PB81-213258
Bibliography on Hazardous
Materials Analysis Methods
Aerospace Corp.
Germantown, MD
Prepared for
Municipal Environmental Research l,ab
Cincinnati, OH
Jun 81
U.S. DEPARTMENT OF COMMERCE
National Technical Information Service
NITS
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P381-213258
EPA 600/2-81-094
June 1981
BIBLIOGRAPHY
ON HAZARDOUS MATERIALS
ANALYSIS METHODS
by
Jean R. Simons
Environment and Conservation Directorate
THE AEROSPACE CORPORATION
Germantown, Maryland
Contract No. 68-03-2609
Project Officer
Michael Gruenfeld
Oil and Hazardous Materials Spills Branch
Solid and Hazardous Waste Research Division
Municipal Environmental Research Laboratory, Cincinnati
Edison, New Jersey 08837
MUNICIPAL ENVIRONMENTAL RESEARCH LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
U. S. ENVIRONMENTAL PROTECTION AGENCY
CINCINNATI, OHIO 45268
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TECHNICAL REPORT DATA
(Please read Jaumcnont on the reverse before eomoleanf)
1. REPORT NO.
EPA-600/2-81-094
ORD Report-
3. RECIPIENT'
PBH
•S ACCESSION NO.
21325 8
4. TITLE AND SUBTITLE
Bibliography on Hazardous Materials Analysis Methods
5. REPORT DATE
.limp 10Q1
5. PERFORMING ORGANIZATION CODE
7 AUTMCR(S)
Jean R. Simons
8. PERFORMING ORGANIZATION REPORT NO.
9. PERFORMING ORGANIZATION NAME AND AOORE5S
Environment and Conservation Directorate
The Aerospace Corporation
Germantown, Maryland 20767
10. PROGRAM ELEMENT NO.
MERL-BBF-nm
3.-BBF
THACT/(
11. CONTRACT/GRANTNC.
68-03-2609
II. SPONSORING AGENCY NAME AND ADDRESS
Municipal Environmental Research Laboratory - Cin., OH
Office of Research and Development
U.S. Environmental Protection Agency
Cincinnati, Ohio 45268
13. TYPE Of REPORT AND PERICD COVERED
Final
14. SPONSORING AGENCY CSOE
EFA/600/14
19. SUPPLEMENTARY NOTES
Project Officer: Michael Gruenfeld
(201) 321-6625
16. ABSTRACT
A comprehensive annotated bibliography of analytical methods for 67 of the
chemicals on the Environmental Protection Agency's Hazardous Substances
List is presented. Literature references were selected and abstracts of analytical
methods were compiled to facilitate rapid and accurate identification of the
substances when discharged into the environment. Literature search procedures are
outlined and general selection criteria for the analytical methods are discussed.
Cross references are included for methods applicable to more than one of the hazardous
substances.
17.
KEY WORDS ANO DOCUMENT ANALYSIS
DESCRIPTORS
b.lDENTIFISRS/OPEN ENDED TERMS C. CCSATI Field/Group
Analytical Methods
Hazardous Waste
Bibliography
7B
7C
13B
13. DISTRIBUTION STATEMENT
Release Unlimited
19. SECURITY CLASS fTTia Xeponf
llnrl actii f i'oH
21.
20. SECURITY CLASS (Tnu pagcf
Unclassified
EPA Form 2220.1 (9-73)
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DISCLAIMER
This report has been reviewed by the Municipal Environmental Research
Laboratory-Cincinnati, U.S. Environmental Protection Agency, and approved
for publication. Approval does not signify that the contents necessarily
reflect the views and policies of the U.S. Environmental Protection Agency,
nor does mention of trade names or commercial products constitute endorse-
ment or recommendation for use.
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FOREWORD
The U.S. Environmental Protection Agency was created because of increasing
public and government concern about the dangers of pollution to the health and
welfare of the American people. Noxious air, foul water, and spoiled land are
tragic testimonies to the deterioration of our natural environment. The com-
plexity of that environment and the interplay of its components require a con-
centrated and integrated attack on the problem.
Research and development is that necessary first step in problem solution;
it involves defining the problem, measuring its impact, and searching for solu-
tions. The Municipal Environmental Research Laboratory develops new and im-
proved technology and systems to prevent, treat, and manage wastewater and solid
and hazardous waste pollutant discharges from municipal and community sources, to
preserve and treat public drinking water supplies, and to minimize the adverse
economic, social, health, and aesthetic effects of pollution. This publication
is one of the products of that research and provides a most vital communications
link between the researcher and the user community.
This report is a product of the above effort. It abstracts and cites pub-
lished methods of chemical analysis for organic and inorganic hazardous materials.
It thereby facilitates rapid selection of appropriate analytical methods pertain-
ing to treatability studies, emergency response actions, and general pollution
monitoring activities. This project is part of the continuing program of the
Oil and Hazardous Materials Spills Branch, MERL-Ci, to assess and mitigate the
environmental impact of oil and hazardous material pollution.
Francis T. Mayo, Director
Municipal Environmental Research
Laboratory
iii
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ABSTRACT
A comprehensive annotated bibliography of analytical methods for 67 of the
chemicals on the Environmental Protection Agency's Hazardous Substances
List is presented. Literature references were selected and abstracts of
analytical methods were compiled to facilitate rapid and accurate
identification of the substances when discharged into the environment.
Literature search procedures are outlined and general selection criteria
for the analytical methods are discussed. Cross references are included
for methods applicable to more than one of the hazardous substances.
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TABLE OF CONTENTS
DISCLAIMER ii
FOREWORD i i i
ABSTRACT iv
TABLE OF CONTENTS v
I. Introduction 1
II. Development of the Bibliography 2
Selection of Target Chemicals 2
Literature Search Procedures 5
Selection Criteria for Analytical Methods 5
III. Description of the Bibliography 7
Organization and Information Content 7
Utilization 7
Limitations 7
IV. References 9
V. Bibliography 10
VI. Index to Compound Names 78
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BIBLIOGRAPHY ON HAZARDOUS MATERIALS ANALYSIS METHODS
I, Introduction
Section 311 (b) C.2) CA) of the Federal Water Pollution Control Act
(Public Law 92-500) charges the Administrator of the Environmental
Protection Agency (EPA) with the development of regulations designating
as hazardous substances such elements and compounds that, when discharged
into or upon navigable waters, present an imminent and substantial danger
to the public health or welfare. Based on toxicological and discharge
potential criteria, the EPA has designated 271 chemicals on its Hazardous
Substances List. Rapid and accurate identification of these chemicals
is essential when an accident involving discharge of these substances
into the environment occurs. To facilitate such identification, the Oil
and Hazardous Materials Spills Branch of the EPA commissioned a review of
the literature to determine the best methods of analysis for these
chemical substances.
This report contains a comprehensive annotated bibliography and
ancillary file of methods of analysis for 67 chemicals on the Hazardous
Substances List. The compounds addressed herein fall into the following
three major categories: 1) pesticides/herbicides, 2) organic compounds,
and 3) inorganic compounds, excluding metal salts.
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II. Development of the Bibliography
Selection of Target Chemicals
A target list of 100 compounds on the Hazardous Substances List
was selected for tentative inclusion in the Bibliography on Hazardous
Materials Analysis Methods. Emphasis was placed on organic compounds
v«hich retain their identity on admixture with cold water, as the
analytical procedures were to be based on the assumption that samples
are recovered from aqueous media. Several inorganic compounds,
excluding metal salts, were then selected to yield the full complement
of 100 compounds. Note that analytical methods for compounds appearing
on both the "Priority Pollutants" list, also known as "Consent Decree"
compounds, and the Hazardous Substances List have been addressed else-
where and were therefore omitted from this bibliography.*
The Priority Pollutants list emanated from a court settlement ,
involving the EPA and several environmentally concerned plaintiffs, and
commonly known as the "EPA Consent Decree". This judicial action
required EPA to publish a list of toxic pollutants for which technology-
based effluent limitations and guidelines would be required.
The EPA Project Officer divided the 100 chemicals into three
different categories, based on priority. Hazardous substances thus
determined to be of highest priority were addressed first. Within the
budgeted manpower limitations for this bibliography, methods of analysis
were assessed for the compounds in all but the lowest priority grouping.
Table 1 comprises a list of the 67 compounds included in the final
bibliography.
*EPA has proposed (Federal Register 44 (233), December 3, 1979)
guidelines establishing test procedures for the analysis of pollutants.
The proposed procedures include one or more analytical methods for
each of the Priority Pollutants except bis(chloromethyl)ether, which
decomposes rapidly in an aqueous medium.
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Table 1. List of Compounds Included in Bibliography on Hazardous
Material Analysis Methods
acetaldehyde
acetone cyanohydrin
ally! alcohol
amyl acetate
aniline
benzoic acid
benzonitrile
benzyl chloride
butyl acetate
butyl amine
butyric acid
captan
carbaryl
carbon disulfide
chlorpyrifos
coumaphos
cresol
cyanogen chloride
2, 4-D acid
2, 4-D ester
diazinon
dicamba
dichlobenil
dichlone
2, 2-dichloropropionic acid
dichlorvos
diethyl amine
dinitrobenzene
diquat
disulfoton
diuron
dodecylbenzenesulfonic acid
eth'ion
ethylenediamine
formic acid
fumaric acid
furfural
guthion
hydrofluoric acid
hydrogen cyanide
isoprene
kelthane
malathion
maleic acid
methoxychlor
methyl mercaptan
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methyl methacrylate
methyl parathion
mevinphos
mexacarbate
naled
paraformaldehyde
parathion
phosphoric acid
propionic acid
pyrethrins
quinoline
resorcinol
strychnine
styrene
2, 4, 5-T acid
2, 4, 5-T ester
tetraethyl lead
trichlorfon
triethylamine
vinyl acetate
xylene
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Literature Search Procedures
The primary data base for the literature searches was the Chemical
Abstracts condensates files available through the Lockheed Dialog
Retrieval Service. The Chemical Abstracts registry number for each
compound was combined with key words such as analysis, identification,
and determination to retrieve pertinent titles of technical publications.
For most compounds, the search was conducted for publications which
appeared during the years 1972 through 1978. The search was extended
through 1970 (Volume 72 of Chemical Abstracts) if the recent literature
did not yield a sufficient number of satisfactory references. In most
cases for which a large number of appropriate references were available,
the search was restricted to English-language publications. Through the
Dialog system, access was gained not only to the chemical and biochemical
journals but also to relevant sources such as NTIS and ASTM publications.
The titles thus retrieved were narrowed to the five to seven articles
for each compound which appeared to be potentially most useful. Abstracts
of these publications were read and considered. After the abstracts were
examined, up to four papers which were expected to include appropriate
analytical methods were ordered for each compound. Some of the papers
thus selected did not contain the desired information. In'those cases,
additional papers were ordered, if available. To accommodate the report
submission schedule, no papers were ordered after May 25, 1979. Up to
three of the "best" methods, according to the criteria enumerated in the
following section of this report, were included in the bibliography.
If no appropriate titles were retrieved, an effort was made to report
a closely related compound, or a compound which can easily be derived from
the desired compound. For example, formaldehyde was substituted for para-
formaldehyde, the polymeric form of the former compound.
Several EPA laboratories were contacted by the Project Officer to
determine whether work was underway in-house to develop analytical methods
for the compounds under consideration and thus to avoid duplication of
effort. The U. S. Coast Guard was similarly queried. This report does
not appear to duplicate any existing reports or work in progress.
Selection Criteria for Analytical Methods
The formal selection criteria for the analytical methods were as
follows:
o practicality of the method for rapid laboratory use (i.e.,
rapid and simple sample processing)
o occupational safety of prescribed reagents
o correctness of quantification data
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o ability to identify the presence, and possibly the source,
of the material
o practicality of the method in relation to the availability
of common laboratory instruments (i.e., mass spectrometer;
vapor phase and high-pressure liquid chromatographs; ultra-
violet/visible, infrared, and nuclear magnetic resonance
spectrophotometers; fluorescence and atomic absorption
spectrometers, etc.)
Several other factors were considered in the selection of analytical
methods. When three good analytical methods for aqueous samples were
not available for a hazardous substance, the order of preference of
sample source has 1) water, 2) sediment, 3) air, and 4) tissue. Super-
imposed on this ranking was a preference for English language articles to
minimize translation problems. Variety in types of analytical methods was
considered desirable. A rapid method for the mere detection of a compound
might complement a more elaborate or time-consuming quantitative method.
Whenever possible, methods were chosen employing different instrumentation
techniques to circumvent delays caused by unavailability or temporary
malfunctioning of a particular piece of equipment; consequently, two gas
chronatographic methods and one spectrophotometric method would be
preferred over three gas chromatographic methods. Lastly, if all other
factors were deemed equal, the most recent publications were selected.
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III. Description of the Bibliography
Organization and Information Content
The bibliography is organized alphabetically by compound name as
indicated in the Hazardous Substances List. The entry for each
compound includes the name, followed by alternate names, abstracts of
up to three analytical methods, and, where applicable, cross references
to methods for other compounds which identify or determine the compound
of interest.
For each method, the general category of analytical method is
reported (e.g., wet chemical, thin-layer chromatography, ultraviolet
spectrophotometry, etc.), followed by the literature reference. The
abstract itself is a summary not of the entire article but of the
analytical procedure and includes the equipment and chemicals required
for the analysis and general sample preparation measures. Information
regarding maximum or minimum detection limits or sample size is given if
these data were reported in the primary literature.
Although each analytical method is designated by the letter A, B,
or C, the letters serve merely as labels for ease in cross-referencing
and are not intended to connote the relative merits of the methods.
Utilization
The abstracts are designed to enable laboratory personnel to
determine quickly which method is most appropriate for a given analysis
problem. The lack of a suitable chromatographic colac:n or reagent
specified in the abstract would immediately be apparent, and cause a
method to be eliminated from further consideration. Information
regarding limits of detection and time required to perform the analysis
is included, where .available, to aid the analyst in selecting a method.
As many of the compounds included in the bibliography are closely
related, the methods are frequently applicable to several compounds.
Cross references are supplied in the following format: "see dia:inon,
method A; coumaphos, B; malathion, A."
An index of the compound names and all of the alternate names
reported in the bibliographic headings provides a means of access to the
analytical methods.
Limitations
When many references (more than 50) were located for a particular
compound, only English-language publications were considered. Therefore,
the "optimal" analytical methods might have been omitted if they appeared
in foreign-language journals.
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The selection was weighted toward recent papers in widely circulated
journals, if all other considerations appeared to be equal. It is
possible that a superior older method could have been excluded.
The analytical procedures were valid and current at the completion.of
literature survey. The user should be aware that the chemical literature
changes and expands rapidly to reflect frequent innovations in sampling,
wet-chemical procedures, and instrumentation.
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IV. References
1. Federal Register 43(49), March 13, 1978
2. Natural Resources Defense Council v. Train, U. S. District
Court, District of Columbia, Consent Decree, Natural Resources
Defense Council, Inc., et al., v. Russell E. Train; Environmental
Defense Fund et al. v. Russell E. Train; Citizens for a Better
Environment et al. v. Russell E. Train; Natural Resources Defense
Council, Inc. v. James A. Agee et al., Nos. 78-2153, 75-172,
75-1698, and 75-1267, June 8, 1976.
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V. Bibliography
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ACETALDEHYDE
o ethanal, ethyl aldehyde, acetic aldehyde
METHOD A - Wet Chemical and Visible Spectrophotometry
o CHARACTERISTIC DETECTION AND DETERMINATION OF ALIPHATIC
ALDEHYDES
o Chem. Pharra. Bull. 1975, 23 (4), 891-894,
S. Tagami, T. Nakamura, T. Nakano, and D. Shiho
o Acetaldehyde forms a red product on reaction with
propionaldehyde C3-phenyl-2-quinoxalinyl)"hydrazone in
95% ethanol. Reaction is complete in 20 minutes and
absorbance of the product is measured at 465 run. The
hydrazone is synthesized from propanal and 2-hydrazino-3-
phenylquinoxaline. Effects of pH and temperature on the
reaction between hydrazone and aliphatic aldehyde are
discussed; aromatic aldehydes, glucose, and ketones do
not react.
o Limits: SxlO"5 to 1x10 M acetaldehyde
METHOD B- Gas Chromatography
o RAPID SEPARATION OF LOWER ALIPHATIC CARBONYL COMPOUNDS
BY GAS-LIQUID-SOLID CHROMATOGRAPHY
o J. Chromatogr. 1978, 152(2), 533-537
Y. Hoshika and G. Muto
o Lower aliphatic carbonyl compounds are separated by gas
Chromatography, with flame ionization detection, on a
column of 5% TCEP on 60/80 mesh Carbopack B. Relative
retention times are reported for the compounds on several
columns.
o Limits: < 300 ng
METHOD C- Titration
O MACRO- AND MICRO-DETERMINATIONS OF ACETALDEHYDE BY
OXIDATION WITH PERMANGANATE IN ACID MEDIUM CONTAINING
FLUORIDE IONS
o Indian J. Chem.1977, 15A(6), 542-544
K. A. Idriss, I. M. Issa, and M. M. Ghoneim
o A standard solution of permanganate in sulfuric acid/
sodium fluoride quantitatively oxidizes acetaldehyde
solution. The direct titration can be performed to a
visual or potentiometric endpoint. The determination can
also be made indirectly by back titration of excess
permanganate against T1(I) or Hg(I).
o Limits: 44 fig
Cross References - See furfural, method A; paraformaldehyde, C.
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ACETONE CYANOHYDRIN
o 2-methyllactonitrile, alpha-hydrojcyisobutyronitrile
METHOD A - Spectrofluorimetry
o DETECTION OF VARIOUS o- SUBSTITUTED NITRILES AND GEM
HALONITROALKANES BY CHEMILUMINESCENCE
o Anal. Chim. Acta 1975, 77, 324-326
H. W. Yurow and S. Sass
o Reaction of OOH~ with a-substituted nitriles gives an
intermediate which oxidizes luminol to a chemiluminescent
species. The nitrile is detected by mixing the sample in
a spectrofluorimetric cell with alkaline luminol and 0.30%
HjO- in tetrasodiura ethylenediaminetetraacetate and measuring
intensity of light at 410 ran. Relative light intensities for
17 compounds are listed.
o Sample size: 0.2 ml at 1.0 mg/ml
NETHODS B fi C - Wet Chemical and Visible Spectrophotometry
o DETECTION OF ACETONE, a-HYDROXYISOBUTYRONITRILE, AND
a-AMINOISOBUTYRONITRILE IN THE PRESENCE OF EACH OTHER:
DETERMINATION OF a-HYDROXYISOBUTYRONITRILE
o Mikrochim. Acta 1974, 00 , 759-764
L. Legradi
o Acetone cyanohydrin is detected in acetone by addition of
p_-nitroaniline diazonium salt solution and 2N sodium
hydroxide to the acetone sample. The dark green color
produced by acetone changes with concentration of the
cyanohydrin. For quantitative determination, absorbance
is measured at 440 run after establishing a calibration
curve. _4
o Limits: 10 % acetone cyanohydrin in acetone
o Copper sulfate solution and ammonia are added to an aqueous
sample. Acetone cyanohydrin weakens or destroys the blue
color of the copper tetraammine complex. For quantitative
determination, absorbance is measured at 560 nm after
establishing a calibration curve.
o Limits: 50 vg for detection.
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ALLYL ALCOHOL
o 2-propen-l-ol, l-propenol-3, vinyl carbinol
METHOD A - Wet Chemical
o ESTIMATION OF ALLYL ALCOHOL BY CHLORAMINE-T
o Talanta 1973, 20(3), 349-351
D. S. Mahadevappa and H. M. K. Naidu
o Allyl alcohol in aqueous solution is estimated by mild
oxidation with standard chloramine-T and iodometric back-
titration of the excess oxidizing agent. The oxidation step
is carried out in 0.5-1.0 M hydrochloric acid. The effects of
pH and the presence of several foreign ions are discussed.
o Sample size: 8-125 mg
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AMYL ACETATE
o amylacetic ester, iso-amylacetate, sec-amylacetate, t>amylacetate,
pear oil, banana oil
METHOD A - Gas Chromatography
o GAS CHROMATOGRAPHIC AND SENSORY ANALYSIS OF VOLATILES FROM
CLING PEACHES
o J. Agric. Food Chem. 1978, 26 (3), 725-732
M. D. Spencer, R. M. Pangborn, and W. G. Jennings
o Isoamyl acetate is one of 30 major volatile compounds
identified in samples of cling peaches that are pureed,
steam distilled, extracted, and analyzed by capillary gas
Chromatography. The column is coated with Carbowax 20M,
and a flame ionization detector is used. Tridecane and
octadecane serve as internal standards.
o Limits: not given
METHOD B- Gas Chromatography and Mass Spectrometry
o DETERMINATION OF BENZALDEHYDE IN WINES AND AMYL ACETATE AND
ISOAMYL ACETATE IN LIQUEURS BY GAS-LIQUID CHROMATOGRAPHY
AND CONFIRMATION BY MASS SPECTROSCOPY
o J. Assoc. Off. Anal. Chem. 1975, 58(3), 582-584
G. E. Martin, P. C. Buscemi, and B. B. Butts
o Liqueur samples are diluted with water, extracted with
pentane, dried, and analyzed by gas Chromatography (with
flame ionization detection) on a column of 10% SP-1000 on
100/120 mesh Chromosorb W (HP). Identification of amyl and
isoamyl acetates is confirmed by mass spectrometry.
o Limits: calibration of the gas chromatograph is linear
for 0-50 ppm of amyl or isoamyl acetate
METHOD C- Gas Chromatography
o GAS CHROMATOGRAPHIC RETENTIONS AS IDENTIFICATION CRITERIA
o Anal. Biochem. 1977, 78(1), 244-251
K. Yabumoto, W. G. Jennings, and M. Yamaguchi
o Over 40 flavor essences recovered from muskmelon are
identified through two-dimensional plots of Kovats indices
measured on two wall-coated open tubular capillary gas
chromatographic columns of different polarity. The coating
materials are Carbowax 20M or methyl silicone SE-30, admixed
with benzyltriphenylphosphonium chloride. Kovats indices
are reported for butyl, isobutyl, amyl, and isoamyl acetates.
o Limits: not given
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ANILINE
o aniline oil, phenylamine, aminobenzene, aminophen, kyanol
METHOD A - High-Pressure Liquid Chromatography
o HIGH-PRESSURE LIQUID CHROMATOGRAPHY OF AROMATIC AMINES
o J. Chromatogr. 1976, (119), 569-579
P. R. Young and H. M. McNair
o Fifty aromatic amines are separated by high-pressure liquid
Chromatography on various silica gels with detection at 254 nm.
For aniline, a Corasil II column is used with chloroform as
the mobil phase. A k1 value of 0.40 is reported.
o Sample size: 2-3 pg
METHOD B- Wet Chemical and Visible Spectrophotonetry
o DETECTION AND SPECTROPHOTOMETRIC DETERMINATION OF SOME
AROMATIC NITROGEN COMPOUNDS WITH p_-DIMETHYLAMINOCINNAMALDEHYDE
o Anal. Chim. Acta 1976, 86, 309-311
M. Qureshi and I. A. Khan
o p_-Dimethylan)inocinnamaldehyde is used with Dowex 50W-X8 resin
beads to detect aniline. A red color appears on the beads
after heating for five minutes. Aniline is determined
quantitatively with the aldehyde reagent, in a mixture of
ethanol and hydrochloric acid. Color develops in 30 minutes,
and absorbance is measured at 520 nm. A variety of compounds
cause no interference in the procedure.
o Limits: detection, 0.10 yg/ml; determination, 3-30 ug
METHOD C- Wet Chemical and Visible Spectrophotometry
o A SIMPLE SIMULTANEOUS COLORIMETRIC DETERMINATION OF PRIMARY
AND SECONDARY AMINES WITH FLUORESCAMINE
o Anal. Lett. 1975, 8(7), 441-448
V. Toome and K. Manhart
o Primary and secondary amines react with fluorescamine to
form, respectively, pyrrolinones or aminoenone chromophores
with long wavelength absorption maxima. A solution of
fluorescamine in dioxane is added to a solution of the
amine or amine mixture in pH 8-8.5 phosphate buffer; reaction
is complete within one minute, and spectrophotometric measure-
ments can be made immediately. Tertiary amines, alcohols,
acids, thiols, and aldehydes do not interfere.
o Limits: For aniline, Beer's Law is obeyed for 0.00-0.05 iimol/ml,
Cross References - See benzonitrile, method A; ethylenediamine, C.
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BENZOIC ACID
o benzenecarboxylic acid, phenylforraic acid, dracylic acid
METHOD A - Wet Chemical and Ultraviolet Spectre-photometry
o DETERMINATION OF BENZOIC AND SORBIC ACIDS IN ORANGE JUICE
o Analyst (London) 1976, 101 (1198), 49-54
T. Gutfinger, R. Ashkenazy, and A. Letan
o Benzoic and sorbic acids are determined under conditions
which prevent their mutual interference. Aqueous or
orange juice solutions of the two acid anions are acidified
with orthophosphoric acid and steam distilled. A portion
of the distillate is oxidized vigorously with potassium
dichromate/sulfuric acid to destroy sorbic acid and volatile
compounds. After redistillation, benzole acid is determined
spectrophotometrically at 225 run against a standard curve.
o Limits: 40-400 ppm in water; 40-1000 ppm in orange juice
METHOD B- Wet Chemical
o MICRODETERMINATION OF BENZOIC AND SALICYLIC ACIDS WITH
GUANIDINE CARBONATE AS A TITRANT
o Microchem. J. 1972, 61(2), 61-62
A. K. Saxena
o Benzoic acid in a water-alcohol mixture is titrated to the
bromcresol purple endpoint with standard guanidine carbonate
solution.
o Limits: 0.061-0.610 rag with maximum error of + 0.005 mg
Cross References - See formic acid, method A; phosphoric acid, A and B.
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BENZONITRILE
o phenyl cyanide, cyanobenzene
METHOD A - Anion-Exchange Chromatography
o NON-AQUEOUS SOLVENT CHROMATOGRAPHY. II. SEPARATION OF BENZENE
DERIVATIVES IN THE ANION-EXCHANGE AND n-BUTYL ALCOHOL SYSTEM
o J. Chromatogr. 1972, 72, 187-191
W. Funasaka, T. Hanai, K. Fujimura, and T. Ando
o The distribution coefficients, Kd', of several mono- and
disubstituted benzene compounds were determined by column
Chromatography (Amberlite CG-400 resin, type I, Cl-form) and
ultraviolet spectrophotometry. Kj'values (in ml/ml) are:
benzonitrile, 1.13; aniline, 4.14; £-xylene, 0.56; m-xylene,
0.55; p_-xylene, 0.51; £-cresol, 4.26; m-cresol, 3.70;
p_-cresol, 3.39; £-dinitrobenzene, 3.62; in-dinitrobenzene,
2.06.
o Limits: not given
METHOD B- Wet Chemical
o MICROGRAM DETECTION OF NITRILES USING RESIN BEADS
o Mikrochim. Acta 1977, 11-16
S. Z. Qureshi and M. S. Rathi
o Benzonitrile is detected via ion exchange resin beads (H+
form) after hydrolysis with dilute sulfuric acid to produce
ammonium ions. The ammonium ions are retained by the resin
and detected by adding sodium hypochlorite and phenol
solutions. N^unsubstituted amides react positively in the
absence of sulfuric acid and can thus be distinguished from
nitriles.
o Limits: 0.002 M_ benzonitrile (10 ug in 0.05 ml)
Cross References - See dinitrobenzene, method B.
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BEN'ZYL CHLORIDE
METHOD \ - Gas Chromatography
o THE GAS-LIQUID CHROMATOGRAPHY OF THE CHLOROETHANES AND
CHLOROTOLUENES
o J. Chromatogr. 1973, 76(1), 101-113
D. A. Solomons and J. S. Ratcliffe
o Mixtures of toluene, benzyl chloride, benzal chloride, and
benzotrichloride are analyzed by gas Chromatography, with
a thermal conductivity detector, on a column of 8% dinonyl
phthalate on 90/100 mesh Anochrom ADS. Benzal chloride is
not completely resolved from benzotrichloride. A calibration
curve is given for quantitative analysis.
o Sample size: O.S pi
METHOD B- Gas Chromatography
o SEPARATION OF BENZYL COMPOUNDS BY GAS-LIQUID CHROMATOGRAPHY
o J. Chromatogr. 1978, (157), 409-411
A. E. Habboush and A. Z. Al-Rubaie
o A mixture of benzyl compounds is separated by gas Chromatography
(flame ionization detector). The following nine stationary
phases are used, at 20% loading, on 80/100 mesh Chromosorb K
as support: OV-1, OV-3, OV-rll, OV-25, DECS, DEGGLU, DEGA,
EGTCP, and Carbowax 6000. The best separations are obtained
with OV-11 and DEGGLU columns.
o Sample size: 0.25 g of each benzyl compound; 0.2 to 0.4 yl
injection
METHOD C- Gas Chromatography
o QUANTITATIVE ANALYSIS OF MIXTURES OF TOLUENE AND ITS SIDE-
CHAIN-CHLORINATED DERIVATIVES BY GAS CHROMATOGRAPHY
o J. Chromatogr. 1975, (114), 247-249
R. Ramakrishnan and N. Subramanian
o Toluene and its side-chain-chlorinated derivatives are analyzed
by gas Chromatography with thermal conductivity detection on
a column of 15% silicone oil DC 200 on Celite 545. Carbon
tetrachloride is used as a standard. Relative retention times
are reported.
o Limits: not given
- 18 -
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BUTYL ACETATE
o acetic acid butyl ester
METHOD A - Gas Chromatography
o GAS-LIQUID CHROMATOGRAPHIC DETERMINATION OF SOLVENTS IN
COMMERCIAL NAIL LACQUER PREPARATIONS
o J. Assoc. Off. Anal. Chem. 1977, 60 (3), 658-662
M. J. Stutsman
o Dilution of commercial nail lacquer samples with isooctane
effects precipitation of resins and pigments from the
solvent mixture. After settling, n-butyl acetate is deter-
mined by temperature-programmed gas chromatography on a
column of 10% PEG 20M on 70/80 mesh Gas-Chrom R. n-Propyl
acetate is the internal standard, and a thermal conductivity
detector is used.
o Limits: linear relationship of peak heights from 15-750 pg
METHOD B- Gas Chromatography
o A NEW PERSONAL SAMPLER FOR ORGANIC VAPORS
o J., Am. Ind. Hyg. Assoc. 1978, 39 (9), 701-708
R. L. Bamberger, G. G. Esposito, B. W. Jacobs, G. E. Podolak,
and J. F. Mazur
o Organic vapors are sampled by collection on an adsorption
substrate contained within a small passive sampler worn by
the worker. For ii-butyl acetate determination, the sample
is desorbed by carbon disulfide and analyzed by gas
chromatography on a column of 10% FFAP. A flame ionization
detector is used.
o Limits: 93% recovery at 37.5 ppm in air.
METHOD C- Gas Chromatography
o A CONVENIENT OPTIMIZED METHOD FOR THE ANALYSIS OF SELECTED
SOLVENT VAPORS IN THE INDUSTRIAL ATMOSPHERE
o Amer. Ind. Hyg. Assoc., J. 1970, 31(2), 225-232
L. D. White, D. G. Taylor, P. A. Mauer, and R. E. Kupel
o Solvent vapors from 10-1. air samples are adsorbed onto
activated charcoal, desorbed by carbon disulfide, and
analyzed by gas chromatography with flame ionization
detection. A column of 10% FFAP on 80/100 mesh acid-washed
DMCS Chromosorb W is used.
o Limits: For 0.5-2.0 TLV, recovery is greater than 90% for
butyl acetate and for xylene.
Cross References - See amyl acetate, method C.
- 19 -
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BUTYLAMINE
o 1-aminobutane
METHOD A - Ligand-Exchange Chromatography
o STUDIES ON LIGAND-EXCHANGE CHROMATOGRAPHY. V. GAS CHROMA-
TOGRAPHIC SEPARATION OF LOWER ALIPHATIC AMINES BY LIGAND
EXCHANGE
o J. Chromatogr. 1975, 114(1), 15-21
K. Fujimura and T. Ando
o An inorganic cation exchanger, zirconium phosphate (ZP-1)
in the Cu form, is used as the stationary phase and
nitrogen containing ammonia and water vapor as the mobile
phase in the gas chromatographic separation of lower
aliphatic amines. A flame ionization detector is used.
The concentration of ammonia plays an important part in
determining both resolution and retention times.
o Samples: aqueous solutions containing 5% of each amine.
METHODS - Ion-Pair Chromatography
o ION-PAIR CHROMATOGRAPHY IN THE LOW CONCENTRATION RANGE BY
USE OF HIGHLY ABSORBING COUNTER IONS
o J. Chromatogr. 1977, 142, 283-297
J. Crommen, B. Fransson, and G. Schill
o A stationary phase containing a counter ion (naphthalene-2-
sulfonate) of high absorbance is used in a high-performance
system for ion-pair chromatography of non-UV-absorbing samples
such as alkylamines. LiChrospher SI-100 is employed as the
support phase. A good separation is obtained for isomeric
six-carbon amines.
o Limits: approximately 1 ng
Cross References - See aniline, method C; diethylamine, A, B, and C;
ethylenediamine, C.
- 20 -
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BUTYRIC ACID
o butanoic acid, ethylacetic acid
METHOD A - Gas Chromatography
0 GASH CHROMATOGRAPHIC ANALYSIS OF C.-C- FATTY ACIDS IN
AQUEOUS MEDIA USING CARBOPACK B-CARBOWAX 20M-PHOSPHORIC
ACID
o J. Chromatogr. 1978, 150(1), 259-262
J. C. DuPreez and P. M. Lategan
o A mixture of six C--C,. fatty acids is separated by gas
chromatography (flame ionization detection) on a column of
3% Carbowax 20M - 0.5% phosphoric acid on Carbopack B.
Standard aqueous samples and a culture medium sample were
analyzed.
o Limits: 8 ppra propionic or butyric acid.
METHOD B - Gas Chromatography
o DIRECT ANALYTICAL PROCEDURE FOR DETERMINATION OF VOLATILE
ORGANIC ACIDS IN RAW MUNICIPAL WASTEWATER
o Water Res. 1978, 12(7), 437-446
N. Narkis and S. Henfeld-Furie
o After addition of solid metaphosphoric acid to raw sewage,
precipitated proteins and suspended solids are removed by
centrifugation. The supernatant is injected onto a column
of 20% Carbowax "20M and 3% phosphoric acid on 60-80 mesh
acid-washed Chromosorb W. A flame ionization detector is
used.
o Limits: approximately 5 mg carboxylic acid per liter.
Cross References - See formic acid, method B; propionic acid, A.
- 21 -
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Orthocide-406, SR-406, Vancide-89
METHOD A - Liquid Chromatography
o CHLORINE-SELECTIVE DETECTION FOR LIQUID CHROMATOGRAPHY WITH
A COULSON ELECTROLYTIC CONDUCTIVITY DETECTOR
o Anal. Chem. 1977, 49 (2), 326-331
J. W. Dolan and J. N. Seiber
o High performance liquid Chromatography on Vydac reversed
phase packing is used with Coulson electrolytic conductivity
detector for selective detection of poorly UV-absorbing
organochlorine compounds in water and crop samples. Little
or no interference is caused by compounds lacking chlorine
or bromine heteroatoms.
o Limits: approximately 50 ng for lindane
METHOD B - Thin Layer Chromatography and Fluorometry
o SIMULTANEOUS DETERMINATION OF CAPTAN AND CAPTAFOL IN APPLES
AND POTATOES BY THIN LAYER CHROMATOGRAPHY AND IN SITU FLUORO-
METRY
o J. Assoc. Off. Anal. Chem. 1977, 60 (6), 1328-1330
Y. Francoeur and V. Mallet
o A crop sample is homogenized and extracted, and captan and
captafol are separated from each other and from co-extractives
by thin layer Chromatography on silica gel H impregnated with
aluminum chloride. After the plates are sprayed with sodium
chlorate and heated, fluorescence is measured directly.
o Limits: 0.02 ppm
METHOD C - Thin Layer Chromatography and Spectrofluorimetry
o THE FLUORIMETRIC DETECTION OF PESTICIDES ON ALUMINUM OXIDE
LAYERS
o J. Chromatogr. 1976, 117 (1), 129-136
G. E. Caissie and V. N. Mallet
o Fluorigenic properties of several pesticides on acidic and
basic aluminum oxide thin layers are noted both before and
after heat treatment of the chromatograms. Wavelengths and
intensities of emissions are noted and compared with
behavior of the compounds on silica gel plates.
o Limits: coumaphos, 0.02 ug; captan, 0.2 vg; guthion, 0.02 ug
Cross References - See dichlone, method A.
- 22 -
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CARBARYL
Sevin
METHOD A - Thin Layer Chromatography and Densitometry
o QUANTITATIVE DETERMINATION OF CARBARYL IN APPLES, LETTUCE,
AND WATER BY DENSITOMETRY OF THIN LAYER CHROMATOGRAMS
o J. Assoc. Off. Anal. Chem. 1978, 61 (3), 616-620
J. Sherma, A. J. Kovalchick, and R. Mack
o Carbaryl residues are extracted from water and separated on
silica gel thin-layer plates. The plates are dipped
successively in potassium hydroxide and p_ - nitrobenzene-
diazonium fluoborate to develop color, scanned with a fiber
optics densitometer, and compared with standards.
o Limits: 50 ng
METHOD B - Wet Chemical and Gas Chromatography
o GAS CHROMATOGRAPHIC DETERMINATION OF MICROAMOUNTS OF CARBARYL
AND 1- NAPHTHOL IN NATURAL WATER AS SOURCES OF WATER SUPPLIES
o J. Chromatogr. 1977, 144 (1), 77-84
K. Nagasawa, H. Uchiyama, A. Ogamo, and T. Shinozuka
o Water samples are extracted with methylene chloride, 'arid
carbaryl and its hydrolysis product, 1- naphthol, are
separated from several known organochlorine contaminants on
Amberlite XAD-8 resin. Heptafluorobutyryl derivatives are
prepared and analyzed on three gas chromatographic columns
with electron capture detection.
o Limits: 2.5-10 ppb for a 1- liter sample
METHOD C - Column Chromatography and High-Pressure Liquid Chromatography
o DIRECT ANALYSIS OF SOME CARBAMATE PESTICIDES IN FOODS BY HIGH-
__PRESSURE LIQUID CHROMATOGRAPHY
o J. Agric. Food Chem. 1977, 25(1), 211-212
J. F. Lawrence
o Pesticide residues are extracted from crops and passed through
a 2% deactivated Florisil column. The carbaraate fraction is
subjected to high-pressure liquid Chromatography on LiChrosorb
Si 60 with ultraviolet detection at 254 nm. Carbaryl and
carbofuran require separation by reversed-phase Chromatography
with Permaphase ODS.
o Limits: carbaryl, 0.9 ng; zectran, 1.0 ng
Cross References - See diazinon, method B; mevinphos, B; mexacarbate, B and C;
parathion, A; trichlorfon, B.
- 23 -
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CARBON DISULFIDE
o carbon bisulfide, dithiocarbonic anhydride
METHOD A - Wet Chemical and Ultraviolet Spectrophotonetry
o SPECTROPHOTOMETRIC DETERMINATION OF CARBON DISULPHIDE AS
THE l,2,3,4-THIATRIAZOL-5-THIOLATE ION
o Anal. Chim. Acta 1977, 92 C2), 393-397
D. W. Franco and P. F. Romanelli
o A spectrophotometric method for the determination of carbon
disulfide in water is based on the quantitative formation of
the l,2,3,4-thiatriazol-5-thiolate ion from carbon disulfide
and azide ion. Absorbance is measured at 313 nm. Adjustments
in procedure are described for analysis in the presence of
cupric ion, other cations, sulfide, sulfite, nitrate, and
nitrite.
o Limits: the system obeys Beer's Law for 2.3-8,6 vg carbon
disulfide/ml.
METHOD B - Wet Chemical and Potentiometry or Atomic Absorption
Spectrophotometry
o DETERMINATION OF CARBON DISULFIDE IN' INDUSTRIAL ATMOSPHERES
BY AN EXTRACTION-ATOMIC ABSORPTION NETHOD
o Anal. Chem. 1975, 47(6), 942-944.
B. M. Kneebone and H. Freiser
Aqueous solutions of carbon disulfide react with pyrrolidine
to yield the dithiocarbamate, which subsequently reacts with
copper (as cupric+sulfate) to form a chelate. The dis-
appearance of Cu is monitored with a solid-state copper
electrode. Alternatively, the chelate can be extracted into
isoamyl acetate and determined by atonic absorption
Spectrophotometry.
o • Limits: 7.0 yg CS_ per sample
METHOD C - Wet Chemical and Gas Chromatography
o DETECTION OF CARBON DISULPHIDE (A DISULFIRAM METABOLITE) IN
EXPIRED AIR BY GAS CHROMATOGRAPHY
o J. Chromatogr. 1974, 92(2), 442-444.
J. Wells and E. Koves
Carbon disulfide is determined by gas chromatography after
conversion to diethyldithiocarbamic acid. Expired air is
bubbled into diethylaraine in acetone and methyl chloride
is added. After work-up, the residue is dissolved in
n_-butyl chloride and analyzed by gas chromatography (with
flame ionization detection) on a column of 1.5% FFAP on
80/100 mesh Varoport 30.
o Limits: sub-microgram quantities can be determined
- 24 -
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CHLORPYRIFOS
o Dursban
METHOD A - Capillary Gas Chromatography
o ANALYSIS OF ORGANOPHOSPHORUS PESTICIDES BY CAPILLARY GAS
CHROMATOGRAPHY WITH FLAME PHOTOMETRIC DETECTION
o J. Chromatogr. 1976, 117 (1), 201-205
W. Krijgsman and C. G. Van de Kamp
o Fifty-nine organophosphorus pesticides are analyzed by
capillary gas Chromatography on SE-50 with flame photometric
detection. Relative retention times are given for two
isothermal conditions and for temperature programming.
o Limits: approximately 100 pg
METHOD B - Thin Layer Chromatography and Fluorimetry
o METALLOFLUORESCENT INDICATORS AS SPRAY REAGENTS FOR THE ^N
SITU DETERMINATION OF ORGANOPHOSPHORUS PESTICIDES ON THIN-
LAYER CHROMATOGRAMS
Anal. Chim. Acta 1972, 60 (1), 13-23
o
o
Water samples are extracted with organic solvent and
chromatographed on silica gel N plates and sprayed with
a quenched solution of palladiura(II) - calcein or palladium-
(II) - calcein blue. Organothiophosphorus insecticides are
determined by displacement of palladium from its indicator
complex, producing fluorescent spots on the plate.
o Limits: malathion, 10-50 ngj ethion, 10 ngj guthion, 10-20 ng;
di-syston, 10 ng; chlorpyrifos, 50-100 ng
Cross References - See dichlone, method A; raexacarbate, A; trichlorfon. B.
- 25 -
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COUMAPHOS
o Co-Ral
METHOD A - Thin Layer Chromatography
o DETECTION OF ORGANOPHOSPHORUS AND CARBAMATE PESTICIDES IN
ADIPOSE TISSUE BY THIN-LAYER AND GAS-LIQUID CHROMATOGRAPHY
o N. Z. J. Sci. 1977, 20 C2), 221,224
M. H. Clear, F, R. Fowler, S, R. B. Solly, and A. R. Ritchie
o Cholinesterase - inhibiting pesticides are extracted from
adipose tissue, filtered at low temperature, and identified
by thin-layer chromatography, treatment with bromine vapor,
and visualization via cholinesterase spray solution.
Confirmation is made by gas-liquid chromatography.
o Limits: 0.001-0.1 mg/kg adipose tissue
Cross References - See captan, method C; chlorpyrifos, A; dichlone, A.
- 26 -
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CRESOL
o cresylic acid, hydroxytoluene
METHOD A - Wet Chemical and Gas Chromatography
o DETERMINATION OF TRACE PHENOLS IN WATER BY GAS CHROMATOGRAPHIC
ANALYSIS OF HEPTAFLUOROBUTYRYL DERIVATIVES
o J. Chromatogr. 1978, 156(1), 143-151
L. L. Lamparski and T. J. Nestrick
o Phenol and substituted phenols are derivatized with hepta-
fluorobutyryliraidazole and determined by gas chromatography
on a nitro-DEGS column. The derivatives are amenable to
detection by electron capture. Sample preparation consists
of benzene extraction of the aqueous medium and subsequent
drying of the organic layer.
o Limits: resorcinol and £-cresol are determined at
concentrations ilOng/ml.
METHOD B - Wet Chemical and Gas Chroiaatography
o TRACE ANALYSIS OF PHENOLS IN WATER BY GAS CHROMATOGRAPHY
o J. Fish. Res. Board Can. 1975, 32(2), 292-294
D. A. J. Murray
o With <5-xylene as internal standard, aqueous samples of
phenols, cresols, and xylenols are extracted with
chloroform, concentrated, and reacted with Tri-Sil concen-
trate to form their trimethylsilyl derivatives. Gas
chromatographic analysis is performed with flame
lonization detection on a column of 5% Imol on Chromosorb W,
acid washed. Calibration is linear in the 0-10 mg/1 range.
o Limits: cresols, 0.025 mg/1; xylenols, 0.050; phenol, 0.100.
METHODC - Gas Chromatography
o THE DIRECT-INJECTION GLC ANALYSIS OF XYLENOLS IN INDUSTRIAL
WASTEWATERS
o Bull. Environ. Contam. Toxicol. 1977, 17(6), 764-767.
R. B. Baird, L. G. Carmona, and R. L. Jenkins
o A direct aqueous injection method is developed for the gas
chromatographic analysis of phenol, cresols,and xylenols in
petroleum waste discharges. A column of 4% dinonylphthalatc
on 80/100 mesh Chromosorb G is used with flame ionization
detection. £-Cresol is resolved from the mixture; m- and
p_-cresol appear as one peak.
o Limits: samples in the mg/1 range.
Cross References - See benzonitrile, method A; resorcinol, C.
- 27 -
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CYANOGEN CHLORIDE
METHOD A- Wet Chemical and Visible Spectrophotometry
o
o
THE DETERMINATION OF CYANOGEN CHLORIDE
Analyst (London) 1972, 97(1158), 691-695
P. L. Bailey and E. Bishop
Hydrochloric acid solutions of 1,4-diaminobenzene and
pyridine react with cyanogen chloride to yield a solution
which absorbs radiation at 515 nm. Interference from
oxidizing chlorine species can be avoided by treatment
of the contaminated cyanogen chloride solution with a
mixture of hydrochloric acid, arsenic(III) oxide, and
potassium bromide. Sulfur dioxide interference is removed
by addition of barium nitrate to the colorimetric reagent.
Limits: cyanogen chloride solutions in the range 10~ to
5x10 M
METHOD B - Wet Chemical and Gas Chromatography
o SENSITIVE GAS CHROMATOGRAPHIC DETERMINATION OF CYANIDE
o Anal. Chem. 1974, 46(7), 924-925
J. C. Valentour, V. Aggarwal, and I. Sunshine
o Cyanide is converted to cyanogen chloride by reaction with
chloramine-T and analyzed by gas chromatography on a column
of 7% Halcomid M-18 on Anakrom ABS. Response is linear up
to 100 ug/ml, and the following ions cause no interference
at 100 ug/ml: chloride, fluoride, bromide, iodide, and
acetate.
o Limits: 0.025 vg cyanide/ml
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2.4-D ACID
o 2,4-dichlorophenoxyacetic acid
METHOD A - Wet Chemical and Gas Chromatography
SIMPLE PROCEDURES FOR THE SIMULTANEOUS GAS CHROMA-
'ALYS?S OF FOUR CHLOROPHENOXY HERBICIDES IN
WATER AND SOIL SAMPLES
o J Agric Food Chem. 1978, 26 (3), 640-643
B. A. Olson, T. C. Sneath, and N. C. Jain
o Water and soil samples containing 2,4-D, 2,4-DP, 2,4,5-T,
and 2,4,5-TP are acidified, extracted into organic solvent,
methylated with BF.-methanol, and analyzed by gas chroma-
tography with electron capture detector. Excellent separation
of 5 compounds was obtained with the following columns:
(1) 3% OV-17 on Gas-Chrom Q (80/100 mesh), (2) 3% Versamide -
900 on Supelcoport (80/100 mesh), (3) 15% QF-1/10% DC-200 on
Chromosorb W (80/100 mesh).
o Limits: 0.001 ppm minimum quantitation level
METHOD B- Wet Chemical and Gas Chromatography
o GAS-LIQUID CHROMATOGRAPHIC METHOD WITH ELECTRON-CAPTURE
DETECTION FOR THE DETERMINATION OF RESIDUES OF SOME
PHENOXYACETIC ACID HERBICIDES IN WATER AS THEIR 2,2,2-
TRICHLOROETHYL ESTERS
oo J. Chromatogr. 1977, 136 (1), 105-111
S. Mierzwa and S. Witek
o o 2,4-D is determined by gas Chromatography after sorption
of an aqueous sample on Amberlite XAD-4, elution with
benzene, and esterification with 20% 2,2,2-trichloroethanol
in trifluoroacetic anhydride/sulfuric acid. Electron capture
detection is used with a column of 10% DC-200 and 15% QF-1
on 80-100 mesh Gas-Chrom Q.
o o Limits: 0.096 ppb 2,4-D in a 1- liter sample
METHOD C - Thin Layer Chromatography and Densitometry
o DETERMINATION OF CHLOROPHENOXY ACID HERBICIDES BY DENSITOMETRY
ON THIN LAYER CHROMATOGRAMS
o o Anal. Chim. Acta 1977, 91 (2), 259-266
J. Shenna and J. Koropchack
o Chlorophenoxy acid herbicides and their salts are extracted
from water with benzene, dried, and spotted on silica gel G
plates that have been impregnated with a silver nitrate
detection reagent solution. After ultraviolet irradiation,
the spots are scanned by a fiber optics densitometer. Linear
calibration curve is obtained in the 100-1000 ng range.
o Limits: 1 ppb
Cross References - See captan, method A; 2,4-D ester, B; dicamba, A, B,
and C; dichlone, A; 2,2-dichloropropionic acid, B; 2,4,5-T
acid, A; 2,4,5-T ester, A; trichlorfon, B.
- 29 -
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2.4-D ESTER
o 2,4-dichlorophenoxyacetic ester
METHOD A - Wet Chemical and Gas Chromatography
o DETERMINATION OF INDIVIDUAL ESTERS OF 2,4-D and 2,4,5-T IN
COMMERCIAL CROPS
o Pestic. Sci. 1977, 8 (2), 157-162
H. E. Munro
o Individual esters of 2,4-D and 2,4,5-T are determined in
purified crop samples by gas Chromatography on a column
of 9% XE60 or 2.5% NPGS on silanized Embacel. The samples
are macerated, steam distilled into a hexane trap, extracted,
and cleaned on a Florisil column. The following mixtures
are separated: 2,4-D-butyl and 2,4,5-T-butyl esters; 2,4-D-
ethyl, 2,4,5-T-butyl, and 2,4,5-T-isobutyl esters.
o Sample size: lug each ester in 100 g plant material
NETHOD B - Wet Chemical and High Pressure Liquid Chromatography
o ISOMER-SPECIFIC ASSAY OF ESTER AND SALT FORMULATIONS OF
2,4-DICHLOROPHENOXYACETIC ACID BY AUTOMATED HIGH PRESSURE
LIQUID CHROMATOGRAPHY
o J. Assoc. Off. Anal. Chem.^ 1977, 60 (4), 868-872
N. E. Skelly, T. S. Stevens, and D. A. Mapes
o 2,4-D is assayed in ester or salt formulations by in situ
saponification (KOH/2-propanol/water), followed by separation
by high pressure liquid Chromatography on Partisil ODS,
10-25 pm. Results are reported as % 2,4-D acid equivalent.
Tne method separates 2,4-D from known impurities and is
applicable to 2,4-D esters of the following alcohols:
methanol, 2-butoxyethanol, l-butoxy-2-propanol, isooctanol,
isobutyl alcohol, and n_ - butyl alcohol.
o Standard solution: 300 mg/25 ml
Cross References - See 2,4-D acid, method C; dichlone. A; dichlorvos, B;
mevinphos, B; 2,4,5-T ester, A.
- 30 -
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DIAZINON
o Dipofene, Diazitol, Basudin, Spectracide
.METHOD A - Reaction Gas Chromatography
O REACTION GAS CHROMATOGRAPHIC ANALYSIS OF PESTICIDES. II.
ON-COLUMN TRANSESTERIFICATION OF ORGANOPHOSPHATES BY METHANOL
o J. Agr. Food Chem. 1973, 21 (4), 621-625
H. A. Moye
o Parathion and diazinon undergo on-column transesterification
with methanol on a gas chromatographic column of 80/100
Porapak P or Q in which the first 6" is packed with sodium
hydroxide-treated glass beads. Alkali flame ionization
detection is used. Peaks were also obtained for transesteri-
fication with ethanol, 1-propanol, and 1-butanol. The
organophosphates are separated from a representative carbamate.
o Limits: 1.0 ng
METHOD B- Gas Chromatography
O A MULTICLASS, MULTIRESIDUE ANALYTICAL METHOD FOR DETERMINING
PESTICIDE RESIDUES IN AIR
o Arch. Environ. Contara. Toxicol. 1975, 3 (1), 55-71
J. Sherma and T. M. Shafik
o Airborne pesticide residues are trapped by ethylene glycol,
extracted by methylene chloride, and fractionated on silica
gel. The fraction containing phosphate compounds is
analyzed by gas Chromatography with flame photometric
detection on 5% OV-210 on Supelcoport, 80-100 mesh. Diazinon
is well separated from malathion.
o Limits: 80 pg diazinon detected by gas Chromatography;
40 pg, csrbaryl; 460 pg, ethion; 400 pg, malathion; 320 pg,
methyl parathion; 80 pg, mexacarbate; 40 pg, parathion
Cross References - See chlorpyrifos, method A; coumaphos, A; dichlone, A;
dichlorvos, B; guthion, A and B; mevinphos, B; trichlorfon, B.
- 31 -
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DICAMBA
o 2-methoxy-3,6-dichlorobenzoic acid
METHOD A - Wet Chemical and Gas Chromatography
o ANALYSIS OF PESTICIDES BY CHEMICAL DERIVATIZATION. III. GAS
CHROMATOGRAPHIC CHARACTERISTICS AND CONDITIONS FOR THE
FORMATION OF PENTAFLUOROBENZYL DERIVATIVES OF TEN HERBICIDAL
ACIDS
o J. Assoc. Offic. Anal. Chem. 1976, 59 (3), 633-636
A. S. Y. Chau and K. Terry
o Herbicidal acids are dissolved in benzene, converted to their
pentafluorobenzyl ester derivatives by pentafluorobenzyl
bromide and potassium carbonate, and analyzed by gas
chromatography with electron capture detection. The best
separation was obtained with a column of 3.6% OV-101 and 5.5%
OV-210 on 80-100 mesh Chromosorb W.
o Limits: 0.8 pg
METHOD B - Wet Chemical and Thin-Layer Chromatography
o DETERMINATION OF SOME ACIDIC HERBICIDES BY THIN-LAYER
CHROMATOGRAPHY
o J. Agric. Food Chem. 1971, 19 (6), 1181-1182
A. Guardigli, W. Chow, and M. S. Lefar
o Six acid herbicides are extracted from tissue, cleaned by
alkaline hydrolysis and extraction, converted to the nitro
derivatives by sodium nitrate in concentrated orthophosphoric
acid, and spotted on thin-layer chromatographic plates
(precoated Merck silica gel F-254). Visualization is
effected by spraying successively with a reducing agent
(stannous chloride), a diazotizing agent, and the Bratton-
Marshall reagent (N-(l-naphthyl)-ethylenediamine dihydrochlonde)
o Limits: O.Sug (approximately 0.05 ppm in a crop residue)
METHOD c - Wet Chemical and Gas Chromatography
b ANALYSIS OF PESTICIDES BY CHEMICAL DERIVATIZATION. I. A
NEW PROCEDURE FOR THE FORMATION OF 2-CHLOROETHYL ESTERS
OF TEN HERBICIDAL ACIDS.
o J. Assoc. Offic. Anal. Chem. 1975, 58 (6), 1294-1301
A. S. Y. Chau and K. Terry
o Ten herbicidal acids are purified by extraction and crystal-
lization and subsequently converted to their 2-chloroethyl
ester derivatives via dicyclohexyl carbodiimide and
2-chloroethanol. Gas chromatography with electron capture
detection on one or more of the follwoing three columns
allowed separation of the ten acids: 3.6% OV-101 and 5.5%
OV-210 on 80-100 mesh Chromosorb W; 3% OV-225 on 80-100 mesh
Chromosorb Q; 11% OV-17 and QF-1 on 80-100 mesh Chromosorb Q.
o Sample size required: 50-500 vg
Cror.s References - See 2,2-»dichloropropionic acid, method B; 2,4,5-T
acid, A.
- 32 -
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DICHLOBENIL
o 2,6-dichlorobenzonitrile, 2,6-DBN
METHOD A - Gas Chromatography
o A MULTI-RESIDUE EXTRACTION PROCEDURE FOR THE GAS CHROMATOGRAPHIC
DETERMINATION OF THE HERBICIDES DICHLOBENIL, DINITRAMINE,
TRIALLATE AND TRIFLURALIN IN SOILS
o J. Chromatogr. 1974, 97 (1), 103-106
A. E. Smith
o Four persistent herbicides are extracted from soil and
analyzed by gas chromatography on 10% OV-1 on Chromosorb
G-HP, 80-100 mesh. Electron capture detection is used.
o Limits: 0.05 ppm in soil
METHOD B - Wet Chemical and Gas Chromatography
0 CONFIRMATION OF SOME ORGANONITROGEN HERBICIDES AND FUNGICIDES
BY CHEMICAL DERIVATIZATION AND GAS CHROMATOGRAPHY
o J. Agric. Food Chem. 1976, 24 (6), 1236-1238
J. F. Lawrence
o Several pesticides are extracted from corn and subjected to
Florisil column cleanup. The fraction containing dichlobenil
is methoxylated (methanolic sodium methoxide) and analyzed
by gas chromatography on 4% SE-30/6% SP-2401 on Chromosorb
W/HP. 80-100 mesh.
o Limits: 0.1 ppm
METHODC - Bioassay
o BIOASSAYS FOR THE DETECTION OF HERBICIDES AND ALGICIDES IN
WATER
o Meded. Fac. Landbouwwet, Rijksuniv. Gent 1977 42 (2 Pt 21
1625-1634 ' }'
R. A. J. Bulcke and J. M. T. Stryckers
o Dichlobenil inhibits root growth of garden cress seeds (Lepidium
sativum L.)- The seeds are placed on filter paper soaked with
herbicide solution,and root length is measured after 48 hours.
EDgQ value is reported.
o Limits: qualitative detection in the range 0.02-0.14 ppm
Cross References - See 2,2-dichloropropionic acid, method B.
- 33 -
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PICHLONE
o Phygon, dichloronaphthoquinone
METHOD A - Gas Chroraatography
o RELATIVE RETENTION RATIOS OF NINETY-FIVE PESTICIDES AND
METABOLITES ON NINE GAS-LIQUID CHROMATOGRAPHIC COLUMNS
OVER A TEMPERATURE RANGE OF 170 TO 204°C IN TWO DETECTION
MODES
o J. Assoc. Offic. Anal. Chera, 1975, 58 (5), 1037-1055
J. F. Thompson, J. B. Mann, A. 0. Apodaca, and E. J. Kantor
o Tables of relative retention data are given for 95 organo-
chlorine and organophosphorus pesticides at temperatures
from 170 to 204 C, in two-degree increments. Nine columns
and two modes of detection (electron capture and flame
photometric) were used. Two chromatograms are generally
sufficient for tentative identification in multiresidue
samples.
METHOD B - Column, Thin-Layer, and Gas Chromatography
o SEPARATION AND IDENTIFICATION OF 20 PESTICIDES IN THEIR
MIXTURE
o Agr. Biol. Chem. 1973, 37 (8), 1959-1962
K. Suzuki, K. Miyashita, H. Nagayoshi, and T. Kashiwa
o Dichlone, diuron, and 18 other pesticides undergo
preliminary separation into 5 groups via column chroma-
tography on silica gel. Each group is developed by two-
dimensional thin-layer chromatography. Individual
components are identified by ultraviolet spectroscopy and
by gas chromatography on a column of 5% QF-1 on 80-100 mesh
Gaschrom Q.
o Limits: approximately 1 mg
METHODC- Thin-Layer Chromatography
o ELECTRON-DONOR-ACCEPTOR COMPLEXING REAGENTS IN THE ANALYSIS
OF PESTICIDES. VI
o Mikrochim. Acta 1973, f5), 641-650
J. D. MacNeil, R. W. Frei, and 0. Hutzinger
0 Dichlone is detected following thin-layer chromatography by
spraying the chromatogram with a reagent that forms a
TT -complex with the pesticide. Colors are produced with
both donors and acceptors. Mass spectrometry is used for
confirmation.
o Saj?ple size: 5 u g
- 34 -
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2;2-DICHLOROPROPION'IC ACID
o Dalapon
METHOD A . Wet Chemical and Gas Chromatography
o DETERMINATION OF RESIDUES OF DALAPON IN SOIL BY GAS
CHROMATOGRAPHY OF THE 1-BUTYL ESTER
o J. Chromatogr. 1975, 106 (2), 409-411
E. G. Cotterill
o Dalapon is extracted from soil (using methanelie sodium
hydroxide) and converted to its ii-butyl ester via 1-butanol
and sulfuric acid. The ester is analyzed with electron
capture detection on a column of 2% OV-17 on Chromosorb
WHP, 80-100 mesh.
o Limits: 0.05 ppm
METHOD B - Bioassay
o THE USE OF THREE SIMPLE, RAPID BIOASSAYS ON FORTY-TWO
HERBICIDES
o Weed Res. 1971, 11(4), 257-262
B. A. Kratky and G. F. Warren
o The following three bioassays were tested as primary
screening methods on 42 herbicides: chlorella bioassay;
root bioassay with sorghum, oat and cucumber; and shoot
bioassay with sorghum and oat. A positive test is one in
which inhibition is 50% or greater.
o Limits: dalapon, 30 ppm in soil; aicamba, dichlobenil,
and 2,4-D, 1 ppm.
METHODC - Gas Chromatography
0 METHODS OF RESIDUE DETERMINATION AT THE BRITISH SUGAR
CORPORATION RESEARCH LABORATORIES
o IIRB (Inst. Int. Rech. Betteravieres) 1973, 6(3), 138-153
R. Parslow
o A sample of sugar beets is macerated with water, ortho-
phosphoric acid, and phosphotungstic acid, extracted with
diethyl ether, and analyzed by gas Chromatography with
electron capture detection. Column composition is 5%
diethylene glycol adipate and 1% orthophosphoric acid on
60/85 mesh celite. Dalapon is confirmed by thin-layer
Chromatography on 60% Kieselghur G/40% Kieselgel G.
o Limits: 0.1 ppm by gas Chromatography
- 35 -
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DICHLORVOS
o 2,2-dichlorovinyl dimethyl phosphate, Vapona
NETHOD A - Thin Layer Chromatography
0 DETECTION AND DETERMINATION OF DICHLOROVOS (DDVP) IN
TOXICOLOGICAL ANALYSIS
o Fresenius1 Z. Anal. Chem. 1977, 285 (1), 48
S. N. Tewari and S. P. Harpalani
o A biological sample is homogenized, extracted and spotted
on -a silica gel plate which is developed and sprayed with
ethanolic thymol blue. The appearance of a violet color
against a blue background (Rf 0.36] indicates dichlorvos.
o Limits: D.2yg
METHOD B - Gel Permeation Chromatography and Gas Chromatography
o AUTOMATED GEL PERMEATION CHROMATOGRAPHY CLEANUP OF ANIMAL
AND PLANT EXTRACTS FOR PESTICIDE RESIDUE DETERMINATION
o J. Assoc. Offic. Anal. Chem. 1976, 59 (1), 174-187
1. D. Johnson, R. H. Waltz, J. P. Ussary, and F. E. Kaiser
o Pesticide residues in fats and oils are separated by gel
permeation Chromatography on Bio-Beads SX-3. Toluene and
ethyl acetate are used to elute sixteen nonionic chlorinated
pesticides, three polychlorinated biphenyls, fourteen
chlorophenoxy herbicide esters, and seven organophosphate
insecticides. For gas Chromatography on the pesticides, a
column of 1.5% OV-17/2.0% OV-210 on Gas-Chrom Q (100-120
mesh) is used.
o Sample Size: 0.5 g lipid
Cross References •* See chlorpyrifos, method A, diclilone, A; trichlorfon, A
and C.
- 36 -
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DIETHYLAMINE
METHOD A - Wet Chemical and Gas Chromatography
o GAS CHROMATOGRAPHIC SEPARATION OF LOWER ALIPHATIC AMINES
o Anal. Chem. 1976, 48 (12), 1716-1717
Y. Hoshika
o Thirteen aliphatic amines are analyzed by gas chroraatography
(with thermal conductivity detector) on a TENAX-GC column,
60/80 mesh. Primary amines are converted to Schiff bases by
reaction with benzaldehyde; secondary and tertiary amines
are analyzed in the form of their free amines.
o Sample size: approximately 10~ mole
METHOD B - Wet Chemical, Gas Chromatography, and Mass Spectrometry
0 THE SEPARATION AND IDENTIFICATION OF SOME ISOMERIC ALKYLAMINES
AS THEIR TRIFLUOROACETYL DERIVATIVES
o J. Chromatogr. 1973, 82 (2), 373-376
B. Crathome and M. J. Saxby
o Trifluoroacetyl derivatives of 7 C. and 10 C_ amines are
prepared and analyzed by gas Chromatography on a DECS
column with flame ionization detection. Diethylamine and
_t-butylamine have identical retention times but are
distinguishable by mass spectrometry. 11-Butylamine appears
as a separate peak,
METHOD C - Wet Chemical, Thin-Layer Chromatography, and Fluorescence
Spectroscopy
o FLUOROMETRIC DETERMINATION OF PRIMARY AND SECONDARY ALIPHATIC
AMINES BY REACTION WITH 9-ISOTHIOCYANATOACRIDINE
o J. Pharm. Sci. 1973, 62 (8), 1370-1371
A. DeLeenheer, J. E. Sinsheimer, and J. H. Burckhalter
o Primary and secondary aliphatic amines are determined by
fluorescence spectroscopy of cyclic derivatives formed by
reaction with 9-isothiocyanatoacridine. Wavelength for
activation is 300 nm and for detection is 520 nm'.
Fluorescence is measured either directly on the reaction "
mixture or after thin-layer chromatographic separation on
silica gel G.
o Limits: 0.2-0.5 nl/ml
Cross References - See aniline, method C.
- 37 -
-------
DINITROBENZENE
dinitrobenzol
METHOD A - Liquid Chromatography
o RETENTION BEHAVIOR OF DINITROBENZENE ISOMERS AND
DIHYDROXYBENZENE ISOMERS ON OCTADECYL AND PHENYL BONDED
PHASE PACKINGS
o J. Chromatogr. Sci. 1978, 16 (9), 438-442
P. K. Tseng and L. B. Rogers
o Dinitrobenzene isomers are separated by liquid chromatography
on Lichrosorb C-g, Bondapak C.g-Porasil B, or Bondapak
phenyl/Porasil B with detection at 254 nm. Various methanol/
water mixtures are used as eluent.
o Sample size: 30-80 yl
METHOD B - Gas Chromatography
o DETERMINATION OF TRACES OF ORGANIC COMPOUNDS IN THE ATMOSPHERE:
ROLE OF DETECTORS IN GAS CHROMATOGRAPHY
o Anal. Chira. Acta 1978, 100, 45-52
J. Mitchell, Jr. and H. D. Deveraux
o Gas chromatographic retention times and relative sensitivity
data for various detectors are reported for 34 organic
compounds. The column employed is 2% Carbowax 20M on 80/100
mesh GasChrom RA.
o Limits: nanogram range
METHOD C- Wet Chemical and Potentiometric Titration
o MICRODETERMINATION OF m-DINITRO COMPOUNDS WITH CYANIDE AND
SILVER ELECTRODES
o Anal. Chem. 1977, 49(1), 45-48.
S. S. M. Hassan
o m-Dinitro compounds react selectively and quantitatively
with 0.2M potassium cyanide. Excess cyanide is titrated
potentiometrically with 0.02M silver nitrate using a
cyanide or silver/sulfide ion-selective electrode. No
interference occurs from other classes of nitrogenous
compounds.
o Sample size: 2-10 mg
Cross References - See benzonitrile, method A.
- 38 -
-------
o Aquacide, Dextrone, Reglone, Diquat dibromide
METHOD A - Wet Chemical and Gas Chromatography
o THE GAS CHROMATOGRAPHIC DETERMINATION OF PARAQUAT IN WATER
o Bull. Environ. Contain. Toxicol. 1972, 8 (6), 363-368
C. J. Soderquist and D. G. Crosby
o Samples obtained from water are catalytically hydrogenated
by sulfuric acid and PtO_ in methanol, extracted into an
organic solvent, and analyzed by flame-ionization gas
chromatography on a column of 10% Triton X-100 plus 1% KOH
on 70/80 AW, DMCS treated Chromosorb G. Diquat and paraquat
can be analyzed simultaneously.
o Limits: <0.1 ppm
f-ETHOD B - Pyrolysis and Gas Chromatography
o A RAPID METHOD FOR THE SIMULTANEOUS DETERMINATION OF PARAQUAT
AND DIQUAT IN POND AND RIVER WATERS BY PYROLYSIS AND GAS
CHROMATOGRAPHY
o Analyst 1975, 100 (1197), 848-853
A. J. Cannard and W. J. Criddle
o Aqueous samples containing paraquat and diquat are pyrolyzed
under carefully controlled conditions in a silica tube
inserted into a Chemical Data Systems Pyroprobe 190. The
pyrolysate is analyzed by gas chromatography on a column of
10% Carbowax 20M plus 2% KOH on Celite (80-100 mesh).
Paraquat does not interfere with the diquat determination
o Limits: 0.01 ppm
METHOD C - Wet Chemical and Gas Chromatography
o
o
DETERMINATION OF DIQUAT AND PARAQUAT RESIDUES IN SOIL BY GAS
CHROMATOGRAPHY
J. Agr. Food Chem. 1974, 22 (5), 865-867
S. U. Khan
Paraquat and diquat residues are extracted from soil, hydro-
genated catalytically over PtO,, and analyzed by gas chroma-
tography with flame ionization or alkali flame ionization
detection. Of several columns that were explored, the best
separation of the two compounds was obtained with 3% Carbowa.x
20M plus 1% KOH on 80-100 mesh Chromosorb WHP.
Limits: 0.01 ppm
- 39 -
-------
DISULFOTON
o Dl-syston
MEJHODA- Wet Chemical, Gas Chromatography, Infrared Spectrophotometry
o ANALYTICAL STUDIES OF DI-SYSTON FORMULATIONS
o J. Assoc. Offic. Anal. Chem. 1972, 55 (5), 918-922
J. C. Cavagnol
o Several analytical methods for determining disulfoton are
presented, including the following: (1) extraction, hydrolysis,
and back titration; (2) infrared Spectrophotometry at 610-750
cm " ; (3) gas Chromatography; (4) extraction and gravimetry;
(5) colorimetry based on phosphorus.
o Limits: none quoted
METHOD B - Wet Chemical and Visible Spectrophotometry
o SEMIAUTOMATED ANALYSIS OF GRANULAR ORGANOPHOSPHORUS PESTICIDE
FORMULATIONS
o J. Agr. Food Chem. 1972, 20 (5), 959-963
T. D. Talbott, J. C. Cavagnol, C. F. Smead, and R. T. Evans
o Granular formulations of disulfoton are extracted with an
acetic acid-bromine mixture and automatically analyzed
colorimetrically for phosphorus via its molybdenum blue
complex. Absorbance is measured at 829 nra.
o Sample size: 1.65 g of 15% granules
Cross References - See captan, method A; chlorpyrifos, A and B; dichlonc, A;
dichlorvos, B; guthion, A and B; parathior., A.
- 40 -
-------
DIURON
o DCMU, DMU
METHOD A - Wet Chemical and Gas Chromatography
o ANALYSIS OF SONE CARBAMATE AND UREA HERBICIDES IN FOODS BY
GAS-LIQUID CHROMATOGRAPHY AFTER ALKYLATION
o J. Agric. Food Chem. 1975, 23 (6), 1106-1109
J. F. Lawrence and G. W. Laver
o Carbamate and urea herbicides are extracted from crops with
ethanol, partitioned between water and chloroform, alkylated
with sodium hydride/methyl iodide, extracted with hexane,
and analyzed by gas chromatography with a Coulson electrolytic
conductivity detector in the nitrogen mode. Column composition
is 4% SE-30/6% QF-1 on Chromosorb WHP (80-100 mesh.)
o Limits: approximately 0.005 ppm
METHOD B - Wet Chemical and Visible Spectrophotometry
o COLORIMETRIC DETERMINATION OF PHENYLAMIDE PESTICIDES IN
NATURAL WATERS
0 J, Assoc, Offic, Anal. Chem. 1972, 55 Q6), 1276-1279
M. A, El-Dib and 0. A. Aly
o A simple rapid colorimetric procedure is given for phenylamide
pesticides obtained from natural waters. The sample is hydro-
lyzed by sulfuric acid to produce corresponding anilines, which
are extracted with chloroform, diazotized, and coupled with
1-naphthol to yield azo.dyes. Absorbance at wavelengths of
maximum absorption are measured on a visible spectrophotometer
and compared with standards. Phenylamides may be analyzed in
the presence of anilines.
o Limits: 0.02 mg/1.
METHOD C - Wet Chemical and Gas Chromatography
o A CHEMICAL CONFIRMATORY TEST FOR ORGANOPHOSPHORUS AND CARBAMATE
INSECTICIDES AND TRIAZINE AND UREA HERBICIDES WITH REACTIVE NH
MOIETIES
o J. Agric. Food Chem. 1975, 23 (2), 325-329
R. Greenhalgh and J. Kovacicova
o Alkylation (sodium hydride/methyl iodide/dimethyl sulfoxide)
followed by gas chromatography is used to confirm organophos-
phorus and carbamate insecticides and urea and triazine herbi-
cides with NH or NH- moieties. An alkali flame ionization
detector is used with a column of 100-120 Gas-Chrom Q coated
with 4% SE-30/6% QF-1. The alkylated derivatives are thermally
stable.
o Residues in crude plant and soil extracts can be confirmed at
the sub part-per-million level.
Cross References - See dichlone, method B.
- 41 -
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DODECYLBENZENESULFONIC ACID
o laurylbenzenesulfonic acid
hETHOD A - Potentiometry
o ION SELECTIVE ELECTRODES RESPONSIVE TO ANIONIC DETERGENTS
o Anal. Chen. 1974, 46(12), 1842-1844
T. Fujinaga, S. Okazaki, and H, Freiser
o Ion-selective electrodes responsive to anionic detergents
are prepared by dipping a platinum wire into an appropriate
coating mixture. For laurylbenzenesulfonate response, the
coating consists of a 3:1 mixture of 10% polyvinyl chloride
in cyclohexanone and a decanol solution of the quaternary
ammonium salt formed by reaction of methyltricaprylammonium
chloride and sodium laurylbenzenesulfonate. The electrode
also responds to the lauryl sulfate and lauryl sulfonate ions,
o Limits: calibration of the potential-response curve is
linear in the concentration range 10" - 10 M.
- 42 -
-------
Nialate, ethyl raethylene phosphorodithioate
METHOD A - Liquid-Liquid Extraction
o GUIDELINES FOR QUANTITATIVE LIQUID-LIQUID EXTRACTION OF
ORGANOPHOSPHATE PESTICIDES FROM WATER
o ASTM Spec. Tech. Publ. 573 (Water Qual. Parameters, Symp.,
1973), pp. 167-182 (1975)
I. H. Suffet, C. Wu, and D. T. L. Wong
o An approach is developed for the quantitative analysis of
aqueous samples of organophosphate pesticides, including
ethion and parathion. Residue analysis includes liquid-
liquid extraction, water and solvent phase separation,
drying, and evaporation. The liquid-liquid extraction step
is optimized. The £ - values determined for pure water
are applicable to natural waters.
o Recovery studies were conducted at the ng/1 level.
Cross References - See chlorpyrifos, methods A and B; diazinon, B;
dichlone, A; dichlorvos, B; guthion, A; mevinphos, B;
trichlorfon, B.
- 43 -
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ETHYLENEDIAMINE
o 1,2-diarainoethane
METHOD \ - Wet Chemical and High-Perfornance Liquid Chromatography
o HIGH-PERFORMANCE LIQUID CHROMATOGRAPHIC SEPARATION AND
QUANTITATION OF POLYFUNCTIONAL AMINES AS THEIR m-TOLUOYL
DERIVATIVES
o J. Chromatogr. 1978, 154 (2), 219-225
S. L. Wellons and M. A. Carey
0 Polyfunctional aliphatic amines are determined at low
levels in water, ammonia, and other amines by high-
performance liquid Chromatography of derivatives measurable
vvith available ultraviolet detectors. Derivatization is
accomplished with m-toluoyl chloride in pyridine. After
extraction with methylene chloride, the amine derivatives
are chromatographed on u-Bondapak C.g.
o Sample size.: 7 mg ethylene diamine before derivatization
METHOD B - Wet Chemical and High-Pressure Liquid Chromatography
o DETERMINATION OF DIAMINES AND POLYAMINES IN TISSUES BY
HIGH-PRESSURE LIQUID CHROMATOGRAPHY
o J. Chromatogr. 1976, 124 (2), 277-285
N. E. Newton, K. Ohno, and M. M. Abdel-Monem
o The dansyl (5-dimethylaminonaphthalene-l-sulfonyl)
derivatives of five diamines obtained from tissue extracts
are prepared and analyzed by high-pressure liquid chroma-
tography on a column of Micropak CN-10. Fluorescence
detection is used. Ethylene diaraine is the internal
standard.
o Sainple size: 0.004 mmoles ethylene diamine
\ETHOD C - Wet Chemical and Visible Spectrophotometry
o SPECTROPHOTOMETRIC DETERMINATION OF MICROGRAM AMOUNTS OF
AMINES WITH CHLORANIL
o Anal. Chim. Acta 1976, 85(1), 189-194
T. S. Al-Ghabsha, S. A. Rahim, and A. Townshend
o Amines and chloranil react at 60-65 C in a pH 9 borate
buffer to yield colored products. Wavelengths for
absorbance measurements of the complexes are given.
o Limits: ethylene diamine, 2 ppm; £-butylamine, 2.5 ppm;
aniline, 10 ppm.
- 44 -
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FORMIC ACID
o methanoic acid
METHOD A - Wet Chemical and Gas Chromatography
o IMPROVED METHOD FOR ASSAY OF FORMIC ACID BY GAS-LIQUID
CHROMATOGRAPHY
o J. Chromatogr, 1978. 151 (31. 374-378
K. S. Bricknell and S. M. Finegold
o Formic acid obtained in a mixture of end-products produced
by bacterial cultures is methylated with boron trifluoride/
methanol and extracted with chloroform. The ester is
converted to dimethylformamide by treatment with dimethyl-
amine and analyzed by gas Chromatography on a Resoflex
column with thermal conductivity or flame ionization
detector. Methyl esters of short-chain volatile fatty acids
do not interfere, but free acetic acid does interfere with
the analysis for dimethylformamide.
o Limits: 2 pmole/ml for thermal conductivity detector;
0.5 umole/ml for flame ionization detector
METHOD B- Wet Chemical and Gas Chromatography
O DETERMINATION OF ORGANIC ACIDS OF LOW RELATIVE MOLECULAR
MASS (C. to C4) IN DILUTE AQUEOUS SOLUTION
o Analyst (London) 1974, 99(1175), 137-142
P. 0. Bethge and K. Lindstrom
o C.-C. carboxylic acids are determined in low concentrations
(5 x 10" M) in polluted water. Samples undergo ion exchange
to remove metal cations and are then neutralized with tetra-n-
butylammonium hydroxide, evaporated, dissolved in acetone,
and converted to their benzyl esters by treatment with benzyl
bromide. The esters are analyzed by gas-liquid Chromatography,
with flame ionization detection, on a column of 3% butane-1,4-
diol succinate polyester on 120/140 mesh Chromosorb W, acid
washed. ii-Hexanoic acid is used as an internal standard.
o Limits: approximately 5 x 10~ mole sample size
METHOD C- Wet Chemical and Gas Chromatography
o GAS CHROMATOGRAPHIC DETERMINATION OF SMALL AMOUNTS OF
FORMIC ACID IN MIXTURES CONTAINING PHENOL, ACETONE, AND
AROMATIC HYDROCARBONS
o J. Chromatogr. 1978, 148(1).. 219-222
W. Czerwirfski and A. Stepien
o Formic acid is isolated from a mixture of aromatic hydro-
carbons and acetone by extraction as its sodium salt. After
acidification and esterification (methanol/anhydrous
hydrogen chloride), the derivative is analyzed by gas
Chromatography on a column of 10% Carbowax 20M on 60-80 mesh
Chromosorb W. A flame ionization detector is used. For
formic acid concentrations between 0.005 and 0.1%, a linear
calibration curve is obtained.
o Limits: 0.01-0.1% formic acid
- 45 -
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FUMARIC ACID
trans-butenedioic acid, trans-l,2-ethylenedi-carboxylic
acid, boletic acid, allomaleic acid
^ETHOD A - Liquid Chromatography
o
o
0
fETHOD B
o
o
o
t-ETHOD C
o
o
SEPARATION OF THE CITRIC ACID CYCLE ACIDS BY LIQUID
CHROMATOGRAPHY
Anal. Chem., 1978, 50 (11). 1420-1423
V. J. Turkelson and M. Richards
A variety of organic acids are analyzed by liquid
Chromatography on Aminex 50W-X4 cation exchange resin.
The column eluent is monitored by ultraviolet spectro-
photometry at 210 nra. As the column is operated in the
hydrogen form, no regeneration of the resin is necessary.
Limits: <1 ppm fumaric acid
- Column and Thin-Layer Chromatography
SEPARATION OF KREBS CYCLE ACIDS IttTH BEADED DIETHYL-
AMINOETHYL CELLULOSE
J. Assoc. Off. Anal. Chem. 1978, 61 (3), 751-752
B. L. Bruinsma and D. Le Tourneau
Organic acids are separated on a column of beaded diethyl-
aminoethyl cellulose (Sephadex A-25, chloride form) without
pH or solvent gradients. After solvent removal in vacuum,
samples can be titrated for quantitative analysis. Iden-
tification of the acids is made by thin-layer Chromatography
on Brinknian cellulose MN300 and development by spraying
with ribose-aniline reagent. The method has been used to
determine acids produced in a culture medium.
Sample size: 0.5 raeq
- Anion Exchange, Wet Chemical and Gas Chromatography
ANALYSIS OF ORGANIC ACIDS IN FRUIT PRODUCTS BY ANION EXCHANGE
ISOLATION AND GAS CHROMATOGRAPHIC DETERMINATION
J. Assoc. Off. Anal. Chem. 1973, 56(5), 1257-1263
D. W. Baker
Alcoholic extracts of fruit products are passed successively
through a cation exchange resin (Bio-Rad AG 50W-X2) and an
anion exchange resin (Bio-Rad AG 1-X2). Acidic compounds
trapped on the anionic column are eluted with formic acid/
acetone, reacted with bis(trimethylsilyl) acetamide or bis-
(trimethylsilyl)trifluoroacetamide to form trimethylsilyl
ether-ester derivatives which are analyzed by gas Chroma-
tography with flame ionization detection. A column of 4% OV-1
on 100/120 mesh Gas-Chrom Q is used,
Sample size: 1 rag
- 46 -
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FURFURAL
o 2 - furaldehyde, pyromucic aldehyde
METHOD A - Wet Chemical and Gas Chromatography
o SENSITIVE GAS CHROMATOGRAPHIC DETERMINATION OF LOWER
ALIPHATIC CARBONYL COMPOUNDS AS THEIR PENTAFLUOROPHENYL-
HYDRAZONES
o J. Chroraatogr. 1978, 152 (1), 224-227
Y. Hoshika and G. Muto
o Twenty-seven lower aliphatic carbonyl compounds are
derivatized with pentafluorophenylhydrazine and analyzed
by gas chromatography. Columns and detectors employed are:
20% Ethofat 60/25 on Shimalite F (20-80 mesh), flame
ionization; 5% SE-30 on Chromosorb W (60-80 mesh), flame
ionization or electron capture; and glass capillary, PEG
20M, flame ionization.
o Sample size: 0.5 mmole carbonyl compound
METHOD B - Wet Chemical and Fluorescence Spectroscopy
o FLUORIMETRIC DETERMINATION OF AROMATIC ALDEHYDES WITH
2,2'-DITHIOBIS(l-AMINONAPHTHALENE)
o Anal. Chira. Acta 1978, 99 (21. 317-324
Y. Ohkura, K. Ohtsubo, K. Zaitsu, and K. Kohashi
o A fluorimetric method for determining aromatic aldehydes
is based on their reaction with 2,2'-dithiobis(l-aminonaph-
thalene) in the presence of tri-ii-butylphosphine, sodium
sulfite, and sodium phosphite. The method is selective for
aromatic aldehydes; almost all other biologically important
substances examined do not fluoresce at the concentrations
employed. For furfural, excitation occurs at a wavelength
of 380 nm and emission at 475 nm.
o Limits: 10 ng/ml
METHOD C- Wet Chemical and Ultraviolet Spectroscopy
o SPECTROPHOTOMETRIC DETERMINATION OF FURFURAL IN VJg QUANTITIES
USING ITS MOLYBDIC ACID COMPLEX
o Fresenius' Z. Anal. Chem. 1975, 276(4), 300
V.K.S. Shukla and J. P. Sharma
o Furfural forms a colorless complex with molybdic acid. The
complex absorbs at 331 nm and its solutions obey Beer's
Law in the range of 100-700 ug.
o Limits: 100-700 wg
- 47 -
-------
GUTHION
o Gusathion, azinphos-methyl
METHOD A- Gas Chromatography
o MULTIRESIDUE ANALYSIS OF FOURTEEN ORGANOPHOSPHORUS
PESTICIDES IN NATURAL WATERS
o J. Assoc. Off. Anal. Chem. 1974, 57 (5), 1033-1042
B. D. Ripley, R. J. Wilkinson, and A. S. Y. Chau
o Fourteen organophosphorus pesticides are determined in
natural water samples by gas chromatography with flame
photometric detection on a column of 11% OV-17/QF-1 on
80-100 mesh Chromosorb Q. Two extraction methods and two
concentration methods are described.
o Limits (sample size, 1A): disulfoton, 0.005 ppb; guthion,
0.10 ppb; diazinon, methyl parathion, malathion, parathion,
and ethion, 0.010 ppb.
METHOD B- Gas Chromatography
o METHOD FOR ORGANOPHOSPHORUS PESTICIDES IN WATER AND
WASTEWATER
o Methods for Benzidine, Chlorinated Organic Compounds,
Per.tachlorophenol and Pesticides in Water and Wastewater
(Interim) 1978, 25-42
U.S. Environmental Protection Agency, Environmental
Monitoring and Support Laboratory, Cincinnati, Ohio
o An aqueous sample is extracted with methylene chloride in
hexane, dried, concentrated, and analyzed by gas chroma-
tography with flame photometric detector. Several
organophosphorus pesticides are resolved on a column of
5% OV-210 or a mixture of 6^ QF-1 and 4% SE-30 on 100/120
mesh Gas-Chrom Q. Cleanup and column variations are
discussed.
o Limits: 0.050-0.100 pg/fc for 1- *. sample; 1 pg/fc for
100-ml. sample
Cross References - See captan, method C; chlorpyrifos, A and B;
dichlone, A; mevinphos, B.
- 48 -
-------
HYDROFLUORIC ACID
o fluohydric acid
METHODA - Potentiometry
o NIOSH ANALYTICAL METHODS FOR SET L
0 NTIS PB-250159, 1976, 40-46
Stanford Research Institute
o Air samples are drawn through sodium hydroxide solution,
diluted with additional sodium hydroxide solution, and
further diluted with total ionic strength activity buffer.
The diluted samples are analyzed using a fluoride ion
specific electrode. Very large amounts of complexing
metals such as aluminum may interfere.
o Limits: method validated for 1.33-4.50 mg/m ; probable
useful range is 0.245-7.35 mg/m for 45-liter sample
METHODB - Coulometric titration
O COULOMETRIC TITRATION OF HYDROFLUORIC ACID WITH A VITREOUS
CARBON WORKING ELECTRODE
o Anal. Chira. Acta 1975, 75(2), 478-485
V. J. Jennings, A. Dodson, and D. Colboume
o A vitreous carbon cathode and silver anode are used in the
coulometric determination of hydrofluoric acid. Nitrogen
is bubbled through a potassium chloride solution, m-cresol
purple solution is added as indicator, and current is passed
through the solution until the color changes to determine
the blank value. The hydrofluoric acid sample is added,
and the electrolysis is continued until the indicator changes
color again.
o Limits: 10" - 10" moles of hydrogen fluoride
METHOD C - Potentiometry
o AN AUTOMATIC POTENTIOMETRIC ANALYZER FOR ATMOSPHERIC HYDROGEN
FLUORIDE DETERMINATIONS
o Anal. Chim. Acta 1976, 85(2), 287-293
M. Mascini
o Hydrogen fluoride is collected from air by sodium carbonate
and measured hourly by washing the absorber with a citrate
buffer and determining fluoride with a fluoride-selective
electrode. In the collector, a large filter impregnated
with citric acid allows gaseous fluoride and gaseous fluoride
adsorbed on particulate matter to pass, but retains particulate
fluoride.
o Limits: 0.1-15 ug/m useful range
- 49 -
-------
HYDROGEN CYANIDE
o hydrocyanic acid
METHOD A - Wet Chemical
o RAPID TEST PAPER METHODS FOR HYDROGEN CYANIDE IN THE
ATMOSPHERE
o Ann. Occup. Hyg. 1971, 14C41, 289-294
R. Hill, J. H. Holt, and B. Miller
o Test paper is treated with a mixture of p-nitrobenzaldehyde
Gin diacetone alcohol) and potassium carbonate, A reddish-
purple color is obtained upon exposure of the paper to an
atmosphere containing 10 ppm hydrogen cyanide. The reagent
is stable and no interference is caused by the presence of
a few hundred ppm of chlorine, ammonia, or nitrogen peroxide,
o Limits: approximately 5 ppm
METHOD B- Potentioraetry
o DEVELOPMENT OF A SOLID SORPTION TUBE AND ANALYTICAL PROCEDURE
FOR HYDROGEN CYANIDE IN THE WORKPLACE ATMOSPHERE
o NTIS PB-253 228, 1976, 1-20
B. C. Cadoff and J. K. Taylor
o Atmospheric hydrogen cyanide is collected on flake sodium
hydroxide in a sorption tube. After removal of the sample
by water, the solution is analyzed potentiometrically with
cyanide and saturated calomel electrodes. The method is
rapid and relatively free of interferences.
o Limits: 10 - 10 M (concentrations greater than 10"3 M
rapidly destroy the cyanide electrode)
METHOD C - Potentiometric Titration
o EVALUATION OF SAMPLING TECHNIQUES FOR CYANIDE EMISSIONS
o J. Am. Ind. Hyg. Assoc. 1978, 39(10), 852-835
K. E. Williams, R. L. Bamberger, and G. G. Esposito
o Mixtures of air, carbon dioxide,, and hydrogen cyanide are
sampled through aqueous sodium hydroxide absorbents and the
absorbents are analyzed potentiometrically (cyanide-
specific electrode) by the method of standard additions.
Hydrogen cyanide is determined in stack emissions containing
up to 10% carbon dioxide. Absorbent temperature has no
significant impact on results.
o Limits: samples containing 5 and 20 ppm hydrogen cyanide are
analyzed successfully.
- 50 -
-------
ISOPRENE
o 2-methyl-l,3-butadiene
METHOD A - Gas Chroraatography
o GAS CHROMATOGRAPHIC ANALYSIS OF AMBIENT AIR FOR LIGHT
HYDROCARBONS USING A CHEMICALLY BONDED STATIONARY PHASE
o Anal. Chem. 1974, 46U2), 1852-1854
H. H. Westberg, R. A. Rasmussen, and M. Holdren
o Ambient air is sampled for light hydrocarbons (C2-C6) in
an apparatus which is adaptable for mobile field units.
The analysis is performed by gas chromatography on
Durapak (n-octane/Porasil C). A sample trap immersed in
liquid oxygen is preceded by a drying loop Canhydrous
lotassium carbonate).
imits: approximately 0.5 ppb.
I
METHOD B- Visible Spectrophotometry
O TETRACYANOETHYLENE ^-COMPLEX CHEMISTRY. INDIRECT SPECTRO-
PHOTOMETRIC DETERMINATION OF DIELS-ALDER-ACTIVE 1,3-DIENES
o Talanta 1973, 20(11), 1085-1096
D. A. Williams and G. H. Schenk
o A colored ir-complex between tetracyanoethylene (TCNE) and
an aromatic compound such as naphthalene or mesitylene is
destroyed by the Diels-Alder reaction of 1,3-dienes with
TCNE. The decrease in absorbance of the complex in the
presence of the 1,3-diene serves as the basis for the
indirect spectrophotometric determination of isoprene.
o Limits: 2.5 x 10" M for the naphthalene-TCNE complex;
2.5 x 10" M for the mesitylene-TCNE complex.
METHOD C- Gas Chromatography
o AN IMPROVED COLUMN FOR BUTADIENE ANALYSIS
o J. Chromatogr. Sci. 1972, 10C12), 737-740
J. W. Carson, J. D. Young, G. Lege', and F. Ewald
o Butadiene plant process streams and gaseous effluent from
naphtha feedstock thermal cracking furnaces in ethylene
plants are analyzed by gas chromatography. Two column
sections are connected in series: 1) 20% dibutyl maleate
on 60/80 Chromosorb P-NAW and 2) 10% bis(2-methoxyethoxy)-
ethyl ether on the same support. C. and C- diolefins are
separable.
o Limits: approximately 3% isoprene by weight.
- 51 -
-------
KELTHANE
o di(p_-chlorophenyl)trichloromethylcarbinol, DTMC, dicofol
METHOD A - Thin Layer Chromatography and Ultraviolet Spectrophotometry
o ISOLATION AND DETERMINATION OF CHLORINATED ORGANIC
PESTICIDES BY THIN-LAYER CHROMATOGRAPHY AND THE APPLICATION
TO TOXICOLOGICAL ANALYSIS
o J. Chromatogr. 1977. 131, 275-284
S. N. Tewari and I. C. Shanna
o Twelve chlorinated organic pesticides are chromatographed
on silica gel G plates, sprayed with a chromogenic reagent,
and exposed to ultraviolet radiation. Results are given
for 26 solvent systems and two chromogenic reagents. Densi-
tometer response is linear from l-10pg.
o Limits: 0.05 ug Kelthane with ethanolic, ammoniacal silver
nitrate spray; 0.5 pg Kelthane with 1% diphenylamine in
ethanol spray
METHOD B - Thin-Layer Chromatography and Ultraviolet Spectrophotometry
o THIN-LAYER CHROMATOGRAPHY OF DDT AND SOME RELATED COMPOUNDS
ON ALUMINUM OXIDE CHROMATOPLATES
o J. Chromatogr. 1972, 64 (1), 135-145
R. H. Bishara, G. S. Born, and J. E. Christian
o DDT and 11 related compounds are separated by two-dimensional
thin-layer Chromatography on aluminum oxide plates. The
plates are activated under ultraviolet radiation, sprayed
with a chromogenic reagent (ammoniacal silver nitrate plus
2-phenoxyethanol), and re-exposed to ultraviolet radiation.
o Limits: O.OSug Kelthane
Cross References - See captan, method A.
- 52 -
-------
MALATHION
o Phosphothion
METHOD A - Gas Chromatography
o Ten NIOSH Analytical Methods, Set 1. U. S. NTIS, PB-271712,
pp. 262-287 (1977)
Stanford Research Institute
o Airborne raalathion is collected on a filter, extracted with
isooctane, and analyzed by gas chromatography (flame photo-
metric detection) on a column of 1.5% OV-17 plus 1.95% OV-210
on 80/100 mesh GasChrom Q.
o Limits: 8-35 mg/m in 106-4. sample
METHOD B - Thin Layer Chromatography and Visible Spectrophotometry
o DETERMINATION OF SOME ORGANOTHIOPHOSPHORUS PESTICIDES WITH
PALLADIUM CHLORIDE, FOLLOWING THEIR SEPARATION BY THIN-LAYER
CHROMATOGRAPHY
o Acta Phann. Jugoslav. 1972, 22 (3), 91-96
D. A. Jovanovic and Z. Prosic
o Malathion, methyl parathion, and bromophos are separated
by thin-layer chromatography on Silica Gel F. After
detection on a sprayed portion of the plate, the corresponding
unsprayed portions are scraped off, dissolved in acetone and
reacted with 0.05% palladium chloride solution. The solution
is made up to volume and the optical density is determined at
320 nm.
o Limits: 0.25 ppm for food samples; 50-150 ug/100 ml water
Cross References - See chlorpyrifos, methods A and B; diazinon, B:
dichlone, A; dichlorvos, 3; guthion, A and B; meviiiphos, A and B;
parathion, A.
- 53 -
-------
MALE1C ACID
o ci£-butenedioic acid, cis^l^-ethylenedicarboxylic acid,
toxilic acid
METHOD A - Liquid Chromatography
o
o
SEPARATION OF MONO- AND DICARBOXYLIC ACIDS BY LIQUID
CHROMATOGRAPHY
J. Chroniatogr. 1975, 115(1), 259-261
M. Richards
A mixture of maleic, furaaric, citraconic, acrylic, and
acetic acids is separated by liquid Chromatography on a
column of Aminex 50W-X4 (30-35 urn), The wavelength
selected for monitoring is 210 nm.
Limits: lug/ml of each component, except acetic acid
(100 ug/ml)
METHOD B - Potentiometry
o ION-SELECTIVE ELECTRODE MEMBRANES RESPONSIVE TO MALEIC AND
PHTHALIC ACIDS
o Bull. Chen. Soc. Jap. 1973, 46(12), 3734-3737
A. Jyo, M. Yonemitsu, and N, Ishibashi
o Ion-selective electrodes responsive to hydrogen maleate
anion are prepared via organic solvent solution of the
anion with Crystal Violet or tris(bathophenanthroline)-
iron(II) ion as the electrode membrane. Solvents successfully
used for the membrane are nitrobenzene, 1,2-dichloroethane,
and chloroform. Fumaric acid does not interfere in the
maleic acid determination, and interferences from acetate,
benzoate, and chloride are low,
o Limits: electrode response is linear down to 10 -10"4'5M
METHOD C - Net Chemical and Visible Spectrophotometry
o SOLVENT EXTRACTION OF ANIONS WITH METAL CHELATE CATIONS -
XVIII. SPECTROPHOTOMETRIC DETERMINATION OF MALEIC ACID IN
THE PRESENCE OF FUMARIC ACID BY SOLVENT EXTRACTION WITH
TRIS(1,10-PHENANTHROLINE)IRON(II) CHELATE CATIONS
o Talanta 1972, 19(4), 415-422
Y. Yamamoto, T. Kumamaru and M. Muranaka
o Maleic acid is selectively extracted into nitrobenzene as
the ion-association complex formed between the hydrogen
maleate anion and the tris(l,10-phenanthroline)iron(II)
cation. The complex is determined at 516.nm, and a linear
relationship is obtained from 10 to 10 M maleic acid.
The optimal pH range is 3-5^. Maleic acid can be determined
in the presence of up to 10~ M fumaric acid.
o Limits: 10"5-10"4 M
- 54 -
-------
METHOXYCHLOR
o DMDT, methoxy-DDT
METHOD A - Wet Chemical and Gas Chromatography
o EVALUATION OF XAD-2 FOR MULTIRESIDUE EXTRACTION OF ORGANO-
CHLORINE PESTICIDES AND POLYCHLORINATED BIPHENYLS FROM
NATURAL WATERS
o J. Assoc. Off. Anal. Chem. 1977, 60 (1), 224-228
J. A. Coburn, I. A. Valdmanis, and A. S. Y. Chau
o Organochlorine pesticides are extracted from water on XAD-2
macroreticular resin, cleaned on a column of deactivated
alumina, and analyzed by gas chromatography (electron
capture detector) on the following columns: (1) 4% SE-30
plus 6% OV-210 on 80-100 mesh Gas-Chrom Q; (2) 1.5% OV-17
plus 1.95% OV-210 on 80-100 mesh Gas-Chrom Q; (3) 3% OV-225
on 80-100 mesh Chromosorb W(HP).
o Limits: 0.1 ug/ml
METHOD B- Gas Chromatography
o RAPID PREPARATION OF MICRO SAMPLE AND GAS-LIQUID CHROMATOGRAPHIC
DETERMINATION OF METHOXYCHLOR RESIDUES IN ANIMAL TISSUES AND
WATER
o J. Assoc. Off. Anal. Chem. 1977, 60 (3), 690-695
J. Solomon and W. L. Lockhart
o Water samples are extracted with 11 - hexane and analyzed by
gas chromatography (electron capture detector) on a column of
2% SE-30 plus 3% QF-1 on 80-100 mesh Chromosorb W(HP). For
tissue samples, extraction is followed by freezing out lipids
and cleanup on a Florisil column.
o Limits: water samples, 1 ppb, 5-ml sample; animal tissue,
10 ppb, 0.1 g sample
METHOD C - Gas Chromatography
o METHOD FOR CHLORINATED HYDROCARBONS IN WATER AND WASTEWATER
o Methods for Benzidine, Chlorinated Organic Compounds,
Pentachlorophenol and Pesticides in Water and Wastewater
(Interim) 1978, 7-24
U.S. Environmental Protection Agency, Environmental Monitoring
and Support Laboratory, Cincinnati, Ohio
o An aqueous sample is extracted with methylene chloride in
hexane, dried, concentrated, and analyzed by gas chromatography,
with electron capture detection, on a column of 5% OV-210 on
100/120 mesh Gas-Chrom-Q. Cleanup and column variations are
discussed.
o Limits: 0.050-0.100 ug/J. for l-i. sample; 1 ug/2 for 100-ral
sample.
Cross References - See dichlone, method A; dichlorvos, B.
- 55 -
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METHYL MERCAPTAN
o methanethiol, mercaptomethane, methyl sulfhydrate,
thiomethyl alcohol
METHOD A - Gas Chromatography
o GAS CHROMATOGRAPHIC DETERMINATION OF SOME SULPHUR GASES AT
THE VOLUMES PER MILLION LEVEL IN AIR USING TENAX-GC
o Analyst (London) 1978, 103(1225), 397-400
D. S. Walker
o A method is reported for the gas chromatographic determination
of hydrogen sulfide, carbonyl sulfide, sulfur dioxide, methyl
mercaptan, and dimethyl sulfide either separately or in
combination. A Tenax-GC column (35-60 mesh) and flame
photometric detector are used.
o Limits: 1-100 ppm (volume)
METHOD B- Gas Chromatography
o SIMULTANEOUS GAS CHROMATOGRAPHIC SEPARATION OF VOLATILE
ORGANIC SULPHUR COMPOUNDS AND Cj-C4 HYDROCARBONS
o J. Chromatogr. 1974, 90(.l), 218-222
F. Raulin and G. Toupance
o Twenty-six volatile sulfur compounds and several C.-C. hydro-
carbons are analyzed simultaneously by gas chromatography on
a column of Durapak OPN - Porasil C, 80-100 mesh. A flame
ionization detector is used. The methanethiol peak is well
resolved.
o Sample size: approximately 5 ug of each compound.
METHOD c- Gas Chromatography
o ANALYSIS OF SULFUR-CONTAINING GASES BY GAS-SOLID CHROMATOGRAPH1
ON A SPECIALLY TREATED PORAPAK QS COLUMN PACKING
o Anal. Chera. 1975, 47(3), 543-545
T. L. C. de Souza, D. C. Lane, and S. P. Bhatia
o A mixture of H2S, COS, SO-, MeSH, Me,S, and Me.S. is cleanly
separated by gas chromatography on a column of acetone-
washed Porapak OS. A flame photometric detector is used.
o Limits: approximately 5 ppm.
- 56 -
-------
METHYL METHACRYLATE
o methacrylic acid methyl ester, methyl-2-methyl-2-propenoate
METHOD A - Proton Magnetic Resonance Spectroscopy
0 DETERMINATION OF METHYL METHACRYLATE IN SURGICAL ACRYLIC
CEMENT
o J. Pharm. Sci. 1976, 65(2), 280-283
E. B. Sheinin, W. R. Benson, and W, L. Brannon
o Methyl methacrylate cement is quantitatively analyzed for
its monomer content by proton magnetic resonance spectres-
copy. The sample is dissolved in deuterated chloroform
and integrals of the vinyl C$ 5.50-6.20) and methoxyl
( 53.38-3.87) regions are determined in quintuplicate.
o Sample size: approximately 10 x 10 x 2mm
METHOD B- Gas Chromatography
o ANALYSIS OF THE INGREDIENTS AND DETERMINATION OF THE RESIDUAL
COMPONENTS OF ACRYLIC BONE CEMENTS
o J. Biomed. Mater. Res. 1977, 11(4), 577-607
G. M. Brauer, D. J. Termini, and G. Dickson
o Cured acrylic bone cement is examined for residual methyl
methacrylate monomer and for water-leachable monomer by gas
Chromatography on a column of 25% Emulphor Ott-870 on acid-
washed, 80/100 mesh Chromosorb W. A flame ionization
detector is used. For the water-leached sample, 0.02%
aqueous ii-hexyl alcohol is used as an internal calibration
standard, and the height of the methyl methacrylate peak
is compared to the alcohol peak. For the residual monomer
determination, 0.1% ethyl methacrylate in methylene chloride
is employed as internal standard.
o Limits: monomer content determined within 0.05% for 0.2-3%
monomer range.
Cross References - See quinoline, method B.
- 57 -
-------
METHYL PARATHION
o Nitrox-80
METHOD A - High Performance Liquid Chromatography
o DETERMINATION OF ETHYL AND METHYL PARATHION IN RUNOFF WATER
WITH HIGH PERFORMANCE LIQUID CHROMATOGRAPHY
o Anal. Chem. 1977, 49 (11), 1551-1554
D. C. Paschal, R. Bicknell, and D. Dresbach
o Aqueous samples are preconcentrated by treatment with XAD-2
resin, dissolved in acetonitrile, and chroraatographed on a
Partisil-ODS reverse phase column. Variable wavelength
detection is used. Of 20 agricultural chemicals tested,
only Fonofos interferes with the analysis for ethyl and
methyl parathion.
o Limits: 2 ppb
METHOD B - Laser Excited Resonance Raman Spectroscopy
o DETECTION OF WATER POLLUTANTS BY LASER EXCITED RESONANCE
RAMAN SPECTROSCOPY: PESTICIDES AND FUNGICIDES
o Appl. Spectrosc. 1978, 32 (1), 98-100
R. J. Thibeau, L. Van Haverbeke, and C. W. Brown
o Raman spectra of aqueous samples of nitrobenzene-based
pesticides and fungicides are recorded using the 488.0 and
457.9 nm Ar laser lines.
o Limits: 7.0 ppm methyl parathion
Grogs References - See chlorpyrifos, method A; diazinon, B; dichlone, A;
dichlorvos, B; guthion, A and B; malathion, B; mevinphos, B;
parathion, A; trichlorfon, B.
- 58 -
-------
MEVINPHOS
o Phosdrin
METHOD A - Resin Trap and Gas Chromatography
o PORTABLE DEVICE WITH XAD-4 RESIN TRAP FOR SAMPLING AIRBORNE
RESIDUES OF SOME ORGANOPHOSPHORUS PESTICIDES
o Anal. Chem. 1973, 50 (8), 1229-1231
J. E. Woodrow and J. N. Seiber
o An XAD-4 resin trap is used for airborne samples of
mevinphos, malathion, and parathion and compared with an
ethylene glycol trap. After extraction from the resin,
the sample is concentrated and analyzed by gas chroma-
tography (alkali flame ionization detector) on a column of
3% OV-17 on 80/100 mesh Chromosorb G.
o Limits: 5 ng/m
METHODS - Gas Chromatography
o EXTRACTION AND CLEANUP OF ORGANOCHLORINE, ORGANOPHOSPHATE,
ORGANONITROGEN, AND HYDROCARBON PESTICIDES IN PRODUCE FOR
DETERMINATION BY GAS-LIQUID CHROMATOGRAPHY
o J. Assoc. Off. Anal. Chem. 1975, 58 (5), 1020-1026
M. A. Luke, J. E. Froberg, and H. T. Masumoto
o Thirty-one pesticides are extracted from produce and analyzed
by gas Chromatography with thermionic or electron capture
detection; preliminary Florisil cleanup is necessary with
electron capture detection. Several standard columns are
employed.
o Limits (in ng): carbaryl, 106; parathion, 0.5; ethion, 0.76-
guthion, 3.6; diazinon, 0.45
Cross References - See captan, method A; dichlone, A.
- 59 -
-------
MEXACARBATE
o Zectran
METHOD A - Hi gh*-Performance Liquid Chromatography
o HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY OF CARBAMATE
PESTICIDES
0 J. Chromatogr. Sci. 1976, 14 (12), 549-556
C. M. Sparacino and J. K. Hines
0 Thirty compounds are separated by high-performance liquid
Chromatography using both normal and reverse-phase modes.
In the normal mode, the best separation for mexacarbate
was obtained using a column of Si-10; for carbaryl, NH--10.
Either P-Cj. or ETH was satisfactory in the reverses-phase mode.
0 Limits: mexacarbate, 10.2 ng; carbaryl, 8.7 ng.
METHODS_ Wet Chemical and Gas Chromatography
o ESTERS OF SULFONIC ACIDS AS DERIVATIVES FOR THE GAS
CHROMATOGRAPHIC ANALYSIS OF CARBAMATE PESTICIDES
o J. Agric. Food Chem. 1975, 23 (3), 415-418
H. A. Moye
o Mexacarbate or carbaryl is reacted with 2,5-dichlorobenzene-
sulfonyl chloride to yield the corresponding sulfonate esters
which are analyzed by gas Chromatography with tritium
electron capture detection. Column packings are 5% LSX-3-0295
or UCW98 on 100-120 Hi-Performance Chromosorb W. Preliminary
work has been carried out on flame photometric detection.
o Limits: 0.1 ppm for mexacarbate; 0.05 ppm for carbaryl
METHOD C- Thin-Layer Chromatography and Fluorescence Spectrophotometry
o ANALYSIS OF CARRAMATES AS FLUORESCENT 1-DIHETHYLAMINONAPHTHALENE-
5-SULFONATE ESTERS
o Intern. J. Environ. Anals. Chem., 1972, 1, 317-325.
J. F. Lawrence and R. W. Frei
o A fluorescent label is introduced into six N-methyl carbamates
by reaction of their aqueous solutions with 1-dimethylamino-
naphthalene-5-sulfonyl chloride (dansyl chloride). After
extraction by ii-hexane, the derivatives are subjected to thin-
layer Chromatography on silica gel G. Two fluorescent spots
are obtained for each carbamate; emission maxima occur at
approximately 530 nm.
o Limits: visual detection, 51 ng; instrumental detection, less
than 1 ng per spot.
Cross References - See carbaryl, method C; diazinon, B.
- 60 -
-------
NALED
o dibrom
Cross References - See chlorpyrifos, method A; dichlone, A.
- 61 -
-------
PARAFORMALDEHYDE
o paraform, formagene, triformol, polymerized formaldehyde,
polyoxymethylene
METHOD A - Wet Chemical and Gas Chromatography
o GAS CHROMATOGRAPHIC DETERMINATION OF METHANAL TRACES IN
PRESENCE OF OTHER VOLATILE CARBONYL COMPOUNDS
o J. Chromatogr. 1978, (153), 530-531
E. Merat
o Methanal is determined in concentrated liquid apple and
smoke flavors in the presence of other volatile carbonyl
compounds by derivatization with 2,4-dinitrophenylhydrazine.
The 2,4-dinitrophenylhydrazone is extracted into benzene
and analyzed by gas Chromatography, with flame ionization
detection, on a column of 4% SE-30 plus 4% 0\M7 on 100/120
mesh Chromosorb W HP. The same support is also used with
10% OV-101 stationary phase,
o Limits: 10 ppm
METHOD B- Gas Chromatography
o DETERMINATION OF THE CYCLIC TRIMER OF FORMALDEHYDE BY
GAS-LIQUID CHROMATOGRAPHY
o Analyst (London) 1978, 103(1230), 979-982
V. B. Kapoor, S. K. Chopra, and S. C. Vishnoi
o A mixture of formaldehyde, 1,3,5-trioxan, methanol, water,
and benzene is separated by gas Chromatography, with thermal
conductivity detection, on a column of 20% polyoxyethylene
sorbitan monooleate on 60/80 mesh Chromosorb P.
o Sample size: 1.0 p£
METHOD C- Wet Chemical and Gas Chromatography
o GAS CHROMATOGRAPHIC SEPARATION OF CARBONYL COMPOUNDS AS THEIR
2,4-DINITROPHENYLHYDRAZONES USING GLASS CAPILLARY COLUMNS
o J. Chromatogr. 1976, 120(2), 379-389
Y. Hoshika and Y. Takata
o 2,4-Dinitrophenylhydrazone derivatives of a mixture of 10
aliphatic aldehydes are separated by capillary gas Chroma-
tography, using SF-96 stationary phase and flame ionization
detection. A 30-1. car exhaust sample is condensed and
dissolved in ethanol. The 2,4-dinitrophenylhydrazone
derivatives are crystallized overnight, purified, and
dissolved in acetone. Anthracene is employed as internal
standard.
o Limits: exhaust sample containing 2.3 ppm formaldehyde and
1.5 ppm acetaldehyde is well resolved.
Cross References - See furfural, method A.
- 62 -
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PARATHION
o DNTP, Niran
METHOD A - Gas Chromatography
o GAS-LIQUID CHROMATOGRAPHY OF AQUEOUS-ALCOHOL SOLUTIONS FOR
INSECTICIDE RESIDUE ANALYSIS
o J. Assoc. Off. Anal. Chem. 1978, 61 (4), 837-840
W. W. Sans
o Aqueous solutions of 20 insecticides are centrifuged, diluted
with methanol and analyzed by gas chromatography (alkali flame
detection) on a column of 10% QF-1 on 100-120 mesh Aeropak 30.
o Limits (in ng): parathion, 0.03; methyl parathion, 0.03;
malathion, 0.03; carbaryl, 3.1; disulfoton, 0.01
METHODB- Gas Chromatography
o ANALYTICAL METHOD FOR PARATHION IN AIR
o Health Lab. Sci. 1976, 13C1), 73-77
D. F. Adams, J. 0. Frohliger, D. Falgout, A. M. Hartley,
J. B. Pate, A. L. Plumley, F. P, Scaringelli, and P. Urone
o Parathion is removed from an air sample by passing a
measured volume through an impinger containing ethylene
glycol. After extraction into hexane, the sample is
analyzed by gas chromatography on a column of 4% SE-30/6%
OV-210 on 80/100 mesh Chromosorb W. A flame photometric
detector is used. ?
o Limits: 5-250 pg/m
Cross References - See chlorpyrifos, method A; diazinon, A and B;
'ethion, A; guthion, A; ujevinphos, A and B; trichlorfon. B
- 63 -
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PHOSPHORIC ACID
o orthophosphoric acid
METHOD A - Catalytic Thermometric Titrimetry
o THE DETERMINATION OF WEAK ACIDS IN AQUEOUS SOLUTION BY
CATALYTIC THERMOMETRIC TITRIMETRY
o Talanta 1976, 23(1), 73-76
E. J. Greenhow and A. A. Shafi
o Weak acids are determined in aqueous solution with dimethyl
sulfoxide as co-solvent and acrylonitrile as indicator.
The titrant is potassium hydroxide in propan-2-ol. A sharp
rise in temperature occurs at the endpoint due to heat
evolved in the anionic polymerization of the indicator.
o Limits: for a 0.1 mmole sample, the concentration limits
are: phosphoric acid, 1%; benzoic acid, 2%; resorcinol, 10%.
METHOD B - Gas Chromatography and Mass Spectrometry
o ORGANIC ACID PROFILES OF HUMAN TISSUE BIOPSIES BY CAPILLARY
GAS CHROMATOGRAPHY-MASS SPECTROMETRY
o J. Chromatogr. 1977, 142, 497-503
S. I. Goodman, P. Helland, 0. Stokke, A. Flatmark, and E.
Jellum
o Tissue specimens are homogenized and extracted to yield a
mixture of acids, which are converted to their trimethylsilyl
derivatives. The derivatives are analyzed by combined gas
Chromatography (glass capillary column coated with SE-30)
and mass spectrometry.
o Limits: Smg tissue sample
METHOD C- Wet Chemical
o MICRODETERMINATION OF THE PHOSPHATE
o Mikrochim. Acta 1974, (4), 561-566.
S. S. M. Hassan and S. A. I. Thoria
ION USING A NEW REACTION
Phosphoric acid and primary and secondary phosphates are
determined by indirect iodometric titration. Phosphate
displaces iodate from calcium iodate in the presence of
ammonia to form the less soluble calcium ammonium phosphate.
The soluble iodate is determined by addition of potassium
iodide and titration of the liberated iodine with sodium
thiosulfate. Fluoride, silicate, sulfate, and arsenate
interfere with the analysis; chloride, bromide, iodide, and
nitrate do not interfere.
Sample size: 2-10 mg
- 64 -
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PROPIONIC ACID
o propanoic acid, methylacetic acid, ethylformic acid
METHOD A - Wet Chemical and Gas Chromatography
o GAS-LIQUID CHROMATOGRAPHY OF SHORT-CHAIN FATTY ACIDS ON
DEXSIL 300GC
o J. Chromatogr. 1972, 74(2), 335-338
M. A. Lambert and C. W. Moss
o A mixture of twelve C.-C- fatty acids is derivatized via
reaction with trifluoroacetic anhydride in boron trifluoride/
butanol. The esters are analyzed by gas chromatography (flame
ionization detection) on a column of 15% Dexsil 300GC on
80-100 mesh DMCS-treated Chromosorb W.
o Limits: 2.5 ug
Cross References - See butyric acid, methods A and B; formic acid, B.
- 65 -
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PYRETHRINS
o
METHOD A -
0
o
Pyrethrin I, Pyrethrin II
Gas Chromatography and Mass Spectrometry
SEPARATION AND ANALYSIS OF THE PYRETHRINS BY COMBINED GAS-
LIQUID CHROMATOGRAPHY-CHEMICAL IONIZATION MASS SPECTROMETRY
J. Assoc. Off. Anal. Chem. 1977, 60 (3), 685-689
R. L. Holmstead and D. M. Soderlund
The six naturally occurring pyrethrin esters and pyrethrins I
and II are separated by gas Chromatography on a column of 5%
OV-25 on 60-80 mesh Chromosorb W. Chemical ionization mass
spectra are also reported.
Limits: 114 ng total to detect all compounds; 11.4 ng total
to detect Pyrethrin I
METHOD B - Gas Chromatography and Mass Spectrometry
o ANALYTICAL STUDIES OF PYRETHRIN FORMULATIONS BY GAS
CHROMATOGRAPHY III. ANALYTICAL RESULTS ON INSECT1CIDALLY
ACTIVE COMPONENTS OF PYRETHRINS FROM VARIOUS WORLD SOURCES
o J. Chromatogr. 1974, 90 (1), 119-128
Y. Kawano, K. H. Yanagihara, and A. Bevenue
o Matrix-programmed flame ionization gas Chromatography is
used to separate the components of pyrethrum extracts on
a column of 2.5% XE-60 on 60-100 mesh Chromosorb W after
Florisil column cleanup of the crude extracts. Mass spectra
in the m/e 50-190 range are given.
o Sample size: 80-120 vg
METHOD C - Gas Chromatography
o USE OF PROGRAMMED TEMPERATURE IN ANALYTICAL DETERMINATION
OF PYRETHRINS BY ELECTRON CAPTURE DETECTOR
o Pyrethrum Post 1971, 11 (1), 29-31
P. Tetenyi, E. Hethelyi, T. Okuda, and I. Szilagyi
o Both isothermal and programmed temperature gas chromatographic
methods are used to analyze pyrethrum extracts. An electron
capture detector is employed with a column of 3% NPGS on
silanized Chromosorb W, 60/80 mesh.
o Sample size: 5 ug pyrethrum extract in 3p£
- 66 -
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QUINOLINE
1-benzazine, benzo(b)pyridine, leuocoline, chinoleine,
leucol
METHOD A - High-Pressure Liquid Chromatography
o SEPARATION OF AZA-ARENES BY HIGH-PRESSURE LIQUID CHROMATOGRAPHY
o J. Chromatogr. Sci. 1977, 15 (1), 32-35
M. Dong and D. C. Locke
o Aza-arenes are separated in 20 minutes by high-pressure
liquid chromatography using reversed-phase or adsorbent
packings. Identification is made by UV (254 ran) or
fluorescence spectrophotometry. The method is applied to
the analysis of airborne particulate matter.
o Limits: 1 ng
METHOD B - Column and Gas Chromatography
o USE OF MACRORETICULAR RESINS IN THE ANALYSIS OF WATER FOR
TRACE ORGANIC CONTAMINANTS
o J. Chromatogr. 1974, 99, 745-762
G. A. Junk, J. J. Richard, M. D. Grieser, D. Witiak, J. L.
Witiak, M. D. Arguello, R. Vick, H. J. Svec, J. S. Fritz,
and G. V. Calder
o Trace organics are isolated from water samples by sorption
on XAD-2 or XAD-4 macroreticular resins and elution with
diethyl ether. After concentration, the eluent is analyzed
by gas chromatography (flame ionization detector) on a
column of 5% OV-1 on 80-100 mesh DMCS-treated Chromosorb W.
o Limits: recovery of quinoline at the 10-100 ppb level is 84%;
methyl methacrylate, 35%.
METHOD C - High-Performance Liquid Chroraatography
o HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY WITH Ag* COMPLEXATION
IN THE MOBILE PHASE
o J. Chromatogr. 1978, 149, 417-430
B. Vonach and G. Schomburg
o Six N-heterocycles, including quinoline, and standard nitrogen-
free polyaromatics are separated by high-performance liquid
chromatography on Nucleosil 5 C 18 with a polar mobile phase
containing silver perchlorate.
Cross References - See strychnine, method C.
- 67 -
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RESORCINOL
o resorcin, 1,3-benzenediol, meta-di-hydroxybenzene
METHOD A - Wet Chemical and Gas Chromatography
o N-METHYLIMIDAZOLE-CATALYZED ACETYLATION OF HYDROXY COMPOUNDS
PRIOR TO GAS CHROMATOGRAPHIC SEPARATION AND DETERMINATION
o Anal. Chem. 1979, 51(1), 27-30
R. Wachowiak and K. A. Connors
o Alcohols, phenols, glycols, and sugars are acetylated with
acetic anhydride in the presence of N-methylimidazole and
determined by gas Chromatography with flame ionization
detection. For phenols, the stationary phase is 5%
Carbowax 20M or 5% OV-17 on Chromosorb W - AW, DMCS, and
ethylene glycol diacetate is employed as an internal
standard.
o Sample size: 0.04g
METHODS - Thin-Layer Chromatography
o
o
TITANIUM CHROMOGENIC REAGENT FOR PHENOLIC COMPOUNDS ON
JHIN-LAYER PLATES.
Chromatogr. 1978, 150(1), 293-294
N. A. M. Eskin and C. Frenkel
Phenolic compounds are detected on thin-layer plates
(silica gel G) by spraying with the chromogenic reagent,
20% titanium tetrachloride in concentrated hydrochloric
acid. For resorcinol, an orange-yellow color develops
immediately.
Limits: 4 ug
METHOD C- Wet Chemical and Gas Chromatography
o THE DETERMINATION OF PHENOLS IN AQUEOUS EFFLUENTS
o Water Res. 1973, 7(9), 1375-1384
R. L. Cooper and K. C. Wheatstone
o Phenol, cresols, xylenols, ethylphenols, and dihydric phenols
are separated by gas-liquid Chromatography after conversion
to their trimethylsilyl ether derivatives. A flame ionization
detector is used with a column of 5% tri-2,4-xylenyl phosphate
on Chromosorb W. (AW-DCMS).
o Limits: 0.1 rag/1.
Cross References - See cresol, method A; dinitrobenzene, A; phosphoric
acid, A.
- 68 -
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STRYCHNINE
METHOD A - Gas Chromatography
o A NEW, RAPID GAS CHROMATOGRAPHY METHOD FOR THE DETECTION OF
BASIC DRUGS IN POSTMORTEM BLOOD, USING A NITROGEN PHOSPHORUS
DETECTOR. PART 1. QUALITATIVE ANALYSIS
o J. Anal. Toxicol. 1978, 2 (1), 26-31
W. 0. Pierce, T. C. Lamoreaux, and F. M. Urry
o Basic drugs are determined in blood by extraction into
n_ - butyl chloride and analysis by gas Chromatography with
a nitrogen phosphorus detector. Retention data are given
for two columns, 3% OV-1 and 3% OV-17, on 100-120 mesh
Chromosorb W.
o Limits: 200-500 ng; 1 ml blood sample
METHOD B - Liquid Chromatography
o HIGH-SPEED LIQUID CHROMATOGRAPHY OF ALKALOIDS. I.
o J. Chromatogr. 1974, 100 (1), 227-230
R. Verpoorte and A. B. Svendsen
o Strychnine is subjected to high-speed liquid Chromatography
on Merckosorb Si 60, with detection at 254 nm. Retention
times are reported for six solvent systems.
o Limits: 25 ng
METHOD C - Wet 'Chemical and Atomic Absorption Spectrometry
o THE INDIRECT ATOMIC ABSORPTION SPECTROMETRIC DETERMINATION
OF SEVERAL ORGANIC BASES USING MOLYBDOPHOSPHORIC ACID
o Microchem. J., 1975, 20 (4) 468-475
S. J. Simon and D. F. Boltz
o Complexation of strychnine or quinoline with molybdophosphoric
acid and subsequent liberation of molybdate permits indirect
determination of the bases by measuring absorbance of
molybdenum at 313 nm in an air/acetylene flame.
o Limits: quinoline, 2 ppm; strychnine, 0.65 ppm
- 69 -
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STYRENE
o vinylbenzene, phenylethylene, styrol, styrolene, cinnamene,
cinnamol
METHOD A - Gas Chromatography
o GAS CHROMATOGRAPHIC DETERMINATION OF SELECTED ORGANIC
COMPOUNDS ADDED TO WASTEWATER
o Environ. Sci. Technol. 1975, 9 (6), 588-590
B. M. Austern, R. A. Dobbs, and J. M. Cohen
o Eleven organic compounds are recovered from wastewater by
extraction with Freon, concentrated, and analyzed by gas
chromatography (hydrogen flame ionization detector) on a
column of 15% Carbowax 4000 on 80-100 mesh Chromosorb WfHPl.
o Limits: 0.5 ng styrene
METHOD B - Wet Chemical and Gas Chromatography
o GAS CHROMATOGRAPHIC DETERMINATION OF STYRENE AS ITS
DIBROMIDE
o J. Chromatogr., Vol. 136, No. 1, pp. 95-103 (1977)
Y. Hoshika
o Styrene from air is collected in a cold trap (liquid
oxygen), extracted with hexane, and brominated with bromine
in chloroform. The dibromide is analyzed by gas chroma-
tography with electron capture detection on a column of 3%
OV-17 on 60-80 mesh Chromosorb W. Interference studies with
138 compounds are reported.
o Limits: 0.1-0.4 ppb from air
Cross References - See xylene, method C
- 70 -
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2.4.S-T ACID
o 2,4,5-tTichlorophenoxyacetic acid
METHOD A - Wet Chemical and Gas Chromatography
o SIMULTANEOUS DETERMINATION OF 2,4-DICHLOROPHENOXYACETIC
ACID, 2,4,5-TRICHLOROPHENOXYACETIC ACID, AND 2-METHOXY-
3,6-DICHLOROBENZOIC ACID IN SOIL AND WATER BY GAS
CHROMATOGRAPHY WITH ELECTRON CAPTURE DETECTOR
o J. Agr. Food Chem. 1974, 22 (3), 453-458
R. Purkayastha
o Soil and water samples of the above herbicides are extracted
with diethyl ether, butylated with diazobutane, cleaned on
a Florisil column, and analyzed by gas Chromatography with
electron capture detector. Columns providing good
sensitivity and resolution are 11% (OV-17/QF-1) or 3% Carbowax
20M on Gas-Chrom Q or Chromosorb W, 80-100 mesh.
o Limits: 0.03-0.05 ppm in soil; no cleanup required for water
samples
Cross References - See 2,4-D acid, method A; dicamba, A and C; dichlorvos, B;
2,4,5-T ester, A.
- 71 -
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2.4.S-T ESTER
o 2,4,5-trichlorophenoxyacetic esters
METHOD A - Resin Sorption, Wet Chemical, and Gas Chromatography
o SIMPLIFIED RESIN SORPTION FOR MEASURING SELECTED
CONTAMINANTS
o J. Am. Water Works Assoc. 1976, 68 (4), 218-222
G. A. Junk, J. J. Richard, H. J. Svec, and J. S. Fritz
o 2,4-D, 2,4,5-T, and their esters are removed from water
samples by XAD-2 resin and eluted with diethyl ether.
One portion of the eluate is hydrolyzed and another is
esterified with diazomethane. Toal chlorophenoxy
herbicide is then determined by gas Chromatography.
o Limits: < 250 ng/1
Cross References - See chlorpyrifos, method A; 2,4-D ester, A;
dichlone, A; dichlorvos, B; 2,4,5-T acid, A.
- 72 -
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TETRAETHYL LEAD
o lead tetraethyl, TEL
METHOD A - Thin-Layer Chromatography and Visible Spectroscopy
o DETECTION AND DETERMINATION OF ALKYL LEAD COMPOUNDS IN
NATURAL WATERS
o Water Pollut. Control (Maidstone, Engl.) 1977, 76(1), 123-128
H. R. Potter, A. W. P. Jarvie and R. N. Markall
o Tetraethyllead is determined by extraction into petroleum
ether, conversion to Et.PbCl- (via iodine monochloride),
extraction of the salt into water, and thin-layer chroma-
tography against an authentic sample. The aqueous extract
can also be converted to a colored product by reaction with
pyridylazoresorcinol; the absorption of the resulting solution
is measured at 515 nm.
Limits: 2 mg/1
of Et2Pb
2+
in the petroleum ether extract
METHOD B- Gas Chromatography and Atomic Absorption Spectrometry
o GAS CHROMATOGRAPHY - ATOMIC ABSORPTION SPECTROMETRY FOR THE
DETERMINATION OF TETRAALKYLLEAD COMPOUNDS
o Anal. Chim. Acta 1976, 85(2), 421-424
Y. K. Chau, P. T. S. Wong, and P. D. Goulden
o A combination of gas Chromatography and atomic absorption
spectrometry is used to determine tetraalkyllead compounds
in which the alkyl substituents are methyl or ethyl. A
column of 3% OV-1 on 'Chromosorb W is used to resolve the
five organometallic compounds, and lead is detected at
217 nm. The response is linear to 200 ng of lead.
o Limits: 0.1 ng lead can be determined with certainty.
METHOD C- Gas Chromatography
o TEN NIOSH ANALYTICAL METHODS. SET 3.
o NTIS PB-275 834, 1977, 75-118.
Stanford Research Institute
o A known volume of air is drawn through an XAD-2 tube to
trap the organic vapors present. After desorption with
pentane, tetraethyllead is determined by gas Chromatography,
with photoionization detection, on a column of 5% Carbowax
20M on 80/100 mesh Chromosorb W, AW. Dodecane or other
suitable internal standard is used.
o Limits: 0.045-0.20 rag/m (as lead)
- 73 -
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TRICHLORFON
o Dipterex, Dylox
METHOD A_ Wet Chemical and Gas Chromatography
o ROUTINE METHODS FOR ANALYSIS OF ORGANOPHOSPHORUS AND
CARBAMATE INSECTICIDES IN SOIL AND RYEGRASS
o Pestic. Sci. 1977, 8 C4) 354-358
P. T. Holland
o Trichlorfon and dichlorvos are extracted from soil, cooled
to precipitate water and waxes, and analyzed by gas
Chromatography (alkali flame ionization detector) on a
column of 3% SE-30 on 80/100 Gaschrom Q. On-column
acetylation with acetic anhydride is employed for analysis
of trichlorfon. Gas chromatographic results are confirmed
by mass spectrometry.
o Limits: 0.2 ng
METHOD B- Plasma Chromatography
O PLASMA CHROMATOGRAPHY OF PESTICIDES
0 J. Chromatogr. Sci. 1975, 13 (.6), 285-290
H. A. Moye
o Twenty-three pesticides and/or metabolites are analyzed at
residue levels by plasma Chromatography. Ion mobility
spectra are presented and applications to analysis of liquid
chromatographic fractions are discussed.
0 Limits: 0.1 ng for trichlorfon, methyl parathion, 2,4-D,
and carbaryl; 0.01 ng for parathion and ethion; 0.001 ng for
diazinon and chlorpyrifos.
METHOD C- Wet Chemical and Gas Chromatography
o THE DETERMINATION OF TRICHLORFON IN WATER
o Fish. Mar. Serv. Res. Dev. Tech. Rep. 714, 1977, 1-14
V. Zitko and D. B. Sergeant
o Trichlorfon is determined indirectly by hydrolysis to
dichlorvos and analysis of the latter by gas Chromatography
and mass spectrometry. The pH of a solution of trichlorfon
in acetone is adjusted by addition of sodium hydroxide
solution. After 1.75 hr the hydrolysis is quenched by
addition of sulfuric acid, and the mixture is extracted
with ethyl acetate and concentrated. Gas chromatographic
columns used are: 3% OV-1 on Chromosorb W, HP, 80/100 mesh
with flame photometric detector; 4% SE-30 on Chromosorb W,
HP, 100/200 mesh with electron capture detector.
o Limits: 1 ug/£ of trichlorfon in an aqueous sample.
Cross References - See chlorpyrifos, method A; coumaphos, A.
- 74 -
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TRIETHYLAMINE
METHOD A - Wet Chemical and Thin-Layer Chromatography
o A NEW SOLVENT SYSTEM FOR THE THIN-LAYER CHROMATOGRAPHIC
SEPARATION OF THE DANSYL DERIVATIVES OF SOME BIOGENIC
AMINES
o J. Chromatogr. 1974, 90C1), 178-180
G. C. Boffey and G. M. Martin
o Twenty-two biogenic amines are derivatized with 1-naphthalene-
sulfonyl chloride Cdansyl chloride) and subjected to thin-
layer chromatography on silica gel. The chromatograms are
developed in the carbon tetrachloride - ethylene glycol
monomethyl ether C85:15, v/v) solvent system, and fluorescence
of the dansyl derivatives is observed at 366 nm.
o Limits: 0.01-1.00 uM sample
Cross References - See butylamine, methods A and B.
- 75 -
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VINYL ACETATE
o acetic acid ethylene ether
METHOD A - Gas Chromatography
o RHODIUM(II) CARBOXYLATES AS NEW SELECTIVE STATIONARY PHASES
IN GAS-LIQUID CHROMATOGRAPHY
o Chromatographia 1972, 5C12J, 301-304
V. Schurig, J. L. Bear, and A. Zlatkis
o Dimeric rhodium (II) benzoate in squalane is employed as a
stationary phase for gas-liquid Chromatography of compounds
containing oxygen functional groups. The carboxylate is
coated on Chromosorb P, AW, DMCS, 100/120 mesh, and a flame
ionization detector is used.
o Limits: not given
METHODB - Wet Chemical
o MICRO DETERMINATION OF OLEFINIC UNSATURATION. REACTION OF
N-BROMOSUCCINIMIDE WITH OLEFINS IN POLAR MEDIUM
o Fresenius1 Z. Anal. Chem. 1972, 260(5), 359-361
V. K. S. Shukla, U. C. Pande, and J. P. Sharma
o Olefinic unsaturation is determined by reacting a solution
of the olefin in glacial acetic acid with a known excess of
N-bromosuccinimide, which is back-titrated iodometrically.
The reaction is rapid (.10 minutes) and observes 2:1 stoichiometry
in the polar medium.
o Sample size: 2-10 mg
Cross References - See acetaldehyde, method B.
- 76 -
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dimethylbenzene, xylol
METHOD A - Gas Chromatography
o
o
o
METHOD B
o
o
METHOD C
o
o
SUSPENSIONS OF CRUDE OILS IN SEA WATER: RAPID METHODS OF
CHARACTERIZING LIGHT HYDROCARBON SOLUTES
Natl. Bur. Stand. (U.S.), Spec. Publ. 409, pp. 127-130 (1974)
R. M. Bean
Aqueous samples containing the xylenes are filtered to
remove insoluble hydrocarbons, extracted with carbon
tetrachloride, and analyzed by gas chromatography on a
column of 4% Carbowax 20M TPA on 100-120 mesh Chromosorb W.
£-Xylene appears as a separate peak, but m- and p_-xylene
are not resolved.
Limits: 0.01 mg/1; sample size, 0.5 1
- Gas Chromatography
SOLVENTS IN SEWAGE AND INDUSTRIAL WASTE WATERS:
IDENTIFICATION AND DETERMINATION
Water Pollut. Control 1974, 73 (6), 656-672
W. K. Ellison and T. E. Wallbank
Aqueous samples of m-xylene undergo preliminary separation
by steam distillation and extraction, followed by gas
chromatography (electron capture detection; 10% Apiezon L
on Chromosorb G, 60/80 mesh) and infrared and ultraviolet
Limits: recovery of 88% with 0.5 mg aliquot in 1-A sample
- Gas Chromatography
GAS CHROMATOGRAPHIC SEPARATION OF STYRENE IN THE PRESENCE
OF XYLENES AND PROPYLBENZENES
Anal. Chem. 1974, 46 (14) 2225*2226
D. M. Ottenstein, D. A. Bartley, and W. R. Supina
For a mixture of nine compounds, including styrene and
the three isomeric xylenes, base line resolution is
obtained by gas chromatography on a column of 5% SP-1200
and 1.75% Bentone 34 on 100-120 mesh Supelcoport. Dual
flame ionization detectors are used.
Limits: a O.lOpJZ. injection of the mixture is well
resolved
Cross References - See benzonitrile, method A; butyl acetate, C;
dinitrobenzene, B; styrene, A.
- 77 -
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VI. Index to Compound Names
Acetaldehyde 11
Acetic acid butyl ester 19
Acetic acid ethylene ester 76
Acetic aldehyde 11
Acetone cyanohydrin 12
Allomaleic acid 46
Allyl alcohol 13
Aminobenzene 15
1-Aminobutane 20
Aminophen 15
Amyl acetate 14
js_o- Amy 1 acetate 14
sec-Amy! acetate 14
t-Amyl acetate 14
Amylacetic ester 14
Aniline 15
Aniline oil 15
Aquacide 39
Azinphos-methyl 48
Banana oil 14
Basudin 31
1-Benzazine 67
Benzenecarboxylic acid 16
1,3-Benzenediol 68
Benzo(b)pyridine 67
Benzole acid 16
Benzonitrile 17
Benzyl chloride 18
Boletic acid 46
Butanoic acid 21
cis^Butenedioic acid 54
trans-Butenedioic acid 46
Butyl acetate 19
Butylamine 20
Butyric acid 21
Captan 22
Carbaryl 23
Carbon bisulfide 24
Carbon disulfide 24
Chinoleine 67
Chlorpyrifos 25
Ci nnamene 70
Cinnamol 70
Co-Ral 26
Coumaphos 26
Cresol 27
Cresylic acid 27
_ 78 -
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Cyanobenzene 17
Cyanogen chloride 28
2,4-0 acid 29
Dalapon 35
2,6-DBN 33
DCMU 41
2,4-D ester 30
Dextrone 39
1,2-01 aminoethane 44
Diazinon 31
Dlazltol 31
Dibrom 61
01camba 32
Dichlobenil 33
Dlchlone 34
2,6-Dichlorobenzonitrile 33
Dichloronaphthoquinone 34
2,4-Dlchlorophenoxyacetlc acid 29
2,4-Dichlorophenoxyacetic ester 30
01 (p_-chlorophenyl)trichloromethylcarbinol 52
2,2-Dichloropropionic acid 35
2,2-Dichlorovinyl dimethyl phosphate 36
Dichlorvos 36
Dlcofol 52
01ethyl amine 37
meta-Di hydroxybenzene 68
01methyl benzene 77
01 nitrobenzene 38
Dlnitrobenzol 38
Dipofene 31
Dipterex 74
Olquat 39
Dlquat dibromide 39
Disulfoton 40
Dl-syston 40
Dithiocarbonic anhydride 24
Diuron 41
DMDT 55
DMU 41
DNTP 63
Dodecylbenzenesulfonic acid 42
Dracylic acid 16
DTMC 52
Oursban 25
Ethanal 11
Ethion 43
Ethylacetic acid 21
Ethyl aldehyde 11
Ethylenediamine 44
- 79 -
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cl^-l.Z-Ethylenedicarboxylic acid 54
trans-1,2-Ethylenedicarboxylic acid 46
Ethyl formic acid 65
Ethyl methylene phosphorodithioate 43
Fluohydric acid 49
Formagene 62
Formaldehyde, polymerized 62
Formic acid 45
Fumaric acid 46
2-Furaldehyde 47
Furfural 47
Gusathion 48
Guthion 48
Hydrocyanic acid 50
Hydrofluoric acid 49
Hydrogen cyanide 50
a!pha-Hydroxyi sobutyroni tri1e 12
Hydroxytoluene 27
Isoprene 51
Kelthane 52
Kyanol 15
Laurylbenzenesulfonic acid 42
Lead tetraethyl 73
Leucol 67
Leuocoline 67
Mai athion 53
Maleic acid 54
Mercaptomethane 56
Methacrylic acid methyl ester 57
Methanethiol 56
Methanoic acid 45
Methoxychlor 55
Methoxy-DDT 55
2-Methoxy-3,6-dichlorobenzoic acid 32
Methyl acetic acid 65
2-Methy!-1,3-butadiene 51
2-Methyllactonitrile 11
Methyl mercaptan 56
Methyl methacrylate 57
Methyl-2-methyl-2-propenoate 57
Methyl parathion 58
Methyl sulfhydrate 56
Mevinphos 59
Mexacarbate 60
Naled 61
Nialate 43
Niran 63
Nitrox-80 58
Orthocide-406 22
Orthophosphoric acid 64
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Paraform 62
Paraformaldehyde 62
Parathion 63
Pear oil 14
Phenylamine 15
Phenyl cyanide 17
Phenylethylene 70
Phenylformic acid 16
Phosdrin 59
Phosphoric acid 64
Phosphothion 53
Phygon 34
Polyoxymethylene 62
Propanoic acid 65
l-Propenol-3 13
2-Propen-l-ol 13
Propionic acid 65
Pyrethrin I 66
Pyrethrin II 66
Pyrethrins 66
Pyromucic aldehyde 47
Quinoline 67
Reglone 39
Resorcin 68
Resorcinol 68
Sevin 23
Spectracide 31
SR-406 22
Strychnine 69
Styrene 70
Styrol 70
Styrolene 70
2,4,5-T acid 71
TEL 73
2,4,5-T ester 72
Tetraethyl lead 73
Thiomethyl alcohol 56
Toxilic acid 54
Trichlorfon 74
2,4,5-Trichlorophenoxyacetic acid 71
2,4,5-Trichlorophenoxyacetic esters 72
Triethyl amine 75
Triformol 62
Vancide-89 22
Vapona 36
Vinyl acetate 76
Vinyl benzene 70
Vinyl carbinol 13
Xylene 77
Xylol 77
Zectran 60
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