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PENGEMBANGAN DAN VALIDASI METODE SPEKTROFOTOMETRI BERDASARKAN REAKSI PENGURAIAN PRUSSIAN BLUE UNTUK ANALISIS KADAR KLOR BEBAS DALAM PRODUK DISINFEKTAN
Abstrak (Bhs. Indonesia)
Latar Belakang: Spektrofotometri merupakan metode sederhana yang dapat dikembangkan untuk penetapan kadar klor. Klor mampu mengoksidasi fero menjadi feri sehingga prussian blue yang terbentuk melalui reaksi antara FeSO4 dengan K3Fe(CN)6 menjadi terurai. Jumlah prussian blue yang terurai akan diukur intensitasnya menggunakan spektrofotometer UV/VIS. Tujuan penelitian ini adalah mengembangkan dan memvalidasi metode spektrofotometri visible berdasarkan reaksi penguraian prussian blue untuk analisis kadar klor dalam produk disinfektan. Metodologi: Metode analisis dimulai dengan menstandarisasi bahan klor yang akan dijadikan larutan kerja. Penentuan panjang gelombang,optimasi pembentukan prussian blue, penetapan operating, dan vaidasi metode. Selanjutnya metode yang telah dikembangkan dan divalidasi diaplikasikan terhadap produk disinfektan berbahan aktif klor yang beredar dipasaran. Hasil Penelitian: Hasil penelitian yang didapatkan yaitu konsentrasi bahan larutan standar adalah 560 mM. Panjang gelombang pengukuran 750 nm. Konsentrasi optimal FeSO4 2 mM, K3Fe(CN)6 3 mM, dan HCl 0,5 M, dengan operating time 15 menit. Parameter validasi yang didapatkan yaitu linearitas (r2) 0,97 pada rentang 2,8-11,2 mM, akurasi (% recovery) 91,67-100,41%, presisi interday (% RSD) 1,87-8,72%, presisi intraday (% RSD) 2,46-11,69%, selektivitas dengan penambahan eksipien mendapatkan % recovery 103,17-105,41%, batas deteksi 0,70 mM, dan batas kuantifikasi 2,34 mM. Hasil aplikasi metode terhadap produk disinfektan berbahan aktif klor menghasilkan % recovery terhadap klaim label sebesar 27,24-86,5 8%. Kesimpulan: Penguraian prussian blue oleh klor dapat dianalisis menggunakan spektrofotometri visible, memenuhi persyaratan parameter validasi linearitas, akurasi, dan selektivitas, namun tidak memenuhi syarat parameter presisi. Aplikasi metode kurang sesuai dengan klaim label.
Abtrak (Bhs. Inggris)
Background: Spectrophotometric determination of chlorine is a simple method to develop. Chlorine can oxidize ferro into ferri, therefore prussian blue that form from the reaction between FeSO4 with K3Fe(CN)6 become decompose. The value of decomposes prussian blue and its intensity will be measured using spectrophotometer UV/VIS. This study aims to develop and validate visible spectrophotometric method using using the prussian blue desomposition reaction for the analysis of free chlorine in disinfectant products. Methodology: The development start with standarized chlorine material for working standart. The measurement wavelenght choosen by scanning the maximum wavelenght of prussian blue that form from dari 1 ml of FeSO4 2 mM, 1 ml of K3Fe(CN)6 2.5 mM, 1 ml of HCl 2 M and chlorine standard 11.2: 2.8 Mm; 1.12 mM respectively in range 400-800nm. The formation of prussian blue optimized by the optimation of FeSO4, K3Fe(CN)6, and HCl concentration. The operating time choosen using chlorine standard 2.8 mM in time range between 0-60 minutes. The conducted validation variables were linearity, range, accuracy, precision, selectivity, detection limit and quantitation limit. Then the method that have been develop and validated were applied for the determination of free chlorine in disinfectant products. Result: The result of this study were, the consentration of reference standard material was 560mM. The measurement wavelength was 750nm, the optimal consentration of FeSO4 was 2 mM, K3Fe(CN)6 was 3 mM and HCl 0.5 M, with 15 minutes operating time. The value of validation variable linearity (r2) was 0.97 on range 2.8-11.2 mM, accuracy (% recovery) was 91.67-100.41%, interday precision (% RSD) was 1.87-8.72%, intraday presicion (% RSD) was 2.46-11.69%, selectivity for excipients with a recovery rate was 103.17-105.41%, limit of detection was 0.70 mM, and limit of quantitation was 2.34 mM. The result of this method application % recovery was 27.24-86.58% from label claim. Conclusion: The decompose prussian blue can be analyzed using visible spectrophotometric, fulfilled the requirement of validation variable like linearity, accuracy, and selectivity, but did not fulfill the precision requirement. The application of this method were not approprite enough with the label claim.
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