aerosol in a small metal foundry

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Quantitative analysis

When the excitement of the samples is monoenergetic, one canuse a mathematical expression that relates the characteristic X-rayintensity with the concentration of a particular element in thefollowing sample:[15]

Ii ¼ Si:ci:f i (1)

X-Ray Spectrom. 2013, 42, 493–501 Copyright © 2013 John W

where Ii represents the intensity of characteristic X-rays detected(cps); Si is the analytical sensitivity of Si X-ray spectrometer(cps μg�1 cm�2); ci is the concentration or superficial densityof the element of interest i in the sample (μg cm�2); and fi is theabsorption factor (dimensionless) for the characteristic X-rays emit-ted by the element of interest in the sample, which has a value of 1in the case such as these when the samples are considered thin(airborne particulate matter deposited on filters).

By means of equation 1, it was possible to verify the concentra-tion of elements present in the sample (in μg cm�2) by determin-ing in advance the elemental sensitivities Si (cpsμg

�1 cm2) withthe help of the certified standard samples. Knowing the concen-tration of elements, the volume of sucked air and the depositionarea of the SPM samples, the concentration of the elements ofinterest in the sample in units of mass per unit volume of suckedair could be determined by the following:

Ci ¼ ci:Ai=Vi (2)

where Ci represents the concentration of airborne particles in theair in units of mass of the element of interest per unit volume ofair (μgm�3), ci is the concentration defined in equation 1, Ai is thearea of deposition of particulate matter in the filter (cm2), and Viis the volume of sucked air (m3).

Limit of detection

The limit of detection LDi for each element i is in direct propor-tion to the continuum or background BGi intensity (cps) under

iley & Sons, Ltd. wileyonlinelibrary.com/journal/xrs

Figure 7. Spectra of the characteristic X-rays emitted by elements in fine(PM2.5) and coarse (PM10–2.5) airborne particles of the sample collectedfrom 15h:50min to 16 h:10min, during the molding process of bronze(the black areas refers to the blank and the Ar peak refers to air argon).


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the peak of that element and in inverse elemental analyticalsensitivity Si (cps μg�1 cm2) according to the equationproposed by van Grieken & Markowics.[16] This equation,together with the ratio between the area Ai of the sampleand the volume of sucked air Vi for this sample, provides thedetection limit in μgm�3:

Elementalanalyticalsensitivity

Si(cps.µg-1.cm2)

Si = 6.288.10-3

Figure 8. Elemental analytical sensitivity Si versus atomic number Z for thMicroMatter/USA.


LDi ¼ 3

Si:

ffiffiffiffiffiffiffiffiBGi

t

r:A

V(3)

where t (s) is the excitation/detection time for the sample.

Elemental analytical sensitivity

The determination of elemental analytical sensitivities wascarried out using certified standard samples, produced by theMicroMatter/USA, containing the known concentrations of K,Ca, Sc, Ti, Mn, Fe, Cu, Zn, and Pb, which were irradiated in thesame geometry of the samples. With the characteristic X-rayintensity of each element contained in these certified standardsamples, the elemental sensitivities were calculated fromequation 1 and subsequently a graph of sensitivity versus atomicnumber was formulated. All elements were evaluated by the KαX-rays, except Pb, which was determined by the Lα X-ray.

Certified standard samples used in validation

To validate the methodology used, it was measured the concentra-tion of elements present in certified standard samples, producedby the National Institute of Standards and Technology - NIST,USA, deposited in cellulose ester membrane, whose certificationcode is SRM 1832 – serial number 227 and SRM 1833 – serialnumber 1062.

Results

Elemental analytical sensitivity and limit of detection

From the curve of the elemental analytical sensitivity of the spec-trometer versus atomic number (Figure 8), it was possible to esti-mate the sensitivity for other elements not available as standardin the laboratory, such as V, Cr, Co, and Ni.

With the estimated values for the analytical sensitivity of theelements, the area of background under the peak of interest,the sucked air volume and the deposition area, the limit of detec-tion of the system for each element of interest (equation 3)contained in the fine and coarse particulate samples were calcu-lated and the values are shown in Table 1.

Zi3- 0.2249.Zi

2+2.2554.Zi - 3.884R2 = 0.9997

e Kα X-rays obtained with the certified standard samples produced by


Table 1. Limit of detection for elements of interest present in thesamples of fine (PM2.5) and coarse (PM10–2.5) suspended particulatematter determined by the Kα characteristic X-rays, except for Pb thatwas determined by the Lα X-ray

Limit of detection (LD, ngm�3)

Element Fine (PM2.5) Coarse (PM10–2.5)

19 K 692.0 57.5

20Ca 382.3 32.0

21Sc 252.8 21.7

22Ti 158.0 14.0

23 V 115.0 9.5

24Cr 83.5 8.2

25Mn 62.5 6.4

26Fe 44.0 3.6

27Co 40.8 3.5

28Ni 32.0 3.4

29Cu 28.1 2.9

30Zn 23.7 2.5

82Pb 54.1 5.8


Certified standard samples

Table 2 compares the values certified by the manufacturer of thesample with their respective CIs and measured values. The resultsare quite consistent, validating the proposed methodology.

Concentration of elements in the SPM and the criticalmoment of casting

Figures 9 and 10 show the changes in concentrations of severalelements in the fine (PM2.5) and coarse (PM10�2.5) fractionsduring smelting and casting of bronze and iron, which startedat 8:30 h and 12:40 h, respectively, with 8 and 5 h to finish. Itwas found that the most critical moment was during the mold-ings (15:30 h to 15:50 h for bronze and 16:40 h to 17:00 h for iron),in which there were high concentrations of potentially toxicelements such as Cr, Mn, Ni, Cu, Zn, and Pb mainly in the finefraction. It is noteworthy that during the molding of bronze andiron, there were peaks of Pb in PM2.5 concentrations reaching42 600 and 57 000 ngm�3, respectively.

Although some elements present sharp peaks of concentration,from the concentration and volume collected in each sample every20min, the mean values in fine and coarse were calculated duringthe 8 and 5h of molding and casting processes of bronze and iron.

Table 2. The concentration of the certified standard samples producedcompared with those measured experimentally

SRM 1832

Element Certification Uncertainty This work

μg cm�2 μg cm�2 μg cm�2

22Ca 19.98 1.343 20.70

23 V 4.53 0.504 4.27

24Mn 4.53 0.504 4.55

27Co 0.99 0.067 1.01

29Cu 2.52 0.168 2.44


With the average values of these two fractions, the average totalSPM (PM10=PM10-2.5 + PM2.5) was calculated.

With reference to Pb, a potentially toxic element for humanhealth even at low concentrations, the average value obtainedfor the bronze in the PM2.5 was 1870 and in the PM10, 2190 ngm�3. For iron, the values were 17 150 and 17 230 ngm�3. Bothare over 500 ngm�3, the maximum allowed in the SPM of aero-dynamic diameters less than 100μm [total suspended particles(TSP)] by the World Health Organization. Furthermore, this maxi-mum value is a quarterly average, which should not be exceededmore than one time per year.[17] Even an average of the 24 h isassumed, the values found for the fine and coarse fractions were623 and 730 ng.m�3 for the bronze, respectively, and 3430 and3446 ngm�3 for iron, well above the limits allowed.

The average values for the concentration of some elements inthe fine and coarse fractions and the total for the period of 8 and5 h for the bronze and iron were higher than the values of con-centration of inorganic, non-carcinogenic, and carcinogenic airpollutants, adopted by the Brazilian National Health Foundation– Fundação Nacional de Saúde.[1] Tables 3 and 4 show Cr, Mn,and Ni, for the bronze and iron, respectively.

Similarly, the total concentration of elements present in thePM10 and PM2.5 in the bronze foundry also showed almost 50%of the concentration limits set by the United States Environmen-tal Protection Agency,[18] i.e. 15 and 50 ngm�3. Table 5 showsthat in the smelting and casting of iron, the values estimatedwere quite high, mainly in the fine fraction, where almost allthe suspended particles were found.

The concentration limit established by the Brazilian NationalCouncil for the Environment – Conselho Nacional do MeioAmbiente [1] for the TSP (considering all the elements – particlesranging in size less than 100μm composed of liquid or solidmaterial in the form of dust, mist, aerosol, smoke, soot, etc.) is60μgm�3. The sum of all elements measured was 24μgm�3

for bronze and 67μgm�3 for casting iron, results that are quiteworrisome, because the comparison was made between TSPand particles smaller than 10μm.

The average concentration of Fe in the smelting and castingof iron was 2100 ngm�3 in the PM2.5 and 800 ngm�3 in thePM10, thus the TSP was 2900 ngm�3. Even with the values ofrelatively high concentrations for Fe, limits for its concentrationin the SPM were not found in the literature or information thatit poses a health risk. The same happened with the Ca (PM2.5 =3800 ngm�3 and PM10-2.5 = 900 ngm�3), for which the maxi-mum levels in the atmosphere have not been established forthe environmental agencies.

by the National Institute of Standards and Technology – NIST, USA,

SRM 1833

Element Certification Uncertainty This work

μg cm�2 μg cm�2 μg cm�2

19 K 17.4 1.18 17.07

22Ti 12.9 0.78 13.19

26Fe 14.3 1.98 15.16

30Zn 3.8 0.79 4.18

82Pb 15.9 1.97 16.79


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Figure 9. Temporal concentration of K, Ca, Ti, V, Cr, Mn, Fe, Ni, Cu, Zn, Sr, and Pb (concentration in ng.m�3 vs time in hours) as fine (PM2.5 ) andcoarse (PM10–2.5 ) suspended particulate matter in the air during the smelting and casting of bronze.


498

As for the elements K, Ti, V, Cu, and Zn, there are noassociated risks of inhalation. However, the inhalation offumes of zinc oxide can result in fever. Other symptomsmay include the following: metallic taste in the mouth,


accompanied by throat dryness and irritation and coughing,accompanied sometimes with difficulty breathing and a feel-ing of weakness and fatigue. The recovery in such cases isusually within two days.[19]


Figure 10. Temporal concentration of Ca, Ti, V, Cr, Mn, Fe, Ni, Cu, Zn, and Pb (concentration in ng.m�3 vs time in hours) as fine (PM2.5 ) and coarse(PM10–2.5 ) suspended particulate matter in the air during the smelting and casting of iron.

Table 3. Mean concentrations found in samples of PM2.5, PM10–2.5, and PM10 in the smelting and casting bronze and the concentration limits ofsome air pollutants total suspended particles adopted by the Brazilian National Health Foundation – Fundação Nacional de Saúde[1]

Element Concentration in PM2.5

(ngm�3)Concentration in PM10-2.5

(ngm�3)Concentration in PM10

(ngm�3)TSP Limits FUNASA

(ng.m�3)

Cr <LD 22 59 1

Mn 106 35 141 50

Ni 82 13 95 40

FUNASA, Fundação Nacional de Saúde; TSP, total suspended particles; and Limit of detection


499

As the raw material for the smelting of iron has no Pb in thechemical composition specified by the manufacturer, an


investigation was made of all materials that are found on the ironcastings, including the raw material itself. Qualitative analysis of


Table 4. Mean concentrations found in samples of PM2.5, PM10–2.5, and PM10 in the smelting and casting iron and the concentration limits of someair pollutants total suspended particles adopted by the Brazilian National Health Foundation – Fundação Nacional de Saúde[1]

Element Concentration in PM2.5

(ngm�3)Concentration in PM10�2.5

(ngm�3)Concentration in PM10

(ngm�3)TSP Limits FUNASA

(ngm�3)

Cr <LD 26 140 1

Mn 289 40 329 50

Ni 463 10 473 40

FUNASA, Fundação Nacional de Saúde; and TSP, total suspended particles

Table 5. Mean concentrations found in samples of PM10 and PM2.5 in the bronze and iron foundries and the concentration limits of atmosphericparticulates adopted by the United States Environmental Protection Agency[18]

Particulate(all elements)

Concentration bronze foundry(μgm�3)

Concentration iron foundry(μgm�3)

Limits USEPA(μgm�3)

PM10 24 3 50

PM2.5 9 64 15

USEPA, United States Environmental Protection Agency.


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these materials was made by EDXRF but without the use of abrass collimator. The materials analyzed were the following:

• Iron (gray and nodular) – raw.• Isothermic powder – prevents rapid cooling of molten mate-

rial into the mold and is placed over the channel of the mold,after being filled with the material.

• Inoculant – placed on the molten material so that it leaves theoven for the ‘pot’ (a container used to receive molten materialfrom the oven, which is then taken to fill the mold).

• Paint finishing – lining of the sand mold for best results infinishing the piece.

• Alloy Fe-Si-Mg – solid material placed in the empty pan beforepouring the molten material with the intention of a better out-come after casting.

Of these samples, only isothermal powder showed the pres-ence of Pb, which probably increased the concentration of leadin airborne particles in the foundry environment. The powder isresponsible for an isothermal slow solidification of liquid metalin order to obtain better quality in the final product, withoutbig cracks or deformities. As this material is placed in the moldchannel shortly after being completely filled with molten metal,there may be volatilization of various chemicals, including lead.

Conclusions

From the results, it is clear that workers are exposed to the atmo-spheric SPM over a long period. This matter contains chemicalswith carcinogenic properties that can also cause lung diseaseand immunological and neurological illnesses, among othershealth problems, when they are in critical concentrations.One can also conclude that in the casting and molding of the

two metals, suspended particles can be derived not only by theelements in the metal to be cast but also by the elements presentin materials that offer a good yield of the casting, such as isother-mal dust.Concentration levels were found that far exceed the limits

adopted by the Brazilian and international agencies, mainly in


the iron foundry, with respect to Pb, Cr, Mn, and Ni in the finefraction, indicating an imminent risk to the health of workers inthe foundry industries and prompting the need for constantmonitoring of air quality (concentration of potentially toxicelements) and the working conditions of employees.

Acknowledgement

Research partially founded by Conselho Nacional deDesenvolvimento Científico e Tecnológico (CNPq) and Fundaçãode Amparo à Pesquisa de São Paulo (FAPESP).

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Evaluation of the concentration of chemical elements in suspended particulate matter inside a small bronze and iron foundry industry, using a streaker sampler and EDXRF