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Advances in the Assessment
of Dietary Intake
Advances in the Assessment
of Dietary Intake
Edited by
Dale A. Schoeller
Margriet S. Westerterp-Plantenga
CRC Press
Taylor & Francis Group
6000 Broken Sound Parkway NW, Suite 300
Boca Raton, FL 33487-2742
This book contains information obtained from authentic and highly regarded sources. Reasonable efforts have been made to
publish reliable data and information, but the author and publisher cannot assume responsibility for the validity of all materials
or the consequences of their use. The authors and publishers have attempted to trace the copyright holders of all material repro-
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Trademark Notice: Product or corporate names may be trademarks or registered trademarks, and are used only for identifica-
tion and explanation without intent to infringe.
This book is dedicated to Dr. Ira Wolinsky, PhD, who conceptualized the
aims of this book and then initiated the process leading to its publication.
Dr. Wolinsky passed away on November 26, 2014, after a long career as an
investigator and an editor. He earned his doctorate in biochemistry from
the University of Kansas, Lawrence, Kansas, and went on to investigate the
role of bone metabolism and human health at Pennsylvania State University,
State College, Pennsylvania. He later moved to the University of Houston,
Houston, Texas, from which he retired as Professor Emeritus in 2005. From
the very beginning of his scientific career, Dr. Wolinsky worked to apply
the advances in basic science to the improvement of clinical science with
respect to both treatment and prevention of human disease. During his
PhD training at the University of Kansas, he applied the state-of-the-art
biochemistry to increasing the health of human teeth. Later at Pennsylvania
State University, he studied the interaction of skeletal muscle and bone to
improve bone health. At the University of Houston, he examined the impact of
weightlessness during space flight in order to prevent the loss of bone density.
Dr. Wolinsky published more than 40 journal articles and selected to expand
the impact of original scientific research on the human condition by authoring
and editing of more than 148 books. This included editing the influential CRC
Series in Modern Nutrition, which he aimed toward a “scholarly audience … to
explain, review, and explore present knowledge and recent trends, developments,
and the advances in nutrition.” Although Dr. Wolinsky welcomed investigator-
initiated book proposals for this series, he went beyond and monitored
novel developments in nutrition recruiting others to create state-of-the-art
volumes that enhanced and expanded upon those key basic developments.
Although I only knew Dr. Wolinsky through our correspondence, it was he
who first engaged my efforts as a coeditor along with Dr. Helen Lane on
a book that encapsulated the breadth of knowledge on nutrition that was
necessary for spaceflight. In 2014, it was again because of Dr. Wolinsky’s
foresight and creativity that I was recruited to coedit this book in an effort
to change the field of diet assessment. He contacted and convinced me
that recent breakthroughs in technology were such that, if focused on diet
assessment in the form of a state-of-the-art book, could help revolutionize
the methods used for dietary assessment. Unfortunately, Dr. Wolinsky passed
away before Dr. Margriet S. Westerterp-Plantenga and I, along with the many
authors of Advances in the Assessment of Dietary Intake, could complete
this book; however, because of his efforts as a creative and engaged editor,
we dedicate this book to the memory of Dr. Wolinsky’s achievements.
Dale A. Schoeller
Margriet S. Westerterp-Plantenga
Coeditors
Contents
Editors ...............................................................................................................................................ix
Contributors ......................................................................................................................................xi
Prologue ........................................................................................................................................... xv
Chapter 4 Strategies for Improving the Validity of the 24-hour Dietary Recall and Food
Record Methods ......................................................................................................... 67
Lisa J. Harnack and Mark A. Pereira
Chapter 6 Meal Patterns, Physical Activity, Sleep, and Circadian Rhythm ............................. 113
Margriet S. Westerterp-Plantenga and Marta Garaulet
Chapter 9 Direct and Indirect Measures of Dietary Intake: Use of Sensors and Modern
Technologies ............................................................................................................. 163
Holly L. McClung, Joseph J. Kehayias, Gary P. Zientara, and Reed W. Hoyt
vii
viii Contents
Chapter 11 Biomarker for Energy Intake: Resting Energy Expenditure and Physical
Activity ................................................................................................................ 199
Klaas R. Westerterp
Chapter 12 Dynamic Modeling of Energy Expenditure to Estimate Dietary Energy Intake..... 211
Diana Thomas and Vincent W. Antonetti
Chapter 18 Targeted and Untargeted Metabolomics for Specific Food Intake Assessment:
Whole Grains as an Example ................................................................................... 315
Carl Brunius, Huaxing Wu, and Rikard Landberg
ix
Contributors
David B. Allison Hamid R. Farshchi
Department of Nutrition Sciences, Nutrition School of Life Sciences
Obesity Research Center Queen’s Medical Centre
University of Alabama at Birmingham University of Nottingham
Birmingham, Alabama Nottingham, United Kingdom
xi
xii Contributors
Sharon I. Kirkpatrick
Suzanne McNutt
School of Public Health and Health Systems
Health Studies Sector
University of Waterloo
Westat, Inc.
Ontario, Canada
Rockville, Maryland
Rikard Landberg
Department of Food Science Edward Melanson
Swedish University of Agricultural Sciences Division of Endocrinology, Metabolism, and
Uppsala, Sweden Diabetes/Division of Geriatric Medicine
University of Colorado
and Aurora, Colorado
Department of Biology and Biological
Engineering Eric Muth
Chalmers University of Technology Department of Psychology
Göteborg, Sweden Clemson University
Clemson, South Carolina
and
Department of Medical Epidemiology and Candice A. Myers
Biostatistics Pennington Biomedical Research Center
Karolinska Institutet Baton Rouge, Louisiana
Stockholm, Sweden
Sarah H. Nash
Ian Macdonald
Alaska Native Tumor Registry
School of Life Sciences
Alaska Native Epidemiology Center
Queen’s Medical Centre
Anchorage, Alaska
University of Nottingham
Nottingham, United Kingdom
Vanessa Neveu
Ameneh Madjd Nutrition and Metabolism Section, Biomarkers
School of Life Sciences Group
Queen’s Medical Centre International Agency for Research on Cancer
University of Nottingham Lyon, France
Nottingham, United Kingdom
Diane M. O’Brien
Corby K. Martin Institute of Arctic Biology
Pennington Biomedical Research Center University of Alaska–Fairbanks
Baton Rouge, Louisiana Fairbanks, Alaska
Contributors xiii
xv
xvi Prologue
balance, which would be disastrous for performance. High-energy drinks, consumed during the
race, contribute significantly to daily intake (Westerterp et al. 1986). Sailors, during offshore races
of several days or weeks, often fail to maintain energy balance due to their work on the deck,
changing and trimming the sails, the continuous need to counterbalance movements of the boat,
the watch system not allowing for a full night’s sleep or a normal frequency, and the order of
meals and activities (Branth et al. 1996). At high-altitude expeditions, it seems to be impossible to
maintain the energy balance above 5000–5500 m. Maintenance of energy balance determines the
success of these expeditions. Experienced negative energy balances are largely due to insufficient
energy intake (Westerterp et al. 1992, 1994, 1996b, 2000). Hypoxia induces a negative energy
balance by reduction of energy intake due to a more rapid increase in satiety and a decrease of
hunger, probably caused by higher hypoxia-induced ventilation and diet-induced thermogenesis
(Westerterp-Plantenga et al. 1999).
As evidenced previously, many of the advances in nutritional science have come from studies
in which dietary assessment was central to the study. It should be noted, however, that epidemio-
logic studies of diet provided only part of the scientific story. Sometimes, the first notion came
from the population dietary assessment data, which could be the last step in generalizing the
findings.
In the face of these shortcomings, experts still diverge in their opinions on dietary assessment
and its traditional tools. Some advocate that “Something is not better than nothing” (Dhurandhar
et al. 2015). Specifically with respect to the energy intake, they argue that “it is time to move
away from the use of self-reports of energy intake as a research tool. They base this on the
evidence that self-reports of energy intake are so poor that they are wholly unacceptable for
scientific research on energy balance and that researchers and sponsors should develop objective
measures of energy intake.”
Other researchers admit that accuracy of reported or recalled absolute intakes fails, yet they
believe that dietary patterns can be recognized, and thus, traditional dietary assessment should still
be employed. It is added, however, that even if dietary assessment is imprinted by some inherent
weaknesses, it should not be discredited and rejected for research purposes. Indeed, the information
should be used with caution, should not be overinterpreted, and would be advantageously used with
other supporting techniques. (Tremblay pers. comm. 2016). Many conclude that a multistep process
should be used to reinforce the outcome of a traditional dietary assessment. Biomarkers and sen-
sors are projected to add useful information that would compensate for shortcomings of traditional
dietary assessment.
major focus for dietary assessment studies. Some success has been made, but further progress will
require a wider perspective. Investigations have shown that not only food patterns but also the
complete lifestyle are related to health and well-being. Thus, habitual physical activity is promoted
along with regular timing of meals, activity, and sleep, and all are in line with the individual’s cir-
cadian rhythm (Westerterp-Plantenga 2016); but exactly what food and exercise and how much of
each remain controversial. To answer this, we need to learn to improve the accuracy and reliability
of dietary assessment, and then how to disentangle that from other confounding lifestyle factors.
Novel methods of dietary assessment are needed to augment the traditional dietary assessment
methods.
ACKNOWLEDGMENTS
We thank Drs. Edith Feskens, Wageningen University, Wageningen, the Netherlands; Barbara
Livingstone, Ulster University, Ulster, Ireland; Martijn Katan, Free University, Amsterdam,
the Netherlands; Ronald Mensink and Klaas Westerterp, Maastricht University, Maastricht, the
Netherlands; Angelo Tremblay, University of Laval, Quebec, Canada; Mikael Fogelholm, University
of Helsinki, Helsinki, Finland; Anne Raben, University of Copenhagen, Copenhagen, Denmark;
Nikhil Dhurandhar, Texas Tech University, Lubbock, Texas; Sally Poppit, University of Auckland,
Auckland, New Zealand; Jennie Brand-Miller, University of Sydney, Sydney, Australia; Margarita
Santiago Torrez, University of New Mexico, Albuquerque, New Mexico; Michele Mendez,
University of North Carolina, Chapel Hill, North Carolina; Jean Jacques, Tufts University, Medford,
Massachusetts; and Natalie M. Racine, University of Wisconsin-Madison, Wisconsin, for their valu-
able contributions.
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1 Benefits and Limitations
of Traditional Self-Report
Instruments
Hamid R. Farshchi, Ian Macdonald,
Ameneh Madjd, and Moira A. Taylor
CONTENTS
1.1 Introduction .............................................................................................................................. 1
1.2 Self-Reported Methods for Assessing Dietary Intake ..............................................................2
1.2.1 Food Records ................................................................................................................2
1.2.1.1 Benefits and Limitations of Food Records ....................................................3
1.2.2 24-hour Dietary Recall .................................................................................................5
1.2.2.1 Benefits and Limitations of 24-hour Dietary Recall ..................................... 5
1.2.3 Diet History .................................................................................................................. 6
1.2.3.1 Benefits and Limitations of Diet History .......................................................6
1.2.4 Food Frequency Questionnaire..................................................................................... 7
1.2.4.1 Benefits and Limitations of Food Frequency Questionnaire ......................... 8
1.3 Key Issues in Evaluating Dietary Intake Assessment Methods ............................................... 8
1.3.1 Misreporting of Foods and the Amounts Consumed ................................................... 9
1.3.2 Attempts to Quantify the Degree of Error in Dietary Intake Assessment ................... 9
1.3.3 Determinants of Underreporting Dietary Intake ........................................................ 10
1.3.3.1 Body Mass Index ......................................................................................... 10
1.3.3.2 Age and Sex ................................................................................................. 10
1.3.3.3 Socioeconomic Levels and Education ......................................................... 10
1.3.3.4 Eating Behaviors .......................................................................................... 11
1.3.3.5 Diet Variation ............................................................................................... 11
1.3.3.6 Appropriate Selection of Administration Techniques ................................. 11
1.4 Conclusions ............................................................................................................................. 12
References ........................................................................................................................................ 12
1.1 INTRODUCTION
Dietary intake is an important and potentially modifiable determinant of health. Associations, in
some cases demonstrated to be causal, have been reported between dietary intake and morbidity and
mortality, for example, relating to cardiovascular diseases (Mente et al. 2009), cancer (Schwingshackl
and Hoffmann 2015), diabetes (Khazrai et al. 2014), and obesity. Accurately assessing dietary intake,
including the pattern and quantity of food, drinks, and supplement consumption is a fundamentally
important element of nutrition and health research, across the spectrum of surveillance, epidemio-
logical, and interventional studies. It is equally important in clinical practice, to be able to accu-
rately establish an individual’s current dietary intake, whether prior to or after giving dietary advice.
Having confidence in the techniques used to assess dietary intake is essential if existing research
outcomes are to be considered valid, and in order to justify funding for further techniques.
1
2 Advances in the Assessment of Dietary Intake
However, dietary intake assessment is not without challenges (Thompson et al. 2015b). Some
caution that traditional techniques may provide incorrect data that may result in misguided health
care policies, future research, and clinical judgment (Dhurandhar et al. 2015). Comparisons
between self-reported intake and estimated energy expenditure measured using doubly-labeled
water (DLW) have shown individual differences ranging from +25% to −76% (Schoeller et al.
1990), which assuming stable body weight, raises questions about their accuracy. It is thus essen-
tial that traditional methods are critically reviewed in order to inform whether there is justification
for their continued use, or to identify priority areas for investing in the development of alternative
techniques.
Dietary intake is a chronic and multidimensional phenomenon that may vary over time in rela-
tion to age, life stage, environment, and many other factors (Thompson et al. 2015b). Assessment
methods are potentially required to establish nutrient intake, food choices, or broader patterns of
eating, hence are attempting to measure what, when, how much, and how often foods and drinks are
consumed. Further steps may then need to be taken to establish, for example, an estimate of nutri-
ents using a food composition database. Food composition tables have many inherent limitations,
for example, some foods may not be included, or the composition of the foods analyzed may differ
from the foods consumed (Chapter 19) (Cantwell et al. 2006).
Many different methods have been developed for assessing dietary intake that vary with respect
to cost and the burden placed on the researcher and respondent. Nutritional biomarkers of intake
have been proposed but are not without limitations, such as weak associations with intake, and
only providing information about one dietary component. (Thompson et al. 2010; Freedman 2011)
(Chapters 15, 16, and 18). Nutrition researchers and practitioners thus may choose to rely on more
traditional, self-reported measures. This chapter describes traditional methods for self-reported
dietary intake assessment, considers benefits and limitations, and focuses on key issues in evaluat-
ing traditional dietary intake assessment methods.
confounding. Successive days may not be independent of each other, for example, if left-over foods
are used, or if a day of high consumption is followed by a day of lower consumption. Nonsuccessive
days may provide a more representative view of typical consumption patterns.
To complete a dietary record, each respondent must be trained in the level of detail required
in order to adequately describe the foods and amounts consumed, including the name of the food
(brand name, if possible), preparation and cooking methods, recipes for home prepared foods,
and portion sizes. This places a considerable burden on the respondent. Dietary records may be
recorded by someone else, such as parents reporting for their children, or staff in a residential care
home providing that they are able to witness when food or drink is consumed.
Dietary records are usually collected using an unstructured diary. For example, there should not be
sections for different meals, as this potentially communicates to the respondent that they should have
such a meal pattern, which may introduce bias. However, some diaries are more structured (Schoeller
et al. 1990; Black et al. 1997; Cantwell et al. 2006; Thompson et al. 2010). These forms contain
checklists consisting of food groups, which the respondent reports on whether he or she consumed
foods from a particular food group. The design of these checklists is similar to FFQs, but the time
of the food intake report consumed is different between these two methods. In FFQ (described in a
later section), subjects are asked about intake over a definite time period like the past year or month,
while checklists should be completed at the time of intake or at the end of a day. A checklist may be
designed to evaluate specific main foods that contribute markedly to consumptions of some nutrients
(Kolar et al. 2005), and also to track food contaminants (Rebro et al. 1998). A high level of motivation
is needed in the respondents, or those who complete the record on their behalf (Willett 1998).
Some protocols insist that the food record should be reviewed by a dietitian or other trained inter-
viewer after one day of recording, and again once the record has been completed. The purpose is to
prompt the recall of foods that may have been omitted (e.g., confectionery), clarify the interpretation of
portion sizes, and add details such as the type of fat used, and amount of salt and sugar added at the point
of consumption (Cantwell et al. 2006). Other protocols may not require this step (Kolar et al. 2005). The
foods and drinks in the food record may then be matched to foods in a food composition database that are
usually accessed with the assistance of computer software, and the program is used to derive variables
such as the mean daily intakes by weight of a micronutrient, or percentage of total energy for a particular
macronutrient. Data entry is time consuming, and it may be necessary to add foods to the database, hav-
ing obtained information about composition from packets or direct from the manufacturer.
are needed to establish habitual intake (Bingham 1987). The number of days required depends
on frequency of food consumed, and will be more important in some cases than others. Liver, for
example, while infrequently consumed in the United Kingdom, is a rich source of iron, a mineral
that can be stored. Insufficient days of recording that do not capture the consumption of this particu-
lar food, might erroneously lead to the conclusion that an individual’s iron intake was inadequate.
However, incomplete records increase significantly as more days of records are kept, and the validity
of the collected information declines in the later days of a seven-day recording period, in contrast to
collected information in the earlier days (Gersovitz et al. 1978).
Food records are unsuitable for individuals who are unable to read and write in the language
selected for the assessment. Although translation may be an option, where basic literacy levels are
low, issues remain. Respondents must be cooperative and motivated for this method to have validity
as there is a large respondent burden (see summary in Table 1.1).
TABLE 1.1
Summary of Benefits and Limitations of Traditional Self-Report Instruments for Dietary
Intake
Benefits Limitations
Food records • Can provide typical meal and food • Can alter eating behaviors
pattern information • May influence on both the food
• Recorded at the time of eating with no type and eaten amount
reliance on memory providing reliable • Requires multiple records to
data intake capture habitual intake
• Intake is quantified • High subject burden
• Recordings made away from home suit • High staff cost and burden
for people with irregular lifestyle habits • Requires literate and motivated
• Allows self-monitoring that can population
influence behavior change
24-hour dietary recall • Intake is quantified • Less accurate measurements of
• Less subject burden portion size
• Does not alter eating behaviors • Relies on subject recall
• Does not require literate population for • High staff cost and burden
interviewer provided version • Requires multiple recalls over
several months to capture
habitual intake
Diet history • Evaluate meal patterns and details of • Rely on subject memory
food intake • May overreport good foods and
• Catch details of the methods of food underreport intake of bad foods
preparation • Quantify the relative amount
• Does not require literacy and not the absolute intake
• Less subject burden • Not suitable for people with
irregular meal pattern
• High staff cost and burden
Food frequency • Less subject burden • Relies on subject recall
questionnaires • Less staff cost and time burden • Not as quantifiably precise
• Does not alter eating behaviors • Requires literate population
• Captures habitual intake • Does not provide meal pattern
• Can be shorter and emphasis on foods information
rich in a specific nutrient or a specific • Bias with overestimation
group of foods, for example, fruits and consumption of good foods or
vegetables underestimation of bad foods
Benefits and Limitations of Traditional Self-Report Instruments 5
literacy can be a limitation. The immediacy of the recall period facilitates recall of foods and drinks;
however, the method does rely on memory that may challenge young children and the elderly. The
burden on the respondent is minimal, so the 24-hour recall method is useful across a wide range
of populations. The 24HR is frequently used in national surveys (Kweon et al. 2014), randomized
clinical trials, and cohort studies (Dauchet et al. 2007; Luke et al. 2011).
Furthermore, in contrast to the food record method, dietary recalls occur after the food has been
consumed, so there is likely to be less impact on dietary habits. Finally, 24HR can be conducted by
telephone or a web-based automated self-administered method (Thompson et al. 2015a) with mini-
mal differences in comparison with interviewer-administered recalls.
However, on the other hand, potential limitations of the 24-hour recall method include inaccura-
cies in the assessment of portion size and individual food intake for a wide range of reasons relating
to knowledge, memory, and the interview conditions. In addition, as a single observation provides
a poor measure of individual intake, so multiple days of recalls may be needed. Although a single
24-hour recall can be used to describe the average dietary intake of a population, multiple recalls
can improve precision (Blanton et al. 2006). Multiple days of recall inevitably increase cost and the
burden placed on the respondent (see summary in Table 1.1).
However, respondents are asked to make many judgments about both the usual foods and the
amounts of those foods consumed. So, respondents may overreport good foods and underreport
intake of bad foods according to their perceptions. In addition, these subjective tasks may be dif-
ficult for many respondents. Burke cautioned that nutrient intakes estimated from these data should
be interpreted as relative rather than absolute. The meal-based approach is not useful for individu-
als who have no particular eating pattern and may be of limited use for individuals who graze (i.e.,
eat throughout the day rather than at defined mealtimes) or shift workers who have varied meal
patterns.
A further limitation of this method is reliance on the memory of the respondent that may result
in recall bias. This may be a particular issue for older individuals who may become fatigued and
unable to complete the interview in one session; a typical session lasts 60–90 minutes. All of these
limitations are also shared with the food frequency method.
Given the need for a trained interviewer, the approach tends to be expensive and vulnerable to
inconsistency in the exact method used. Poor standardization has resulted in difficulties in repro-
ducing studies, and in comparing between studies (see summary in Table 1.1).
Finally, it is important to consider how missing data will be treated, especially in self-administered
questionnaires. Zero values may be entered; having made the assumption that failure to answer
questions relates to foods that respondents rarely or never consume (Rimm et al. 1992). Imputation
of frequency values for unanswered questions is the other solution for this issue (Parr et al. 2008).
However, it is now unclear whether imputation improves FFQ analyses (Fraser et al. 2009).
As a tool designed to obtain the habitual dietary intake, FFQs have been used commonly in epi-
demiological studies evaluating relations between diet and disease. In this case the aim may be to
rank the intake of respondents relative to others, or as quantiles, as opposed to determining absolute
intake. Two well-known FFQs (Willett et al. 1985; Block et al. 1986) with some adaptations have
been used in many national studies (Lamb et al. 2007; Barclay et al. 2008).
Ethylene
It was known from the work of certain French chemists that in the
presence of such a catalyst as kaolin, ethyl alcohol is dehydrated at an
elevated temperature to ethylene. The process as finally developed by
American chemists consisted essentially in introducing mixtures of
alcohol vapor and steam, in the ratio of one to one by weight, into an
8-inch iron tube with a 3-inch core, in contact with clay at 500-600° C.
The use of steam rendered the temperature control more uniform and
thus each unit had a greater capacity of a higher grade product. The
gaseous products were removed through a water-cooled surface
condenser. One unit of this type had a demonstrated capacity of 400
cubic feet per hour of ethylene, between 92 and 95 per cent pure,
while the conversion efficiency (alcohol to ethylene) was about 85 per
cent. The Edgewood plant consisted of 40 such units. This would have
yielded sufficient ethylene to make 40 tons of mustard gas per 24-hour
day.
The English procedure consisted in the use of phosphoric acid,
absorbed onto coke. An American furnace was designed and built
which gave 2,000 cubic feet per hour of ethylene, with a purity of 98 to
99 per cent. This furnace was not used on a large scale, because of
the satisfactory nature of the kaolin furnaces.
Fig. 30.—Experimental Installation for the Production
of Ethylene by Kaolin Procedure.
Capacity 400-600 cu. ft. Ethylene per hr.
Sulfur Chloride
Since chlorine was prepared at Edgewood, it was logical that some
of this chlorine should be utilized in the preparation of sulfur chloride.
The plant constructed consisted of 30 tanks (78 inches in diameter
and 35 feet long), each capable of producing 20,000 pounds of
monochloride per day. The tanks are partially filled with sulfur and
chlorine passed in. The reaction proceeds rapidly with sufficient heat
to keep the sulfur in a molten condition. If the chlorine is passed in too
rapidly, the heat generated may be sufficient to boil off the sulfur
chloride formed. Hence water pipes are provided so that a supply of
cold water may be sprayed upon the tanks, keeping the temperature
within the proper limits.
Fig. 31.—Row of Furnaces for the Preparation of
Ethylene.
“Preparation of Dihydroxyethylsulfide—To
prepare the hydroxysulfide, the theoretical quantity of
sodium sulfide, either in the form of the anhydrous
salt or as crystals, was added to the 18 to 20 per cent
solution of chlorhydrin. After the addition of the
sulfide, the mixture was heated to about 90° to 100°.
It was then pumped to an evaporator, and heated
until all the water was driven off. The glycol was next
filtered from the salt which separated, and distilled in
a vacuum. The yield of glycol was about 90 per cent
of the theoretical, calculated from the chlorhydrin.
“Preparation of Dichlorethylsulfide—The
thiodiglycol was taken from the rail to two large
storage tanks and thence drawn by vacuum direct to
the reaction vessel. Each reaction vessel was placed
in a separate cubicle ventilated both from above and
below and fitted with glass windows for inspection.
The vessels themselves were made of 1¼ in. cast
iron and lined with 10 mm. lead. They were 2.5 m.
high and 2.8 m. in diameter. These tanks were
jacketed so that they could be heated by water and
steam, and the reaction was carried out at 50°. The
hydrochloric acid coming from the main pipe was
passed through sulfuric acid so that the rate could be
observed, and passed in by means of 12 glass tubes
of about 2 cm. diameter. The rate of flow was
maintained at as high a rate as possible to procure
absorption. The vapors from the reaction were led
from the vessel through a pipe into a collecting room,
and then through a scrubber containing charcoal and
water, through a separator, and then, finally, into the
chimney. These exhaust gases were drawn off by
means of a fan which was also connected with the
lower part of the chamber in which the reaction
vessels were set, so that all the gases had to pass
through the scrubber before going to the chimney.
When the reaction was completed, the oil was
removed by means of a vacuum, induced by a water
pump, into a cast iron washing vessel.
“The hydrochloric acid layer was removed to a
stoneware receiver, also by vacuum. A glass enabled
the operator to avoid drawing oil over with the acid.
The pan was fitted with a thermometer to the interior
as well as to the jacket. For testing the material
during reaction, provision was made for drawing
some up by vacuum to a hydrometer contained in a
glass funnel. The final test at this point read 126° Tw.
Another portion could be drawn up to a test glass and
hydrochloric acid passed through it in full view. A float
contained in a glass outer tube served to show the
level of the liquid in the vessel. The pans in which the
operation is carried on, as well as those employed for
washing and distilling the product, were of a standard
pattern employed in many other operations in the
works.
“The washer consisted of a cast iron vessel, lead
lined, and was 2.5 m. in diameter, 2 m. deep, and
fitted with a dome cover and stirring gear. Lead pipes
served for the introduction of sodium carbonate
solution and water. Similar pipes were fitted for
drawing these off by means of a vacuum. A manhole
on the cover, with a flat top, was fitted with light and
sight glasses to which were fitted a small steam coil
for keeping them clear. The washed oil is drawn off to
a distillation still, which is a cast iron vessel
homogeneously lead coated, 1.5 m. in diameter and
2 m. deep, fitted with a lead heating coil and
connected through a spiral lead condenser and
receiver to a vacuum pump. The water is distilled
from the oil at a pressure of from 62 to 70 mm.
absolute pressure. When dried, the oil is sent by
vacuum to a mixing vessel, similar in most respects
to the washing vessel, in which it is mixed with an
appointed quantity of solvent, which, in this factory,
was usually chlorobenzene but occasionally carbon
tetrachloride. The relative quantities varied with the
time of year, and instructions were sent from Berlin
on this point. Thence the mixture was passed to a
storage tank and into tank-wagons.”
Properties
Dichloroethylsulfide (mustard gas) is a colorless, oily liquid, which
has a faint mustard odor. The pure material is said to have an odor
very suggestive of that of water cress. While the odor is more or less
characteristic, it is possible to have extremely dangerous amounts of
the gas in a neighborhood without being detected through its odors. It
still seems to be an open question whether mustard gas paralyzes the
sense of smell. One can find opinions on both sides.
Mustard gas boils at 215°-217° C. at atmospheric pressure, so that
it is at once seen to be a very persistent gas. It distills without
decomposition at this temperature but is best purified by vacuum
distillation, or by distillation with steam. A still for the vacuum
distillation of mustard gas has been described by Streeter.[20]
Mustard gas melts, when pure, at 13° to 14° C. (The ordinary
summer temperature is 20°-25° C.). The ordinary product, as obtained
from the “reactor,” melts from 9°-10° C. In order that the product in the
shell might be liquid at all temperatures, winter as well as summer, the
Germans added from 10 to 30 per cent of chlorobenzene, later using a
mixture of chlorobenzene and nitrobenzene and still later pure
nitrobenzene. Carbon tetrachloride has also been used as a means of
lowering the melting point. Many other mixtures, such as chloropicrin,
hydrocyanic acid, bromoacetone, etc., were tested, but were not used.
The effect on the melting point of mustard gas is shown in the
following table:
Chemical Properties
Mustard gas is very slowly decomposed by water, owing to its very
slight solubility. The products are dihydroxyethylsulfide and
hydrochloric acid:
Detection
At first the only method of detecting mustard gas was through the
sense of smell. It was then believed that concentrations which could
not be detected in this way were harmless. Later this proved not to be
the case, and more delicate methods had to be devised. In the
laboratory and in the field these tests were not very satisfactory,
because most of them depended upon the presence of chlorine, and
the majority of the war gases contained chlorine or one of the other
halogens. The Lantern Test depended upon the accumulation of the
halogen upon a copper gauze and the subsequent heating of the
gauze in a Bunsen flame. This test could be made to detect one part
of mustard gas in ten million parts of air. Another field detector devised
by the Chemical Warfare Service consisted in the use of selenious
acid. Here again the lack of specificity is apparent, for while certain
halogen compounds did not give the test, arsine and organic
arsenicals gave a positive reaction and often in a shorter time than
mustard gas.
The Germans are said to have had plates covered with a yellow
composition which had the property of turning black in the presence of
mustard gas. These plates were lowered into the bottom of recently
captured trenches and if, after a few minutes, they turned black, the
presence of mustard gas was suspected. It is also stated that the
characteristic yellow paint on the olive of the mustard gas shell had
the same composition, and was useful in detecting leaky shell.
According to a deserter’s statement, however, reliance upon this test
resulted in casualties in several instances.
A white paint has also been reported which turned red in the
presence of mustard gas. This color change was not characteristic, for
tests made by our Army showed that other oils (aniline, turpentine,
linseed) were found to produce the same effect.
The Chemical Warfare Service was able to develop an enamel and
an oil paint which were very sensitive detectors of mustard gas. Both
of these were yellow and became dark red in contact with mustard
gas. The change was practically instantaneous. The enamel consisted
of chrome yellow as pigment mixed with oil scarlet and another dye,
and a lacquer vehicle, which is essentially a solution of nitrocellulose
in amyl acetate. One gallon of this enamel will cover 946,500 sq. cm.,
or a surface equivalent to a band 3 cm. wide on 12,500 seven cm.
shell.
The paint was composed of a mixture of 50 per cent raw linseed oil
and 50 per cent Japan drier, with the above dye mixture added to the
required consistency. In contact with liquid mustard gas, this changes
to a deep crimson in 4 seconds. Furthermore, in contact with
arsenicals, this paint changes to a color varying from deep purple to
dark green, the color change being almost instantaneous and very
sensitive, even to the vapors of these compounds. Other substances
have no effect upon the paint.
For field work, however, nothing was found equal to the trained
nose, and it is questionable if any of the mechanical means described
will be used in the field.
Physiological Action
One of the most interesting phases of mustard gas is its peculiar
physiological action. This has been studied extensively, both as relates
to the toxicity and to the skin or blistering effect.
Toxicity
When one considers the high boiling point of mustard gas, and its
consequent low vapor pressure, he is likely to conclude that such a
substance would be of comparatively little value as a toxic or poison
gas. While it is true that an important part of the military value of
mustard gas has been because of its vesicant properties, the fact still
remains that it is one of our most toxic war gases. The following
comparison with a few of the other gases indicates this:
Mg. per Liter
Mice Dogs
Mustard gas 0.2 0.05
Phosgene 0.3 ···
Hydrocyanic acid 0.2 0.1
Chloropicrin 1.5 0.8
··· 3.0
When an animal is exposed to the vapors of mustard gas in high
concentration, it subsequently shows a complexity of symptoms, which
may be divided into two classes:
(1) The local effects on the eyes, skin and respiratory tract. These
are well recognized and consist mainly of conjunctivitis and superficial
necrosis of the cornea; hyperemia, œdema and later, necrosis of the
skin, leading to a skin lesion of great chronicity; and congestion and
necrosis of the epithelial lining of the trachea and bronchi.
(2) The systemic effects due to the absorption of the substance into
the blood stream, and its distribution to the various tissues of the body.
The most striking observation about the symptoms of mustard gas
poisoning is the latent period which elapses after exposure before any
serious objective or subjective effects are noted. The developments of
the effects are then quite slow, unless very high superlethal doses
have been inhaled.
At first it was a very serious question whether or not the temporary
blindness resulting from mustard gas would not be permanent. Later,
as the depth and seriousness of some of the body burns became well
known, it was a seven-day wonder that no permanent blindness
occurred.
The reason seems to be largely a mechanical one. The constant
winking of the eyelids apparently washes the mustard gas off the
eyeball and carries it away so that not enough remains to burn to the
depth necessary to cause permanent blindness.
Due to the very slight concentrations ordinarily encountered in the
field, resulting from a very slow rate of evaporation, the death rate is
very low, probably under 1 per cent among the Americans gassed with
mustard during the war.
If, on the other hand, the gas be widely and very finely dispersed
by a heavy charge of explosive in the shell, the gas is very deadly. In
such cases the injured breathe in minute particles of the liquid and
thus get hundreds of times the amount of gas that would be inhaled as
vapor. This so-called “high explosive mustard gas shell” was a
German development in the very last months of the war. Its effects
were great enough to make it certain that in the future large numbers
of these shell will be used.
The similarity of the symptoms and pathological effects after the
inhalation of large amounts of the vapor and those following an
injection of an olive oil or water solution of mustard gas led Marshall
and his associates to conclude that in high concentrations mustard
gas is absorbed through the lungs. A further bit of evidence consists in
the isolation of the hydrolysis product, dihydroxyethylsulfide, in the
urine of animals poisoned by inhalation of mustard gas. This product is
not toxic and is not responsible for the effects of mustard gas.
Hydrochloric acid, however, does produce very definite effects upon
the animal and may cause death.
From these facts Marshall[21] has proposed the following
mechanism of the action of mustard gas:
“Dichlorethylsulphide is very slightly soluble in
water and very freely soluble in organic solvents, or
has a high lipoid solubility or partition coefficient. It
would, therefore, be expected to penetrate cells very
readily. Its rapid powers of penetration are practically
proven by its effects upon the skin. Having
penetrated within the living cell, it would undoubtedly
hydrolyze. The liberation of free hydrochloric acid
within the cell would produce serious effects and
might account for the actions of dichlorethylsulphide.
To summarize, then, the mechanism of the action of
dichlorethylsulphide appears to be as follows: