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Determination of total sulfur in geothermal water by inductively coupled plasma-atomic emission spectrometry
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Abstract: Sulfur speciation and concentration in geothermal water are of great significance for the research and utilization of the water resources. In most situations, it is necessary to determine the total sulfur in geothermal water. In this study, the method was established for the determination of determining total sulfur content — the inductively coupled plasma-atomic emission spectrometry (ICP-AES), with the wavelength of 182.034 nm selected in spectral line of sulfur. It was identified that the optimal working conditions of the ICP-AES instrument were 1 200 W for high frequency generator power 9 mm for vertical observation height, 0.30 MPa atomizer pressure, and 50 r/min analytical pump speed. The matrix interference of the method was eliminated by the matrix matching method. Using this method, sulfur detection limit and minimum quantitative detection limit were 0.028 mg/L and 0.110 mg/L, respectively, whilst the linear range was 0.0–100.0 mg/L. The recovery rate of sample was between 90.67% and 108.7%, and the relative standard deviation (RSD) was between 0.36% and 2.14%. The method was used to analyze the actual samples and the results were basically consistent with the industry standard method. With high analysis efficiency, the method has low detection limit and minimum quantitative detection limit, wide linear range, good precision and accuracy, and provides an important detection method for the determination of total sulfur in geothermal water.
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Figure 1. Relative intensity and average background intensity of 3 spectral lines of sulfur
Figure 2. Influence of high frequency generator power on the intensity of sulfur standard solution and blank solution
Figure 3. Influence of vertical observation height on the intensity of sulfur standard solution and blank solution
Figure 4. Influence of atomizer pressure and analytical pump speed on the spectral intensity ratio (I1/I0) of sulfur standard solution and blank solution
Table 1. Working conditions of instrument
Working conditions Parameter Working conditions Parameter High frequency generator power（W） 1 200 Auxiliary air flow（L/min） 0.50 Atomizer pressure（MPa） 0.30 Integration time（s） 15 Vertical observation height（mm） 9 Stable schedule（s） 5 Analytical pump speed（r/min） 50.0 Flushing pump speed（r/min） 50.0 
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Table 2. Selection of different atomizer pressure and analytical pump speed
Atomizer pressure（MPa） Analytical pump speed（r/min） Atomizer pressure（MPa） Analytical pump speed（r/min） A1 0.10 25 A9 0.30 25 A2 0.10 50 A10 0.30 50 A3 0.10 75 A11 0.30 75 A4 0.10 100 A12 0.30 100 A5 0.20 25 A13 0.40 25 A6 0.20 50 A14 0.40 50 A7 0.20 75 A15 0.40 75 A8 0.20 100 A16 0.40 100
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Table 3. Determination results of total sulfur in geothermal water samples by matrix matching method and standard addition method (n=6)
Linear regression equation Correlation coefficient Linear range (mg/L) Sample 1# (mg/L) Sample 2# (mg/L) Sample 3# (mg/L) Matrix matching method Y=77.378x+14.592 0.9999 0.0–100.0 3.056 8.410 29.802 Standard addition method Y=70.220x+131.58 0.9999 0.0–100.0 2.997 8.277 30.441 Relative deviation（%） -- -- -- 1.95 1.59 2.12
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Table 4. Method detection limit, lower limit of determination and linear range compared with DZ/T 0064.51-2021
ICP Spectroscopy（as total sulphur）（this study） Ion chromatography（as SO42−）（DZ/T 0064.51-2021） Detection limit (mg/L) 0.028 0.10 Minimum quantitative detection limit (mg/L) 0.110 0.30 Linear range (mg/L) 0.0–100.0 0.30–50.00
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Table 5. Method precision and accuracy test (n=6)
Sample number Measured value（mg/L） Average value（mg/L） RSD
（%）Added value（mg/L） Recovery rate（%） RSD
（%）B1# 8.89, 9.05, 9.15, 9.10, 8.78, 9.12 9.02 1.63 10.0 91.60–101.1 1.89 B2# 13.70, 13.74, 13.29, 13.54, 13.57, 13.11 13.49 1.82 15.0 95.87–108.7 2.14 B3# 40.75, 40.87, 41.04, 41.01, 40.97, 40.68 40.89 0.36 10.0 91.20–103.9 0.88 B4# 21.66, 20.96, 21.14, 21.65, 21.78, 21.10 21.38 1.65 5.0 91.40–108.0 1.13 B5# 240.5, 237.2, 239.7, 236.2, 244.1, 241.9 239.9 1.22 45.0 90.67–107.4 1.15
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Table 6. Determination of total sulfur in geothermal water samples from different regions (n=6)
Sample number ICP Spectroscopy DZ/T 0064.51-2021 Relative deviation（%） Measured value（mg/L） RSD（%） Measured value（mg/L） RSD（%） C1# 22.96 1.20 23.40 0.69 1.89 C2# 54.78 1.04 53.49 1.48 2.39 C3# 89.58 2.84 90.35 0.63 0.85 C4# 1.98 1.41 2.05 3.75 3.73 C5# 2383 0.31 2401 2.53 0.75 C6# 71.68 1.07 71.47 0.65 0.30
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