顶空-气相色谱法测定固定污染源废气中三甲胺的含量
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摘要
按照HJ/T 55或GB/T 16157的相关规定,用固定量0.12mol·L~(-1)盐酸溶液吸收采集固定污染源废气中三甲胺。分取样品溶液10.00mL,移至顶空瓶中,加入氯化钠3.2g和硫酸钾1.0g,并用微量注射器加入质量分数为50%的NaOH溶液500μL和氨水100μL,立即密封顶空瓶,在顶空平衡温度为80℃,平衡时间为30min的条件下进行顶空采样。选择CP-Volamine石英毛细管色谱柱进行三甲胺及其他5种研究的脂肪胺类化合物的定量分离,采用氢火焰离子化检测器(FID)进行检测。分别按HJ/T 55及GB/T 16157规定的方法各取三甲胺标准气体20L,分别进行7组平行试验,测得前一采样方法的检出限[t_(n-1,0.99))×s]为0.004mg·m~(-3),后一采样方法的检出限[t_(n-1,0.99))×s]为0.02mg·m~(-3)。另取高浓度(0.510μmol·mol~(-1))、中浓度(0.102μmol·mol~(-1))及低浓度(0.010 2μmol·mol~(-1))等3种浓度的三甲胺标准气体,按规定方法采样并分析6次,计算得三甲胺的回收率在90.1%～108%之间,测定值的相对标准偏差(n=6)在2.2%～6.7%之间。应用此方法分析实际样品,测定结果表明该方法能满足国家标准GB 14554-93及天津市和上海市两地方标准对恶臭污染物排放的规定,并配合上述标准的执行。
Trimethylamine(TMA)in exhaust gas at stationary pollutive sources were collected either by the method given in HJ/T 55 or GB/T 16157 with definite amount of 0.12 mol·L~(-1) HCl solution as absorbent.An aliquot of 10.00 mL of the dil.HCl solution containing TMA was taken and transferred into the head-space flask of the GC instrument,and 3.2 g of NaCl and 1.0 g K_2SO_4 were added and 500μL of NaOH(w,50%)solution,together with 100μL of aq.ammonia were added successively.The head-space flask was then sealed hermetically and the HS-sampling was carried out at 80 ℃ for 30 min.CP-Volamine quartz capillary chromatographic column was selected for quantitative separation of TMA and other 5 aliphatic amines added for testing.FID was adopted for detection of response signals.To test for detection limit of the proposed method with collection of TMA in exhaust gas by the methods given in HJ/T 55 and GB/T 16157,20 Lof TMA standard gas were collected by the 2 methods separately,and 7 sets of parallel determinations were performed by the GC analysis by taking 10.00 mL aliquots from the HCl solution absorbed with TMA.Detection limit [t_(n-1,0.99))×s]of 0.004 mg· m~(-3) was found for collection of TMA by the method given in HJ/T 55,and detection limit[t_(n-1,0.99))×s]of 0.02 mg·m~(-3) was found for collection of TMA by the method given in GB/T 16157.Standard TMA gas samples with 3 concentration levels of 0.510μmol·mol-1,0.102μmol·mol~(-1) and 0.010 2μmol·mol~(-1) were collected and analyzed by thd given method for 6 parallel determinations,and values of recovery found were in the range of 90.1%-108%,and RSDs found were ranged from 2.2%to 6.7%.As shown by the results obtained by analyzing several substantial samples,the proposed method was feasible to be used in supervision and controlling the ejection of TMA in atmosphere,and was effective in meeting with the requirements given in the national standard GB 14554-93 and in local standards of Shanghai and Tianjin Muncipalities,pertaining regulations of ejection of stenchy pollutants.
Trimethylamine(TMA)in exhaust gas at stationary pollutive sources were collected either by the method given in HJ/T 55 or GB/T 16157 with definite amount of 0.12 mol·L~(-1) HCl solution as absorbent.An aliquot of 10.00 mL of the dil.HCl solution containing TMA was taken and transferred into the head-space flask of the GC instrument,and 3.2 g of NaCl and 1.0 g K_2SO_4 were added and 500μL of NaOH(w,50%)solution,together with 100μL of aq.ammonia were added successively.The head-space flask was then sealed hermetically and the HS-sampling was carried out at 80 ℃ for 30 min.CP-Volamine quartz capillary chromatographic column was selected for quantitative separation of TMA and other 5 aliphatic amines added for testing.FID was adopted for detection of response signals.To test for detection limit of the proposed method with collection of TMA in exhaust gas by the methods given in HJ/T 55 and GB/T 16157,20 Lof TMA standard gas were collected by the 2 methods separately,and 7 sets of parallel determinations were performed by the GC analysis by taking 10.00 mL aliquots from the HCl solution absorbed with TMA.Detection limit [t_(n-1,0.99))×s]of 0.004 mg· m~(-3) was found for collection of TMA by the method given in HJ/T 55,and detection limit[t_(n-1,0.99))×s]of 0.02 mg·m~(-3) was found for collection of TMA by the method given in GB/T 16157.Standard TMA gas samples with 3 concentration levels of 0.510μmol·mol-1,0.102μmol·mol~(-1) and 0.010 2μmol·mol~(-1) were collected and analyzed by thd given method for 6 parallel determinations,and values of recovery found were in the range of 90.1%-108%,and RSDs found were ranged from 2.2%to 6.7%.As shown by the results obtained by analyzing several substantial samples,the proposed method was feasible to be used in supervision and controlling the ejection of TMA in atmosphere,and was effective in meeting with the requirements given in the national standard GB 14554-93 and in local standards of Shanghai and Tianjin Muncipalities,pertaining regulations of ejection of stenchy pollutants.
引文
[1]夏元洵．化学物质毒性全书[M]．上海：上海科学技术文献出版社，1991:254-256.
[2] CAS Reg.No.75-50-3 Acute exposure guideline levels(AEGLs)for trimethylamine[S].
[3]王亘，翟增秀，耿静，等．40种典型恶臭物质嗅阈值测定[J]．安全与环境学报，2015,15(6):348-351.
[4] GB 14554-93恶臭污染物排放标准[S].
[5] DB 12/-059-95恶臭污染物排放标准[S].
[6] DB 31/1025-2016恶臭（异味）污染物排放标准[S].
[7] GB/T 14676-93空气质量三甲胺的测定气相色谱法[S].
[8] National Institute for Occupational Safety and Health NIOSH pocket guide to chemical hazards-trimethylamine[S].
[9]邓迈华．离子色谱法同时测定空气中的氨、二甲胺、三甲胺[J]．福建分析测试，2009,18(2):77-78.
[10]冯忆，顾海东，周振梅．环境中三甲胺的气相色谱测定[J]．环境监测管理与技术，1999,11(2):28-29.
[11]朱仁康，王逸虹，侯定远．甲胺、二甲胺及三甲胺的气相色谱测定[J]．中国环境监测，2000,16(1):20-22.
[2] CAS Reg.No.75-50-3 Acute exposure guideline levels(AEGLs)for trimethylamine[S].
[3]王亘，翟增秀，耿静，等．40种典型恶臭物质嗅阈值测定[J]．安全与环境学报，2015,15(6):348-351.
[4] GB 14554-93恶臭污染物排放标准[S].
[5] DB 12/-059-95恶臭污染物排放标准[S].
[6] DB 31/1025-2016恶臭（异味）污染物排放标准[S].
[7] GB/T 14676-93空气质量三甲胺的测定气相色谱法[S].
[8] National Institute for Occupational Safety and Health NIOSH pocket guide to chemical hazards-trimethylamine[S].
[9]邓迈华．离子色谱法同时测定空气中的氨、二甲胺、三甲胺[J]．福建分析测试，2009,18(2):77-78.
[10]冯忆，顾海东，周振梅．环境中三甲胺的气相色谱测定[J]．环境监测管理与技术，1999,11(2):28-29.
[11]朱仁康，王逸虹，侯定远．甲胺、二甲胺及三甲胺的气相色谱测定[J]．中国环境监测，2000,16(1):20-22.