ASTM E411-2017 red 1780 Standard Test Method for Trace Quantities of Carbonyl Compounds with 2 4-Dinitrophenylhydrazine《用2 4-二硝基苯肼测定羰基化合物痕量的标准试验方法》.pdf
《ASTM E411-2017 red 1780 Standard Test Method for Trace Quantities of Carbonyl Compounds with 2 4-Dinitrophenylhydrazine《用2 4-二硝基苯肼测定羰基化合物痕量的标准试验方法》.pdf》由会员分享,可在线阅读,更多相关《ASTM E411-2017 red 1780 Standard Test Method for Trace Quantities of Carbonyl Compounds with 2 4-Dinitrophenylhydrazine《用2 4-二硝基苯肼测定羰基化合物痕量的标准试验方法》.pdf(5页珍藏版)》请在麦多课文档分享上搜索。
1、Designation: E411 12E411 17Standard Test Method forTrace Quantities of Carbonyl Compounds with 2,4-Dinitrophenylhydrazine1This standard is issued under the fixed designation E411; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the
2、 year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1. Scope*1.1 This test method covers the determination of total carbonyl in the range from 0.5 to 50 g calculated as CO.1
3、.2 This test method is intended to be general and does not include steps for sample preparation.1.3 Acetals that hydrolyze under the conditions of the test are also determined.1.4 Carbonyl derivatives such as acetals and imines that are easily hydrolyzed may be determined by an alternative procedure
4、.1.5 The developed color is not stable and must be measured within a specified period.NOTE 1Other test methods for the determination of traces of carbonyl compounds are given in Test Methods D1089, D1612, D2119, and D2191.1.6 Review the current appropriate Material Safety Data Sheets (MSDS)(SDS) for
5、 detailed information concerning toxicity, firstaid procedures, and safety precautions.1.7 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.1.8 This standard does not purport to address all of the safety concerns, if any, assoc
6、iated with its use. It is the responsibilityof the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatorylimitations prior to use. Specific hazards statements are given in Note 4Section 7 and Section 8.1.9 This international standard
7、was developed in accordance with internationally recognized principles on standardizationestablished in the Decision on Principles for the Development of International Standards, Guides and Recommendations issuedby the World Trade Organization Technical Barriers to Trade (TBT) Committee.2. Reference
8、d Documents2.1 ASTM Standards:2D1089 Method of Test for Carbonyl Content of Butadiene (Withdrawn 1984)3D1193 Specification for Reagent WaterD1612 Test Method for Acetone in Methanol (Withdrawn 2011)3D2119 Test Method for Aldehydes in Styrene MonomerD2191 Test Method for Acetaldehyde Content of Vinyl
9、 AcetateE60 Practice for Analysis of Metals, Ores, and Related Materials by SpectrophotometryE180 Practice for Determining the Precision of ASTM Methods for Analysis and Testing of Industrial and Specialty Chemicals(Withdrawn 2009)3E300 Practice for Sampling Industrial Chemicals3. Summary of Test Me
10、thod3.1 The sample containing traces of carbonyl compounds is reacted with an acidic solution of 2,4-dinitrophenylhydrazine toform the hydrazone which, upon reaction with potassium hydroxide, forms a wine-red color, presumably due to a resonating1 This test method is under the jurisdiction of ASTM C
11、ommittee D16 on Aromatic Hydrocarbons Aromatic, Industrial, Specialty and Related Chemicals and is the directresponsibility of Subcommittee D16.15 on Industrial and Specialty General Standards.Current edition approved April 1, 2012April 15, 2017. Published June 2012April 2017. Originally approved in
12、 1970. Last previous edition approved in 20052012 asE411 05.E411 12. DOI: 10.1520/E0411-12.10.1520/E0411-17.2 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standardsvolume information, refer to the stand
13、ards Document Summary page on the ASTM website.3 The last approved version of this historical standard is referenced on www.astm.org.This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version
14、. Becauseit may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current versionof the standard as published by ASTM is to be considered the official document.*A Summary of Changes section
15、 appears at the end of this standardCopyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States1quinoidal ion. The intensity of the red color, which is a function of the carbonyl concentration, is determined photometrically andthe amount of carbo
16、nyl is read directly from a previously prepared calibration curve. This test method is based upon the work ofLappin and Clark.44. Significance and Use4.1 This test method is applicable to the determination of trace amounts of aldehydes and ketones in aqueous solutions and awide variety of organic so
17、lvents.5. Interferences5.1 This test method has been found to be relatively free from interferences. It is necessary, however, to test a sample to ensurethat it does not interfere.5.2 Carbonyl compounds containing conjugated unsaturation interfere by absorbing at a different wavelength than othercar
18、bonyl compounds.5.3 Acetals that are only partially hydrolyzed under the conditions of the test will interfere. A higher reaction temperature isrequired to effect complete hydrolysis.5.4 Certain carbonyl compounds such as diisobutyl ketone have been found to undergo incomplete reactions and thus giv
19、e lowresults. These compounds may be determined if a suitable calibration is made using the compound in question.5.5 Because of the extreme sensitivity of this test method, it is necessary to perform the test in a room from which acetone orother carbonyl compound vapors are excluded.6. Apparatus6.1
20、Spectrophotometer or Photometer, capable of measuring light absorption at 480 nm and holding a 1-cm cell.NOTE 2If a filter photometer is used, a narrow band filter having its maximum transmission at approximately 480 nm should be used. A discussionof photometers and photometric practice is given in
21、Practice E60.6.2 Absorption Cells, 1-cm.6.3 All glassware must be cleaned before use. Rinse thoroughly with water and finally with methanol. Do not use acetone todry the glassware.NOTE 3The precision and bias reported in this test method were determined using chromic acid cleaning solution to clean
22、the glassware. The effecton precision and bias of using other cleaning materials has not been determined.7. Reagents7.1 Purity of ReagentsUnless otherwise indicated, it is intended that all reagents shall conform to the specifications of theCommittee on Analytical Reagents of the American Chemical S
23、ociety, where such specifications are available.5 Other grades maybe used, provided it is first ascertained that the reagent is of sufficiently high purity to permit its use without lessening the accuracyof the determination.7.2 Purity of WaterUnless otherwise indicated, references to water shall be
24、 understood to mean Types II or III reagent wateras defined in Specification D1193.7.3 Methanol, Carbonyl-freeTo 4 L of methanol add 20 g of 2,4-dinitrophenylhydrazine and 2 mL of hydrochloric acid (HCl,sp gr 1.19). Reflux for 2 h and then distill using a 2 to 3-ft fractionating column. Discard the
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