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INDUSTRIAL TRAINING
2017
INDUCTIVELY COUPLED
PLASMA OPTICAL EMISSION
SPECTOMETRY (ICP-OES)
PRESENT BY:
NURIDAYAH BINTI YUSMAIDI
WEEK 1 & 2 • ICP-OES THEORY
• SAMPLE PREPARATION OF EA
• FERTILIZER ANALYSIS
WEEK 3 & 4 SOIL ANALYSIS
WEEK 5 ICP-OES THEORY
INTRODUCTION
• Type of emission spectroscopy that uses the
inductively coupled plasma
• It is a flame technique
• The intensity of this emission is indicative of the
concentration of the element within the sample
• Calibration: Mangenese solution
Check nitrogen and argon gas
PART OF INSTRUMENT
Remove water from air
compressor
Regulator: control
of noncorrosive
Dryer: to remove
moisture Check the water level of
chiller water
AUTOSAMPLERCOMPUTER
Designed to
transform
raw data
into
information
Collect
samples
COMPONENTS OF ICP
Delivers
sample
into
nebulizer
Converting a
liquid into a
fine spray
PUMPNEBULIZER
INJECTOR
CHAMBER
Remove droplets
produced by the
nebulizer
Place sample in
high pressure
flow
TORCH
Tubing for
plasma and
auxiliary
gas flow
Act as a spacer
between the torch
RF coil
TORCH BONNET
RADIALAXIAL
Side view of
plasma
End view
of
plasma
Torch, injector,
bonnet torch,
radial and axial
was set up
STEP 1: SYSTEM CHECK LIST
HOW USING WinLab32 FOR RUN ICP-OES??
STEP 2: FILE
FILE
OPEN
METHOD
CLICK
STEP 3: PLASMA
PLASMA
CLICK
ON
STEP 4: TOOLS
TOOLS
CLICK
SPECTROMETER
CONTROL
INITIALIZE OPTICS
ALIGN VIEW
STEP 5: TOOLS
STEP 6: CALIBRATION
DATA AND CALCULATION: BASED ON ONE SAMPLE
OF FERTILIZER
Sample ID A/S Loc Date Time
Analyte
Name Int (Corr)
RSD
(Corr Int)
SD (Corr
Int)
Conc
(Calib)
Conc
(Samp)
Reported
Conc
(Calib) Reported Conc (Samp)
Calib Blank 1 1 05-02-17 1:52:54 PM P 213.617 14.4235457 6.457346 0.931378 [0.00]
Calib Blank 1 1 05-02-17 1:52:54 PM K 766.490 18820.7249 2.285483 430.1444 [0.00]
Calib Blank 1 1 05-02-17 1:52:54 PM Mg 285.213 -463.70613 6.533916 30.29817 [0.00]
Calib Blank 1 1 05-02-17 1:52:54 PM B 249.677 30111.9796 0.244815 73.71873 [0.00]
S1 33 05-02-17 1:57:27 PM P 213.617 351082.482 0.671362 2357.034 [158.4]
S1 33 05-02-17 1:57:27 PM K 766.490 6006884.89 0.581678 34940.74 [200]
S1 33 05-02-17 1:57:27 PM Mg 285.213 2299070.57 0.009609 220.9133 [30]
S1 33 05-02-17 1:57:27 PM B 249.677 360518.244 0.765572 2760.028 [2]
S2 34 05-02-17 2:01:15 PM P 213.617 1537716.75 0.056084 862.4073 [634.17]
S2 34 05-02-17 2:01:15 PM K 766.490 25495615.6 0.424443 108214.3 [800]
S2 34 05-02-17 2:01:15 PM Mg 285.213 11193576.8 0.859641 96224.63 [150]
S2 34 05-02-17 2:01:15 PM B 249.677 1989438.61 1.955102 38895.55 [10]
S3 35 05-02-17 2:05:03 PM P 213.617 2267715.79 0.252416 5724.087 [951]
S3 35 05-02-17 2:05:03 PM K 766.490 37909821.9 0.816761 309632.8 [1200]
S3 35 05-02-17 2:05:03 PM Mg 285.213 17467052 0.27787 48535.69 [250]
S3 35 05-02-17 2:05:03 PM B 249.677 3050847.97 0.653446 19935.66 [15] %P2O5 %K2O %MgO %B2O3
QC F15/10 5 05-02-17 2:08:56 PM P 213.617 257151.976 2.530687 6507.711 110.9262 110.9262 110.9 110.9 5.07922
QC F15/10 5 05-02-17 2:08:56 PM K 766.490 27132931.3 0.079279 21510.65 857.8097 857.8097 857.8 857.8 20.67298
QC F15/10 5 05-02-17 2:08:56 PM Mg 285.213 5155926.77 1.686524 86955.92 70.70965 70.70965 70.71 70.71 2.347572
QC F15/10 5 05-02-17 2:08:56 PM B 249.677 862541.565 0.646395 5575.429 4.35837 4.35837 4.358 4.358 0.280655
BLANK 38 05-02-17 2:12:53 PM P 213.617 86.9382419 18.04484 15.68787 4.097573 4.097573 4.098 4.098 0.000938
BLANK 38 05-02-17 2:12:53 PM K 766.490 14654.35 3.597323 527.1643 4.292732 4.292732 4.293 4.293 0.000517
BLANK 38 05-02-17 2:12:53 PM Mg 285.213 36282.3952 0.113541 41.19531 -2.18262 -2.18262 -2.183 -2.183
-
0.000362
BLANK 38 05-02-17 2:12:53 PM B 249.677 30602.727 1.794585 549.1918 0.278291 0.278291 0.278 0.278 8.95E-05
QC F15/10 39 05-02-17 2:17:20 PM P 213.617 250696.412 0.442589 1109.555 108.2434 108.2434 108.2 108.2 4.95556
QC F15/10 39 05-02-17 2:17:20 PM K 766.490 26057616.9 0.948126 247059 823.9654 823.9654 824 824 19.8584
QC F15/10 39 05-02-17 2:17:20 PM Mg 285.213 4935491.66 0.368125 18168.8 67.57115 67.57115 67.57 67.57 2.243324
QC F15/10 39 05-02-17 2:17:20 PM B 249.677 723577.686 0.783142 5666.643 3.676849 3.676849 3.677 3.677 0.236799
BKILANG_R4_272/K_17 40 05-02-17 2:21:11 PM P 213.617 131308.767 0.221019 290.2168 58.62947 58.62947 58.63 58.63 2.685254
BKILANG_R4_272/K_17 40 05-02-17 2:21:11 PM K 766.490 10553758.9 0.750208 79175.18 335.9991 335.9991 336 336 8.0976
BKILANG_R4_272/K_17 40 05-02-17 2:21:11 PM Mg 285.213 1123883.39 0.329213 3699.975 13.30239 13.30239 13.3 13.3 0.44156
BKILANG_R4_272/K_17 40 05-02-17 2:21:11 PM B 249.677 34466.5758 1.223829 421.8121 0.29724 0.29724 0.297 0.297 0.019127
CALCULATION: % P2O5
• ppm – concentration
• f – factor
• FACTOR P2O5
= (Molecular Weight P2O5)
Atomic Weight 2P
= [2(30.973762) + 5(15.9994)]
2(30.973762
= 2.29
CALCULATION: FACTOR P2O5
CONCLUSION ICP-OES
Measure almost all the elements
Lower detection limit
Multiple quantitative

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INDUSTRIAL TRAINING ICP-OES ANALYSIS

  • 1. INDUSTRIAL TRAINING 2017 INDUCTIVELY COUPLED PLASMA OPTICAL EMISSION SPECTOMETRY (ICP-OES) PRESENT BY: NURIDAYAH BINTI YUSMAIDI
  • 2. WEEK 1 & 2 • ICP-OES THEORY • SAMPLE PREPARATION OF EA • FERTILIZER ANALYSIS WEEK 3 & 4 SOIL ANALYSIS WEEK 5 ICP-OES THEORY INTRODUCTION
  • 3. • Type of emission spectroscopy that uses the inductively coupled plasma • It is a flame technique • The intensity of this emission is indicative of the concentration of the element within the sample • Calibration: Mangenese solution
  • 4. Check nitrogen and argon gas PART OF INSTRUMENT Remove water from air compressor Regulator: control of noncorrosive Dryer: to remove moisture Check the water level of chiller water
  • 5. AUTOSAMPLERCOMPUTER Designed to transform raw data into information Collect samples COMPONENTS OF ICP Delivers sample into nebulizer Converting a liquid into a fine spray PUMPNEBULIZER
  • 6. INJECTOR CHAMBER Remove droplets produced by the nebulizer Place sample in high pressure flow TORCH Tubing for plasma and auxiliary gas flow Act as a spacer between the torch RF coil TORCH BONNET
  • 7. RADIALAXIAL Side view of plasma End view of plasma Torch, injector, bonnet torch, radial and axial was set up
  • 8. STEP 1: SYSTEM CHECK LIST HOW USING WinLab32 FOR RUN ICP-OES??
  • 14. DATA AND CALCULATION: BASED ON ONE SAMPLE OF FERTILIZER Sample ID A/S Loc Date Time Analyte Name Int (Corr) RSD (Corr Int) SD (Corr Int) Conc (Calib) Conc (Samp) Reported Conc (Calib) Reported Conc (Samp) Calib Blank 1 1 05-02-17 1:52:54 PM P 213.617 14.4235457 6.457346 0.931378 [0.00] Calib Blank 1 1 05-02-17 1:52:54 PM K 766.490 18820.7249 2.285483 430.1444 [0.00] Calib Blank 1 1 05-02-17 1:52:54 PM Mg 285.213 -463.70613 6.533916 30.29817 [0.00] Calib Blank 1 1 05-02-17 1:52:54 PM B 249.677 30111.9796 0.244815 73.71873 [0.00] S1 33 05-02-17 1:57:27 PM P 213.617 351082.482 0.671362 2357.034 [158.4] S1 33 05-02-17 1:57:27 PM K 766.490 6006884.89 0.581678 34940.74 [200] S1 33 05-02-17 1:57:27 PM Mg 285.213 2299070.57 0.009609 220.9133 [30] S1 33 05-02-17 1:57:27 PM B 249.677 360518.244 0.765572 2760.028 [2] S2 34 05-02-17 2:01:15 PM P 213.617 1537716.75 0.056084 862.4073 [634.17] S2 34 05-02-17 2:01:15 PM K 766.490 25495615.6 0.424443 108214.3 [800] S2 34 05-02-17 2:01:15 PM Mg 285.213 11193576.8 0.859641 96224.63 [150] S2 34 05-02-17 2:01:15 PM B 249.677 1989438.61 1.955102 38895.55 [10] S3 35 05-02-17 2:05:03 PM P 213.617 2267715.79 0.252416 5724.087 [951] S3 35 05-02-17 2:05:03 PM K 766.490 37909821.9 0.816761 309632.8 [1200] S3 35 05-02-17 2:05:03 PM Mg 285.213 17467052 0.27787 48535.69 [250] S3 35 05-02-17 2:05:03 PM B 249.677 3050847.97 0.653446 19935.66 [15] %P2O5 %K2O %MgO %B2O3 QC F15/10 5 05-02-17 2:08:56 PM P 213.617 257151.976 2.530687 6507.711 110.9262 110.9262 110.9 110.9 5.07922 QC F15/10 5 05-02-17 2:08:56 PM K 766.490 27132931.3 0.079279 21510.65 857.8097 857.8097 857.8 857.8 20.67298 QC F15/10 5 05-02-17 2:08:56 PM Mg 285.213 5155926.77 1.686524 86955.92 70.70965 70.70965 70.71 70.71 2.347572 QC F15/10 5 05-02-17 2:08:56 PM B 249.677 862541.565 0.646395 5575.429 4.35837 4.35837 4.358 4.358 0.280655 BLANK 38 05-02-17 2:12:53 PM P 213.617 86.9382419 18.04484 15.68787 4.097573 4.097573 4.098 4.098 0.000938 BLANK 38 05-02-17 2:12:53 PM K 766.490 14654.35 3.597323 527.1643 4.292732 4.292732 4.293 4.293 0.000517 BLANK 38 05-02-17 2:12:53 PM Mg 285.213 36282.3952 0.113541 41.19531 -2.18262 -2.18262 -2.183 -2.183 - 0.000362 BLANK 38 05-02-17 2:12:53 PM B 249.677 30602.727 1.794585 549.1918 0.278291 0.278291 0.278 0.278 8.95E-05 QC F15/10 39 05-02-17 2:17:20 PM P 213.617 250696.412 0.442589 1109.555 108.2434 108.2434 108.2 108.2 4.95556 QC F15/10 39 05-02-17 2:17:20 PM K 766.490 26057616.9 0.948126 247059 823.9654 823.9654 824 824 19.8584 QC F15/10 39 05-02-17 2:17:20 PM Mg 285.213 4935491.66 0.368125 18168.8 67.57115 67.57115 67.57 67.57 2.243324 QC F15/10 39 05-02-17 2:17:20 PM B 249.677 723577.686 0.783142 5666.643 3.676849 3.676849 3.677 3.677 0.236799 BKILANG_R4_272/K_17 40 05-02-17 2:21:11 PM P 213.617 131308.767 0.221019 290.2168 58.62947 58.62947 58.63 58.63 2.685254 BKILANG_R4_272/K_17 40 05-02-17 2:21:11 PM K 766.490 10553758.9 0.750208 79175.18 335.9991 335.9991 336 336 8.0976 BKILANG_R4_272/K_17 40 05-02-17 2:21:11 PM Mg 285.213 1123883.39 0.329213 3699.975 13.30239 13.30239 13.3 13.3 0.44156 BKILANG_R4_272/K_17 40 05-02-17 2:21:11 PM B 249.677 34466.5758 1.223829 421.8121 0.29724 0.29724 0.297 0.297 0.019127
  • 15. CALCULATION: % P2O5 • ppm – concentration • f – factor
  • 16. • FACTOR P2O5 = (Molecular Weight P2O5) Atomic Weight 2P = [2(30.973762) + 5(15.9994)] 2(30.973762 = 2.29 CALCULATION: FACTOR P2O5
  • 17. CONCLUSION ICP-OES Measure almost all the elements Lower detection limit Multiple quantitative