FR No : 19-1/P3KLL

Revisi : 1

EVALUASI DATA VERIFIKASI METODE PENGUJIAN

1. Informasi Umum

Parameter : Ortofosfat
Acuan Metode : Standar Method, APHA No. 4500 P.E - 2017
Rentang Pengukuran : 0,05-1,5 mg/L
Peralatan : Spektrofotometer HITACHI 3010
Nama Analis : Rany Ramadhani (air sungai)

Tanggal Pengujian : 29 Maret- 1 April 2021

2. Penentuan Linearitas Kurva Kalibrasi

Larutan
Konsentrasi (mg/L) Absorbansi
Standar
Kurva Kalibrasi Orto Fosfat
std 1 0.00 0.002
std 2 0.05 0.013 0.3
f(x) = 0.192465733235077 x + 0.004329403095063
std 3 0.1 0.021 R² = 0.998972763104851
std 4 0.2 0.042 0.25
std 5 0.40 0.084
std 6 0.60 0.123 0.2
std 7 0.80 0.16
std 8 1.00 0.2
0.15
std 9 1.20 0.238
std 10 1.40 0.275
0.1
std 11 1.50 0.285
Method Slope 0.1925
Intercept 0.0043 0.05
Correlation Determination (R) 0.9990
Correlation Coefficien ( r ) 0.9995 0
Batas keberterimaan r ≥ 0.995 0.00 0.20 0.40 0.60 0.80 1.00 1.20 1.40 1.60
Kesimpulan Diterima
4. Penentuan Method Detection Limit (MDL)
Kons spike - sampel + Kons.
Vol sampel Vol spike Vol Total
Pengulangan Sampel Kons spl (mg/L) Target sampel % Recovery standar Standar
(mL) (mL) (mL)
(mg/L) (mg/L) (mg/L) (mg/L)
1 0.211 0.312 148.6 0.045
2 0.210 0.312 148.6 0.046
3 0.209 0.309 147.1 0.045
4 0.209 0.21 0.313 149.0 0.044 50 0.50 10 50
5 0.210 0.308 146.7 0.047
6 0.211 0.312 148.6 0.048
7 0.211 0.313 149.0 0.049
Rerata 0.311 1556.4
Standar Deviasi (SD) 0.0020
MDL = 3.143xSD 0.0062
LoQ = 10xSD 0.0198
Signal/noise (S/N) 157.5295
% RSD 0.6348
Batas Keberterimaan
1) MDL < Spike < 10 MDL 0.006 < 0.02 < 0.06 Diterima
2) Signal/noise (S/N): 2.5 < S/N < 10 157.5295 Ditolak
3) %RSD ≤ 20% 0.6348 Diterima
4) %R = 100% ± 20% 1556.4 Diterima
5) %RSD < 2/3 Horwitz 0.6348 < 36.1432 Diterima
6) Repetability: %RSD < 1/2 Horwitz 0.6348 < 26.9726 Diterima
7) Reproducibility: %RSD < 2/3 Horwitz 0.6348 < 36.1432 Diterima
KESIMPULAN MDL 0.006 mg/L
KESIMPULAN LoQ 0.020 mg/L
5.Penentuan Trueness, Bias dan Presisi Metode
CRM ERA P 245 - 500
1,29 ± 2,59 %
( 0,629 - 0,662 )

Pengulangan Hasil (mg/L) %R %Bias

1 0.654 130.80 30.80
2 0.655 131.00 31.00
3 0.655 131.00 31.00
4 0.657 131.40 31.40
5 0.657 131.40 31.40
6 0.657 131.40 31.40
7 0.658 131.60 31.60
Rerata 0.656 131.229 31.23
Simpangan Baku ( sd ) 0.0015
%RSD 0.22
% Trueness 131.23
Batas Keberterimaan
1) %RSD < 24.11 0.22 Diterima
2) %R ≈ 80% - 120% 131.229 Diterima
3. Penentuan Limit Of Linearity (LOL)
Larutan
Konsentrasi (mg/L) ABS 1 ABS 2 ABS 3 ABS 4 ABS 5 ABS 6 ABS 7 ABS 8 ABS 9 ABS 10 SD
Standar
std 1 0.01 0.0110 0.0120 0.0130 0.0130 0.0120 0.0110 0.0130 0.0130 0.0130 0.0130 0.0008
std 2 0.02
std 3 0.04
std 4 0.08
std 5 0.10
std 6 0.20
std 7 0.40
std 8 0.06
std 9 0.08
std 10 1.00 0.0980 0.0980 0.0981 0.0981 0.0982 0.0982 0.0980 0.0980 0.0985 0.0982 0.0002
Evaluasi :
SD 2
 12 12 
FhitungSD 0.0345
Fhitung  SD
2 2

SD2
Derajat kebebasan, df = n - 1 dan tingkat kepercayaan 99%, α = 0.01 maka Ftabel = F(0,99; 9; 9) = 5.3510
Batas keberterimaan: Fhitung < Ftabel
Kesimpulan Uji F = Diterima Maka, LOL= 1 ppm
4. Reprodusibilitas

spike - sampel + Kons.

Kons Target Vol sampel Vol spike Vol Total
Pengulangan Sampel Kons spl (mg/L) sampel % Recovery standar Standar
(mg/L) (mL) (mL) (mL)
(mg/L) (mg/L) (mg/L)
1 0.027 0.017 85.0 0.044
2 0.027 0.019 95.0 0.046
3 0.028 0.017 85.0 0.045
4 0.028 0.02 0.016 80.0 0.044 50 0.10 10 50
5 0.028 0.019 95.0 0.047
6 0.028 0.019 95.0 0.047
7 0.027 0.022 110.0 0.049
Rerata 0.018 92.1
Standar Deviasi (SD) 0.0020
MDL = 3.143xSD 0.0062
LoQ = 10xSD 0.0199
Signal/noise (S/N) 9.2696
% RSD 10.7879
Batas Keberterimaan
1) MDL < Spike < 10 MDL 0.006 < 0.02 < 0.06 Diterima
2) Signal/noise (S/N): 2.5 < S/N < 10 9.2696 Diterima
3) %RSD ≤ 20% 10.7879 Diterima
4) %R = 100% ± 20% 92.1 Diterima
5) %RSD < 2/3 Horwitz 10.7879 < 55.3107 Diterima
6) Repetability: %RSD < 1/2 Horwitz 10.7879 < 41.2767 Diterima
7) Reproducibility: %RSD < 2/3 Horwitz 10.7879 < 55.3107 Diterima
KESIMPULAN MDL 0.006 mg/L
KESIMPULAN LoQ 0.020 mg/L

spike - sampel + Kons.

Kons Target Vol sampel Vol spike Vol Total
Pengulangan Sampel Kons spl (mg/L) sampel % Recovery standar Standar
(mg/L) (mL) (mL) (mL)
(mg/L) (mg/L) (mg/L)
1 0.027 0.019 95.0 0.046
2 0.027 0.019 95.0 0.046
3 0.028 0.017 85.0 0.045
4 0.028 0.02 0.016 80.0 0.044 50 0.10 10 50
5 0.028 0.018 90.0 0.046
6 0.028 0.020 100.0 0.048
7 0.027 0.022 110.0 0.049
Rerata 0.019 93.57
Standar Deviasi (SD) 0.0020
MDL = 3.143xSD 0.0062
LoQ = 10xSD 0.0198
Signal/noise (S/N) 9.4706
% RSD 10.5590
Batas Keberterimaan
1) MDL < Spike < 10 MDL 0.006 < 0.02 < 0.06 Diterima
2) Signal/noise (S/N): 2.5 < S/N < 10 9.4706 Diterima
3) %RSD ≤ 20% 10.5590 Diterima
4) %R = 100% ± 20% 93.6 Diterima
5) %RSD < 2/3 Horwitz 10.5590 < 55.1828 Diterima
6) Repetability: %RSD < 1/2 Horwitz 10.5590 < 41.1812 Diterima
7) Reproducibility: %RSD < 2/3 Horwitz 10.5590 < 55.1828 Diterima
KESIMPULAN MDL 0.006 mg/L
KESIMPULAN LoQ 0.020 mg/L

Pengulangan Hasil Pengujian (µg/L)

Pengujian Sampel Analis-1 Analis-2
Spl-01 0.017 0.019
Spl-02 0.019 0.019
Spl-03 0.017 0.017
Spl-04 0.016 0.016
Spl-05 0.019 0.018
Spl-06 0.019 0.020
Spl-07 0.022 0.022
Rerata 0.018 0.019
Standar Deviasi (SD) 0.0020 0.0020
RSDr 10.79 10.56
Grand mean 0.019
SDR 0.0019
RSDR 10.28
0,67 Horwitz Value (PRSDR) 55.246
Batas Keberterimaan
RSDr < 0.67PRSDR 10,00 < 55,215
5.1 Penentuan Repetabilitas dan Reprodusibilitas Kadar Rendah (0,02 mg/L)

Repeatabilitas (0,5%CV Horwitz)

No Abs Kadar (mg/L) Rerata %RPD %R
Hasil Kesimpulan
1 0.01 0.019
0.020 -5.13 97.5 14.47 Diterima
0.01 0.020
2 0.01 0.020
0.020 0.00 100.0 14.41 Diterima
0.01 0.020
3 0.01 0.020
0.020 0.00 100.0 14.41 Diterima
0.01 0.020
4 0.01 0.019
0.019 0.00 95.0 14.53 Diterima
0.01 0.019
5 0.01 0.019
0.019 0.00 95.0 14.53 Diterima
0.01 0.019
6 0.01 0.019
0.019 0.00 95.0 14.53 Diterima
0.01 0.019
7 0.01 0.017
0.017 0.00 85.0 14.77 Diterima
0.01 0.017
Rerata 0.019
Standar Deviasi (sd) 0.0010
%RSD 5.23
0,67%CV Horwitz 19.455
Batas Keberterimaan
%RSD < 0.67%CV Horwitz
Diterima
 5.2 Penentuan Repeatabilitas dan Reprodusibilitas Kadar Tengah (0,5 mg/L)

Repeatabilitas (0,5%CV Horwitz)

No Abs Kadar (mg/L) Rerata %RPD %R
Hasil Kesimpulan
1
0.205 0.453
0.453 0.00 90.6 9.01 Diterima
0.205 0.453
2 0.205 0.453
0.453 0.00 90.6 9.01 Diterima
0.205 0.453
3 0.206 0.455
0.455 0.22 91.0 9.01 Diterima
0.206 0.455
4 0.211 0.466
0.467 0.64 93.3 8.97 Diterima
0.211 0.467
5 0.211 0.467
0.469 0.00 93.7 8.97 Diterima
x1  0.212 x0.470
2
6 0.213 0.471
0.471 0.00 94.2 8.96 Diterima 
1 0.213 0.471 1
7 0.205 
0.454
n 1
0.205 0.454
0.454 n
-99.63 90.8 9.01
2
Diterima

Rerata 0.460
Standar Deviasi (sd) 0.0078
%RSD 1.70
0,67%CV Horwitz 12.049
Batas Keberterimaan
%RSD < 0.67%CV Horwitz Diterima
 5.3 Penentuan Repeatabilitas dan Reprodusibilitas Kadar Tinggi (1 mg/L)

Repeatabilitas (0,5%CV Horwitz)

No Abs Kadar (mg/L) Rerata %RPD %R
Hasil Kesimpulan
1
0.443 0.982
0.983 0.10 98.3 8.02 Diterima
0.443 0.983
2 0.443 0.984
0.984 -0.10 98.4 8.02 Diterima
0.443 0.983
3 0.444 0.985
0.985 0.00 98.5 8.02 Diterima
0.444 0.985
4 0.444 0.986
0.987 0.10 98.7 8.02 Diterima
0.445 0.987
5 0.442 0.981
0.983 0.31 98.3 8.02 Diterima
x1  0.444 x0.984
2
6 0.444 0.985
0.985 0.00 98.5 8.02 Diterima 
1 0.444 0.985 1
7 0.445 
0.987
n 1
0.444 0.986
0.987 n
-0.10 98.7 8.02
2
Diterima

Rerata 0.985
Standar Deviasi (sd) 0.0018
%RSD 0.18
0,67%CV Horwitz 10.745
Batas Keberterimaan
%RSD < 0.67%CV Horwitz Diterima

Kesimpulan : Metode terverifikasi sesuai persyaratan teknis dan dapat diterapkan di laboratorium pengujian

Mengetahui,
Penyelia Lab. Air Deputi Manajer Teknis
(Oktaria Diah P) ( Ernawita Nazir)
FR No : 19-1/P3KLL
Revisi : 1

EVALUASI DATA VERIFIKASI METODE PENGUJIAN

1. Informasi Umum

Parameter : Ortofosfat
Acuan Metode : Standar Method
Rentang Pengukuran : 0,01-1 mg/L
Peralatan : Spektrofotometer HITACHI 3010
Nama Analis : Oktaria Diah Pitalokasari

Tanggal Pengujian : 27 Desember s/d 19 Februari 2018

2. Penentuan Linearitas Kurva Kalibrasi

Larutan
Konsentrasi (mg/L) Absorbansi
Standar Kurva Kalibrasi Orto Fosfat
std 1 0.00 0.009
std 2 0.01 0.014 0.3
std 3 0.02 0.020 f(x) = 0.192465733235077 x + 0.004329403095063
R² = 0.998972763104851
std 4 0.04 0.033 0.25
std 5 0.08 0.053
std 6 0.10 0.074 0.2
std 7 0.20 0.133
std 8 0.40 0.255 0.15
std 9 0.60 0.393
std 10 0.80 0.512
0.1
std 11 1.00 0.650
Method Slope 0.6385
Intercept 0.0064 0.05
Correlation Determination (R) 0.9997
Correlation Coefficien ( r ) 0.9998 0
0.00 0.20 0.40 0.60 0.80 1.00 1.20
Batas keberterimaan r ≥ 0.995
Kesimpulan Diterima

3. Penentuan Method Detection Limit (MDL)

Kons spike - sampel +
Pengulangan Sampel Kons spl (mg/L) Target sampel % Recovery standar
(mg/L) (mg/L) (mg/L)
1 0.027 0.018 90.0 0.045
2 0.027 0.019 95.0 0.046
3 0.028 0.017 85.0 0.045
4 0.028 0.02 0.016 80.0 0.044
5 0.028 0.019 95.0 0.047
6 0.028 0.020 100.0 0.048
7 0.027 0.022 110.0 0.049
Rerata 0.019 93.6
Standar Deviasi (SD) 0.0020
MDL = 3.143xSD 0.0062
LoQ = 10xSD 0.0198
Signal/noise (S/N) 9.4706
% RSD 10.5590
Batas Keberterimaan
1) MDL < Spike < 10 MDL 0.006 < 0.02 <
2) Signal/noise (S/N): 2.5 < S/N < 10 9.4706
3) %RSD ≤ 20% 10.5590
4) %R = 100% ± 20% 93.6
5) %RSD < 2/3 Horwitz 10.5590 <
6) Repetability: %RSD < 1/2 Horwitz 10.5590 <
7) Reproducibility: %RSD < 2/3 Horwitz 10.5590 <
KESIMPULAN MDL 0.006
KESIMPULAN LoQ 0.020

5.Penentuan Trueness, Bias dan Presisi Metode

CRM ERA P 245 - 500
1,29 ± 2,59 %
( 0,629 -SD
0,662
2
)
Fhitung  1

SD22
Pengulangan Hasil (mg/L) %R %Bias
1 0.654 130.80 30.80
2 0.655 131.00 31.00
3 0.655 131.00 31.00
4 0.657 131.40 31.40
5 0.657 131.40 31.40
6 0.657 131.40 31.40
7 0.658 131.60 31.60
Rerata 0.656 131.229 31.23
Simpangan Baku ( sd ) 0.0015
%RSD 0.22
% Trueness 131.23
Batas Keberterimaan
1) %RSD < 24.11 0.22 Diterima
2) %R ≈ 80% - 120% 131.229 Diterima

6. Penentuan Limit Of Linearity (LOL)

Larutan
Konsentrasi (mg/L) ABS 1 ABS 2 ABS 3 ABS 4 ABS 5
Standar
std 1 0.01 0.0110 0.0120 0.0130 0.0130 0.0120
std 2 0.02
std 3 0.04
std 4 0.08
std 5 0.10
std 6 0.20
std 7 0.40
std 8 0.06
std 9 0.08
std 10 1.00 0.0980 0.0980 0.0981 0.0981 0.0982
Evaluasi :
SD 2
 12 12 
FhitungSD 0.0345
Fhitung  SD
2 2

SD 2
Derajat kebebasan, df = n - 1 dan tingkat kepercayaan 99%, α = 0.01 maka Ftabel = F(0,99; 9; 9) =
Batas keberterimaan: Fhitung < Ftabel
Kesimpulan Uji F = Diterima Maka, LOL= 1 ppm
TODE PENGUJIAN

alibrasi Orto Fosfat

004329403095063

0 0.80 1.00 1.20 1.40 1.60

Kons.
Vol sampel Vol spike Vol Total
Standar
(mL) (mL) (mL)
(mg/L)

50 0.10 10 50
 0.06 Diterima
Diterima
Diterima
Diterima
55.1828 Diterima
41.1812 Diterima
55.1828 Diterima
mg/L
mg/L

ABS 6 ABS 7 ABS 8 ABS 9 ABS 10 SD

0.0110 0.0130 0.0130 0.0130 0.0130 0.0008

0.0982 0.0980 0.0980 0.0985 0.0982 0.0002

5.3510