CAJ | 학술논문

建立稳定性同位素内标-吹扫捕集-气相色谱-质谱联用法( GC-MS)分析多种水体中硫化物,为预警异味水质突发事件和开展相关研究奠定基础。水样脱氯过滤后,加入同位素内标与氯化钠,吹扫捕集装置40℃氮气吹扫10 min,200℃脱附2 min,吹扫流量40 mL/min。色谱柱：DB-624,进样口温度270℃,分流比20：1,载气高纯He,流速3.8 mL/min。升温条件：35℃(5 min),6℃/min升至120℃,20℃/min升至210℃。传输线( AUX)温度为280℃。质谱条件：离子源温度230℃,四极杆温度150℃,电子能量70 eV。以保留时间和质谱全扫描方式进行定性分析,质量范围m/z 45~450；选择离子监测定量；基质加标验证方法的准确度与精密度。乙硫醇、二甲基硫和二甲基二硫在0.6~21.3μg/L范围内线性良好。 ET, DMS和DMDS的检出限分别为0.088,0.13和0.10μg/L。5种水体高、低浓度加标,回收率为90.7%~118.0%, RSD为2.7%~9.8%。本方法采用稳定同位素内标法,具有较好的准确性、稳定性和实用性,可用于地表水、地下水和生活饮用水等多种水体中含硫嗅味物质的分析。
건립은정성동위소내표-취소포집-기상색보-질보련용법( GC-MS)분석다충수체중류화물,위예경이미수질돌발사건화개전상관연구전정기출。수양탈록과려후,가입동위소내표여록화납,취소포집장치40℃담기취소10 min,200℃탈부2 min,취소류량40 mL/min。색보주：DB-624,진양구온도270℃,분류비20：1,재기고순He,류속3.8 mL/min。승온조건：35℃(5 min),6℃/min승지120℃,20℃/min승지210℃。전수선( AUX)온도위280℃。질보조건：리자원온도230℃,사겁간온도150℃,전자능량70 eV。이보류시간화질보전소묘방식진행정성분석,질량범위m/z 45~450；선택리자감측정량；기질가표험증방법적준학도여정밀도。을류순、이갑기류화이갑기이류재0.6~21.3μg/L범위내선성량호。 ET, DMS화DMDS적검출한분별위0.088,0.13화0.10μg/L。5충수체고、저농도가표,회수솔위90.7%~118.0%, RSD위2.7%~9.8%。본방법채용은정동위소내표법,구유교호적준학성、은정성화실용성,가용우지표수、지하수화생활음용수등다충수체중함류후미물질적분석。
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 ℃, desorpbed 2 min at 200 ℃. The purging flow was 40 mL/min. Chromatographic column:DB-624, inlet temperature 270 ℃, split ratio 20:1, high purity He as carrier gas, flow rate 3. 8 mL/min. Temperature programmed condition: 35 ℃ ( 5 min ) , 6 ℃/min to 120 ℃, 20 ℃/min to 210 ℃. AUX temperature was 280 ℃. Mass spectrometric conditions were as follows: ion source temperature 230 ℃, quadrupole temperature 150℃, 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 μg/L. The limits of detection were 0. 09, 0. 13 and 0. 10 μg/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.