JEOL : Analysis of Simazine and Thiobencarb by GC-MS method using hydrogen carrier gas
March 18, 2024 at 06:16 am
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JMS-Q1600GC UltraQuad™ SQ-Zeta
1. Overview
Helium (He), which is widely used as a carrier gas for GC, may face problems such as temporary price increases or unstable supply conditions due to various reasons, and when supply delays occur, it is necessary to consider using another type of carrier gas as an alternative. Hydrogen and nitrogen are the main alternative gases being considered. Hydrogen, in particular, has a wide linear velocity range for optimum separation and is suitable as a carrier gas for GC. In this report, simazine and thiobencarb, pesticides subject to environmental standards for water pollution, were measured with hydrogen carrier gas. The results show good linearity of the calibration curve and reproducibility at the lower limit of quantification.
2. Methods
Samples were prepared with simazine and thiobencarb at concentrations of 0.01, 0.05, 0.1, and 0.2 mg/L as test solutions. Measurements were made using a gas chromatograph quadrupole mass spectrometer "JMS-Q1600GC UltraQuad™ SQ-Zeta". Table 1 shows the measurement conditions. A calibration curve was created under these measurement conditions, and the coefficient of variation was calculated by continuously measuring a 0.01 mg/L sample with n=5 trials.
Table. 1 Measurement Condition
Parameter
Value
GC
Column
VF-5ms (Agilent Technologies, Inc.),
length 30 m, inner diameter 0.25 mm, film thickness 0.25 μm
Oven temp.
50°C (1 min)→ 20°C/min→300°C (1 min), Total 14.5 min
The mass spectra (upper) and library spectra (lower) of simazine and thiobencarb acquired with hydrogen carrier gas are shown in Figure 1. The agreement of the library search in both cases was over 850 (maximum 999), and there was no significant difference in the mass spectra.
Figure 1. Mass spectra of Simazine and Thiobencarb acquired by hydrogen carrier gas (upper), and NIST Library data (lower)
3.2. Confirmation of calibration curve and reproducibility
Calibration curves for simazine and thiobencarb are shown in Figure 2. The correlation coefficients of the calibration curves were more than 0.999. SIM chromatograms and the coefficients of variation at quantitation values when a 0.01 mg/L sample was measured continuously at n=5 are respectively shown in Figure 3 and Table 2. Coefficients of variation of less than 10% were obtained for both simazine and thiobencarb. The environmental standard for simazine and thiobencarb is 0.003 mg/L for the lowest simazine, and assuming the concentration factor in the solid phase extraction-GC-MS method based on Notification No. 59 of the Environment Agency in 1971, Appendix Table 6, it was confirmed that less than 1/10 of the standard value can be measured.
Figure 2. Calibration curve of Simazine and Thiobencarb
Figure 3. SIM chromatogram of Simazine and Thiobencarb at 0.01mg/L concentration by Hydrogen
Table 2. Coefficient variation (C.V.) of Simazine and Thiobencarb at 0.01 mg/L
Compound name
Quantitation value (mg/L)
C.V.%
#1
#2
#3
#4
#5
Simazine
0.0101
0.0101
0.0092
0.0101
0.0101
4.1
Thiobencarb
0.0099
0.0098
0.0086
0.0099
0.0099
5.9
Summary
Using hydrogen carrier gas, measurements were made for simazine and thiobencarb, pesticides subject to environmental standards related to water pollution, and it was confirmed that less than 1/10 of the standard value could be measured.
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18 March 2024 and is solely responsible for the information contained therein. Distributed by
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