Sains Malaysiana 48(5)(2019): 1011–1018

http://dx.doi.org/10.17576/jsm-2019-4805-09

 

Development of an HPLC Method for Formic Acid Analysis through Peak Exclusion Approach

(Pembangunan Kaedah HPLC bagi Analisis Asid Formik melalui Pendekatan Pengecualian Puncak)

 

DANIYAL HASAN¹, IRAM MAHMOOD^2*, ISHFAQ AHMAD³, FARAH AZIZ⁴ & ISHAQ AHMAD^5,6

 

¹School of Chemical and Materials Engineering, National University of Science and Technology, Sector H-12, Islamabad, Pakistan

 

²Department of Industrial Engineering, College of Engineering, King Khalid University, Abha 61413, Kingdom of Saudi Arabia

 

³Department of Mathematics and Statistics, Faculty of Basic and Applied Sciences, International Islamic University, Islamabad, Pakistan

 

⁴Department of Public Health, Faculty of Applied Medical Sciences, King Khalid University Khamis Mushait, Kingdom of Saudi Arabia

 

⁵National Center for Physics, Islamabad, 44000, Pakistan

 

⁶NPU-NCP Joint International Research Center for Advanced Nanomaterials and Defects Engineering, Northwestern Polytechnical University, Xi’an 710072, China

 

Received: 6 February 2019/Accepted: 7 March 2019

 

ABSTRACT

High Performance Liquid Chromatography (HPLC) is a chemical analysis technique that gives both the quantitative and qualitative analysis of liquid samples. A certain set of parameters, called HPLC method, are defined for analysis of every discrete mixture. Often literature is not available or specifically reported expensive HPLC apparatus is not available for every set of mixtures. Present study concentrated on analysis of formic acid from a mixture of methanol, formaldehyde and water. Formic acid is a basic carboxylic acid that has growing industrial and commercial uses, especially as a refrigerant. A C-18 column was utilized for the analysis by optimizing the parameters like dimensions of the stationary column, nature of mobile phase, flow rate of mobile phase and wavelength of the ultraviolet detector. Comprehendible and reproducible results for the analysis of formic acid were obtained on 25 cm long C-18 stationary column, by tuning the combined effect of water as mobile phase at a flow rate of 1 mL/min and by excluding the unnecessary peaks at 250 nm wavelength of ultraviolet detector, called peak exclusion approach. The calibration curve was found to be linear over the range of 1.25 % v/v formic acid solution in methanol up to 100 % pure formic acid. Limit of detection (LOD) and limit of quantitation (LOQ) were found to be 2.25 % and 6.83 %, respectively.

 

Keywords: C-18 columns; calibration; flow rate; formic acid; peak exclusion

 

ABSTRAK

Kromatografi Cecair Prestasi Tinggi (HPLC) adalah teknik analisis kimia yang memberikan analisis kuantitatif dan kualitatif bagi sampel cecair. Satu set parameter yang dipanggil kaedah HPLC ditakrifkan untuk analisis setiap campuran diskret. Selalunya, kajian kepustakawan tidak diperoleh atau dilaporkan secara khusus untuk setiap set campuran kerana radas HPLC yang mahal. Kajian terkini tertumpu kepada analisis asid formik daripada campuran metanol, formaldehid dan air. Asid formik adalah asid karboksilik asas yang digunakan secara meluas di dalam industri dan komersial, khususnya sebagai bahan penyejuk. Kolum C-18 telah digunakan untuk analisis dengan mengoptimumkan parameter seperti dimensi kolum pegun, jenis fasa mudah alih, kadar aliran fasa mudah alih dan panjang gelombang pengesan ultraungu. Keputusan yang boleh difahami dan boleh ulang untuk analisis asid formik telah diperoleh pada 25 cm panjang kolum pegun C-18, oleh penalaan kesan gabungan air sebagai fasa bergerak pada kadar aliran 1 mL/min dan tidak termasuk puncak tak perlu pada 250 nm panjang gelombang pengesan ultraungu, dikenali sebagai pendekatan pengecualian puncak. Lengkung tentukuran didapati linear ke atas julat larutan asid formik 1.25 % v/v dalam metanol sehingga 100 % asid formik tulen. Had pengesanan (LOD) dan had pengiraaan (LOQ) masing-masing ialah 2.25% dan 6.83%.

 

Kata kunci: Asid formik; kadar aliran; kolum C-18; penentukuran; pengecualian puncak

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*Corresponding author; email: irahmad@kku.edu.sa