Quantification of the micronutrient profile in Moringa oleifera tree leaves using calibration free laser induced breakdown spectroscopy

Patent metadata

Field	Value
Publication number	US-11635386-B2
Application number	US-202117535081-A
Country	US
Kind code	B2
Filing date	Nov 24, 2021
Priority date	Nov 25, 2020
Publication date	Apr 25, 2023
Grant date	Apr 25, 2023

Abstract

Method for quantifying the micronutrient profile of Moringa oleifera tree leaves (MOLs) using calibration free laser induced breakdown spectroscopy (CF-LIBS).

First claim

The invention claimed is:

1. A method of determining the micronutrient profile of a Moringa oleifera leaf comprising:
drying the Moringa oleifera leaf at a temperature less than 100° C. to form a dried leaf;
grinding the dried leaf to form a homogeneous mixture;
compressing the homogeneous mixture into a pellet comprising a chromophore;
analyzing the elemental composition of said pellets with calibration free laser-induced breakdown spectroscopy (CF-LIBS); and
wherein the analyzing is carried out with a CF-LIBS algorithm configured to calculate the quantity of a plurality of elements selected from the group Ca, Cu, Fe, K, Mg, Mn, Na, P, S, and Zn present in the pellets; and
wherein the CF-LIBS is performed using a pulsed laser having a pulse width of 5 to 10 ns, a repetition rate of 15 to 25 Hz, a time delay of 290 to 350 ns, and a laser energy of 10 to 30 mJ.

2. The method of claim 1 , further comprising:
determining the concentration of a set of elements in an Nth sample of Moringa oleifera leaves using laser-induced breakdown spectroscopy to produce an Nth sample element profile, wherein the calculating comprises mixing variable amounts of the first through Nth samples to produce a composite dose comprising at least two of the first through Nth samples.

3. The method of claim 1 , wherein the spectra of at least 2 laser pulses are accumulated to get the average CF-LIBS spectrum.

4. The method of claim 1 , wherein the pellets are mounted on the top of a two-dimensional motorized translational stage during CF-LIBS analysis.

5. The method of claim 1 , wherein the detected element during CF-LIBS analysis is Ca and at least one atomic line at 422.6, 445.4, 393.3 and 315.8 nm is monitored; and
the optimum gated time delay of the pulsed laser is 300 ns.

6. The method of claim 1 , wherein the detected element during CF-LIBS analysis is K and at least one atomic line at 404.7, 766.4, and 769.8 nm is monitored; and
the optimum gated time delay of the pulsed laser is 332 ns.

7. The method of claim 1 , wherein the detected element during CF-LIBS analysis is Cu and the atomic line at 324.7 nm is monitored.

8. The method of claim 1 , wherein the detected element during CF-LIBS analysis is Fe and at least one atomic line at 248.3, 259.9, and 275.5 nm is monitored.

9. The method of claim 1 , wherein the detected element during CF-LIBS analysis is Mg and at least one atomic line at 279.5, 280.2, and 285.2 nm is monitored.

10. The method of claim 1 , wherein the detected element during CF-LIBS analysis is Mn and at least one atomic line at 403.0, 259.3, and 257.6 nm is monitored.

11. The method of claim 1 , wherein the detected element during CF-LIBS analysis is Na and at least one atomic line at 328.5, 588.9, and 589.5 nm is monitored.

12. The method of claim 1 , wherein the detected element during CF-LIBS analysis is P and at least one atomic line at 253.5 and 255.3 nm is monitored.

13. The method of claim 1 , wherein the detected element during CF-LIBS analysis is S and at least one atomic line at 543.2 and 545.3 nm is monitored.

14. The method of claim 1 , wherein the detected element during CF-LIBS analysis is Zn and at least one atomic line at 250.1, 255.7, and 334.5 nm is monitored.

15. The method of claim 1 , wherein the sensitivity is sufficient to detect 1 mg/L of at least one of Ca, Cu, Fe, K, Mg, Mn, Na, P, S, and Zn in the Moringa oleifera leaves.

16. The method of claim 1 , wherein the CF-LIBS algorithm assumes the sample is in local thermodynamic equilibrium (LTE); and
LTE is determined by the number density of electrons and electron temperature in the plasma during the CF-LIBS measurements; and
the electron temperature is between 9,000 to 10,000 K; and
the number density of electrons is 0.10×10 16 to 0.50×10 17 cm −3 .

17. The method of claim 1 further comprising:
validating the micronutrient profile results of CF-LIBS by comparing to the standard method of elemental detection using ICP-OES wherein the relative accuracy is in the range of 0.01 to 0.50.

18. The method of claim 1 , wherein the chromophore is a fused ring aromatic compound.

19. The method of claim 18 , wherein the fused ring aromatic compound is selected from the group comprising substituted naphthalene, fluorene, and fluorenone derivatives.

20. The method of claim 1 , wherein the chromophore is mixed into the homogeneous mixture before being compressed into a pellet and/or the chromophore is coated onto the side of the pellet onto which the laser will be focused.

Assignees

• Univ King Fahd Pet & Minerals
• Univ Imam Abdulrahman Bin Faisal

Inventors

• Gondal Mohammad A
• Al-Messiere Munirah Abdullah
• Khan Firdos Alam
• Rehman Suriya
• Baykal Abdulhadi
• Al-Dakheel Reem Khalid

Classifications

• G01N2201/06113

  Coherent sources; lasers · CPC title

• G01N1/286

  involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising (microtomes G01N1/06; pulverising in general B02C; mixing in general B01F) · CPC title

• G01N1/44

  Sample treatment involving radiation, e.g. heat · CPC title

• G01N21/718 Primary

  Laser microanalysis, i.e. with formation of sample plasma · CPC title

• G01N2001/388

  mixing the sample with a tracer · CPC title