气相色谱法测定白酒中氰化物的不确定度评定
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摘要
目的评定气相色谱法测定白酒中氰化物的不确定度。方法分析气相色谱法测定白酒中氰化物的全过程,确认不确定度的来源和大小,合成不确定度,计算扩展不确定度并报出结果。结果白酒中氰化物的含量为13.8 mg/L,扩展不确定度为1.0 mg/L(P=95%, k=2)。结论通过对不确定度的来源分析及各分量的量化评定,回收率与标准曲线拟合对不确定度的影响较大,标准溶液、样品制备和测量重复性对不确定度的影响较小。
Objective To evaluate the uncertainty in determination of cyanide in liquor by gas chromatography.Methods The whole process of determination of cyanide in liquor was analyzed by gas chromatography, the source and value of uncertainty were confirmed, calculated the synthetic uncertainty was synthesized, and the extended uncertainty was calculated and the results were reported. Results The content of cyanide in liquor was 13.8 mg/L,and the expansion of uncertainty was 1.0 mg/L(P=95%, k=2). Conclusion Through the analysis of the source of uncertainty and the quantitative evaluation of each component, the recovery rate and the standard curve fitting have a great influence on the uncertainty. The standard solution, sample preparation and measurement repeatability have little effects on the uncertainty.
Objective To evaluate the uncertainty in determination of cyanide in liquor by gas chromatography.Methods The whole process of determination of cyanide in liquor was analyzed by gas chromatography, the source and value of uncertainty were confirmed, calculated the synthetic uncertainty was synthesized, and the extended uncertainty was calculated and the results were reported. Results The content of cyanide in liquor was 13.8 mg/L,and the expansion of uncertainty was 1.0 mg/L(P=95%, k=2). Conclusion Through the analysis of the source of uncertainty and the quantitative evaluation of each component, the recovery rate and the standard curve fitting have a great influence on the uncertainty. The standard solution, sample preparation and measurement repeatability have little effects on the uncertainty.
引文
[1]韦小烨,黄一帆,陈桂鸾,等.流动注射法测定鲜木薯中氰化物[J].化学分析计量,2018,27(3):20-23.Wei XY,Huang YF,Chen GL,et al.Determination of cyanide in fresh cassava by flow injection method[J].Chem Anal Meter,2018,27(3):20-23.
[2]刘芯韵,张坤,易啸,等.离子色谱法测定蒸馏酒中氰化物含量的方法性能分析[J].食品与发酵科技,2017,53(2):94-95,126.Liu XY,Zhang K,Yi X,et al.Method performance analysis of determination of cyanide in distilled wines by ion chromatography[J].Food Ferment Sci Technol,2017,53(2):94-95,126.
[3]李悦,何颖,李彦懿,等.紫外-可见分光光度法测定3种酒中氰化物的浓度[J].酿酒科技,2017,(8):128-131.Li Y,He Y,Li YY,et al.Determination of cyanides concentration in 3kinds of alcoholic drinks by UV-Vis spectrophotometry[J].Liquor-Mak Sci Technol,2017,(8):128-131.
[4]杜利君,刘晓林,高媛惠,等.顶空气相色谱法快速测定酒中氰化物含量[J].食品研究与开发,2017,38(11):131-133.Du LJ,Liu XY,Gao YH,et al.Determination of cyanide in wine by headspace gas chromatography[J].Food Res Dev,2017,38(11):131-133.
[5]Shigetoshi K,Takeaki N,Keiko K.Determination of cyanide and thiocyanate in blood by gas chromatography and gas chromatography-mass spectrometry[J].J Chromatogr B,1996,675(1):27-32.
[6]阎冠洲,钟其顶,李国辉,等.顶空气相色谱测定白酒中氰化物方法研究[J].酿酒科技,2013,(3):89-92.Yan GZ,Zhong QD,Li GH,et al.Study on the determination of cyanide content in liquor by headspace gas chromatography[J].Liquor-Mak Sci Technol,2013,(3):89-92.
[7]方诚,凌芳,郑琦,等.异烟酸-吡唑啉酮光度法测定硫酸铵中氰化物[J].化学试剂,2017,39(11):1193-1195,1200.Fang C,Ling F,Zheng Q,et al.Isonicotinic acid-pyrazolone spectrophotometric determination of cyanide in ammonium sulfate[J].Chem Reag,2017,39(11):1193-1195,1200.
[8]张建,苏利进,李凯,等.GC-MS定性/HS-20顶空结合GC定量测定酒中痕量氰化物[J].酿酒科技,2014(07):105-108.Zhang J,Su LJ,Li K,et al.GC-MS qualitative/hs-20 headspace coupled with gc quantitativedetection of trace cyanide content in liquor[J].Liquor-Mak Sci Technol,2014,(7):105-108.
[9]GB 5009.36-2016食品安全国家标准食品中氰化物的测定[S].GB 5009.36-2016 National food safety standard-Determination of cyanide in food[S].
[10]李南,何海茵,郑悦珊,等.顶空气相色谱法测定白酒中氰化物含量[J].食品安全质量检测学报,2019,10(1):240-244.Li N,He HY,Zheng YS,et al.Determination of cyanide content in liquor by headspace gas chromatography[J].J Food Saf Qual,2019,10(1):240-244.
[11]费业泰.误差理论的研究与进展[J].计量技术,1998,(8):40-41.Fei YT.Research and development of error theory[J].Metrol Technol,1998,(8):40.
[12]尚德军,王军.测量不确定度的研究和应用进展[J].理化检验(化学分册),2004,(10):623-627.Shang DJ,Wang J.Research and application progress of measurement uncertainty[J].Phys Test Chem Anal(Part B:Chem Anal),2004,(10):623-627.
[13]朱坚民,王中宇,夏新涛,等.测量不确定度评定的研究进展与展望[J].河南科技大学学报(自然科学版),2000,21(2):21-24.Zhu JM,Wang ZY,Xia XT,et al.Research progress and prospect of measurement uncertainty evaluation[J]J Luoyang Inst Technol,2000,21(2):21-24.
[14]安平,刘浩峰,华广胜.检测实验室测量不确定度评定与应用现状[J].中国检验检测,2018,26(6):60-63.An P,Liu HF,Hua GS.Evaluation and application status of measurement uncertainty in testing laboratory[J].China Inspect Test,2018,26(6):60-63.
[15]向德磊.金属铟中锡的ICP-AES测定方法不确定度评定及在产品符合性判定中的应用[J].矿产与地质,2016,30(3):509-512.Xiang DL.Evaluation of uncertainty in determination of tin in metal indium by icp-aes and its application in product conformity determination[J].Mineral Res Geol,2016,30(3):509-512.
[16]赵娜,孙轶,王奇锋,等.浅谈测量不确定度的评定在环境与可靠性实验室中的应用[J].数字通信世界,2018,(12):165,169.Zhao N,Sun W,Wang QF,et al.Discussion on the application of measurement uncertainty in the environment and reliability laboratory[J].Digit Commun World,2018,(12):165,169.
[17]吴小松,曹玉发,姜雪,等.白酒中氰化物含量测定及其不确定度评定[J].中国酿造,2013,32(5):82-85.Wu XS,Cao YF,Jiang X,et al.Determination of cyanide content in liquor and its uncertainty evaluation[J].China Brew,2013,32(5):82-85.
[18]JJF 1059.1-2012测量不确定度评定与表示[S].JJF 1059.12012 Evaluation and expression of uncertainty in measurement[S].
[19]CNAS-GL 006化学分析中不确定度的评估指南[S].CNAS-GL 006 Guidance on evaluating the uncertainty in chemical analysis[S].
[2]刘芯韵,张坤,易啸,等.离子色谱法测定蒸馏酒中氰化物含量的方法性能分析[J].食品与发酵科技,2017,53(2):94-95,126.Liu XY,Zhang K,Yi X,et al.Method performance analysis of determination of cyanide in distilled wines by ion chromatography[J].Food Ferment Sci Technol,2017,53(2):94-95,126.
[3]李悦,何颖,李彦懿,等.紫外-可见分光光度法测定3种酒中氰化物的浓度[J].酿酒科技,2017,(8):128-131.Li Y,He Y,Li YY,et al.Determination of cyanides concentration in 3kinds of alcoholic drinks by UV-Vis spectrophotometry[J].Liquor-Mak Sci Technol,2017,(8):128-131.
[4]杜利君,刘晓林,高媛惠,等.顶空气相色谱法快速测定酒中氰化物含量[J].食品研究与开发,2017,38(11):131-133.Du LJ,Liu XY,Gao YH,et al.Determination of cyanide in wine by headspace gas chromatography[J].Food Res Dev,2017,38(11):131-133.
[5]Shigetoshi K,Takeaki N,Keiko K.Determination of cyanide and thiocyanate in blood by gas chromatography and gas chromatography-mass spectrometry[J].J Chromatogr B,1996,675(1):27-32.
[6]阎冠洲,钟其顶,李国辉,等.顶空气相色谱测定白酒中氰化物方法研究[J].酿酒科技,2013,(3):89-92.Yan GZ,Zhong QD,Li GH,et al.Study on the determination of cyanide content in liquor by headspace gas chromatography[J].Liquor-Mak Sci Technol,2013,(3):89-92.
[7]方诚,凌芳,郑琦,等.异烟酸-吡唑啉酮光度法测定硫酸铵中氰化物[J].化学试剂,2017,39(11):1193-1195,1200.Fang C,Ling F,Zheng Q,et al.Isonicotinic acid-pyrazolone spectrophotometric determination of cyanide in ammonium sulfate[J].Chem Reag,2017,39(11):1193-1195,1200.
[8]张建,苏利进,李凯,等.GC-MS定性/HS-20顶空结合GC定量测定酒中痕量氰化物[J].酿酒科技,2014(07):105-108.Zhang J,Su LJ,Li K,et al.GC-MS qualitative/hs-20 headspace coupled with gc quantitativedetection of trace cyanide content in liquor[J].Liquor-Mak Sci Technol,2014,(7):105-108.
[9]GB 5009.36-2016食品安全国家标准食品中氰化物的测定[S].GB 5009.36-2016 National food safety standard-Determination of cyanide in food[S].
[10]李南,何海茵,郑悦珊,等.顶空气相色谱法测定白酒中氰化物含量[J].食品安全质量检测学报,2019,10(1):240-244.Li N,He HY,Zheng YS,et al.Determination of cyanide content in liquor by headspace gas chromatography[J].J Food Saf Qual,2019,10(1):240-244.
[11]费业泰.误差理论的研究与进展[J].计量技术,1998,(8):40-41.Fei YT.Research and development of error theory[J].Metrol Technol,1998,(8):40.
[12]尚德军,王军.测量不确定度的研究和应用进展[J].理化检验(化学分册),2004,(10):623-627.Shang DJ,Wang J.Research and application progress of measurement uncertainty[J].Phys Test Chem Anal(Part B:Chem Anal),2004,(10):623-627.
[13]朱坚民,王中宇,夏新涛,等.测量不确定度评定的研究进展与展望[J].河南科技大学学报(自然科学版),2000,21(2):21-24.Zhu JM,Wang ZY,Xia XT,et al.Research progress and prospect of measurement uncertainty evaluation[J]J Luoyang Inst Technol,2000,21(2):21-24.
[14]安平,刘浩峰,华广胜.检测实验室测量不确定度评定与应用现状[J].中国检验检测,2018,26(6):60-63.An P,Liu HF,Hua GS.Evaluation and application status of measurement uncertainty in testing laboratory[J].China Inspect Test,2018,26(6):60-63.
[15]向德磊.金属铟中锡的ICP-AES测定方法不确定度评定及在产品符合性判定中的应用[J].矿产与地质,2016,30(3):509-512.Xiang DL.Evaluation of uncertainty in determination of tin in metal indium by icp-aes and its application in product conformity determination[J].Mineral Res Geol,2016,30(3):509-512.
[16]赵娜,孙轶,王奇锋,等.浅谈测量不确定度的评定在环境与可靠性实验室中的应用[J].数字通信世界,2018,(12):165,169.Zhao N,Sun W,Wang QF,et al.Discussion on the application of measurement uncertainty in the environment and reliability laboratory[J].Digit Commun World,2018,(12):165,169.
[17]吴小松,曹玉发,姜雪,等.白酒中氰化物含量测定及其不确定度评定[J].中国酿造,2013,32(5):82-85.Wu XS,Cao YF,Jiang X,et al.Determination of cyanide content in liquor and its uncertainty evaluation[J].China Brew,2013,32(5):82-85.
[18]JJF 1059.1-2012测量不确定度评定与表示[S].JJF 1059.12012 Evaluation and expression of uncertainty in measurement[S].
[19]CNAS-GL 006化学分析中不确定度的评估指南[S].CNAS-GL 006 Guidance on evaluating the uncertainty in chemical analysis[S].
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