Paula Rivera-Quintero, Gregory S. Patience, Nicolas A. Patience, Daria C. Boffito, Xavier Banquy, Dalma Schieppati
{"title":"化学工程实验方法卡尔费休滴定法","authors":"Paula Rivera-Quintero, Gregory S. Patience, Nicolas A. Patience, Daria C. Boffito, Xavier Banquy, Dalma Schieppati","doi":"10.1002/cjce.25295","DOIUrl":null,"url":null,"abstract":"<p>Karl Fischer titration (KF) measures the water content in organic and inorganic compounds. Water reacts with a titrant solution containing iodine and a sulphurous monoalkyl ester to produce a monoalkyl sulphate ester and HI. In volumetric titrators, a burette injects the titrant directly into a cell while coulometric titrators generate titrant in situ. Regardless of the volume of the sample, volumetric titration is limited to 100 mg, while coulometric titration is best suited for <span></span><math>\n <mrow>\n <mo>></mo>\n <mn>2</mn>\n <mspace></mspace>\n <mi>mg</mi>\n </mrow></math>. KF is fast (<span></span><math>\n <mrow>\n <mo><</mo>\n <mn>2</mn>\n <mspace></mspace>\n <mi>min</mi>\n </mrow></math>), considered accurate (<span></span><math>\n <mrow>\n <mo>±</mo>\n <mn>5</mn>\n <mo>%</mo>\n </mrow></math>), and precise (<span></span><math>\n <mrow>\n <mo><</mo>\n <mn>1</mn>\n <mspace></mspace>\n <mo>%</mo>\n </mrow></math>). However, factors such as humidity, non-standard analytes (hexane, isopropanol, ethylene glycol), tritrant composition, and temperature compromise its repeatability: the % sample standard deviation, <span></span><math>\n <mrow>\n <mi>s</mi>\n </mrow></math> (<span></span><math>\n <mrow>\n <mi>n</mi>\n <mo>=</mo>\n <mn>4</mn>\n </mrow></math>), varied from 2% to 60% (<span></span><math>\n <mrow>\n <mover>\n <mi>s</mi>\n <mo>¯</mo>\n </mover>\n <mo>=</mo>\n <mn>22</mn>\n <mo>%</mo>\n <mo>,</mo>\n <msub>\n <mi>n</mi>\n <mtext>conditions</mtext>\n </msub>\n <mo>=</mo>\n <mn>19</mn>\n </mrow></math>). This high variability is, in part, due to the experimental design that included samples and conditions ill-suited for the technique. However, even for the tests for which KF is suitable, <span></span><math>\n <mrow>\n <mover>\n <mi>s</mi>\n <mo>¯</mo>\n </mover>\n <mo>></mo>\n <mn>10</mn>\n <mo>%</mo>\n </mrow></math>. Certain compounds react with the titrant, which increases the variability. The main sources of error affecting the analysis are ambient moisture, pH, solvent, sample handling, and titration speed. As of 2023, the Web of Science has indexed 1332 articles with Karl Fischer as a key word (Topic), but more than 3600 mentioning the technique (All fields). A bibliometric analysis classifies these contributions into five clusters: spectroscopy, stability, temperature, solubility, and mixtures.</p>","PeriodicalId":9400,"journal":{"name":"Canadian Journal of Chemical Engineering","volume":"102 9","pages":"2980-2997"},"PeriodicalIF":1.6000,"publicationDate":"2024-05-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://onlinelibrary.wiley.com/doi/epdf/10.1002/cjce.25295","citationCount":"0","resultStr":"{\"title\":\"Experimental methods in chemical engineering: Karl Fischer titration\",\"authors\":\"Paula Rivera-Quintero, Gregory S. Patience, Nicolas A. Patience, Daria C. Boffito, Xavier Banquy, Dalma Schieppati\",\"doi\":\"10.1002/cjce.25295\",\"DOIUrl\":null,\"url\":null,\"abstract\":\"<p>Karl Fischer titration (KF) measures the water content in organic and inorganic compounds. Water reacts with a titrant solution containing iodine and a sulphurous monoalkyl ester to produce a monoalkyl sulphate ester and HI. In volumetric titrators, a burette injects the titrant directly into a cell while coulometric titrators generate titrant in situ. Regardless of the volume of the sample, volumetric titration is limited to 100 mg, while coulometric titration is best suited for <span></span><math>\\n <mrow>\\n <mo>></mo>\\n <mn>2</mn>\\n <mspace></mspace>\\n <mi>mg</mi>\\n </mrow></math>. KF is fast (<span></span><math>\\n <mrow>\\n <mo><</mo>\\n <mn>2</mn>\\n <mspace></mspace>\\n <mi>min</mi>\\n </mrow></math>), considered accurate (<span></span><math>\\n <mrow>\\n <mo>±</mo>\\n <mn>5</mn>\\n <mo>%</mo>\\n </mrow></math>), and precise (<span></span><math>\\n <mrow>\\n <mo><</mo>\\n <mn>1</mn>\\n <mspace></mspace>\\n <mo>%</mo>\\n </mrow></math>). However, factors such as humidity, non-standard analytes (hexane, isopropanol, ethylene glycol), tritrant composition, and temperature compromise its repeatability: the % sample standard deviation, <span></span><math>\\n <mrow>\\n <mi>s</mi>\\n </mrow></math> (<span></span><math>\\n <mrow>\\n <mi>n</mi>\\n <mo>=</mo>\\n <mn>4</mn>\\n </mrow></math>), varied from 2% to 60% (<span></span><math>\\n <mrow>\\n <mover>\\n <mi>s</mi>\\n <mo>¯</mo>\\n </mover>\\n <mo>=</mo>\\n <mn>22</mn>\\n <mo>%</mo>\\n <mo>,</mo>\\n <msub>\\n <mi>n</mi>\\n <mtext>conditions</mtext>\\n </msub>\\n <mo>=</mo>\\n <mn>19</mn>\\n </mrow></math>). This high variability is, in part, due to the experimental design that included samples and conditions ill-suited for the technique. However, even for the tests for which KF is suitable, <span></span><math>\\n <mrow>\\n <mover>\\n <mi>s</mi>\\n <mo>¯</mo>\\n </mover>\\n <mo>></mo>\\n <mn>10</mn>\\n <mo>%</mo>\\n </mrow></math>. Certain compounds react with the titrant, which increases the variability. The main sources of error affecting the analysis are ambient moisture, pH, solvent, sample handling, and titration speed. As of 2023, the Web of Science has indexed 1332 articles with Karl Fischer as a key word (Topic), but more than 3600 mentioning the technique (All fields). A bibliometric analysis classifies these contributions into five clusters: spectroscopy, stability, temperature, solubility, and mixtures.</p>\",\"PeriodicalId\":9400,\"journal\":{\"name\":\"Canadian Journal of Chemical Engineering\",\"volume\":\"102 9\",\"pages\":\"2980-2997\"},\"PeriodicalIF\":1.6000,\"publicationDate\":\"2024-05-02\",\"publicationTypes\":\"Journal Article\",\"fieldsOfStudy\":null,\"isOpenAccess\":false,\"openAccessPdf\":\"https://onlinelibrary.wiley.com/doi/epdf/10.1002/cjce.25295\",\"citationCount\":\"0\",\"resultStr\":null,\"platform\":\"Semanticscholar\",\"paperid\":null,\"PeriodicalName\":\"Canadian Journal of Chemical Engineering\",\"FirstCategoryId\":\"5\",\"ListUrlMain\":\"https://onlinelibrary.wiley.com/doi/10.1002/cjce.25295\",\"RegionNum\":4,\"RegionCategory\":\"工程技术\",\"ArticlePicture\":[],\"TitleCN\":null,\"AbstractTextCN\":null,\"PMCID\":null,\"EPubDate\":\"\",\"PubModel\":\"\",\"JCR\":\"Q3\",\"JCRName\":\"ENGINEERING, CHEMICAL\",\"Score\":null,\"Total\":0}","platform":"Semanticscholar","paperid":null,"PeriodicalName":"Canadian Journal of Chemical Engineering","FirstCategoryId":"5","ListUrlMain":"https://onlinelibrary.wiley.com/doi/10.1002/cjce.25295","RegionNum":4,"RegionCategory":"工程技术","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":null,"EPubDate":"","PubModel":"","JCR":"Q3","JCRName":"ENGINEERING, CHEMICAL","Score":null,"Total":0}
Experimental methods in chemical engineering: Karl Fischer titration
Karl Fischer titration (KF) measures the water content in organic and inorganic compounds. Water reacts with a titrant solution containing iodine and a sulphurous monoalkyl ester to produce a monoalkyl sulphate ester and HI. In volumetric titrators, a burette injects the titrant directly into a cell while coulometric titrators generate titrant in situ. Regardless of the volume of the sample, volumetric titration is limited to 100 mg, while coulometric titration is best suited for . KF is fast (), considered accurate (), and precise (). However, factors such as humidity, non-standard analytes (hexane, isopropanol, ethylene glycol), tritrant composition, and temperature compromise its repeatability: the % sample standard deviation, (), varied from 2% to 60% (). This high variability is, in part, due to the experimental design that included samples and conditions ill-suited for the technique. However, even for the tests for which KF is suitable, . Certain compounds react with the titrant, which increases the variability. The main sources of error affecting the analysis are ambient moisture, pH, solvent, sample handling, and titration speed. As of 2023, the Web of Science has indexed 1332 articles with Karl Fischer as a key word (Topic), but more than 3600 mentioning the technique (All fields). A bibliometric analysis classifies these contributions into five clusters: spectroscopy, stability, temperature, solubility, and mixtures.
期刊介绍:
The Canadian Journal of Chemical Engineering (CJChE) publishes original research articles, new theoretical interpretation or experimental findings and critical reviews in the science or industrial practice of chemical and biochemical processes. Preference is given to papers having a clearly indicated scope and applicability in any of the following areas: Fluid mechanics, heat and mass transfer, multiphase flows, separations processes, thermodynamics, process systems engineering, reactors and reaction kinetics, catalysis, interfacial phenomena, electrochemical phenomena, bioengineering, minerals processing and natural products and environmental and energy engineering. Papers that merely describe or present a conventional or routine analysis of existing processes will not be considered.