Uncertainty Cu Low Conc

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QA/QC LABORATORY
Approval Date: 06/11/2023
Review Cycle: 3 Years Uncertainty for Copper (Cu) Determination for Low Concentration Sample_
Author: Sr. Chemist - Iso Tech.
Management & Doc Control
Author Pos ID: 50004177
Estimasi Ketidakpastian Metode Penetapan Tembaga (Cu)
Approval: Manager - Qa & Qc untuk Sampel Konsentrasi Rendah
Approval Pos ID: 50000346
1. PROSEDUR (PROCEDURE)
CDC-QAC-012-P012 Prosedur Ketidakpastian Pengukuran.
CDC-QAC-012-P012 Uncertainty Measurement Procedure.
2. IDENTIFIKASI SUMBER KETIDAKPASTIAN (Fish Bone)
Balance Volume AAS
Calibration Repeatibility
Calibration
Temperature Reproducibility
Au in the sample
Intermediate standard Reproducibility Slope
COA standard Repeatibility Calibration Curve
Standard Solution Operator

Concentration Sample
3. PERHITUNGAN (CALCULATION)
3.1. Ketidakpastian Asal Timbangan
Uncertainty of Balance
a. Ketidakpastian kalibrasi (µkal)
Uncertainty of Calibration (µkal)
Ketidakpastian timbangan analitik berdasarkan sertifikat kalibrasi ± 0.00017 g dengan
k=2
Uncertainty of analytical balance based on calibration certificate ± 0.00017 g with k=2
µkal = ketidakpastian timbangan: 2
balance uncertainty: 2
= 0.00017: 2
= 0.000085 g
b. Ketidakpastian penimbangan (µm)
Uncertainty of sample weight (µm)
Ketidakpastian berat sampel (µm)
Uncertainty of sample weight (µm)
µm = √ (µ kal)2+(µ kal)2
= √ (0.000085)2 +(0.000085)2
= 0.00012 g
3.2. Ketidakpastian Asal Alat Gelas
Uncertainty Of Glassware
Alat gelas yang digunakan adalah Labu Volumetri 500 mL
The glassware used is a Volumetric Flask 500 mL
a. Ketidakpastian kalibrasi (µkal)
Uncertainty of Calibration (µkal)
Ketidakpastian labu volumetri berdasarkan sertifikat kalibrasi ± 0.087 mL dengan k = 2
Uncertainty of volumetric flask based on calibration certificate ± 0.087 mL with k = 2
DOKUMEN INI DIKONTROL DALAM FORMAT HARDCOPY_
THIS DOCUMENT IS CONTROLLED IN HARDCOPY FORMAT
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QA/QC LABORATORY
µkal = ketidakpastian labu volumetri: √ 3

µkal = uncertainty of volumetric flask: √ 3
= 0.087: √ 3
= 0.05023 mL
b. Ketidakpastian efek temperature (µtemp)
Temperature influence uncertainty (µtemp)
Variasi temperature di Lab ± 3°C
Temperature variation in lab ± 3°C
Koefisien muai air = 0.00021/°C
Water expansion coefficient = 0.00021/°C
µtem = ((variasi temperature) x (koefisien muai air) x (volume labu volumetri)) / √ 3
= ((temperature variation) x (water expansion coefficient ) x (volumetric flask size))
/√ 3
= (3°C x 0.00021/°C x 500 mL) / √ 3 ¿
= 0.181865 mL
c. Ketidakpastian labu volumetri 500 mL
Uncertainty of volumetric flask 500 mL
µLV500 = √ (µ kal)2+(µtem)2
= √ (0.050229)2 +(0.181865)2
= 0.188674 mL
3.3. Ketidakpastian Asal Larutan Standar
Uncertainty of Standard Solution
Deret standar (ppm) Konsentrasi standar /terkonversi (%)
Standard series (ppm) Standard concentration /converted (%)
0.00 0.000
1.00 0.250
2.00 0.500
3.00 0.750
Representative untuk larutan standar tersebut adalah 1 ppm, cara pembuatannya:
Representative for standard solution above is 1 ppm, how to make:
Konsentrasi induk Dipipet Labu volumetri Konsentrasi larutan
Parent solution Pipetted Volumeteric flask Solution Concentration
1000 ppm 1 mL 1000 mL 1 ppm
3.3.1. Standar Tengah

Intermediate standard
a. Labu Volumetri 1000 mL
Volumetric flask 1000mL
Ketidakpastian labu volumetri berdasarkan sertifikat kalibrasi ± 0.14 mL dengan k = 2
Uncertainty of volumetric flask based on calibration certificate ± 0.14 mL with k = 2
µkal = ketidakpastian labu volumetri 1000 mL: √ 3
uncertainty of volumetric flask 1000 mL: √ 3

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QA/QC LABORATORY
= 0.14: √ 3
= 0.080829 mL
Variasi temperature di Lab ± 3°
Temperature variation in Lab ± 3°C
µtem = ((variasi temperature) x (koefisien muai air) x (volume labu volumetri)) / √ 3
((temperature variation) x (water expansion coefficient) x (volumetric flask
size)) /√ 3
= (3°C x 0.00021/°C x 1000 mL) / √ 3 ¿
= 0.363731 mL
Ketidakpastian labu volumetri 1000 mL
Uncertainty of volumetric flask 1000 mL
µLV1000 = √ (µ kal)2+(µtem)2
= √ (0,08082)2 +( 0,36373)2
= 0,372603 mL
b. Pipet Volumetri 1 mL
Volumetric pipetted 1 mL
Ketidakpastian pipet volumetri berdasarkan sertifikat kalibrasi ± 0.003 mL dengan k=2
Uncertainty of volumetric pipette based on calibration certificate ± 0.003 mL with k=2
µkal = ketidakpastian pipet volumetri 1 mL: √ 3
uncertainty of volumetric pipette 1 mL: √ 3
= 0.003: √ 3
= 0.001732 mL
Variasi temperature di Lab ± 3°C
Temperature variation in Lab ± 3°C
µtem = ((variasi temperature) x (koefisien muai air) x (volume pipet volumetri)) / √ 3
((temperature variation) x (water expansion coefficient) x (pipette volumetric
size)) / √ 3
= (3°C x 0.00021/°C x 1 mL) / √ 3 ¿
= 0.000364 mL
Ketidakpastian labu volumetri 1 mL
Uncertainty of volumetric pipette 1 mL
µLV1 = √ (µ kal)2+(µtem)2
= √ (0.001732)2 +(0.000364)2
= 0.00177 mL
3.3.2. COA standard Cu 1000 ppm

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QA/QC LABORATORY
Standard COA Cu 1000 ppm

Larutan induk Cu 1000 ppm
Parent solution Cu 1000 ppm
Volume labu volumetri = 1000 mL
Volumetric flask size = 1000 mL
Ketidakpastian Cu (pada sertifikat) = 5 dengan k = 2
Uncertainty Cu (on certificate) = 5 with k = 2
µtipe B = ketidakpastian Cu: k
uncertainty Cu: k
= 5:2
= 2.5 ppm
Ketidakpastian Volume (mL) Value u/V (u/V)^2

µLV1000 1000 0.372603453 0.000372603 1.38833E-07
µPV1 1 0.001769831 0.001769831 3.1323E-06
µC1000 1000 2.5 0.0025 0.00000625
√√ ( )( ) (
µ LV 1000 2 µP V 1 2 µC 1000
)
2
µC1 = C1 + +
V 1000 V1 V 1000
= 1 (1.38833E-07)+(3.1323E-06)+(0.00000625)
= 0.003086 ppm
Ketidakpastian µC1 merupakan representative dari 3 deret standar yang digunakan,
sehingga hasil µC1 dibagi 3.
The uncertainty µC1 is representative of the 3 standard series used, so the results of µC1 are
divided by 3.
µtipe A = µC1: 3
= 0.003086: 3
= 0.001028 ppm
3.4. Ketidakpastian Asal Alat AAS
Uncertainty of AAS
3.4.1. Repeatability
Sample: Inh Head
Date:16 July 2023
Sampl Concentrati Sampl Concentrati Sampl Concentrati
e on e on e on
1 0.321 11 0.319 21 0.320
2 0.321 12 0.321 22 0.322
3 0.320 13 0.319 23 0.322
4 0.321 14 0.323 24 0.318
5 0.319 15 0.321 25 0.324
6 0.318 16 0.322 26 0.319
7 0.319 17 0.320 27 0.318
8 0.318 18 0.319 28 0.322
9 0.323 19 0.320 29 0.319

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QA/QC LABORATORY
10 0.322 20 0.319 30 0.318

Average 0.320
SD 0.00172
RSD 0.54
= SD: √ n
µRepeatability
= 0.00172: √ 30
= 0.000313 %
3.4.2. Reproducibility
Sample: Inh Head
Date:16 July 2023
AAS Perkin AAS
Sample Sample
Elmer Agilent
1 0.315 1 0.316
2 0.315 2 0.317
3 0.315 3 0.317
4 0.316 4 0.316
5 0.317 5 0.317
6 0.315 6 0.317
7 0.315 7 0.316
8 0.316 8 0.316
9 0.317 9 0.316
10 0.317 10 0.316
Average 0.316
SD 0.00079
RSD 0.24931
= SD: √ n
µReproducibility
= 0.00079: √ 20
= 0.000176 %
3.5. Ketidakpastian Asal Kurva Kalibrasi
Uncertainty In Calibration Curves
a. Deret standar kalibrasi
Standard calibration series
Nama Konsentrasi Absorbansi
Blank 0.000 0.0000
Standar 1 0.250 0.0838
Standar 2 0.500 0.1675
Standar 3 0.750 0.2428

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0.3000
0.2500
f(x) = 0.32988 x + 0.000869999999999996
0.2000 R² = 0.999839380065267
0.1500
0.1000
0.0500
0.0000
0.000 0.100 0.200 0.300 0.400 0.500 0.600 0.700 0.800
b. Hasil pembacaan smpel

Sample reading results
Y sample = 0.1065
Cx diperoleh dari kurva kalibrasi dengan persamaan garis y=ax+ b
Cx obtained from the calibration curve with the equation of the line y=ax+ b
Dimana α = 0.3299, b = 0.0009
y sampel−b 0.1065 – 0.0009
Cx = =
a 0.3299
= 0.320 %
Cs = Cx
= 0.320 %
Keterangan :
Remarks:
Cx = Konsentrasi Cu dari kurva kalibrasi (%)
= Cu concentration from calibration curves (%)
Cs = Konsentrasi Cu dalam sampel (%)
= Cu concentration in sample (%)
c. Perhitungan ketidakpastian kurva kalibrasi
Uncertainty calculation of calibration curves
xi yi xi2 xi.yi yc yi-yc (yi-yc)2 xi-xaverage (xi-x average)2

0.0008
0 0 0.00000 0.00000 7 -0.00087 0.0000007569 -0.375 0.140625
0.0833
0.250 0.0838 0.06250 0.02095 4 0.00046 0.0000002116 -0.125 0.015625
0.1658
0.500 0.1675 0.25000 0.08375 1 0.00169 0.0000028561 0.125 0.015625
0.2482
0.750 0.2470 0.56250 0.18525 8 -0.00128 0.0000016384 0.375 0.140625
Jumlah 1.500 0.498 0.875 0.290 0.498 0.000 0.000 0.000 0.313
Averag
e 0.375 0.125 0.219 0.072 0.125 0.000 0.000 0.000 0.078
ysample = 0.1065

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QA/QC LABORATORY
ysample – yiaverage = 0.1065 – 0.1246

= -0.0181
Sy/x =
√ ∑ ( yi− yc)2
n−2
=
√ 0.0000047061
4−2
= 0.00165 %
=
√
0.001534 1 1 (−0.0596)2
0.3248 30 + 4 + 0.32992 . 0.125000
√
S y /x 1 1 ( ysampel− yaverage)
2 = 0.00271 %
µCx = + + 2
a m n a . ∑ (xi−xi average)2
Keterangan:
xi = konsentrasi larutan standar (%)
xi = standard solution concentration (%)
yi = absorbansi larutan standar
yi = standard solution absorbance
α = slope
b = intersept
yc = absorbansi dari persamaan regresi linear
yc = absorbance from the linear regression equation
Sy/x = simpangan baku residual (%)
Sy/x = residual standard deviation (%)
m = jumlah pengulangan sampel
m = number of sample repetitions
n = jumlah larutan standar
n = number of standard solutions
3.6. Ketidakpastian Asal Operator
Operator Uncertainty
3.6.1. Repeatability
Sample: Inh Head
Date:16 July 2023
Sampl Concentrati Sampl Concentrati Sampl Concentrati
e on e on e on
1 0.321 11 0.319 21 0.320
2 0.321 12 0.321 22 0.322
3 0.320 13 0.319 23 0.322
4 0.321 14 0.323 24 0.318
5 0.319 15 0.321 25 0.324
6 0.318 16 0.322 26 0.319
7 0.319 17 0.320 27 0.318

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QA/QC LABORATORY
8 0.318 18 0.319 28 0.322

9 0.323 19 0.320 29 0.319
10 0.322 20 0.319 30 0.318
Average 0.320
SD 0.00172
RSD 0.54
µRepeatibility = SD: √ n
= 0.00172: √ 30
= 0.000313 %
3.6.2. Reproducibility
Sample: Inh Head
Date:16 July 2023
I Gede I Nyoman
Sampel Sampel
Budiartha Triana
1 0.315 1 0.316
2 0.315 2 0.317
3 0.315 3 0.317
4 0.316 4 0.316
5 0.317 5 0.317
6 0.315 6 0.317
7 0.315 7 0.316
8 0.316 8 0.316
9 0.317 9 0.316
10 0.317 10 0.316
Average 0.316
SD 0.000788
RSD 0.24931
= SD: √ n
µReproducibility
= 0.000788: √ 20
= 0.000176 %
3.7. Ketidakpastian Gabungan
Combined Uncertainty
Parameter x Satuan µ µ/x (µ/x)2
Ketidakpastian timbangan
0.2000 g 0.000120 0.00060 3.613E-07
Balance uncertainty
Ketidakpastian alat gelas
500 mL 0.188674 0.00038 1.424E-07
Glassware uncertainty
Ketidakpastian Larutan Standar
1 mg/L 0.001029 0.00103 1.058E-06
Uncertainty of Standard Solution
Ketidakpastian AAS Repeatibility
0.320 % 0.000313 0.00098 9.568E-07
Uncertainty of AAS Repeatability
Ketidakpastian AAS Reproducibility
0.316 % 0.000477 0.00157 2.472E-06
Uncertainty of AAS Reproducibility
Ketidakpastian Kurva kalibrasi 0.320 % 0.002712 0.00847 7.170E-05

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QA/QC LABORATORY
Uncertainty of Calibration Curves

Ketidakpastian Operator Repeatibility
0.320 % 0.000313 0.00098 9.568E-07
Uncertainty of Operator Repeatability
Ketidakpastian Operator Reproducibility
0.316 % 0.000176 0.00056 3.108E-07
Uncertainty of Operator Reproducibility
0.0000780
JUMLAH
Cs = 0.320 %
√
2
µCs = Cs ∑ ( µ )
x
= 0.320 √ 0.000125136
= 0.0028 %
Untuk tingkat kepercayaan = 95% digunakan faktor k=2:
For the confidence level = 95%, the factor k = 2 is used:
µCs = k. µCs
= 2. 0.0028 %
= 0.006 %
4. KESIMPULAN (CONCLUSION)
Jadi, estimasi ketidakpastian metode penetapan Cu dalam sampel Head menggunakan metode
CDC-QAC-012-S030 adalah ± 0.006 % dengan tingkat kepercayaan 95%.
The estimated uncertainty of the method for determining Cu in Head samples using the CDC-
QAC-012-S030 procedure is ± 0.006 % ppm with a 95% confidence level.
Disahkan di/Approval Location :

Tanggal:/Date :
Dibuat oleh_Author: Diperiksa oleh_Checked by:
Sr. Chemist – Research & Sr. Chemist - Quality Control & Statistic
Continuous Improvement
Disahkan oleh_Approved by:

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QA/QC Lab Manager


Uncertainty Cu Low Conc

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Page: 1 of 10 Version: 1.0

COA standard Repeatibility Calibration Curve

Standard Solution Operator

µkal = ketidakpastian labu volumetri: √ 3

3.3.1. Standar Tengah

DOKUMEN INI DIKONTROL DALAM FORMAT HARDCOPY_

3.3.2. COA standard Cu 1000 ppm

DOKUMEN INI DIKONTROL DALAM FORMAT HARDCOPY_

Standard COA Cu 1000 ppm

Ketidakpastian Volume (mL) Value u/V (u/V)^2

DOKUMEN INI DIKONTROL DALAM FORMAT HARDCOPY_

10 0.322 20 0.319 30 0.318

DOKUMEN INI DIKONTROL DALAM FORMAT HARDCOPY_

b. Hasil pembacaan smpel

xi yi xi2 xi.yi yc yi-yc (yi-yc)2 xi-xaverage (xi-x average)2

DOKUMEN INI DIKONTROL DALAM FORMAT HARDCOPY_

ysample – yiaverage = 0.1065 – 0.1246

DOKUMEN INI DIKONTROL DALAM FORMAT HARDCOPY_

8 0.318 18 0.319 28 0.322

DOKUMEN INI DIKONTROL DALAM FORMAT HARDCOPY_

Uncertainty of Calibration Curves

Disahkan di/Approval Location :

Dibuat oleh_Author: Diperiksa oleh_Checked by:

Disahkan oleh_Approved by:

DOKUMEN INI DIKONTROL DALAM FORMAT HARDCOPY_

QA/QC Lab Manager

DOKUMEN INI DIKONTROL DALAM FORMAT HARDCOPY_

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