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Full Download Book Goldsmiths Assisted Ventilation of The Neonate An Evidence Based Approach To Newborn Respiratory Care PDF
Full Download Book Goldsmiths Assisted Ventilation of The Neonate An Evidence Based Approach To Newborn Respiratory Care PDF
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Assisted Ventilation
of the Neonate
An Evidence-Based Approach to Newborn Respiratory Care
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GOLDSMITH’S
Assisted Ventilation
of the Neonate 7 th Edition
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This book and the individual contributions contained in it are protected under copyright by the Publisher
(other than as may be noted herein).
Notices
Knowledge and best practice in this field are constantly changing. As new research and experience broaden
our understanding, changes in research methods, professional practices, or medical treatment may
become necessary.
Practitioners and researchers must always rely on their own experience and knowledge in evaluating
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contained in the material herein.
Previous editions copyrighted 2017, 2011, 2003, 1996, 1988, and 1981.
Printed in India
v
vi CONTRIBUTORS
Assisted Ventilation of the Neonate is one of the few textbooks in noninvasive ventilation strategies, a better understanding of
our subspecialty that I consider iconic. The first edition of this transitional and postnatal physiological disturbances, smarter
book was published 40 years ago, and at least two generations clinicians, and increasingly sophisticated ventilators. However,
of trainees and practicing neonatologists have considered it the increasingly complex ventilators allowing multiple modes of
“bible” of respiratory management of critically ill infants. ventilation has increased the opportunity for operator errors
As I think back to the beginning of my training in the 1970s, because of the number of ventilator decisions clinicians must
I am amazed how much progress has been made in respiratory make. As with every edition of this textbook, the editors and
support of the newborn infant. The first large case series authors provide a clear way forward to take much of the guess-
of “near-terminal” preterm neonates with “hyaline membrane work out of mechanical ventilation.
disease” by Papadopoulos and Swyer in 1964 provided a frame- The seventh edition of this textbook has the subtitle of “an
work for ventilation to reverse acid–base disturbances but was evidence-based approach.” The editors have successfully inte-
associated with almost 100% mortality. It is noteworthy that grated the “art” of ventilation with current best evidence. As a
Patrick Bouvier Kennedy (President John F. Kennedy’s son) born foundation to those sections, there are in-depth discussions of
at 34 weeks’ gestation was treated with hyperbaric oxygen rather respiratory physiology and control of breathing, pulmonary
than positive-pressure ventilation and is a prime example of the function testing, newer radiographic techniques to assess lung
skepticism surrounding ventilation of the newborn infant in the pathology, use of oxygen, and delivery room stabilization. Each
mid-1960s. The problem was twofold. First, there was a general of the newest strategies for ventilating neonates is presented
lack of understanding of neonatal respiratory physiology and in great detail along with how to manage infants with diverse
disease pathophysiology, including the importance of positive respiratory diseases. Finally, the editors have wisely chosen to
end expiratory pressure and surfactant in maintaining alveolar include chapters on home ventilation, transport, intraopera-
stability. Second, most neonatal intensive care units were using tive management of the neonate, ethical and medical-legal
ventilators designed for adults in modes that were never meant issues, pharmacotherapies, nursing care, and respiratory care
for newborns. Beginning in the 1970s, a new generation of ven- in resource-limited setting.
tilators designed for neonates became commercially available. The seventh edition of Goldsmith’s Assisted Ventilation of the
However, those ventilators were still not refined. They did not Neonate, edited by Martin Keszler and K. Suresh Gautham, is an
allow infants to breathe when the ventilator was not cycling outstanding compendium of well-written chapters, which not only
(intermittent mandatory ventilation was not available) or were guides care providers in how to care for neonates with respiratory
associated with difficult regulation of delivered tidal volumes, diseases but also provides the basis for their recommendations.
resulting in pneumothoraces and chronic lung injury. Since the The editors of this book and authors of the chapters are to be con-
initial publication of Assisted Ventilation of the Neonate, the mor- gratulated for producing another superb edition.
tality rate for infants with respiratory distress syndrome has
plummeted. The improvement in mortality is multifactorial but Richard A. Polin, MD
is likely secondary to a variety of clinical advancements (includ- William T. Speck Professor of Pediatrics
ing widespread administration of surfactant), greater use of Columbia University, College of Physicians and Surgeons
x
P RIENFA
DECX
E
In 1978, before there were exogenous surfactants, inhaled nitric frequency ventilation), unplanned extubations, plugged endo-
oxide, high-frequency ventilators, and other modern therapies, tracheal tubes, nasal trauma with continuous positive airway
a young overly confident neonatologist (JPG) thought that pressure (CPAP) devices, and others. In the past 40 plus years,
there needed to be a primer on newborn assisted ventilation for pharmacological, nutritional, technological, and philosophical
physicians, nurses, and respiratory therapists entrusted with advances in the care of newborns, especially the extremely pre-
treating respiratory failure in fragile neonates. In the preceding mature, have continued to refine the way we manage neonatal
decade, ventilation of neonates was undertaken only in major respiratory failure. Microprocessor-based machinery, informa-
medical centers, and in 1963, the late preterm son of the Presi- tion technology, an emphasis on safety, quality improvement,
dent of the United States, John F. Kennedy, died of lack of ade- and evidence-based medicine have affected our practice as they
quate respiratory support. As the first edition of this text was have all of medical care. However, the wide variance in out-
being written, assisted ventilation had become widely available comes of this most vulnerable population is striking among
in hundreds of hospitals in the United States and around the even the most sophisticated university-based neonatal intensive
world. Even in the early days of this new subspecialty called care units (NICUs). The Vermont Oxford Network, through
neonatology, respiratory support was an essential part of neo- their Nightingale data collecting system, reports that in the
natal intensive care. However, there was little guidance in stan- most advanced NICUs (Type C, n 5 158), BPD secondary to
dard neonatal textbooks regarding the proper techniques in assisted ventilation varied in 2020 from a median of 20.7% in
neonatal ventilatory support. The initial publication was con- the first quartile to 38% in the third quartile in neonates born
ceived to fill a void and provide a reference to the caretakers in under 1500 g or 32 weeks’ gestation. Literature reports of BPD
this new and exciting field but was not intended as a “license in vary even more widely, documenting a reported incidence of
assisted ventilation” for the novice. The neonatologist, only 5% to 6% in one institution to as high as 50% to 60% in others.
2 years out of his fellowship, recruited his young partner (EHK) Mere survival is no longer the only goal; the emphasis of
and they prevailed upon their former teachers and mentors to neonatal critical care has changed to improving functional out-
write most of the chapters of the text, while they served mostly comes of even the smallest premature infant. While the thresh-
as organizers in this initial project. The result exceeded their old of viability has been lowered only modestly in the past
most optimistic expectations in creating a “how to” guide for decade, there have been decreases in morbidities, even at the
successful ventilation of the distressed newborn. The first edi- smallest weights and lowest gestational ages. However, the large
tion, published in 1981, was modeled after the iconic text of institutional variation in morbidities such as BPD, even in the
Marshall Klaus and Avroy Fanaroff, Care of the High-Risk era of widespread administration of antenatal corticosteroid
Neonate, which was the standard clinical reference for practic- administration to mothers, can no longer be attributed to dif-
ing neonatal caregivers at the time. Dr. Klaus wrote the fore- ferences in the populations treated. The uniform application of
word, and the first edition of Assisted Ventilation of the Neonate evidence-based therapies and quality improvement programs
was born. has shown significant improvements in outcomes, but unfortu-
The preface to the first edition started with a quotation from nately, not in all centers. We have recognized that much of
Dr. Sydney S. Gellis, then considered the Dean of Pediatrics in neonatal lung injury (i.e., ventilator induced lung injury) is due
the United States: to our ventilatory techniques and occurs predominantly in the
“As far as I am concerned, the whole area of ventilation of most premature infants. Our perception of the ventilator has
infants with respiratory distress syndrome is one of chaos. shifted from that of a lifesaving machine to a tool that can also
Claims and counterclaims about the best and least harmful cause harm—a double-edged sword. However, the causes of
method of ventilating the premature infant make me light- this morbidity are multifactorial, and its prevention remains
headed. I can’t wait for the solution or solutions to premature controversial and elusive. This is not a new concept. As early as
birth, and I look forward to the day when this gadgetry will 1745, Fothergill cautioned regarding the deleterious effects of
come to an end and the neonatologists will be retired.” mechanical ventilation: “Mouth to mouth resuscitation may
Year Book of Pediatrics (1977) be better than using a mechanical bellows to inflate the lung
because . . . the lungs of one man may bear, without injury, as
After over four decades and seven editions of the text, we are great a force as those of another can exert, which by the bellows
still looking for the solutions to premature birth despite de- cannot always be determined” (J Philos Trans R Soc, Lond.
cades of research on how to prevent it, and neonatal respiratory 1745). Specifically, attempts to decrease the incidence of BPD
support is still a mainstay of neonatal intensive care. Initially, have concentrated on ventilatory approaches such as earlier and
there were concerns regarding the experience and competence more extensive use of CPAP, noninvasive ventilation, volume-
of those managing these new ventilation devices with an unac- targeted modes, various devices to synchronize ventilator and
ceptable rate of complications such as bronchopulmonary spontaneous breathing, and adjuncts such as caffeine and vita-
dysplasia (BPD), pulmonary air leaks (especially with high min A. Yet, some of these therapies remain unproven in large
xi
xii PREFACE
clinical trials, and the national incidence of BPD in large monitoring methods of the newborn in respiratory distress,
databases for very low birth weight infants exceeds 30%. Thus, including chapters on physical assessment, imaging, blood gas
until there are social, pharmacological, and technical solutions monitoring, and pulmonary function and graphics. Essential
to prematurity, neonatal caregivers will continue to be chal- aspects of respiratory support are covered in the third section
lenged to provide respiratory support for the smallest prema- with discussions on delivery room management, oxygen ther-
ture infants without causing lifelong pulmonary or central apy, and all types of ventilatory modes and strategies. A new
nervous system injury. chapter on respiratory gas conditioning has been added to this
In this, the seventh edition, the transition to two new editors, section. Adjunctive interventions such as pulmonary and nurs-
Dr. Keszler and Dr. Gautham, has been completed. Martin ing care, nutritional support, and pharmacologic therapies are
Keszler, MD, Professor of Pediatrics and Medical Director of the subjects of the fourth section. The fifth section reviews spe-
Respiratory Care at Brown University, is internationally re- cial situations and outcomes, including chapters on BPD care,
nowned for his work in neonatal ventilation. Kanekal Suresh surgical and medical considerations of the airway, intraopera-
Gautham, MD, DM, MS, is the Chairman of Pediatrics and tive management, and new chapters on persistent pulmonary
Pediatrician-in-Chief at Nemours Children’s Hospital and a hypertension and congenital diaphragmatic hernia. Finally, the
Professor of Pediatrics at the University of Central Florida sixth section reviews complications, transition from hospital to
College of Medicine, Orlando, FL. He is a Deputy Editor of The home, pulmonary and neurologic outcomes, care in resource
Joint Commission Journal on Quality and Safety, is a Senior limited settings, and a new final chapter on gaps in knowledge
Editor for the Neonatal Review Group of the Cochrane and future directions.
Collaboration, and is regarded as one of the foremost authori- During the four-plus decade and seven-edition life of this
ties on quality improvement in neonatal care. text, neonatology has grown and evolved in the nearly 1000
Since the sixth edition, new ventilatory devices have been NICUs in the United States. The two young neonatologists, now
introduced, and support has continued to shift from an invasive past-due for retirement, have turned over the leadership of this
to a noninvasive approach, which has resulted in significant and future editions of the text to the new editors. We have seen
improvements in some outcomes, but also new challenges for new and unproven therapies come and go, and despite our
providers. Recent improvements to ventilatory devices have frustration at not being able to prevent death or morbidity in
also not come without cost. The new generation of ventilators all our patients, we continue to advocate for evidence-based
has added a new level of complexity as well as expense to neo- care and robust clinical trials before the application of new de-
natal care. While some clinicians may be attracted to the ad- vices and therapies. We hope this text will stimulate its readers
vanced features of new devices, the new technology may pose to continue to search for better therapies as they use the wis-
risks to patients as devices may not be fully understood or mis- dom of these pages in their clinical practice. We are honored to
applied by multiple caretakers at the bedside. More commonly, have Dr. Richard Polin, the American Academy of Pediatrics
many of the new ventilator features are infrequently used in 2021 Apgar Award winner and editor/author of his own classic
clinical practice. Unfortunately, many providers do not use or text on Fetal and Neonatal Physiology, favor us with the fore-
understand how to apply important adjuncts to care, such word to this edition. And as we wait for the solution(s) to
as pulmonary graphics. Hopefully, these deficiencies can be prematurity, we should heed the wisdom of the old Lancet edi-
addressed by texts such as this. torial: “The tedious argument about the virtues of respirators
The seventh edition of Assisted Ventilation of the Neonate has not invented over those readily available can be ended, now that
been extensively updated and rewritten, with many new con- it is abundantly clear that the success of such apparatus de-
tributors and several new chapters. The text is divided into six pends on the skill with which it is used” (Lancet. 1965;2:1227).
sections. The first section covers general principles and con-
cepts and includes chapters on physiologic principles, ethical Jay P. Goldsmith, MD, FAAP
and medical-legal aspects of respiratory care, and quality and November 2021
safety. The second section reviews assessment, diagnosis, and
CONTENTS
SECTION 1 History, Pulmonary Physiology, and 20 Basic Modes of Synchronized Ventilation, 232
General Considerations Martin Keszler and Mark C. Mammel
21 Principles of Lung-Protective Ventilation, 241
1 Introduction and Historical Aspects,1 Anton H. van Kaam
Jay P. Goldsmith and Tonse N. K. Raju 22 Volume-Targeted Ventilation, 249
2 Physiologic Principles,11 Martin Keszler, MD and Kabir Abubakar, MBBS
Martin Keszler and Kabir Abubakar 23 Special Techniques of Respiratory Support, 263
3 Control of Ventilation, 33 Nelson Claure and Eduardo Bancalari
Richard J. Martin and Eric C. Eichenwald 24 High-Frequency Ventilation, 269
4 Ethical Issues in Assisted Ventilation of the Neonate, 39 Martin Keszler, J. Jane Pillow, and Sherry E. Courtney
Matthew Drago and Mark R. Mercurio 25 Mechanical Ventilation: Disease-Specific
5 Evidence-Based Respiratory Care, 47 Strategies, 288
Krithika Lingappan and K. Suresh Gautham Bradley A. Yoder and Peter H. Grubb
6 Quality and Safety in Respiratory Care, 56 26 Weaning and Extubation From Mechanical
K. Suresh Gautham and Grant Joseph Dat Chiu Shafer Ventilation, 303
7 Medical and Legal Aspects of Respiratory Care, 64 Wissam Shalish, Guilherme Sant’Anna, and Martin Keszler
Jonathan M. Fanaroff 27 Common Devices Used for Mechanical Ventilation, 315
Robert L. Chatburn and Waldemar A. Carlo
28 Extracorporeal Membrane Oxygenation, 351
SECTION 2 Patient Evaluation and Monitoring Robert M. Arensman, Billie Lou Short, Nathaniel Koo, and Andrew
Mudreac
8 Physical Examination, 70
Edward G. Shepherd and Leif D. Nelin
9 Imaging: Radiography, Lung Ultrasound, and Other
SECTION 4 B
edside Care, Nutritional
Imaging Modalities, 76
Erik A. Jensen, María V. Fraga, David M. Biko, Francesco Raimondi,
and Pharmacologic Support
and Haresh Kirpalani
29 Respiratory Care of the Newborn, 363
10 Blood Gases: Technical Aspects and Interpretation, 94 Robert DiBlasi
Colm Travers and Namasivayam Ambalavanan
30 Nursing Care, 384
11 Noninvasive Monitoring of Gas Exchange, 111 Debbie Fraser
Bobby Mathew and Satyan Lakshminrusimha
31 Nutritional Support, 397
12 Pulmonary Function and Graphics, 124 Laura D. Brown, Camilia R. Martin, and Sarah N. Taylor
Georg Schmölzer, MD, PhD and Helmut Hummler, MD, MBA
32 Pharmacologic Therapies, 408
13 Airway Evaluation: Bronchoscopy, Laryngoscopy, Jegen Kandasamy and Waldemar A. Carlo
and Tracheal Aspirates, 144 33 Common Hemodynamic Problems in the Neonate
Clarice Clemmens, Erik B. Hysinger, and Joseph Piccione
Requiring Respiratory Support, 424
Keith J. Barrington and Eugene M. Dempsey
SECTION 3 D
elivery Room Stabilization, Oxygen
Therapy, and Respiratory Support
SECTION 5 T reatment of Specific Conditions,
14 Delivery Room Stabilization and Respiratory Support, 151 Surgical Interventions and Other
Louise S Owen, Gary Weiner, and Peter G Davis Considerations
15 Exogenous Surfactant Therapy, 172
K. Suresh Gautham and Roger F. Soll 34 Diagnosis and Management of Persistent Pulmonary
16 Oxygen Therapy, 185 Hypertension of the Newborn, 429
Maximo Vento Satyan Lakshminrusimha and Martin Keszler
17 Respiratory Gas Conditioning, 196 35 Care of the Infant with Congenital Diaphragmatic
Andreas Schulze Hernia, 446
18 Noninvasive Respiratory Support, 201 Satyan Lakshminrusimha, Martin Keszler, and Bradley A Yoder
Brett J. Manley, Peter G. Davis, Bradley A. Yoder, and Louise S. Owen 36 Management of the Infant With Bronchopulmonary
19 Overview of Assisted Ventilation, 221 Dysplasia, 458
Martin Keszler Huayan Zhang and Nicolas Bamat
xiii
xiv CONTENTS
37 Medical and Surgical Interventions for Respiratory 42 Discharge and Transition to Home Care, 526
Distress and Airway Management, 473 Lawrence Rhein
Nathaniel Koo, Thomas Sims, Robert M. Arensman, Nishant Srinivasan, 43 Neurologic Effects of Respiratory Support in the
Saurabhkumar Patel, Akhil Maheshwari, and Namasivayam Ambalavanan Neonatal Intensive Care Unit, 532
38 Intraoperative Management of the Neonate, 491 Vivien Yap and Jeffrey M. Perlman
Christopher E. Colby, Raymond C. Stetson, and Malinda N. Harris 44 Pulmonary and Neurodevelopmental Outcomes Following
Ventilation, 541
Allison H. Payne, Monika Bhola, Gulgun Yalcinkaya,
SECTION 6 Complications of Respiratory Support, and Michele C. Walsh
Special Considerations, and Outcomes 45 Gaps in Knowledge and Future
Directions for Research, 549
39 Complications of Respiratory Support, 501 Tonse N.K. Raju, Payam Vali, and K. Suresh Gautham
Lakshmi Katakam
40 Neonatal Respiratory Care in Resource-Limited Appendices, 565
Countries, 505 Jay P. Goldsmith
Amuchou Soraisham and Nalini Singhal Index, 587
41 Transport of the Ventilated Infant, 516
Robert M. Insoft
SECTION 1 History, Pulmonary Physiology, and General Considerations
1
Introduction and Historical Aspects
Jay P. Goldsmith and Tonse N. K. Raju
KEY POINTS treated with the most advanced therapy of the era, hyperbaric
oxygen,2 but he died of progressive hypoxemia. There was no
• The birth and early death of a premature son to President John F. Kennedy
neonatal-specific ventilator in the United States to treat the
and Jacqueline Kennedy in 1963 focused the world’s attention on prematu-
young Kennedy at the time. In response to his death, The New
rity and the treatment of hyaline membrane disease (HMD), leading to the
research and development of pulmonary surfactants, ventilatory devices York Times reported: “About all that can be done for a victim of
and improved ventilatory techniques that heralded the modern era of hyaline membrane disease is to monitor the infant’s blood
neonatology. chemistry and try to keep it near normal levels.”1 The Kennedy
• Although the first reference to providing assisted ventilation to a child is tragedy, followed only 3 months later by the president’s assas-
found in the Old Testament, the first 15 centuries ad of recorded attempts sination, stimulated a heightening of interest and research in
to ventilate the neonate or child were crude and generally unsuccessful. neonatal respiratory diseases and the treatment of prematurity.
• The early understanding of general cardiorespiratory physiology in the This interest resulted in increased federal funding in these areas
fifteenth through nineteenth centuries led to some anecdotal success of as well as the proliferation of special areas (neonatal intensive
basic ventilatory devices that improved neonatal resuscitation efforts and care units [NICUs]) for the care of sick and premature infants
offered some long term respiratory support to children.
at birth in hospitals around the country.
• The first half of the twentieth century witnessed the introduction of many
With the possible exception of pediatric oncology, no branch
devices that proved mostly unsuccessful in the respiratory treatment of
neonates with respiratory failure. In the second half of this century, of medicine has seen such dramatic progress in the last half
improved understanding of the physiology of respiratory distress syndrome, century as has the field of neonatal-perinatal medicine. Less
the application of end expiratory pressure, and enhancing pulmonary matu- than five decades ago, many centers would not routinely resus-
ration with antenatal steroids and pulmonary surfactant therapy were major citate infants under 28 weeks of gestation and, in some cases,
advances in the treatment of premature lung disease. even those under 1500 g birth weight. A dramatic shift in the
• The major reduction in morbidity and mortality from respiratory failure of physician response and public expectations of care to the very
newborns seen from 1970 to 2010 has been followed by only modest (,1500 g) and extremely low birth weight (,1000 g) newborn
improvement in the last decade. Further gains in reducing chronic pulmo- occurred largely because of significant advances in perinatal
nary morbidities associated with assisted ventilation will depend on trans- and neonatal care during this period. The improvements in the
lational research and quality improvement initiatives from the bench to the
neonatal areas of respiratory, nutritional, and cardiac care as
bedside.
well as other technological advances gave support to the per-
ception that most preterm infants can be treated effectively
and saved from the disorders of prematurity, but also that an
overwhelming majority survive without significant long-term
The birth of a premature son to President John F. Kennedy and disabilities. Specifically, the major technologic advances in
Jacqueline Kennedy on August 7, 1963, focused the world’s at- ventilatory support, especially over the past two decades, have
tention on prematurity and the treatment of hyaline membrane helped push the concept of the borderline of viability well into
disease (HMD), then the current appellation for respiratory the mid second trimester of pregnancy.3 Improved perinatal
distress syndrome (RDS). Patrick Bouvier Kennedy was born by care also helped contribute to improved neonatal outcomes,
cesarean section at 34 weeks’ gestation at Otis Air Force Base especially the improved assessment of fetal wellbeing, enhanc-
Hospital in Massachusetts. He weighed 2.1 kg and was trans- ing fetal lung maturation and optimizing the time and method
ported to Boston’s Massachusetts General Hospital, where he of delivery. The results of these advances have made death from
died at 39 hours of age (Fig. 1.1).1 The Kennedy baby was respiratory failure relatively infrequent in the neonatal period
1
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When the matters are too pasty to be divided in the mortar they should be divided by means
of a knife or a spatula. They should then be incorporated with a known weight of inert,
pulverulent matter such as fine sand, with which they should be thoroughly mixed and in
subsequent calculations the quantity of sand or other inert matter added must be taken into
consideration. Usually a pasty state of a fertilizer is due to the humidity of the mixture. In this
case a considerable volume of the sample is taken and dried and then reduced to a pulverulent
state. In the subsequent calculations, however, the percentage of moisture lost must be taken
into consideration.
Before drying a sample it is necessary to take into consideration whether or not the product
will be modified by desiccation as would be the case, for instance, with superphosphates. With
these, which are often in a state more or less agglomerated, it is recommended to introduce into
them, in order to divide them, a certain quantity of calcium sulfate in order to obtain them in a
pulverulent state.
In the case of animal débris they should be divided as finely as possible with the aid of
scissors and then passed through a drug mill if dry enough. They are then mixed by hand and
may finally be obtained in a state of considerable homogeneity.
When fertilizers are in a pasty state more or less liquid, they are dried at 100°, first
introducing a little oxalic acid in case they contain any volatile ammoniacal compounds. The
product of desiccation is then passed through a mill. Before treating in this way it is necessary to
be sure that the composition will not be altered by drying. In the case of a mixture containing
superphosphates and nitrate, for instance, drying would eliminate the nitric acid. In such a case
the free phosphoric acid should be neutralized with a base like lime. In the case of fertilizers
containing both nitrates and volatile ammoniacal compounds the addition of oxalic acid might
also set free nitric acid during the desiccation. In such a case it is necessary to dry two samples;
one with the addition of oxalic acid for the purpose of estimating the ammonia, and the other
without the acid for the purpose of estimating the nitrate. A qualitative analysis should precede
all the operations so as to determine the nature of the material to be operated on.
14. German Method.—In the method pursued by the German experiment stations it is
directed:[8]
(1) Dry samples of fertilizers must be passed through a sieve and afterwards well mixed.
(2) With moist fertilizers, which can not be subjected to the above process, the preparation
should consist in a careful and thorough mixing, without sieving.
(3) On the arrival of the samples in the laboratory their weight should be determined. The
half of the sample is prepared for analysis and the other part, to the amount of a kilo, should be
placed in a glass vessel, closed air-tight, and placed in a cool place for at least a quarter of a
year from the time of its reception, in order that it may be subjected to any subsequent
investigations which may be demanded.
(4) In the case of raw phosphates and bone-black the amount of water which they contain
should be determined at from 105° to 110°. Samples which in drying lose ammonia in any way,
should have this ammonia determined.
(5) Samples which are sent to other laboratories for control analyses, should be sent
securely packed in air-tight glass bottles.
(6) The weight of the samples sent should be entered in the certificates of analysis.
(7) Samples which, on pulverizing, change their content of water, must have the water
content estimated in both the coarse and powdered condition and the results of the analysis
must be calculated to the water content of the original coarse substance.
15. Special Cases.—Many cases arise of such a nature as to make it impossible to lay
down any rule which can be followed with success. As in almost every other process in
agricultural chemistry the analyst in such cases must be guided by his judgment and
experience. Keeping in view the main object, viz., to secure in a few grams of material a fair
representation of large masses he will generally be able to reach the required result by following
the broad principles already outlined. In many cases the details of the work and the adaptations
necessary to success must be left to his own determination.
16. Drying Samples of Fertilizers.—The determination of the uncombined moisture in a
sample of fertilizer is not an easy task. In some cases, as in powdered minerals, drying to
constant weight at the temperature of boiling water is sufficient. In organic matters containing
volatile nitrogenous compounds, these must first be fixed by oxalic or sulfuric acid, before the
desiccation begins. If any excess of sulfuric acid be added, however, drying at 100° becomes
almost impossible. Particular precautions must be observed in drying superphosphates. In
drying samples preparatory to grinding for analysis, it is best to stop the process as soon as the
materials can be pulverized. In general, samples should be dried only to determine water, and
the analytical processes should be performed on the undried portions. It is not necessary, as a
rule, to dry samples of fertilizers in an inert atmosphere, such as hydrogen or carbon dioxid.
Drying in vacuo may be practiced when it is desired to secure a speedy desiccation or one at a
low temperature.
17. Official Methods.—The Official Agricultural Chemists direct, in the case of potash salts,
sodium nitrate, and ammonium sulfate, to heat from one to five grams in a flat platinum or
aluminum dish at 130° until the weight is constant.[9] The loss in weight is taken to represent the
water. In all other cases heat two grams, or five grams if the sample be very coarse, for five
hours in a steam-bath.
In the German stations in the case of untreated phosphates and bone-black the moisture is
estimated at from 105° to 110°. Samples which lose ammonia should have the weight of
ammonia given off at that temperature, determined separately.
For purposes of comparison it would be far better to have all contents of moisture
determined at the boiling-point of water. While this varies with the altitude and barometric
pressure yet it is quite certain that the loss on drying to constant weight at all altitudes is
practically the same. Where the atmospheric pressure is diminished for any cause the water
escapes all the more easily. This, practically, is a complete compensation for the diminished
temperature at which water boils.
Where the samples contain no ingredient capable of attacking aluminum, they can be
conveniently dried, in circular dishes of this metal about seven centimeters in diameter and one
centimeter deep, to constant weight, at the temperature of boiling water.
18. Moisture in Monocalcium Phosphates.—In certain fertilizers, especially
superphosphates, containing the monocalcium salt, the estimation of water is a matter of
extreme difficulty on account of the presence of free acids and of progressive changes in the
sample due to different degrees of heat.
Stoklasa has studied these changes and reaches the following results[10]:
A chemically pure monocalcium phosphate of the following composition, viz.,
CaO 22.36 per cent.
P₂O₅ 56.67 “ “
H₂O 21.53 “ “
was subjected to progressive dryings. The loss of water after ten hours was 1.83 per cent; after
twenty hours, 2.46 per cent; after thirty hours, 5.21 per cent; after forty hours, 6.32 per cent;
after fifty hours, 6.43 per cent. This loss of water remained constant at 6.43 per cent. This loss
represents one molecule of water as compared with the total molecular magnitude of the mass
treated. A calcium phosphate, therefore, of the following composition, CaH₄(PO₄)₂·H₂O loses,
after forty hours, drying at 100°, its water of crystallization. The calcium phosphate produced by
this method forms opaque crystals which are not hygroscopic and which give, on analysis, the
following numbers:
CaO 24.02 per cent.
P₂O₅ 16.74 “ “
H₂O 15.09 “ “
The temperature can be raised to 105° without marked change. If the temperature be raised
to 200° the decomposition of the molecule is hastened according to the following formula:
COMPLETE ANALYSIS OF
MINERAL PHOSPHATES.
19. Constituents to be Determined.—The most important point in the analysis of mineral
phosphates is to determine their content of phosphoric acid. Of equal scientific interest,
however, and often of great commercial importance is the determination of the percentage of
other acids and bases present. The analyst is often called on, in the examination of these
bodies, to make known the content of water both free and combined, of organic and volatile
matter, of carbon dioxid, sulfur, chlorin, fluorin, silica, iron, alumina, calcium, manganese,
magnesia, and the alkalies. The estimation of some of these bodies presents problems of
considerable difficulty, and it would be vain to suppose that the best possible methods are now
known. Especially is this the case with the processes which relate to the estimation of the
fluorin, silica, iron, alumina, and lime. The phosphoric acid, however, which is the chief
constituent from a commercial point of view, it is believed, can now be determined with a high
degree of precision. Often the estimation of some of the less important constituents is of great
interest in determining the origin of the deposits, especially in the case of fluorin. While the
merchant is content with knowing the percentage of phosphoric acid and the manufacturer asks
in addition only some knowledge of the quantity of iron, alumina, and lime the analyst in most
cases is only content with a complete knowledge of the constitution of the sample at his
disposal.
20. Direct Estimation of the Phosphoric Acid.—It often happens, in the case of a mineral
phosphate, that the only determination desired is of the phosphoric acid. In this instance the
analyst may proceed as follows: If the qualitative test shows the usual amount of phosphoric
acid, two grams of the sample passed through a sieve, with a millimeter mesh, are placed in a
beaker and thoroughly moistened with water. The addition of water is to secure an even action
of the hydrochloric acid on the carbonates present. The beaker is covered with a watch-glass
and a little hydrochloric acid is added from time to time until all effervescence has ceased. There
are then added about thirty cubic centimeters of aqua regia and the mixture raised to the boiling-
point on a sand-bath or over a lamp. The heating is continued until chlorin is no longer given off
and solution is complete. The volume of the solution is then made up to 200 cubic centimeters
without filtering, filtered, and an aliquot part of the filtrate, usually fifty cubic centimeters,
representing half a gram of the original sample, taken for the determination of the phosphoric
acid according to the method of the Official Agricultural Chemists. The small quantity of
insoluble material does not introduce any appreciable error into the process when the volume is
made up to 200 or 250 cubic centimeters.
21. Method of the Official Agricultural Chemists for Total Phosphoric Acid.—To the hot
solution, for every decigram of phosphorus pentoxid which may be present, add fifty cubic
centimeters of the molybdic solution. Digest at 65° for an hour, filter, and wash with water or
ammonium nitrate solution[11]. Test the filtrate by renewed digestion with additional molybdate
reagent. Dissolve the precipitate on the filter with ammonia in hot water and wash into a beaker,
making the volume of filtrate and washings not more than 100 cubic centimeters. Nearly
neutralize with hydrochloric acid, cool, and add magnesia mixture from a burette at the rate of
about one drop a second, stirring vigorously, meanwhile. The quantity of magnesia mixture to be
added is not prescribed in the official method but it should always be in excess of the amount
necessary for complete precipitation. For each decigram of phosphorus pentoxid, from eight to
ten cubic centimeters should be used. Fifteen minutes after the last of the magnesia mixture has
been stirred in, thirty cubic centimeters of ammonia of 0.95 specific gravity are added and the
beaker set aside for two hours or longer. The ammonium magnesium phosphate is separated by
filtration, dried, ignited gently at first, and finally over a blast-lamp and weighed as magnesium
pyrophosphate. The factors for calculating the phosphorus pentoxid and tricalcium phosphate
from the weight of pyrophosphate are given below on the two bases; viz., hydrogen equals 1,
and oxygen equals 16.
H = 1.
Mg₂P₂O₇ × 0.63976 = P₂O₅
Mg₂P₂O₇ × 1.3964 = Ca₃(PO₄)₂
P₂O₅ × 2.1827 = Ca₃(PO₄)₂
O = 16.
Mg₂P₂O₇ × 0.63792 = P₂O₅
Mg₂P₂O₇ × 1.3926 = Ca₃(PO₄)₂
P₂O₅ × 2.1831 = Ca₃(PO₄)₂
22. Preparation of Solutions.—Molybdic Solution.—Dissolve 100 grams of molybdic acid in
400 grams or 417 cubic centimeters of ammonia, of 0.96 specific gravity, and pour the solution
thus obtained into 1,500 grams or 1,250 cubic centimeters of nitric acid, of 1.20 specific gravity.
Keep the mixture in a warm place for several days, or until a portion heated to 40° deposits no
yellow precipitate of ammonium phosphomolybdate. Decant the solution from any sediment and
preserve in glass-stoppered vessels.
Magnesia Mixture.—Dissolve twenty-two grams of recently ignited calcined magnesia in
dilute hydrochloric acid, avoiding an excess of the latter. Add a little calcined magnesia in
excess, and boil a few minutes to precipitate iron, alumina, and phosphoric acid; filter, add 280
grams of ammonium chlorid, 700 cubic centimeters of ammonia of specific gravity 0.96, and
water enough to make a volume of two liters. Instead of the solution of twenty-two grams of
calcined magnesia, 110 grams of crystallized magnesium chlorid may be used.
Dilute Ammonia for Washing.—One volume of ammonia, of 0.96 specific gravity, mixed with
three volumes of water, or usually one volume of concentrated ammonia with six volumes of
water.
23. Use of Tartaric Acid in Phosphoric Acid Estimation.—In the presence of iron the
molybdate mixture is likely to carry down some ferric oxid with the yellow precipitate. To prevent
this, and also hinder the separation of molybdic acid in the solution on long standing, tartaric
acid has been recommended.
Jüptner has found that the presence of tartaric acid does not interfere with the separation of
the yellow precipitate, as some authorities assert.[12] Even 100 grams of the acid in one liter of
molybdate solution produce no disturbing effect. Molybdate solution treated with tartaric acid did
not show any separation of molybdic acid when kept for a year at room temperatures. The
presence of tartaric acid, therefore, is highly recommended by him to prevent the danger of
obtaining both ferric oxid and molybdic acid with the yellow precipitate.
24. Water and Organic Matters.—The sample, according to the practice of Chatard, should
be ground fine enough to leave no residue on an eighty mesh sieve, and should be thoroughly
mixed by passing it three times through a forty mesh sieve[13].
Two grams are weighed into a tared platinum crucible. This, with its lid, is placed in an air-
bath at 105°, and heated for at least three hours. The lid is then put on, and the crucible is
placed in a desiccator and weighed as soon as cold. The loss in weight is the moisture.
Wyatt recommends that two grams of the fine material be heated in ground watch-glasses,
the edges of which are separated so as to allow the escape of the moisture.[14] The heating is
continued for three hours at 110°, the watch-glasses then closed and held by the clip, cooled in
a desiccator, and weighed. This method is excellent for very hygroscopic bodies, but where
quick-acting balances are used, scarcely necessary for a powdered mineral.
The residue from the moisture determination is gradually heated to full redness over a
bunsen, and then ignited over the blast-lamp. This operation is repeated after weighing until a
constant weight is obtained. The loss (after deducting the percentage of carbon dioxid as found
in another portion) may be taken as water and organic matter. This method is sufficient for all
practical purposes; but when minerals containing fluorin are strongly ignited, a part of the fluorin
is expelled; hence, if more accurate determinations are required, the loss of fluorin must be
taken into account. In this laboratory it has been proved that a pure calcium fluorid undergoes
progressive decomposition at a bright red heat with formation of lime.
Wyatt directs that the combined water and organic matters be determined in the residue from
the moisture estimation as follows: The residue is brushed into a weighed platinum crucible,
which is heated over a small bunsen for ten minutes and then brought to full heat of a blast-lamp
for five minutes. After cooling, the total loss is determined by weighing. After deducting the
carbon dioxid determined in a separate portion, the residual loss is regarded as due to
combined moisture and organic matter.
25. Carbon Dioxid.—Many forms of compact apparatus have been devised for this
estimation, but none of them is satisfactory if accurate results are desired.[15] Not to mention
other objections, many phosphates must be heated nearly to the boiling-point with dilute acid to
effect complete decomposition of the carbonates. The distillation method described by
Gooch[16] is excellent, and when once the apparatus is set up, its work will be found to be rapid
and satisfactory.
Wyatt regards the estimation of carbon dioxid as one of the most important for factory use.
The carbonates present in a sample indicate the loss of an equivalent amount of acid in the
process of conversion into superphosphate.[17]
The apparatus employed for estimating carbon dioxid may be any one of those in ordinary
use for this purpose. The principle of the process depends on the liberation of the gas with a
mineral acid, its proper desiccation, and subsequent absorption by a caustic alkali, best in
solution.
The apparatus of Knorr, described in volume first, page 338, may be conveniently used. The
weight of the sample to be used should be regulated by the content of carbonate. When this is
very high, from one to two grams will be found sufficient; when low, a larger quantity must be
used. Hydrochloric is preferred as the solvent acid. Those forms of apparatus which are
weighed as a whole and the carbon dioxid determined by reweighing after its expulsion, are not
as reliable as the absorption apparatus mentioned.
26. Soluble and Insoluble Matter.—Five grams of the fine phosphate are put into a beaker,
twenty-five cubic centimeters of nitric acid, (specific gravity 1.20) and 12.5 cubic centimeters of
hydrochloric acid (specific gravity 1.12) are added. The beaker, covered with a watch-glass, is
placed upon the water-bath for thirty minutes[18]. The contents of the beaker are well stirred
from time to time, and at the end of the period the beaker is removed from the bath, filled with
cold water, well stirred, and allowed to settle. The solution is next filtered into a half liter flask,
and the residue is thoroughly washed with cold water, partially dried, and then ignited, (finishing
with the blast-lamp) and brought to constant weight. The figures thus obtained will, however, be
incorrect, because the fluorin liberated during the solution of the phosphates dissolves a portion
of the silica. Hence, the results are too low. Nevertheless, as the same action would occur in the
manufacture of a superphosphate from the material, the determination may be considered, as a
fair approximation to commercial practice. The ignited residue must be tested for phosphorus
pentoxid.
27. Preparation of the Solution.—The flask containing the filtrate is filled to the mark with
cold water, and the solution is thoroughly mixed by twice pouring into a dry beaker and returning
it to the flask. Cold water is used for washing the residue, since if hot water be used, the
sesquichlorids are apt to become basic and insoluble, and hence to remain in the residue and
on the filter paper. Besides, as the flask is to be filled to the mark, the contents must be cold
before any volumetric measurements can be made.
28. Silica and Insoluble Bodies.—Wyatt describes the following method for determining the
total insoluble or siliceous matters in a mineral phosphate[19]. Five grams of the fine sample are
placed in a porcelain dish with about thirty cubic centimeters of aqua regia. The dish is covered
with a funnel, placed on a sand-bath and, after solution is complete, evaporated to dryness with
care to prevent sputtering. When dry the residue is moistened with hydrochloric acid and again
dried, rubbing meanwhile to a fine powder. The heat of the bath is then increased to 125° and
maintained at this temperature for about ten minutes. When cool, the residue is treated with fifty
cubic centimeters of hydrochloric acid for fifteen minutes. The acid is then diluted and filtered on
a gooch, which is washed with hot water until the filtrate amounts to a quarter of a liter. The
residue in the crucible is dried, ignited, and weighed. This method, unless the solution be
subsequently boiled with nitric acid, may not retain all the phosphoric acid in the ortho form.
It is difficult to estimate the total silica by the ordinary methods of mineral analysis. This is
due to the fact that in an acid solution of a substance containing silicates and fluorids the whole
of the silica or the fluorin, as the case may be may escape as silicofluorid on evaporation. Again,
it is not easy to decompose calcium phosphate by fusing with sodium carbonate. If an attempt
be made to do this, however, the process should be conducted as follows: A portion of the
sample is ground to an impalpable powder in an agate mortar. From one to two grams of the
substance are mixed with five times its weight of sodium carbonate and fused with the
precautions given in standard works on quantitative analysis. The fused mass is digested in
water, boiled, and filtered, and the residue washed first with boiling water and afterwards with
ammonium carbonate. The filtrate contains all the fluorin as sodium fluorid and, in addition to
this, sodium carbonate, silicate, and aluminate. Mix the filtrate with ammonium carbonate and
heat for some time, replacing the ammonium carbonate which evaporates. Separate by filtration
the silicic acid hydrate and aluminum hydroxid which are formed and wash them with
ammonium carbonate. To separate the last portions of silica from the filtrate, add a solution of
zinc oxid in ammonia. Evaporate until no more ammonia escapes and separate, by filtration, the
zinc silicate and oxid. Determine the silica in this precipitate by dissolving in nitric acid,
evaporating to dryness, taking up with nitric acid and separating the undissolved silica by
filtration. In the alkaline filtrate the fluorin may be estimated by the usual method as calcium salt.
29. Estimation of Lime.—One hundred cubic centimeters of the solution (containing one
gram of the original substance) are evaporated in a beaker to about fifty cubic centimeters; ten
cubic centimeters of dilute sulfuric acid (one to five) are added; and the evaporation is continued
on the water-bath until a considerable crop of crystals of gypsum has formed[20]. The solution is
then allowed to cool, when it generally becomes pasty, owing to the separation of additional
gypsum. When it is cold, 150 cubic centimeters of ninety-five per cent alcohol are slowly added,
with continual stirring, and the whole is allowed to stand for three hours, being stirred from time
to time. After three hours, it is filtered, with the aid of a filter-pump, into a distillation flask, and
the beautifully crystalline precipitate, which does not adhere to the beaker, is washed with
ninety-five per cent alcohol. The filter, with the precipitate, is gently removed from the funnel and
inverted into a platinum crucible, so that, by squeezing the point of the filter, the precipitate is
made to fall into the crucible, and the paper can be pressed down smoothly upon it. On gentle
heating of the crucible, the remaining alcohol burns off, and when the paper has been
completely destroyed, the heat is raised to the full power of a bunsen for about five minutes.
After cooling in a desiccator the crucible containing the calcium sulfate, is weighed. The filtration
may also be accomplished on asbestos felt.
30. The Ammonium Oxalate Method.—This method has been extensively used in this
country in commercial work, and is best carried out as described by Wyatt.[21] The total filtrates
from the iron and alumina precipitates, secured as described in paragraph 33, are well mixed
and concentrated to a volume of about 100 cubic centimeters. There are added about twenty
cubic centimeters of a saturated solution of ammonium oxalate, and after stirring, the mixture is
allowed to cool and remain at rest for six hours. The supernatant liquid is poured through a filter,
the residue washed three times by decantation with hot water and brought upon the filter. The
beaker and precipitate are washed at least three times. The precipitate is dried and ignited at
low redness for ten minutes. The temperature is then raised by a blast and the ignition
continued for five minutes longer, or until the lime is obtained as oxid. The precipitate is likely to
contain magnesia. The magnesia is estimated in the filtrates from the lime determination by first
mixing them and concentrating to 100 cubic centimeters, which, after cooling, are made strongly
alkaline with ammonia. After allowing to stand for twelve hours the ammonium magnesium
phosphate is collected and reduced to magnesium pyrophosphate by the usual processes. If
one gram of the original material has been used the pyrophosphate obtained, multiplied by 0.36,
will give the weight of magnesia contained therein.
31. Lime Method of Immendorff.—The tedious processes required to determine the lime in
the presence of iron, alumina, and large quantities of phosphoric acid are well known to
analysts. Immendorff has published a method, accompanied by the necessary experimental
data, based on the comparative insolubility of calcium oxalate in very dilute solution of
hydrochloric acid. He has shown in the data given that the lime is all precipitated in the
conditions named and that the precipitate, when properly prepared, is not contaminated with
weighable amounts of the other substances found in the original solution[22]. The ease with
which oxalic acid can be determined volumetrically with potassium permanganate solution aids
greatly in the time-saving advantages of the process.
In a hydrochloric acid solution of a mineral phosphate an aliquot part of the filtrate
representing about 250 milligrams of calcium oxid, usually about twenty-five cubic centimeters,
should be taken for the analysis. Ammonia is added in slight excess and then the acid reaction
restored with hydrochloric until shown plainly by litmus. The solution is then heated and the lime
thrown down by adding a solution of ammonium oxalate in excess. In order to secure a greater
dilution of the hydrochloric acid after the precipitation has been made, water should be added
until the volume is half a liter. Before filtering, the whole should be cooled to room temperature.
The precipitate should be washed first with cold and afterwards with warm water. The well-
washed precipitate is dissolved in hot dilute sulfuric acid and the solution, while hot, titrated with
a standard solution of potassium permanganate set by a solution of ammonio-ferrous sulfate.
If one cubic centimeter of the permanganate represent 0.005 gram of iron it will correspond
almost exactly to 0.0035 gram of calcium oxid.
Example.—Sample of rather poor mineral phosphate, five grams in
half a liter. Strength of potassium permanganate, one cubic centimeter
equivalent to 0.00697 gram of iron and to 0.003484 gram of calcium
oxid.
Twenty-five cubic centimeters of the solution, representing one
quarter of a gram, in which the lime was precipitated as above described,
required 9.6 cubic centimeters of the potassium permanganate to
saturate the oxalic acid. Then