ASTM E411-12
(Test Method)Standard Test Method for Trace Quantities of Carbonyl Compounds with 2,4-Dinitrophenylhydrazine
Standard Test Method for Trace Quantities of Carbonyl Compounds with 2,4-Dinitrophenylhydrazine
SIGNIFICANCE AND USE
This test method is applicable to the determination of trace amounts of aldehydes and ketones in aqueous solutions and a wide variety of organic solvents.
SCOPE
1.1 This test method covers the determination of total carbonyl in the range from 0.5 to 50 μg calculated as CO.
1.2 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.
1.5 The developed color is not stable and must be measured within a specified period.
Note 1—Other 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) for detailed information concerning toxicity, first aid 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, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. Specific hazards statements are given in Note 4 and Section 8.
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Designation: E411 − 12
Standard Test Method for
Trace Quantities of Carbonyl Compounds with 2,4-
1
Dinitrophenylhydrazine
This standard is issued under the fixed designation E411; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope* D1089Method of Test for Carbonyl Content of Butadiene
3
(Withdrawn 1984)
1.1 This test method covers the determination of total
D1193Specification for Reagent Water
carbonyl in the range from 0.5 to 50 µg calculated as CO.
D1612Test Method for Acetone in Methanol (Withdrawn
3
1.2 This test method is intended to be general and does not
2011)
include steps for sample preparation.
D2119Test Method for Aldehydes in Styrene Monomer
D2191Test Method for Acetaldehyde Content of Vinyl
1.3 Acetals that hydrolyze under the conditions of the test
Acetate
are also determined.
E60Practice for Analysis of Metals, Ores, and Related
1.4 Carbonyl derivatives such as acetals and imines that are
Materials by Spectrophotometry
easily hydrolyzed may be determined by an alternative proce-
E180Practice for Determining the Precision of ASTM
dure.
Methods for Analysis and Testing of Industrial and Spe-
3
1.5 The developed color is not stable and must be measured
cialty Chemicals (Withdrawn 2009)
within a specified period.
E300Practice for Sampling Industrial Chemicals
NOTE1—Othertestmethodsforthedeterminationoftracesofcarbonyl
3. Summary of Test Method
compoundsaregiveninTestMethodsD1089,D1612,D2119,andD2191.
3.1 The sample containing traces of carbonyl compounds is
1.6 Review the current appropriate Material Safety Data
reacted with an acidic solution of 2,4-dinitrophenylhydrazine
Sheets (MSDS) for detailed information concerning toxicity,
to form the hydrazone which, upon reaction with potassium
first aid procedures, and safety precautions.
hydroxide, forms a wine-red color, presumably due to a
1.7 The values stated in SI units are to be regarded as
resonating quinoidal ion. The intensity of the red color, which
standard. No other units of measurement are included in this
is a function of the carbonyl concentration, is determined
standard.
photometrically and the amount of carbonyl is read directly
1.8 This standard does not purport to address all of the from a previously prepared calibration curve.This test method
4
safety concerns, if any, associated with its use. It is the
is based upon the work of Lappin and Clark.
responsibility of the user of this standard to establish appro-
4. Significance and Use
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use. Specific hazards
4.1 This test method is applicable to the determination of
statements are given in Note 4 and Section 8.
trace amounts of aldehydes and ketones in aqueous solutions
and a wide variety of organic solvents.
2. Referenced Documents
5. Interferences
2
2.1 ASTM Standards:
5.1 This test method has been found to be relatively free
from interferences. It is necessary, however, to test a sample to
ensure that it does not interfere.
1
This test method is under the jurisdiction of ASTM Committee D16 on
Aromatic Hydrocarbons and Related Chemicals and is the direct responsibility of
5.2 Carbonyl compounds containing conjugated unsatura-
Subcommittee D16.15 on Industrial and Specialty General Standards.
tion interfere by absorbing at a different wavelength than other
Current edition approved April 1, 2012. Published June 2012. Originally
carbonyl compounds.
approved in 1970. Last previous edition approved in 2005 as E411–05. DOI:
10.1520/E0411-12.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
3
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM The last approved version of this historical standard is referenced on
Standards volume information, refer to the standard’s Document Summary page on www.astm.org.
4
the ASTM website. Lappin, G. R., and Clark, L. C., Analytical Chemistry, Vol 23, 1951, p. 541.
*A Summary of Changes section appears at the end of this standard
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1
---------------------- Page: 1 ----------------------
E411 − 12
5.3 Acetals that are only partially hydrolyzed under the 7.4 Potassium Hydroxide Solution (100 g/L)—Dissolve 100
conditions of the test will interfere.Ahigher reaction tempera- gofpotassiumhydroxide(KOH)in200mLofwater.Cooland
ture is required to effect complete hydrolysis. dilute to 1 L with methanol.
5.4 Certain carbonyl compounds such as diisobutyl ketone 7.5 2,4-Dinitrophenylhydrazine (1
...
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. Because
it 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 version
of the standard as published by ASTM is to be considered the official document.
Designation:E411–05 Designation:E411–12
Standard Test Method for
Trace Quantities of Carbonyl Compounds with 2,4-
1
Dinitrophenylhydrazine
This standard is issued under the fixed designation E411; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript 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 µg calculated as CO.
1.2 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.
1.5 The developed color is not stable and must be measured within a specified period.
NOTE 1—Other 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) for detailed information concerning toxicity, first aid
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, associated with its use. It is the responsibility
of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory
limitations prior to use. Specific hazards statements are given in Note 4 and Section 8.
2. Referenced Documents
2
2.1 ASTM Standards:
D1089 Test Method of Test for Carbonyl Content of Butadiene3
D1193 Specification for Reagent Water
D1612 Test Method for Acetone in Methanol
D2119 Test Method for Aldehydes in Styrene Monomer
D2191 Test Method for Acetaldehyde Content of Vinyl Acetate
E60 Practice for Analysis of Metals, Ores, and Related Materials by Spectrophotometry
E180 Practice for Determining the Precision ofASTM Methods forAnalysis and Testing of Industrial and Specialty Chemicals
E300 Practice for Sampling Industrial Chemicals
3. Summary of Test Method
3.1 The sample containing traces of carbonyl compounds is reacted with an acidic solution of 2,4-dinitrophenylhydrazine to
form the hydrazone which, upon reaction with potassium hydroxide, forms a wine-red color, presumably due to a resonating
quinoidal ion. The intensity of the red color, which is a function of the carbonyl concentration, is determined photometrically and
the amount of carbonyl is read directly from a previously prepared calibration curve. This test method is based upon the work of
3
Lappin and Clark.
4. Significance and Use
4.1 This test method is applicable to the determination of trace amounts of aldehydes and ketones in aqueous solutions and a
wide variety of organic solvents.
1
This test method is under the jurisdiction of ASTM Committee E15 on Industrial and Specialty Chemicals and is the direct responsibility of Subcommittee E15.01 on
General Standards.
Current edition approved MarchApril 1, 2005.2012. Published April 2005.June 2012. Originally approved in 1970. Last previous edition approved in 20042005 as
E411 – 045. DOI: 10.1520/E0411-05.10.1520/E0411-12.
2
For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at service@astm.org. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
3
Lappin, G. R., and Clark, L. C., Analytical Chemistry, Vol 23, 1951, p. 541.
*A Summary of Changes section appears at the end of this standard.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
1
---------------------- Page: 1 ----------------------
E411–12
5. Interferences
5.1 This test method has been found to be relatively free from interferences. It is necessary, however, to test a sample to ensure
that it does not interfere.
5.2 Carbonyl compounds containing conjugated unsaturation interfere by absorbing at a different wavelength than other
carbonyl compounds.
5.3 Acetals that are only partially hydrolyzed under the conditions of the test will interfere. A higher reaction temperature is
required to effect complete hydrolysis.
5.4 Certain carbonyl compounds such as
...
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