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摘要
A stable isotope internal standard. purge and trap. GC. MS analytical method of sulfides in a variety of water was established for the early warning odor water emergencies and researches. Water samples were dechlorinated, filtered and added sodium chloride and isotope internal standard, and purged 10 min by nitrogen at 40 degrees C, desorpbed 2 min at 200 degrees C. The purging flow was 40 mL/min. Chromatographic column: DB-624, inlet temperature 270 degrees C, split ratio 20. 1, high purity He as carrier gas, flow rate 3. 8 mL/min. Temperature programmed condition: 35 degrees C (5 min), 6 degrees C/min to 120 degrees C, 20 degrees C/min to 210 degrees C. AUX temperature was 280 degrees C. Mass spectrometric conditions were as follows: ion source temperature 230 degrees C, quadrupole temperature 150 degrees C, electrical energy 70 eV. Qualitative analysis was carried out by retention time and mass spectrometric scan in the mass range of 45-450 and quantified by select ion monitoring method. The accuracy and precision were determined by matrix spike. The results showed that ethyl thiol, dimethyl sulfide and dimethyl disulfide had good linear at range of 0. 6-21. 3 mu g/L. The limits of detection were 0. 09, 0. 13 and 0. 10 mu g/L, respectively. The recovery of high and low spike concentration in 5 kinds of water samples were 90. 7%-118. 0% with the RSDs of 2. 7%-9. 8%. The method could be used for the analysis of surface water, groundwater and drinking water containing sulfide by using isotope internal standard with good accuracy, stability and practicability.
- 出版日期2014-5
- 单位福建省疾病预防控制中心
