Abstract
The analytical method for methylmercury in sediment samples was performed using an hyphenated system of gas chromatograph coupled atomic fluorescence detector (GC-AFS). Methylmercury in sediment samples was leached and extracted into dichloromethane with the assistance of HNO3, KCl and CuSO4. Dichloromethane was evaporated resulting in the relocation of MeHg to the aqueous phase. MeHg was then extracted in the form of diethyldithiocarmate complex into hexane followed by the alkylation processes with Grignard reagents, butyl magnesium chloride and ethyl magnesium chloride. The alkylation reactions were optimized with respect to the mounts of Grignard reagents, the reaction temperature and time for the best alkylation yields and least extent of trans-alkylation and degradation of the alkylated products. The alkylated MeHg compounds were analyzed by GC-AFS. The analytical method for methylmercury was validated using certified reference material ERM-CC580. The instrumental limit of detection was 1.4 pg as Hg. The method limits of detection for EtMgCl and BuMgCl were 0.18 were 0.18 ng/g and 0.19 ng/g, respectively. This method can be used to analyze MeHg in sediment samples.
Highlights
Các nghiên cứu càng về sau tập trung vào xác định Hg nguyên dạng đặc biệt là methyl thủy ngân (MeHg) trong các đối tượng có hàm lượng Hg rất thấp, thí dụ các mẫu môi trường như nước và bùn lắng, vì thế yêu cầu về độ nhạy của phương pháp/thiết bị phân tích ngày càng cao
The alkylated MeHg compounds were and extracted into dichloromethane with the analyzed by GC-AFS
The analytical method for assistance of HNO3, KCl and CuSO4. methylmercury was validated using certified Dichloromethane was evaporated resulting in the reference material ERM-CC580
Summary
Phương pháp phân tích methyl thủy ngân (MeHg) đuợc nghiên cứu trên hệ thống sắc ký khí ghép nối đầu dò huỳnh quang nguyên tử (GCAFS). MeHg được alkyl hóa bằng hai loại tác chất Grignard, butyl magnesium chloride (BuMgCl) và ethyl magnesium chloride (EtMgCl). Giới hạn phát hiện của thiết bị GC-AFS và của phương pháp phân tích sử dụng hai tác chất alkyl hóa lần lượt là 1,4 pg; 0,18 ng/g MeHg đối với tác chất EtMgCl và 0,19 ng/g MeHg đối với tác chất BuMgCl. Phương pháp này có thể đuợc ứng dụng để xác định methyl thủy ngân trong đất, bùn thải và bùn lắng. Từ khóa: đầu dò huỳnh quang nguyên tử, methyl thủy ngân, sắc ký khí, bùn lắng, tác chất Grignard
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