CN111007182A - 一种气相色谱法测定2,2-二氟乙醇中杂质的方法 - Google Patents
一种气相色谱法测定2,2-二氟乙醇中杂质的方法 Download PDFInfo
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- CN111007182A CN111007182A CN201911390778.7A CN201911390778A CN111007182A CN 111007182 A CN111007182 A CN 111007182A CN 201911390778 A CN201911390778 A CN 201911390778A CN 111007182 A CN111007182 A CN 111007182A
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- 239000012535 impurity Substances 0.000 title claims abstract description 43
- VOGSDFLJZPNWHY-UHFFFAOYSA-N 2,2-difluoroethanol Chemical compound OCC(F)F VOGSDFLJZPNWHY-UHFFFAOYSA-N 0.000 title claims abstract description 42
- 238000000034 method Methods 0.000 title claims abstract description 35
- 238000004817 gas chromatography Methods 0.000 title claims abstract description 18
- 239000012159 carrier gas Substances 0.000 claims abstract description 21
- 238000004519 manufacturing process Methods 0.000 claims abstract description 13
- KURKJXZWCPWPFX-UHFFFAOYSA-N 2,2-difluoroacetyl chloride Chemical compound FC(F)C(Cl)=O KURKJXZWCPWPFX-UHFFFAOYSA-N 0.000 claims abstract description 7
- JVYROUWXXSWCMI-UHFFFAOYSA-N 2-bromo-1,1-difluoroethane Chemical compound FC(F)CBr JVYROUWXXSWCMI-UHFFFAOYSA-N 0.000 claims abstract description 7
- PBWZKZYHONABLN-UHFFFAOYSA-N difluoroacetic acid Chemical compound OC(=O)C(F)F PBWZKZYHONABLN-UHFFFAOYSA-N 0.000 claims abstract description 7
- GZKHDVAKKLTJPO-UHFFFAOYSA-N ethyl 2,2-difluoroacetate Chemical compound CCOC(=O)C(F)F GZKHDVAKKLTJPO-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000009834 vaporization Methods 0.000 claims abstract description 6
- 230000008016 vaporization Effects 0.000 claims abstract description 6
- SCYULBFZEHDVBN-UHFFFAOYSA-N 1,1-Dichloroethane Chemical compound CC(Cl)Cl SCYULBFZEHDVBN-UHFFFAOYSA-N 0.000 claims abstract description 5
- 229960003750 ethyl chloride Drugs 0.000 claims abstract description 5
- 239000000126 substance Substances 0.000 claims abstract description 5
- 230000005526 G1 to G0 transition Effects 0.000 claims abstract description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 14
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims description 13
- 229910052731 fluorine Inorganic materials 0.000 claims description 13
- 239000011737 fluorine Substances 0.000 claims description 13
- 239000007789 gas Substances 0.000 claims description 11
- 239000001257 hydrogen Substances 0.000 claims description 10
- 229910052739 hydrogen Inorganic materials 0.000 claims description 10
- 238000010606 normalization Methods 0.000 claims description 9
- 229910052757 nitrogen Inorganic materials 0.000 claims description 7
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 6
- 238000004364 calculation method Methods 0.000 claims description 5
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- 150000001335 aliphatic alkanes Chemical class 0.000 claims description 3
- 150000001336 alkenes Chemical class 0.000 claims description 3
- 150000001345 alkine derivatives Chemical class 0.000 claims description 3
- 238000009826 distribution Methods 0.000 claims description 3
- 238000012545 processing Methods 0.000 claims description 3
- 230000003321 amplification Effects 0.000 claims description 2
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- 150000002431 hydrogen Chemical class 0.000 claims description 2
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- 238000004458 analytical method Methods 0.000 abstract description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- 239000000543 intermediate Substances 0.000 description 4
- VUYQBMXVCZBVHP-UHFFFAOYSA-N 1,1-difluoroethanol Chemical compound CC(O)(F)F VUYQBMXVCZBVHP-UHFFFAOYSA-N 0.000 description 3
- 239000003814 drug Substances 0.000 description 3
- 229920000642 polymer Polymers 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- ATEBGNALLCMSGS-UHFFFAOYSA-N 2-chloro-1,1-difluoroethane Chemical compound FC(F)CCl ATEBGNALLCMSGS-UHFFFAOYSA-N 0.000 description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 125000006006 difluoroethoxy group Chemical group 0.000 description 2
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- SYJGKVOENHZYMQ-UHFFFAOYSA-N Penoxsulam Chemical compound N1=C2C(OC)=CN=C(OC)N2N=C1NS(=O)(=O)C1=C(OCC(F)F)C=CC=C1C(F)(F)F SYJGKVOENHZYMQ-UHFFFAOYSA-N 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 125000001931 aliphatic group Chemical group 0.000 description 1
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- 125000001028 difluoromethyl group Chemical group [H]C(F)(F)* 0.000 description 1
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- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/86—Signal analysis
- G01N30/8675—Evaluation, i.e. decoding of the signal into analytical information
- G01N30/8679—Target compound analysis, i.e. whereby a limited number of peaks is analysed
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- General Health & Medical Sciences (AREA)
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Pathology (AREA)
- Biochemistry (AREA)
- Immunology (AREA)
- General Physics & Mathematics (AREA)
- Engineering & Computer Science (AREA)
- Library & Information Science (AREA)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
Description
序号 | 参数 | 结果 |
1 | 色谱柱 | DB-35(30mX320μmX0.25μm)毛细管柱 |
2 | 色谱柱柱温 | 初始温度50℃保持5min,以10℃/min升温至220℃保持3min |
3 | 检测器 | 氢火焰离子化检测器(FID) |
4 | 载气 | 体积百分比为99.999%的氮气 |
5 | 燃气 | 体积百分比为99.999%的氢气,流量30mL/min |
6 | 助燃气 | 空气,流量为300mL/min |
7 | 载气流量 | 0.7mL/min |
8 | 进样量 | 0.3μL |
9 | 分流比 | 50:1 |
10 | 汽化室温度 | 250℃ |
11 | 检测器 | 250℃ |
序号 | 组分 | 保留时间(min) | 含量(%) |
1 | 二氟乙酰氯 | 5.03 | 7.27 |
2 | 1,1-二氟-2-氯乙烷 | 5.56 | 28.81 |
3 | 1,1-二氟-2-溴乙烷 | 6.12 | 17.40 |
4 | 2,2-二氟乙醇 | 6.76 | 20.01 |
5 | 2,2-二氯乙烷 | 6.85 | 16.06 |
6 | 二氟乙酸乙酯 | 7.44 | 1.22 |
7 | 二氟乙酸 | 7.60 | 9.23 |
序号 | 组分 | 保留时间(min) | 含量(%) |
1 | 二氟乙酰氯 | 5.04 | 7.26 |
2 | 1,1-二氟-2-氯乙烷 | 5.56 | 28.83 |
3 | 1,1-二氟-2-溴乙烷 | 6.11 | 17.38 |
4 | 2,2-二氟乙醇 | 6.72 | 20.00 |
5 | 2,2-二氯乙烷 | 6.84 | 16.02 |
6 | 二氟乙酸乙酯 | 7.44 | 1.21 |
7 | 二氟乙酸 | 7.59 | 9.20 |
Claims (7)
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CN111007182A true CN111007182A (zh) | 2020-04-14 |
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Citations (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102426208A (zh) * | 2011-11-11 | 2012-04-25 | 巨化集团公司 | 四氟乙烷-β-磺内酯的气相色谱分析方法 |
US20130150325A1 (en) * | 2011-07-21 | 2013-06-13 | Bayer Intellectual Property Gmbh | 3-(Fluorovinyl)pyrazoles and their use |
CN104359997A (zh) * | 2014-10-11 | 2015-02-18 | 广东省东莞市质量监督检测中心 | 顶空-气相色谱质谱法测定溶剂型木器涂料中的低沸点卤代烃的方法 |
CN104359985A (zh) * | 2014-10-11 | 2015-02-18 | 广东省东莞市质量监督检测中心 | 一种人工田径场地合成材料面层卤代烃的测定方法 |
CN104761446A (zh) * | 2015-04-15 | 2015-07-08 | 江西盛伟实业有限公司 | 2-溴-2,2-二氟乙酰氯、2-溴-2,2-二氟乙酸酯的制备方法以及废弃物二氟三氯乙烷的回收处理方法 |
CN105929097A (zh) * | 2016-06-25 | 2016-09-07 | 江苏正大清江制药有限公司 | 一种测定盐酸右美托咪啶中氯甲烷、氯乙烷的方法 |
CN108267520A (zh) * | 2017-12-27 | 2018-07-10 | 江苏联环药业股份有限公司 | 一种采用fid检测器检测特丁酮生产工艺中的残留溶剂二氯乙烷的方法 |
-
2019
- 2019-12-30 CN CN201911390778.7A patent/CN111007182B/zh active Active
Patent Citations (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US20130150325A1 (en) * | 2011-07-21 | 2013-06-13 | Bayer Intellectual Property Gmbh | 3-(Fluorovinyl)pyrazoles and their use |
CN102426208A (zh) * | 2011-11-11 | 2012-04-25 | 巨化集团公司 | 四氟乙烷-β-磺内酯的气相色谱分析方法 |
CN104359997A (zh) * | 2014-10-11 | 2015-02-18 | 广东省东莞市质量监督检测中心 | 顶空-气相色谱质谱法测定溶剂型木器涂料中的低沸点卤代烃的方法 |
CN104359985A (zh) * | 2014-10-11 | 2015-02-18 | 广东省东莞市质量监督检测中心 | 一种人工田径场地合成材料面层卤代烃的测定方法 |
CN104761446A (zh) * | 2015-04-15 | 2015-07-08 | 江西盛伟实业有限公司 | 2-溴-2,2-二氟乙酰氯、2-溴-2,2-二氟乙酸酯的制备方法以及废弃物二氟三氯乙烷的回收处理方法 |
CN105929097A (zh) * | 2016-06-25 | 2016-09-07 | 江苏正大清江制药有限公司 | 一种测定盐酸右美托咪啶中氯甲烷、氯乙烷的方法 |
CN108267520A (zh) * | 2017-12-27 | 2018-07-10 | 江苏联环药业股份有限公司 | 一种采用fid检测器检测特丁酮生产工艺中的残留溶剂二氯乙烷的方法 |
Non-Patent Citations (4)
Title |
---|
SUTHERLAND, F: "Determination of ultra trace levels of 1, 2-dichloroethane in air by sample enrichment micromachined gas chromatography-differential mobility detection", 《JOURNAL OF CHROMATOGRAPHIC SCIENCE》 * |
周圆: "温室气体CFCs、HFCs、SF6和CF4的分析方法与应用研究", 《中国优秀博硕士学位论文全文数据库(硕士) 工程科技I辑》 * |
宋鸣 等: "气相色谱一质谱法检测胃内容物中氟乙酸", 《中国卫生检验杂志》 * |
郭立峰 等: "GC-MS和GC-ECD和 同时在线观测本底大气中的HCFC-142b", 《环境科学》 * |
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