Penerapan Desain Eksperimen Plackett-Burman dan Box-Behnken pada Analisis Voltametri Pulsa Diferensial untuk Penentuan Kadar Senyawa Kompleks Gd-DTPA

Santhy Wyantuti, Ravenna Aristantia, Yeni Wahyuni Hartati, Husein H Bahti

Abstract

Gadolinium merupakan salah satu golongan unsur tanah jarang yang menarik karena memiliki sifat paramagnetik yang tinggi. Pengkhelatan gadolinium dengan ligan dietilentriaminpentaasetat (DTPA) menghasilkan senyawa yang berguna dalam bidang kesehatan. Tujuan dari penelitian ini adalah menentukan kandungan unsur tanah jarang gadolinium sebagai kompleks dengan ligan DTPA secara voltametri pulsa diferensial dengan penerapan desain eksperimen Plackett-Burman dan Box-Behnken. Desain eksperimen Plackett-Burman digunakan untuk menyeleksi parameter yang memiliki relevansi positif terhadap respon arus. Parameter yang terpilih kemudian dioptimasi melalui desain eksperimen Box-Behnken sehingga diperoleh kondisi optimum tiap parameter. Parameter yang terseleksi meliputi konsentrasi ligan DTPA, waktu deposisi dan waktu kesetimbangan dengan nilai tiap parameter pada kondisi optimum masing-masing yaitu 150, 13 mgL-1, 60 detik dan 30 detik.  Berdasarkan hasil pengukuran pada kondisi optimum didapat nilai presisi dan akurasi untuk kompleks Gd-DTPA yaitu 99,79% dan 93,42% dengan nilai limit deteksi dan kuantisasi untuk kompleks Gd-DTPA yaitu 3,97 mg/L dan 10,71 mg/L.

 

The Application of Experimental Designs of Plackett-Burman and Box-Behnken in Differential Pulse Voltammetry Analysis for Gd-DTPA Complex Detection. Gadolinium is one of rare earth elements that is interesting because it has high paramagnetic properties. The gadolinium chelating with diethylentriaminpentaacetic acid (DTPA) ligands produces useful compounds in the health field. The purpose of this experiment is to determine amount of gadolinium as complex with DTPA on differential pulse voltammetry by applying Plackett-Burman and Box-Behnken experimental design. The method employed experimental design of Plackett-Burman to select factors, which have positive relevance to response. The selected factors are optimized based on experimental design of Box-Behnken to obtain the optimum condition each factors. The selected factors are ligand concentration, deposition time and equilibrium time with optimum value of 150 mgL-1, 60 s and 30 s, respectively. Based on the result of measurement at optimum condition, the precision and accuracy value for Gd-DTPA complex is 99.79% and 93.42% with detection and quantization limit value for Gd-DTPA complex is 3.97 mg/L and 10.71 mg/L.

Keywords

box-Behnken; dietilentriaminpentaasetat; gadolinium; plackett-burman; voltametri pulsa diferensial.

Full Text:

PDF

References

Baş, D. and Boyacı, İ.H., 2007. Modeling and optimization I: Usability of Response Surface Methodology. Journal of Food Engineering. 78, 836–845. doi: 10.1016/j.jfoodeng.2005.11.024.

Bank, T., Roth, E., Tinker, P., and Granite, E., 2016. Analysis of Rare Earth Elements in Geologic Samples using Inductively Coupled Plasma Mass Spectrometry. Conference Paper. 10, 1-7.

Cuéllar, M., Pfaffen, V., and Ortiz, P.I., 2016. Application of Multi Factorial Experimental Design to Successfully Model and Optimize Inorganic Chromium Speciation by Square Wave Voltammetry. Journal of Electroanalytical Chemistry. 765, 37–44. doi: 10.1016/j.jelechem.2015.07.050.

Fisher, A. and Kara, D., 2016. Determination of Rare Earth Elements in Natural Water Samples – A Review of Sample Separation, Preconcentration and Direct Methodologies. Analytica Chimica Acta. 935, 1–29. doi: 10.1016/j.aca.2016.05.052.

Hendrati, D., Purnamasari, E. S., Effendi, S., and Wyantuti, S., 2018. Pemantapan Proses Sintesis Ligan Dibutilditiokarbamat (DBDTK) Sebagai Pengekstrak Logam Tanah Jarang Berdasarkan Desain Eksperimen. ALCHEMY Jurnal Penelitian Kimia 14(1), 195-203. doi: 10.20961/alchemy.14.1.15006.195-203.

Quinlan, K.R. and Lin, D.K.J., 2015. Run Order Considerations for Plackett and Burman Designs. Journal of Statistical Planning and Inference. 165, 56–62. doi: 10.1016/j.jspi.2015.04.001.

Suyanta, Sunarto, Sari, L.P., Wardani, N.I., and Isa, I.M,. 2014. Differential Adsorptive Stripping Voltametric Determination of Ultra Trace Lanthanum(III) based on Carbon Paste Electrode Modified with 3-Methyl-2-hydrazinobenzothiazole. International Journal of Electrochemical Science. 9, 7763–7772.

Wyantuti S., Pratomo U., Hartati Y. W., Anggraeni A., Bahti H. H., 2018. Fast and Simultaneously Detection of Sm, Eu, Gd, Tb and Dy using Combination of Voltammetry Method and Multivariate Analysis. Res. J. Chem. Environ., 22, 302–306

Xie, F., Zhang, T.A., Dreisinger, D., and Doyle, F., 2014. A Critical Review on Solvent Extraction of Rare Earths from Aqueous Solutions. Minerals Engineering. 56, 10–28. doi: 10.1016/j.mineng.2013.10.021.

Yu, X.L. and He, Y., 2017. Application of Box-Behnken Designs in Parameters Optimization of Differential Pulse Anodic Stripping Voltammetry for Lead(II) Determination in Two Electrolytes. Scientific Reports. 7, 1–8. doi: 10.1038/s41598-017-03030-2.

Zinoubi, K., Majdoub, H., Barhoumi, H., Bou, S.,and Ja, N., 2017. Determination of Trace Heavy Metal Ions by Anodic Stripping Voltammetry using Nano Fibrillated Cellulose Modified Electrode. 799, 70–77. doi: 10.1016/j.jelechem.2017.05.039.

DOI: https://doi.org/10.20961/alchemy.16.1.35166.140-151

Refbacks

  • There are currently no refbacks.