an approach to determine the efficiency of libs system in ......intensity, toxic grave metals...

J. Sci. Technol. Environ. Inform. 03(01): 178-190 | Rahman et al. (2016) EISSN: 2409-7632, www.journalbinet.com DOI: http://dx.doi.org/10.18801/jstei.030116.20

Published with open access at www.journalbinet.com 178

Volume 03, Issue 01, Article no. 20, pp. 178-190 Rahman et al. (2016) http://www.journalbinet.com/jstei-volume-03.html Original Research Paper

An approach to determine the efficiency of LIBS system in aqueous solution using optical instruments

Md. Bulu Rahman1, Md. Masum Billah2*, Khondokar Nazmus Sakib3, M. A. Malek1, Sheikh Dobir Hossain2 and Abul F. M. Yusuf Haider4 1Dept. of Electrical and Electronic Engineering, Green University of Bangladesh, Dhaka -1207 2Dept. of Physics, Jessore University of Science and Technology, Jessore- 7408 3Dept. of Physics, Mawlana Bhashani Science and Technology University, Tangail- 1902 4Dept. of Physics, Center for Advanced Research in Sciences, University of Dhaka, Bangladesh Article info. ABSTRACT Key Words:

LIBS, Atomic emission Spectroscopy, Liquid absorbent, Background intensity, Toxic grave metals

Received: 01.02.2016 Published: 20.04.2016

Corresponding author*: [email protected]

Laser induced breakdown spectroscopy (LIBS) has been applied to determine its Limit of Detection (LOD) in aqueous solution. It was based on only one single-pulse laser system where we used a wood slice as the liquid absorbent to make over liquid sample analysis using the technique of LIBS. Using this approach, it is obvious to achieve good reproducibility and high detection sensitivity. More than twenty readings of the background emission were taken to calculate the LOD. The calculated value of the background intensity (σ) was 42.435 and the value of the gradient (S) of the calibration curve of Pb element in aqueous solution fitted with straight line through origin was 178.57 mg-1L. The LOD was determined and its experimentally calculated value in our study was 712ppb(parts per billion) with orders better than those determined by directly analyzing liquid samples focusing the laser light on a liquid surface In addition, the wood slice is very uncomplicated to handle and this study provides a more sensible approach for rapid and susceptible metal component investigation in aqueous solutions using laser induced breakdown spectroscopy, which is really functional in various fields to analyze metal elements in aqueous solution, especially for monitoring toxic grave metals in aqueous solution.

Citation (APA): Rahman, M. B., Billah, M. M., Sakib, K. N., Malek, M. A., Hossain, S. D. & Haider, A. F. M. Y. (2016).

An approach to determine the efficiency of LIBS system in aqueous solution using optical instruments. Journal

of Science, Technology and Environment Informatics, 03(01), 178-190.

© 2016, Rahman et al. This is an open access article distributed under terms of the Creative Common Attribution 4.0 International License.



I. Introduction

In LIBS (Laser induced breakdown spectroscopy) method, a pulse of laser of very short duration (several nanoseconds to femtoseconds) and with a high energy density is focused onto a very small spot at the exterior of the sample under study. Absorbing this high energy, the temperature of this locally heated region rises rapidly to the vaporization temperature of the material, on the order of few tens of thousands Kelvin. So, a very small amount of material (range of nano-gram to pico-gram) is ablated and turned to optically induced plasma, frequently called Laser Induced Plasma (LIP) or laser spark.

After the laser pulse has terminated (typically within 10 ns), the plasma decays over an interval of one to few microseconds, depending on the energy of the laser pulse. Soon after the initiation, a strong continuum background emission is seen. This continuum is just the white light coming from the plasma and carries very little spectroscopic information. As the plasma decays, these spectra are followed by the characteristic emission spectra from neutrals and ionic species within the plasma. Eventually weak molecular emissions come out due to the formation of molecules by the recombination of atoms. The analysis of LIBS is just concerned with the characteristic emissions resulting from the neutral atoms and the ions, carrying the signature of the constituents within the specimen. If these emissions are captured by a spectrometer-detector system and analyzed by the help of a standard atomic spectra database, the constituent elements of the specimen can be identified. This is why, a gated detector is usually used in the LIBS setup, which ensures that initial strong continuum plasma background and the final molecular emissions are prevented. Thus inspection of the LIBS spectrum gives instantaneous qualitative information about the composition of the sample and by performing calibration, quantitative information can also be obtained. This is the basis of LIBS.

To analyze a liquid sample directly, we can either focus the laser beam on the surface of a steady or dynamic liquid (Berman and Wolf, 1998; Fichet et al., 2001; St-onge et al., 2004). In the bulk of liquid (Pearman and Angel, 2003; Giacomo et al., 2004) or on the exterior of a liquid jet. When we focus the laser pulse on the liquid surface,liquid splashes and severely interferes with optical detection and if it is focused in the bulk of liquid, the plasma is cramped by the surrounding liquid and it leads to a rapid quenching of the atomic emission. Because of these difficulties, the recognition sensitivity of LIBS for a given metallic element in waters usually several hundred ppm (parts per million) or more in environment. For example, the detection limit was found to be 75ppm for lead (Godwal et al., 2007), 500ppm for Cd and 12.5ppm for Pb in the case of single-pulse LIBS analysis in water; and no mercury was detected even at 1000ppm (Knopp et al., 1996) concentrations in water. Therefore, conventional single pulse LIBS system is not suitable for detecting the toxic elements in environment, whether if these metals are presents in the order of ppm or sub-ppm levels in environment.

For quantitative determination of the concentration of trace toxic heavy metals in water, asensitive and in situ elemental analysis method (Wal et al., 1999; Arca et al., 1997) is very important to monitor environmental pollution and to analyze industrial waste-water.

Lead is an extremely toxic element that can adversely affect the human health. Lead is being used in different industries in Bangladesh namely gasoline, car battery manufacturing and recycling, paints factory, electroplating industry etc. Therefore, in order to further study, we attempted to ascertain the LOD of our system in water by the LIBS technique.

II. Materials and Methods

In Figure 01, the schematic diagram of LIBS system we have used is shown. For this system, the excitation laser used is a Q-switched Nd: YAG laser system (experiment performed in Spectra-Physics LAB-170-10) having an output at a fundamental wavelength of 1064 nm, pulse duration of 8ns, repetition rate of 10 Hz and pulse energy of 850 mJ. The laser is also designed with harmonic generators which are capable of generating the second and third harmonics of the fundamental wavelength at 532 nm and 355 nm by means of KDP crystals and producing energies of 450 mJ and 220 mJ per pulse, respectively. A chiller has been used in this experiment in purpose to control the



temperature of the laser system. The chiller was placed outside the laboratory. Two pipelines were used to ensure the in and out flow of the water from the chiller to the laser setup. Intense, transient plasma is produced by focusing the laser beam by using a glass convex lens of 100 mm focal length (f1) on the sample. The diameter (D) of the laser beam is approximately 50mm. So the f-number of the setup is f = f1/ D = 2.

Figure 01. Schematic illustration of the experimental LIBS method is directly copied from our previous article related to this research (Haider et al., 2014).

Sample processing

A solder is a fusible metal alloy which was used to join metal work pieces. Lead solder are commercially available with tin concentrations between 5% and 70% by weight. One of the common alloys (Sn-60% + Pb-40%) had been used in our experiment to identify the lead line correctly for further study and investigation. It melts at 188°C. That is why; we kept the Lead solder in an electric oven at 200°C about two hours for melting. After melting, the sample was coagulated, and then a reasonable size of pellet was made to perform LIBS experiment. We can use wood slice (Chen et al., 2008; Chen et al., 2010), saw dust, resin, CaO (Diaz Pace et al., 2006) etc. to carry out fast and sensitive trace poisonous heavy metal analysis in aqueous solutions (Giacomo et al., 2007; Lo and Cheung, 2002; Fang and Ahmed, 2007) using LIBS. Aqueous solution with different known concentration (0.375ppm-1000ppm) of lead was prepared in the laboratory using de-ionized water as a solvent. One type of commercially and easily available non-contaminated wood slice (ply wood) was chosen as an absorbent. Wood slice was chosen because it is easily available and easy to handle. The wood slice was cut into small pieces with the dimensions 5cm x 3 cm x 3 mm. At first the wood slice was dried for three hours at 140o C in an electric oven.



Then, it was dipped into the aqueous solution of Lead and stirred for 15 minutes in order to absorb the solution in matrix. After this, the chips were taken out and put on the table for overnight to dry normally. Finally the sample was kept in an electric oven to dry at 120oC before mounted on the sample stage for analysis.

III. Results and Discussion The acquired LIBS spectra of the pellet of a Lead Solder are shown in the following figures:

216 218 220 222 224 226

0

1000

2000

3000

4000

5000

6000

Pb

I Sn

I

Sn

I

Pb

II

Sn

I Sn

I

Sn

I

Cu

I

Pb

I

Inte

nsity

Wavelength (nm)

224 226 228 230 232 234

-500

0

500

1000

1500

2000

2500

3000

3500

4000

Co

II

Fe

I

Sn

I

Sn

I

Sn

I

Sn

I

Sn

I

Inte

nsity

Wavelenth (nm)

Figure 02 (A) Figure 02 (B)

Figure 02 (C) Figure 02 (D)

232 234 236 238 240 242 244

0

1000

2000

3000

4000

5000

6000

7000

Sn

I

Sn

I

Pb

I

Pb

I

Sn

I

Pb

I

Sn

I

Inte

nsity

Wavelength (nm)

242 244 246 248 250 252

-1000

0

1000

2000

3000

4000

5000

6000

7000

Pb

I

Pb

I

Pb

I

Sn

I

Sn

I

Sn

I

Inte

nsity

Wavelength (nm)



Figure 02 (E) Figure 02 (F)

Figure 02 (G) Figure 02 (H)

250 252 254 256 258 260 262

-1000

0

1000

2000

3000

4000

5000

6000

7000

8000

Sb

IS

n I

Pb

I

Sn

I

Sn

I

Sb

IS

n I

Inte

nsity

Wavelength (nm)

260 262 264 266 268 270

0

2000

4000

6000

8000

10000

12000

14000

Sn

IP

b I

Al II

Pb

I

Pb

I

Wavelength (nm)In

tensity

268 270 272 274 276 278 280

-2000

0

2000

4000

6000

8000

10000

12000

14000

Sn I

Sn I

Inte

nsity

Wavelength (nm)278 280 282 284 286 288

-2000

0

2000

4000

6000

8000

10000

12000

14000

16000

18000

20000

Sn I

Sn I

Sn I

Sn I

Pb I

Pb I

Pb I

Pb I

Inte

nsity

Wavelength (nm)



Figure 02 (I) Figure 02 (J)

306 308 310 312 314 316

-100

0

100

200

300

400

500

600

700

Fe I

Sn

I

Inte

nsity

Wavelength (nm)

Figure 02 (K) Figure 02 (L)

Figure 02 (M) Figure 02 (N)

286 288 290 292 294 296 298

0

500

1000

1500

2000

2500

Sn I

Cu

II

Inte

nsity

Wavelength (nm)

296 298 300 302 304 306

0

5000

10000

15000

20000

Sn I

Sn I

Inte

nsity

Wavelength (nm)

314 316 318 320 322 324

-2000

0

2000

4000

6000

8000

10000

12000

14000

16000 Sn I

Inte

nsity

Wavelength (nm)

322 324 326 328 330 332 334

-2000

0

2000

4000

6000

8000

10000

12000

14000

16000

18000

Fe

I

Sn

I

Inte

nsity

Wavelength (nm)

332 334 336 338 340 342

0

1000

2000

3000

4000

5000

Ag

I

Sn

II

Sn

I

Inte

nsity

Wavelength (nm)



Figure 02 (O) Figure 02 (P)

Figure 02 (Q) Figure 02 (R)

Figure 02 (S) Figure 02 (T)

From these spectra we first measured the wavelength and intensity of the corresponding peaks. Then, we compared the measured intensity to the intensity of the NIST (US National Bureau of Standards and

350 352 354 356 358 360

-2000

0

2000

4000

6000

8000

10000

12000

14000 Pb

I

Inte

nsity

Wavelength (nm)

350 360 370 380 390 400

0

20000

40000

60000

80000

100000

Sn

I

Pb

I

Pb

IP

b I

Pb

I

Pb

I

Inte

nsity

Wavelength (nm)

390 400 410 420 430

0

100000

200000

300000

400000

Pb

I

Inte

nsity

Wavelength (nm)

430 440 450 460 470

-20000

0

20000

40000

60000

80000

100000

120000

140000 Sn

I

Pb

II

Inte

nsity

Wavelength (nm)

465 470 475 480 485 490 495 500 505 510

0

20000

40000

60000

80000

100000

Pb

I

Inte

nsity

Wavelength (nm)

505 510 515 520 525 530 535 540 545 550

0

5000

10000

15000

20000

25000

Mo

I Pb

I

Fe

I

Cu

I

Pb

I

Inte

nsity

Wavelength (nm)



Technology database (NIST Atomic Spectra Database, 2014) data (Anonymous source) to approximately identify the elements in the aqueous solution. Doing this, we obtained the following data, which are given below in a table. We did not show the line of other elements, because it was important for us to identify all the lead lines (Pandhiji and Rai, 2009) correctly for further study and we used these lead lines as standard data.

Table 01. Data for Identified Lead lines in Lead solder

Major Elements

Measured wavelength

nm

NIST wavelength nm

Measured intensity

NIST Intensity

Difference in wavelength,

Δ = ( - )nm

Pb l 216.940 217.0000 1958 500 0.06 Pb ll 220.317 220.3534 5103 10 0.0364 Pb l 261.394 261.4175 12350 900 0.0235 Pb l 280.192 280.1995 17917 25000 3398 Pb l 282.304 282.3189 9467 14000 0.0149 Pb l 283.306 283.3053 14143 35000 -0.0007 Pb l 287.312 287.3311 4284 14000 0.0191 Pb l 357.234 357.2729 13741 35000 0.0389

Pb l 363.821 363.9568 56545 50000 0.1358 Pb l 367.055 367.1491 12779 20000 0.0941 Pb l 368.189 368.3462 86133.99 70000 0.1572 Pb l 373.858 373.9935 46743 25000 0.1355 Pb l 405.581 405.7807 413365 95000 0.1997 Pb ll 438.575 438.6460 11929 20 0.071

Pb I 405.977 406.2136 79559.99 14000 0.2366 Pb l 500.496 500.5416 88102 1000 0.0456 Pb l 520.028 520.1437 23534 2000 0.1157 Pb ll 560.842 560.8850 33717 20 0.043 Pb l 600.190 600.1862 14930 2000 -0.0038 Pb ll 665.902 666.0200 9613 50 0.118 Pb l 722.800 722.8965 113468.98 20000 0.0965

LIBS spectra at different concentration of lead

The acquired LIBS spectra of wooden chip, dipped into lead nitrate solution at different concentrations of lead are shown in below.

Figure 03(A). Spectrum for 1000ppm Pb solution Figure 03(B). spectrum for 500ppm Pb solution

390 400 410 420

0

10000

20000

30000

40000

50000

60000

70000

Pb

I

Sr

II

Ca II

Ca II

Ca IIn

ten

sit

y

Wavelength (nm)

390 400 410 420-20000

0

20000

40000

60000

80000

100000

120000

140000

Pb

I

Sr

II

Sr

IIC

a I

Ca II

Ca II

Inte

nsit

y

Wavelength (nm)



Figure 03(C). Spectrum for 250ppm Pb solution Figure 03(D): Spectrum for 125ppm Pb solution

Figure 03(E). Spectrum for 50ppm Pb solution Figure 3(F). Spectrum for 25ppm Pb solution

Figure 03(G). Spectrum for 12.5ppm Pb solution Figure 03(H). spectrum for 6.25ppm Pb solution

390 400 410 420

0

50000

100000

150000

200000

250000

300000

Sr

II

Sr

II

Pb

I

Ca II

Ca II

Ca I

Inte

nsit

y

Wavelength (nm)

390 400 410 420-50000

0

50000

100000

150000

200000

250000

300000

350000

Sr

II

Sr

II

Pb

I

Ca II

Ca II

Ca I

Inte

nsit

y

Wavelength (nm)

390 400 410 420

0

50000

100000

150000

200000

250000

300000

Ca I

Sr

II

Sr

IIPb

I

Ca II

Ca II

Inte

nsit

y

Wavelength (nm)

390 400 410 420-50000

0

50000

100000

150000

200000

250000

300000

350000

400000

Ca I

Sr

II

Sr

II

Pb

I

Ca II

Ca II

Inte

nsit

y

Wavelength (nm)

390 400 410 420 430

-50000

0

50000

100000

150000

200000

250000

300000

350000

400000

Sr

II

Sr

II

Pb

I

Ca

I

Ca

II

Ca

II

Inte

nsity

Wavelength(nm)

390 400 410 420

0

100000

200000

300000

400000

500000

600000

700000

Sr

II

Sr

II

Pb

I

Ca I

Ca II

Ca II

Inte

nsit

y

Wavelength (nm)



Figure 03 (I). Spectrum for 3.125ppm Pb solution Figure 03 (J): Spectrum for 1.5625ppm Pb solution

Figure 03 (K). Spectrum for 0.75ppm Pb solution Figure 3(L). Spectrum for 0.375ppm Pb solution

From the above spectra, we see that lines of different elements Ca, Sr, Pb come. Wood is an organic matter. Calcium and strontium are the essential components of wood; this is the reason behind the origins of these two lines in the spectra. The lines for carbon having wavelength 193.09nm and 247.85nm were not shown in graphs since we did not take any spectrum at these wavelengths. The origin of lead (Pb I) of wavelength 405.7807nm in these spectra is obviously due to the lead nitrate solution. It is the strongest line having highest intensity of 950000 units. Calibration curve

From the above spectra, we measured line intensity of Pb and Ca, and obtained the following data. We also normalized the data by subtracting the background intensity.

390 400 410 4200

100000

200000

300000

400000

500000

600000

Pb

I

Sr II

Sr II

Ca I

Ca II

Ca II

Inte

nsit

y

Wavelength (nm)

390 400 410 4200

100000

200000

300000

400000

Ca I

Sr

II

Sr

II

Pb

I

Ca II

Ca II

Inte

nsit

y

Wavelength (nm)

390 400 410 4200

100000

200000

300000

400000

Ca I

Sr

II

Sr

II

Pb

I

Ca II

Ca II

Inte

nsit

y

Wavelength (nm)

390 400 410 420 430

0

100000

200000

300000

400000

500000

600000

Pb

I

Sr

II

Sr

II

Ca

I

Ca

II

Ca

II

Inte

nsity

Wavelength (nm)



Concentration(mg/L) Intensity

ratio:

1000 0.087791632 500 0.074929668 250 0.140408526 125 0.19636052 62.5 0.180346157 50 0.141993377 25 0.126184135

12.5 0.065411848 6.125 0.006756646 3.125 0.007298779

1.5625 0.006486621 0.78125 0.004574713

0.390625 0.002115405 0 5 10 15 20 25

0.00

0.02

0.04

0.06

0.08

0.10

0.12

0.14

0.16

Graph of Ratio of intensity Pb/Ca vs Conc of Pb

Linear Regression through origin for Data1_A:

Y = B * X

Parameter Value Error

------------------------------------------------------------

B 0.0056 1.89714E-4

------------------------------------------------------------

R SD N P

------------------------------------------------------------

0.997 0.00535 6



By Laser-based technique”. I express my gratitude to AIF-HEQEP-UGC-WB for higher education quality enhancement in Bangladesh.

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How to cite this article? APA (American Psychological Association)

Rahman, M. B., Billah, M. M., Sakib, K. N., Malek, M. A., Hossain, S. D., & Haider, A. F. M. Y. (2016). An approach to determine the efficiency of LIBS system in aqueous solution using optical instruments. Journal of Science, Technology and Environment Informatics, 03(01), 178-190. MLA (Modern Language Association)

Rahman, M. B., Billah, M. M., Sakib, K. N., Malek, M. A., Hossain, S. D., & Haider, A. F. M. Y. “An approach to determine the efficiency of LIBS system in aqueous solution using optical instruments.” Journal of Science, Technology and Environment Informatics, 03.01 (2016): 178-190. Chicago/Turabian

Rahman, M. B., Billah, M. M., Sakib, K. N., Malek, M. A., Hossain, S. D., & Haider, A. F. M. Y. “An approach to determine the efficiency of LIBS system in aqueous solution using optical instruments.” Journal of Science, Technology and Environment Informatics, 03, no. 01 (2016): 178-190.

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an approach to determine the efficiency of libs system in ......intensity, toxic grave metals...

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