Malaysian Journal of Analytical Sciences Vol 25 No 2 (2021): 311 - 323

 

 

 

 

INFLUENCE OF MINERALS ON CONTROL MEASUREMENT OF AMMONIUM, NITRITE, NITRATE AND PHOSPHATE USING UV-SPECTROPHOTOMETER

 

(Pengaruh Mineral Terhadap Pengukuran Kawalan bagi Ammonium, Nitrit, Nitrat dan Fosfat Menggunakan Spektrofotometer UV)

 

Md. Salatul Islam Mozumder*, Shehab Shahreyar, Saiful Islam, Md. Delowar Hossain

 

Department of Chemical Engineering and Polymer Science,

Shahjalal University of Science and Technology, Sylhet-3114, Bangladesh

 

*Corresponding author:  salatul-cep@sust.edu

 

 

Received: 12 February 2021; Accepted: 30 March 2021; Published:  25 April 2021

 

 

Abstract

Interference of different minerals on UV-spectrophotometric determination of ammonium nitrogen (NH4+-N), nitrite-nitrogen (NO2−-N), nitrate-nitrogen (NO3−-N) and phosphate (PO43-) was investigated in this study. Iron, magnesium and sodium acetate had significant interference in Nesslerization of NH4+-N which was needed to adopt standard protocol for the accurate determination of NH4+-N. However, adding 5 times higher Nessler reagent compared to standard method was used to overcome the limitations due to interference of minerals. In determination of NO2−-N through sulphanilmide method, magnesium and iron did not show any significant affect. Presence of 5 g/L sodium acetate reduced the slope of calibration curve of NO2−-N from 0.603 to 0.224. Presence of sodium, either in form of sodium acetate or sodium chloride, reduced the absorbance of sulphanilmide method for NO2−-N determination. Increasing sodium acetate concentration from 2 to 10 g/L, the absorbance of 4 mg/L NO2−-N was reduced by 5 times: 1.50 to 0.34. Identical absorbance for 4 mg/L NO2−-N was found in the presence of 0.84 g/L NaCl (≈ 0.33 g/L Na+) and 2 g/L Na-acetate (≈ 0.56 g/L Na+) which indicated that chlorine also had interference on NO2−-N measurement. The complex formed by nitration of salicylic acid was not interfered by the presence of potassium, phosphate, sodium, magnesium, iron and sodium acetate; almost the same slope (0.0095) was observed for both with and without presence of minerals. In addition, Ammonium molybdate method for the determination of PO43- was a robust method since the measurement was not affected in the presence of minerals.

 

Keywords:   UV-spectrophotometer, Nesslerization, sulphanilmide method, salicylic acid method, ammonium-molybdate method

 

Abstrak

Gangguan mineral berbeza dalam penentuan ammonium nitrogen (NH4+-N), nitrit-nitrogen (NO2−-N), nitrat-nitrogen (NO3−-N) dan fosfat (PO43-) melalui spektrofotometrik-UV telah disiasat dalam kajian ini. Ferum, magnesium dan natrium asetat menghasilkan gangguan yang signifikan tindak balas Nessler bagi NH4+-N yang perlu di adaptasi dalam protokol piawai bagi penentuan tepat NH4+-N. Walau bagaimanapun, penambahan 5 kali ganda reagen Nessler berbanding kaedah piawai telah digunakan untuk mengatasi kelemahan iaitu gangguan dari mineral. Dalam penentuan NO2−-N menggunakan kaedah sulfanilmida, magnesium dan ferum tidak menunjukkan kesan yang signifikan. Kehadiran 5 g/L natrium asetat mengurangkan cerun lengkung kalibrasi NO2−-N dari julat 0.603 hingga 0.224. Kehadiran sodium, sama ada dalam bentuk natrium asetat atau natrium klorida, mengurangkan  serapan  bagi  kaedah sulfanilmida dalam penentuan NO2−-N.  Peningkatan  kepekatan  natrium  asetat  dari  julat 2 hingga 10 g/L, serapan 4 mg/L NO2−-N menurun sebanyak 5 kali ganda: 1.50 hingga 0.34. Serapan sama bagi 4 mg/L NO2−-N diperolehi dengan kehadiran 0.84 g/L NaCl (≈ 0.33 g/L Na+) dan 2 g/L Na-asetat (≈ 0.56 g/L Na+) telah menjelaskan klorin memberi gangguan kepada pengukuran NO2−-N. Kompleks yang terhasil melalui penitratan oleh asid salisilik tidak diganggu oleh kehadiran kalium, fosfat, natrium, magnesium, ferum dan natrium asetat, kecerunan yang sama (0.0095) telah diperhatikan bagi kehadiran mineral atau sebaliknya. Selanjutnyam kaedah ammonium molibidat bagi penentuan PO43- diketahui kaedah teguh kerana pengukuran tidak diganggu dengan kehadiran mineral.

 

Kata kunci:     spektrofotometer UV, tindak balas Nessler, kaedah sulfanilmida, kaedah asid salisilik, kaedah ammonium-molibdat

 

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