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Analytical Assessment of E-Cigarettes. From Contents To Chemical and Particle Exposure Profiles Konstantinos E. Farsalinos
Analytical Assessment of E-Cigarettes. From Contents To Chemical and Particle Exposure Profiles Konstantinos E. Farsalinos
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Analytical Assessment of e-Cigarettes
Emerging Issues in Analytical Chemistry
Series Editor
Brian F. Thomas
Konstantinos E. Farsalinos
Onassis Cardiac Surgery Center, Athens, Greece and University of Patras,
Patras, Greece
I. Gene Gillman
Enthalpy Analytical, Inc., Durham, NC, United States
Stephen S. Hecht
University of Minnesota, Minneapolis, MN, United States
Riccardo Polosa
University of Catania, Catania, Italy
Jonathan Thornburg
RTI International, Research Triangle Park, NC, United States
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material herein.
ISBN: 978-0-12-811241-0
N.L. Benowitz
University of Calilfornia, San Francisco, San Francisco, CA,
United States
K.E. Farsalinos
Onassis Cardiac Surgery Center, Athens, Greece and University of Patras,
Patras, Greece
I. Gene Gillman
Enthalpy Analytical, Inc., Durham, NC, United States
S.S. Hecht
University of Minnesota, Minneapolis, MN, United States
R. Polosa
University of Catania, Catania, Italy
J. Thornburg
RTI International, Research Triangle Park, NC, United States
FOREWORD
N.L. Benowitz
Professor of Medicine and Bioengineering & Therapeutic Sciences
Chief, Division of Clinical Pharmacology
University of California, San Francisco
San Francisco, CA, United States
October 2016
CHAPTER 1
Introduction to e-Cigarettes
K.E. Farsalinos
INTRODUCTION
e-Cigarettes were recently invented and developed as an alternative-to-
smoking method of nicotine intake. They are electronic devices with
three main parts: a battery, an atomizer composed of a wick and metal
coil, and a liquid (“e-liquid”) stored inside the atomizer. The function
is to aerosolize the liquid, producing a visible aerosol which the user
inhales. This is achieved by heating the metal coil inside the atomizer
by an electrical current from the battery. e-Cigarettes are commonly
called electronic nicotine-delivery devices (ENDS). However, because
they can be used with non-nicotine e-liquids, the term ENDS is inaccu-
rate and does not represent the whole spectrum of e-Cigarette devices
and use patterns.
Figure 1.1 Types of e-Cigarettes. First generation: (A) disposable cigalike; (B) rechargeable cigalike and
replacement prefilled cartomizers. Second generation: (C) eGo-type battery; (D) tank-type atomizers; (E) tank-
type atomizer with replacement coil and wick head. Third generation: (F) box-shape variable-wattage battery
device; (G) tank-type atomizer with replacement head; (H) rebuildable atomizer.
Introduction to e-Cigarettes 3
RESEARCH ON e-CIGARETTES
Intense research on all aspects related to e-Cigarettes, including
chemistry, toxicology, clinical effects, and population effects, is ongoing.
6 Analytical Assessment of e-Cigarettes
REFERENCES
1. United States Patent Application Publication. Electronic atomization cigarette. Publication
No: US 2007/0267031 A1; November 22, 2007.
2. United States Patent Office. Electric vaporizer. Publication No: 1,775,947; September 16, 1930.
3. United States Patent Office. Therapeutic apparatus. Publication No: 1,968,509; July 31, 1934.
4. United States Patent Office. Vaporizing unit for therapeutic apparatus. Publication No:
2,057,353; October 13, 1936.
Introduction to e-Cigarettes 7
5. United States Patent Office. Smokeless non-tobacco cigarette. Publication No: 3,200,819;
August 17, 1965.
6. Farsalinos KE, Polosa R. Safety evaluation and risk assessment of electronic cigarettes as
tobacco cigarette substitutes: a systematic review. Ther Adv Drug Saf 2014;5:67 86.
7. Farsalinos KE, Yannovits N, Sarri T, Voudris V, Poulas K. Protocol proposal for, and eval-
uation of, consistency in nicotine delivery from the liquid to the aerosol of electronic cigar-
ettes atomizers: regulatory implications. Addiction 2016;111:1069 76.
8. Nides MA, Leischow SJ, Bhatter M, Simmons M. Nicotine blood levels and short-term smok-
ing reduction with an electronic nicotine delivery system. Am J Health Behav 2014;38:265 74.
9. Farsalinos KE, Spyrou A, Tsimopoulou K, Stefopoulos C, Romagna G, Voudris V.
Nicotine absorption from electronic cigarette use: comparison between first and new-
generation devices. Sci Rep 2014;4:4133.
10. Dawkins L, Turner J, Roberts A, Soar K. Vaping” profiles and preferences: an online survey
of electronic cigarette users. Addiction 2013;108:1115 25.
11. Etter JF. Throat hit in users of the electronic cigarette: an exploratory study. Psychol Addict
Behav 2016;30:93 100.
12. Farsalinos KE, Romagna G, Tsiapras D, Kyrzopoulos S, Voudris V. Characteristics, per-
ceived side effects and benefits of electronic cigarette use: a worldwide survey of more than
19,000 consumers. Int J Environ Res Public Health 2014;11:4356 73.
13. Lopez AA, Hiler MM, Soule EK, Ramôa CP, Karaoghlanian NV, Lipato T, et al. Effects of
electronic cigarette liquid nicotine concentration on plasma nicotine and puff topography in
tobacco cigarette smokers: a preliminary report. Nicotine Tob Res 2016;18:720 3.
14. Farsalinos KE, Voudris V, Poulas K. Are metals emitted from electronic cigarettes a reason
for health concern? A risk-assessment analysis of currently available literature. Int J Environ
Res Public Health 2015;12:5215 32.
15. Zhu SH, Sun JY, Bonnevie E, Cummins SE, Gamst A, Yin L, et al. Four hundred and sixty
brands of e-cigarettes and counting: implications for product regulation. Tob Control 2014;23
(Suppl. 3):iii3 9.
16. Marshall BDL, Wood E. Toward a comprehensive approach to HIV prevention for people
who use drugs. J Acquir Immune Defic Syndr 2010;55(Suppl 1):S23 26.
17. Beyrer C, Malinowska-Sempruch K, Kamarulzaman A, Kazatchkine M, Sidibe M,
Strathdee SA. Time to act: a call for comprehensive responses to HIV in people who use
drugs. Lancet 2010;376:551 63.
18. World Health Organization, United Nations Office on Drugs and Crime, Joint United Nations
Program on HIV/AIDS. HO, UNODC, UNAIDS technical guide for countries to set targets for
universal access to HIV prevention, treatment and care for injecting drug users: 2012 revision.
19. Harm Reduction International. Global state of harm reduction 2014. Available from: https://
www.hri.global/contents/1524.
20. Wilson DP, Donald B, Shattock AJ, Wilson D, Fraser-Hurt N. The cost-effectiveness of
harm reduction. Int J Drug Policy 2015;26(Suppl. 1):S5 11.
21. Russell MA. Low-tar medium-nicotine cigarettes: a new approach to safer smoking. Br Med J
1976;1:1430 3.
22. Luo J, Ye W, Zendehdel K, Adami J, Adami HO, Boffetta P, et al. Oral use of Swedish
moist snuff (snus) and risk for cancer of the mouth, lung, and pancreas in male construction
workers: a retrospective cohort study. Lancet 2007;369:2015 20.
23. Lee PN, Hamling J. Systematic review of the relation between smokeless tobacco and cancer
in Europe and North America. BMC Med 2009;7:36.
8 Analytical Assessment of e-Cigarettes
I. Gene Gillman
INTRODUCTION
In the preparation of this chapter, the author read approximately 150
peer-reviewed publications and a large number of recent conference
proceedings. Two things became apparent: (1) electronic nicotine deliv-
ery systems (ENDS) are evolving rapidly as manufacturers innovate,
and the peer-reviewed literature does not adequately reflect products
on the market. (2) Published findings of analytical testing and analysis
of ENDS tend to show thermal decomposition products at either very
low or very high levels, with little agreement in the middle. To address
the first issue, recent conference proceedings are cited to fill gaps in the
literature. The second issue is addressed only when required to high-
light differences in testing methodologies. The objective is primarily to
explain the results and implications of ENDS aerosol testing.
Definitive advice on the choice and appropriateness of particular test
methods must await further developments.
All current ENDS deliver nicotine in the form of a heated aerosol
commonly comprised of propylene glycol (PG), glycerin (GLY), water,
and flavoring. The modern ENDS arose from a 2003 invention by
Chinese pharmacist Lik Hon,1 but the concept of delivering nicotine in
a heated PG or GLY aerosol has been around since at least 1960.2
Technical challenges, including battery technology, delayed commer-
cialization until the 21st century. ENDS are increasingly popular, with
millions of users in the United States and Europe,35 and are often a
replacement for combustible cigarettes.6 The aerosol is called a vapor,
and usage is called vaping. This is inaccurate, because “vapor” refers
to a gaseous state, while the aerosol from ENDS is a complex suspen-
sion of fine particles, not pure gas phase vapor compounds. The
ENDS aerosol is a complex mixture containing semiliquid particulate
matter along with gas phase compounds. Unlike combustible cigarette
Analytical Assessment of e-Cigarettes. DOI: http://dx.doi.org/10.1016/B978-0-12-811241-0.00002-4
Copyright © 2017 Elsevier Inc. All rights reserved.
10 Analytical Assessment of e-Cigarettes
A cigalike operates when the user draws air through it, which triggers
an airflow sensor and activates a battery that powers an atomizer to
produce an aerosol from liquid in the cartomizer (Fig. 2.1). Advanced
devices function in much the same way except that power is applied to
the atomizer coil only when a button is depressed by the user.
Analytical Testing of e-Cigarette Aerosol 11
Figure 2.2 Diagram of cartomizer used in cigalike ENDS. (1) Battery connecter, (2 and 3) nonresistance wires,
(4) resistance heating wire, (5) liquid reservoir with absorbent material, (6) aerosol exit, and (7) mouth end.
The power supply unit and tank-based atomizer are available from
many suppliers and are usually interchangeable, allowing the user to
select different vendors for the two components. Fig. 2.3 is a diagram
of a rechargeable, variable power, temperature-controlled power
supply unit.
One type of refillable tank-based atomizer is the clearomizer. It
is usually cylindrical in shape with a clear plastic or glass tank and a
separate wick, usually silica, that transfers the liquid from the tank to
the heating coil. A clear tank allows the user to see the level of liquid.
The wick may be placed at either the top or bottom of the tank
(Fig. 2.4, Tanks A and B). Top coil tanks require longer wicks and
thus have poor liquid-wicking rates, are more prone to dry puffing,
and are limited in the maximum power that can be applied.
Figure 2.3 Diagram of a rechargeable, variable power, temperature-controlled ENDS power supply unit.
Figure 2.4 Examples of two top coil clearomizers (Tanks A and B) and a bottom coil cartomizer (Tank C).
Wicking material (not shown) extends into the atomizer.
Variable wattage devices can put out consistent vapor even if the
resistance of the heating coil changes. Temperature-limiting and
temperature-controlled ENDS use heating wires that undergo signifi-
cant, repeatable changes in resistance when the temperature changes.
Typical materials are pure nickel, pure titanium, and stainless steel.
The resistance of the wire is an intrinsic property that varies only with
temperature, so there is no time lag as happens with an external sensor.
A resistance-based temperature-controlled device can react to changes
in temperature as fast as the controller can sample the resistance of the
coil, often hundreds or thousands of times per second. The measured
resistance of the atomizer coil can be used to determine coil tempera-
ture, as shown in Fig. 2.5, using the mathematical formula
Rmeasured 5 Rref ½1 1 αðTactual 2 Tref Þ, where Rref and Tref are the resis-
tance of the conductor material at a reference temperature, usually
20 C, and α is the temperature coefficient of resistance for the conduc-
tor. As of 2016, it is estimated that half of all new large ENDS have
some form of temperature control or temperature limiting. However,
because of the increased technical sophistication that current imple-
mentations require of the user and the relative scarcity of temperature
sensing consumables and atomizers, fewer than 20% of devices that are
NICOTINE IN LIQUIDS
Almost all ENDS deliver nicotine. Unlike in tobacco products that
include the whole leaf, the amount of added nicotine via ENDS is con-
trolled by the producer of the liquid. Nicotine content is communi-
cated to the consumer in several ways. Prefilled devices may list total
nicotine amount or the nicotine concentration of the liquid in units of
mg/mL, mg/gram, or percent nicotine by weight. Refill liquids typically
list mg/mL or percent nicotine by volume. The yield of aerosol among
ENDS varies from less than 2 mg/puff to over 40 mg/puff, depending
on the type of device and power level. Nicotine in commercial liquids
and prefilled devices varies from 3 mg/mL on the low end to 50 mg/mL
on the very high end. Three to 6 mg/mL nicotine-containing liquids are
commonly used in highest yielding ENDS and 2550 mg/mL in lower
yielding prefilled cigalikes. By matching nicotine liquid content to
device yield, consumers are exposed to a narrower range of nicotine
Analytical Testing of e-Cigarette Aerosol 17
amount per puff than might be obvious from the range of nicotine
content available on the market. Use of a 50 mg/mL liquid would be
very unpleasant in a high-yielding fourth-generation ENDS but
acceptable in a cigalike. However, the level listed on the labels of ciga-
like cartridges and refill solutions is often significantly different from
measured values.1120 The Salt Lake County Health Department21
recently tested the amount of nicotine in 153 liquid samples from local
retail shops and reported that 61% differed by at least 10% from the
labeled content, with discrepancies that ranged from 88% less to 840%
more than stated. Of the 33 samples that listed the nicotine amount as
zero, 1 contained 7.35 mg/mL. Given the number of reports that have
found that nicotine content in the refill liquids or prefilled devices does
not match the labeled amounts, it appears that a large percentage of
commercial products are not accurately labeled. Table 2.2 summarizes
historical nicotine test results for refill solutions; there appears to be
little improvement over time in the accuracy of labeling.
the nicotine and ethylene glycol (EG) and diethylene glycol (DEG)
from the PG or GLY; (3) thermal decomposition products formed dur-
ing the heating of the liquid and subsequent formation of the aerosol,
including aldehydes and volatile organic compounds (VOCs), and
(4) leachable materials that transfer from the device or tank into the
liquid. These contaminants may include a range of materials such as
plasticizers and metals.35 While there have been few systematic studies
on the transfer of compounds from the liquid into the aerosol and even
fewer that determine a wide range of HPHCs in both the liquid and
the aerosol, it stands to reason that compounds with physical proper-
ties similar to nicotine, PG, or GLY will transfer from the liquid into
the aerosol. Further, several compounds that are unlikely to form as
the result of thermal decomposition have been found in some aerosol
samples—e.g., polyaromatic compounds (PAHs) in tobacco-flavored
liquids.36,37 PAHs are products of combustion38 and are only formed
at temperatures unlikely to be obtained in ENDS;39 if they are found
in ENDS aerosols they should be treated as contaminants that trans-
ferred from the ingredients present in the liquid, not as compounds
that formed during the production of the aerosol.
CONTAMINANTS IN LIQUIDS
When the liquid is heated, it and compounds contained in it will be
transferred into the aerosol. Compounds with boiling points similar to
PG and GLY are thought to transfer in a nearly quantitative man-
ner,40 while compounds with significantly higher boiling points will
likely transfer at lower rates. Little is known about the transfer effi-
ciency of many compounds, but unpublished data from our laboratory
show that polar compounds like caffeine do not transfer efficiently.
Table 2.3 is a summary of reported compounds found in liquids. The
list is broken into four classes based on the suspected origin of each
compound.
Frank kept his promise of writing to his friend Mr. Jackson, from time
to time, as he had opportunity. One of his letters, written four years
after his arrival in the Dairy Plains, contained the most important
news he had yet had occasion to send of the state of himself and his
family.
“Respected Sir,
“I have often thought and called myself bold in what I have said to
you in my letters, but you have always taken it kindly. This kindness
makes me more bold than ever, especially as to two things that I am
going to write about, when I have a little explained our present
condition.
“My employer and I are about to part; which you will be surprised
to hear, as there is a full year remaining of the time I bound myself to
serve. It is through no quarrel, however; Mr. Stapleton having been a
good master to me, unless for wanting more work out of me than
mortal arm could do; for which, however, he was always willing to
pay me well. The fact is, sir, he is a daring and a bustling man, such
as they say are always to be found in new countries, wanting, as
soon as they have got all pretty comfortable about them, to go
further into the wilds and begin again. I see the good of there being
such men, but do not wish to be one; so, when Stapleton offered me
any wages I liked to go with him, I said ‘No,’ having only engaged to
serve him on this spot; and thus I find myself at liberty a year sooner
than I expected. He offered me an introduction that would get me
good terms from the gentleman that has taken his pretty place; but
not knowing yet what sort of person he is, and there being, thank
God! far more work in my way to be done at any price than I can get
through, I wish to keep myself free. To finish about myself first,—I am
building a sort of double house, in the middle of a very pretty piece of
land. One end of the house is for myself, and the other for my father,
against his time is up. It would do your heart good, sir, to see how he
has everything comfortable about him, though he goes on
complaining, to be sure, that this is not the old country. My step-
mother too has succeeded finely with her fruit this year, and there is
as good cider of hers in every cottage as any in Worcestershire, and
such flowers as she grows make the place look like a paradise.
“Allow me now, sir, to go on as if we were talking as we have often
done over the churchyard gate, or by your door; and not as if this
letter had to travel over the wide sea before it reaches you. I should
like to know whether it has ever happened to you to fancy gentlemen
like yourself coming over to this place? I am sure, if such would think
of it, it would be the best thing for the society here, and might prove
so to themselves, in cases where they are not very well off, and have
little to leave that they care for. You make no secret, sir, of its being
difficult for your family to live on such a curacy as yours, and you
have even talked of settling your sons abroad as they grow up. If you
would send them,—or (what is better) bring them here,—they shall
be made welcome, and watched over and taken care of as they
ought to be by those who owe so much to their father. Indeed, sir,
this might prove a pleasant settlement in a very few years to you and
yours. There are now eleven farms and other dwellings within three
miles, and more building every year; and Launceston is within reach.
The people about us are mostly very intelligent, and it is a good sign
that they are crying out continually for a settled clergyman and a
school; and, if we cannot get so much, for a library. You would find a
good house, with a stable, and a horse in it; a garden, and two or
three fields; a school-room with five-and-twenty scholars, whose
parents would pay you well both for your teaching and your Sunday
services. We should ask you too, to choose a little library at our
expense, and should add to it, under your direction, every year; so
that your children as well as those of the settlers should have every
advantage. You will find further particulars of what we can offer you
in the public letter which accompanies this.
“My fear is, that the consideration of the young ladies will deter
you, should you otherwise be disposed to listen to our plan; and,
indeed, England seems at first sight the best place for daughters that
have lost their mother. But I have great hopes that these plains may
be like an English county before your young ladies have grown up.
When once gentlemen, especially clergymen, begin to come, more
follow; and this is all we want to make the Dairy Plains like parts of
Sussex or Dorsetshire. We have specimens of each class, up to the
thriving farmer and wool-grower. There is also a surveyor, and a
surgeon is coming, they say; though he is the last person wanted,
except for an accident now and then, for we really have no sickness.
If, in addition to these, we could have over a tanner or two, a coal-
master, a vine-grower, a store-keeper, and so on, each with his
proper labourers, ours would be as flourishing a settlement as any in
the world. There is coal in plenty, and a fine market in every
direction, if we had but people to work it; and the same may be said
of slate, and bark, and hides. Some Portuguese vine-dressers are
making a fine thing of a vineyard in the south of the island; and why
not here, instead of our having to import spirits in such quantities as
make drunkards of too many of our labourers? The commoner sorts
of wine we might make would soon drive out spirits, to our great
benefit in every way. As for clothing, utensils, and other things that
are brought to great perfection and cheapness in England, we had
better go on buying there; and I have no doubt they will be as glad of
our productions as we of their manufactures. You will be pleased to
hear that there are already twenty-six vessels belonging to the
island, and that upwards of thirty traded with us from Great Britain
last year; and that 1,000,000 lbs. of wool were sent there within the
twelve months. All these things I mention to show what a rising
country this is, and how well worth the while of many a man above
the rank of labourers and artizans to come to. If you should think of
doing so, sir, it would be the best piece of news that could reach the
Dairy Plains from any part of the world. You should have the
heartiest welcome from some whom you are pleased to call old
friends.
“Perhaps, sir, you may remember saying something to me about
the difficulty of getting a wife here. I have never tried, because there
was one in England, as you know, that I always hoped might keep
herself single till we should agree that she should follow me out.
Through all these long four years we have had this in view, and now
I shall have a house ready for her by the time she can come; and
this is the other liberty I told you I was about to take. If you should
really come, perhaps, knowing her steadiness so well, you would let
her cross with you, waiting on the young ladies during the voyage,
for the expense of which I will be answerable. Whether you join us or
not, I have little doubt you will kindly put her in the way of coming
with the least possible delay; and you may depend on my meeting
her before she lands.
“I have said nothing of Ellen, because you will see her letter to
grandfather. I have left it to her to send money this time, as I have
other use, you see, for my own.
“It is a load off my mind, sir, to have written what has been deep
down in it for so long. It is a great while to wait for an answer; and if
there should be disappointment both ways, I hardly know how I shall
bear it. But I am pretty sure of what is to me the chief thing; and if
you come too, I wonder what we can manage to find to wish for next.
It pleased God to give Ellen and me our hardships early, and to take
us out of them before our hearts and tempers were hurt; like so
many at home, better perhaps than ourselves. If He should try us
any more, we have good reason now to be patient; and in the
meanwhile, we desire to save others from what we had to go through
for a short time, and therefore write as we do about coming over.
”Frank Castle.
“P.S. There are fine downs here for the young gentlemen to fly
their kites, just behind the house you would have. Ellen will take care
that Miss Maria shall have a pretty poultry-yard; and Susan is taming
an opossum mouse for the other little lady.”
TRUE CITIZENSHIP.
A Tale.
BY
HARRIET MARTINEAU.
LONDON:
CHARLES FOX, 67, PATERNOSTER-ROW.
1832.
CONTENTS.
1. Novelty 1
2. Pastime 18
3. Discussion 29
4. More Novelty 45
5. Observing at hand 62
6. Observing afar 70
7. One for Himself 87
8. Consequences 108
9. Each for All 118
FOR EACH AND FOR ALL.
Chapter I.
NOVELTY.
The season was more than half over, and was about to be
pronounced remarkably dull, when a promise of novelty was given
out in the shape of a rumour that lord F—— and his lady, who had
been travelling abroad from the day of their marriage, had arrived in
town, and that the bride’s first appearance would take place at the
Duke of A——’s ball on the 20th. This information was circulated in
various forms of words, all bearing a relation to what lady F—— had
been before she was lady F——. At the clubs, in the shops, in
drawing-rooms and boudoirs, it was related that lady F——’s debut
would take place on the 20th. Her first appearance on a new stage,
—her return from a tour in the provinces,—her first night in a new
character, all were referred to the 20th, in a manner which should
prevent any one forgetting that lady F—— had quitted a profession
on her marriage. The curiosity was not confined to mothers and
daughters, to whose observation an extraordinary marriage is the
most exciting circumstance that life affords: in this case, the interest
was shared by their husbands and fathers. Some wondered how the
proud old earl would stand the introduction of his daughter-in-law
into his own society; and others, who had told lord F—— that he was
a lucky fellow to have won such a glorious creature, speculated,
notwithstanding, on the awkwardnesses and difficulties which must
hourly arise from the choice of one so far below him in rank. He was
an odd personage, however,—lord F——; and there was no telling
how he would think and feel on occasions when everybody else felt