Arsenic, Selenium, Antimony Ultra-Trace Analysis
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About this ebook
Dr. Paul H. Ramses Gouda, is a globally renowned chemist who authored several science books and papers. He has been credited with the foundation of several analytical laboratory procedures utilizing Atomic Absorption and Inductively Coupled Plasma for ultra trace analysis of As, Se, Sb &Hg. These Methods were officially adopted by EPL and by other agencies, and as routinely practiced in the scientific arena they were named after him.
The author, who first attended medical school before specializing in analytical chemistry, has acquired two science doctorates. His contributions to the scientific community include several papers in pharmaceutical and medicinal research, including a recent invention of new pharmaceutical compounds based on the unique concept of the chemical manipulation of hormonal and neurological compounds.
This is a university textbook and a chemist reference.
A must for every library and every analytical laboratory.
Tour the authors books at www.goudabooks.com
Dr.Paul Gouda
Dr. Paul Gouda, is a research scientist and an analytical chemist, He holds two doctorates in medicinal pharmaceutical research and analytical chemistry. He is the scientist behind 3 new pharmaceutical products designed on the unique concept of chemical manipulation of neurological hormonal compounds. He has written several scientific papers and the books. His most recent book is a medical study in gender pre-selection “Choosing the sex of your baby: made simple, made certain.” He has also produced a book similar to this paper, on Hg analysis “Hydrargyrum, Hg analysis from diphenylthiocarbozone to cold vapor.” Visit his laboratory business at www.optimumgreen.com and his books at www.goudabooks.com.
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Arsenic, Selenium, Antimony Ultra-Trace Analysis - Dr.Paul Gouda
Arsenic
Selenium
Antimony
Ultra-trace chemical analysis
Related notes on bench wet-chemistry and
Spectroscopy techniques.
¡Universe, Inc.
Bloomington
Dr. Paul H. Ramses Gouda
C.Chem., P.R.M.D., Ph.D.
As, Se & Sb analysis:
Atomic Absorption
Inductively Coupled Plasma
Bench methodology
The laboratory methodology of ultra trace analysis of As, Se & Sb in environmental, medical & commercial samples.
A university textbook and a laboratory manual.
Front cover by Pelé Gouda
Graphic design, cartoon illustration and video animation.
Dr. Gouda’s scholastic and professional chemist career, his globally adopted analytical laboratory methods, and his experience as a lead scientist; promise this book to be a reference for every chemist and a must for every university.
Prof. Dr. Samuel Hein, Ph.D.
Brock University.
Image477.JPGTo order additional copies of this book please visit your local branch of any of the following chain bookstores:
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This book is also available online at:
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Because of the dynamic nature of the internet, any web addresses or links contained in this book may have changed since publication and may no longer be valid.
The views expressed in this work are solely those of the author and may not reflect the views of the publisher, and the publisher hereby disclaims any responsibility for them.
To the greatest man who has ever walked the surface of this earth, my father.
Copyright © 1994 & 2012 by Paul Gouda.
All rights reserved. No part of this book may be used, reproduced, translated, or transmitted in any form or by any means, electronic, graphical, or mechanical. This includes photocopying, recording, or using any information retrieval system, without a written permission from the author.
The preceding statement excludes the obviously permitted public use of the scientific facts utilized by this book, as well as the use of the scientific notes that have been published by the author via science sites and journals. The author also permits the use of short quotations of the material for reviews and non-commercial scholastic assignments.
ISBN: 978-1-4759-4802-8 (sc)
ISBN: 978-1-4759-4803-5 (ebk)
Canadian Intellectual Property Office.
Certificate of registration of copyright number: 1097823 Paul Gouda, Owner & Author.
Issued pursuant to sections 49 & 53 of the Copyright Act.
Library and Archives Canada Cataloguing in Publication
Gouda, Paul
Arsenic, selenium, antimony : ultra trace analysis / Paul Gouda. Includes index.
1. Arsenic—Analysis. 2. Selenium—Analysis. 3. Antimony—Analysis. 4. Ultratrace analysis. I. Title.
QP519.9.U48G68 2011 543 C2011-901291-X
American Library of Congress Control Number: 2012916152
Preface
The business of chemical analysis of environmental, medical and commercial samples has recently witnessed a large market demand as well as extensive scientific research and development.
Image484.JPGThe days of high ppm level analysis done by a lab technician via a routine bench procedure involving mere volumetric titration, gravimetric precipitation and basic AAS at ppm level are long gone. Remember the days when we used to analyze, say, Hg, via such methods as diphenylthiocarbozone? Today’s market demands qualified analytical chemists and state of the art instrumentation to deal with trace ppb and ppt detection level.
Lake water, seafood, soil, pharmaceutical products and many other samples are sent daily to analytical laboratories for several inorganic and organic analysis, and are subjected to improved regulations that specify the new acceptable limits.
Many may have heard about arsenic as a poisonous element we see in films, but many may not realize how common some elements such as arsenic, selenium and antimony are in nature, and in a variety of forms.
A few years ago, a lady friend was making coffee. As she ran out of filter papers, she innocently used a paper towel. The hot water went through the coffee and the acting filter paper as usual, but she never thought that paper towel could contain a high level of arsenic.
Why would they add arsenic to paper towels?
she asked. They don’t.
I explained. Products such as paper towels are made from recycled newspapers and other scrap wood sources and dry leaves and branches-which (like soil) may contain high levels of arsenic.
Products such as coffee paper-filters, are purified via such techniques as ion exchange and other chemical procedures-to extract arsenic. Paper towels, however, are meant for external use, and are not meant to be subjected to boiling water for one to then drink the extract! I explained.
It is of course true that the form of arsenic, selenium or antimony makes all the difference as to whether they are harmful to us or to what degree. It is also true that soaking a paper towel in boiling water may extract other chemicals that are not meant to be ingested; but that’s a different subject. Our subject here is As, Se, Sb; and one must also understand that not every form of these elements is actually a threat to our body or can be absorbed into our body. Some of these forms, especially the metallic elements, are not particularly or practically harmful to humans, while other forms are easily absorbed into our body if ingested.
It is the harmful form of such parameter that is subjected here to our chemical study.
Image493.JPGAs I indicated, we are now more health conscious than ever, and the standard of specifications (though still needs to be tightened in North America to meet the better standard in Europe)-is still much higher than it used to be.
This paper deals with inorganic and organic parameters of arsenic, selenium and antimony.
These elements are common in nature: in soil, wood trees
and wood-related products and in other sources; and in a variety of forms, both organic and inorganic.
Clearly agricultural soil is always a concern as vegetation will absorb such elements from the soil.
As well, potable water, residential sites, food and pharmaceutical products and others, each has its specific allowable limit of As, Se and Sb. Hence, the role of the analytical laboratory methodology and the appropriate analytical procedure to secure the suitable DL detection level
or detection limit
for the specific case, are a must..
The methods and the studies to follow were utilized, revolutionized and produced by Canadian chemist, Dr. Paul Gouda of Ontario, Canada; and have been well received and adopted by the scientific arena, including analytical laboratories.
The book also introduces five AAS Atomic Absorption Spectroscopy
and ICP Inductively Coupled Plasma
methods-with emphasis on Hydride Generation AAS.
These five methods were created by and have been named after the inventor chemist Dr. Paul Gouda.
This book was first produced in 1994 as a laboratory manual for bench chemists during the author’s employment as a head chemist at B.R.M.
A large portion of the material was posted in 1998-with the author’s permission-by an online science society site.
It was then published in 2001 by Great Canadian books
as a science reference.
This 3rd edition is published by Penguin Group, Iuniverse Bloomington in 2012.
Table of contents
Preface
SOP Introduction
Atomic Absorption-
Principal / theory
Hydride generation technique &
Graphite furnace tube
techniques.
Instrumentation
Digestion scheme
Calibration & Correlation coefficiency Reagents
Standards & special solutions Quality control Precautions
Analytical notes / synopsis Oxidation states
Common compounds
Oxidation of selenides
Ferric selenite
Ferrous sulfate use
Selenium halides & selenosulfates
Selenides and selenites
Thiosulfate titration
Monohaliodes Se2X2, the dihalides SeX2, the tetrahalides Selenium oxyhalides SeOX2
Permonoselenic acid H2SeO5, perdiselenic acid H2Se2O8 and Pyroselenic acid H2Se2O7
Sodium selenocyanate NaSeCN Selenocyanogen SeCN / (SeCN)2,
Selenium selenosulfate Na2SeSO3. Arsenopyrite AsFeS
Tetrahedrally hybridized arsenic Trigonal-bipyramidal or octahedral valence states
Permanganate method and the potassium bromate titration Arsenious sulfide
Primarily orthoarsenic acid, H3AsO4 Arsine [hydrogen arsenide, arsenic trihydride]
Arsine hexahydrate AsH3.6H2O Arsenic monohydride As2H2 or AsH
Tetrachlorophenylarsorane C6H5AsCL4 and Dichlorophenylarsine C6H5AsCL2.
Trihalides, but arsenic pentafluoride
Arsenic pentoxide As2O5 Hydrolysis of haloarsines Hetrocyclic organoarsines Arsines methylarsine CH3AsH2
Mimetite, Pb5Cl(AsO3)3 Erythrite, CO3(AsO4)28H2O Proustite, Ag3AsS3
Specific halogen compounds with valence +3 and +5
Crystals of H3As04(H20)0.5 Monosodium methyl arsenate Arsenic pentoxide and tribromide Arsenic trisulfide, trioxide and triiodide
Arsenate minerals Arsenide minerals Stibine SbH3
Antimonate { SbO4³-} and sodium borohydride role Stibiconite Sb3O6(OH)x, cervantite Sb2O4 or Sb2O3 / Sb2O5
Dicyclohexylstibine
Chlorodicyclohexylstibine
Phenylstibine and diphenylstibine
Diphenylstibine
The role of dialkylstibinic acids
Diazonium salt
Antimony pentachloride and aryltetrachloroantimony compound Valentenite and senarmonite Sb2O3 and kermesite Sb2S3. Trifluoromethylarsine CF3AsH2 Diarylantimony trichloride Tetraantimony dichloride pentoxide
Proustite
Copper arsenate hydroxide or basic copper arsenate
Monosodium methyl arsenate & Sodium arsenate
Arsenic pentachloride
Arsenic pentafluoride
Arsenic pentoxide
Arsenic tribromide
Arsenic trifluoride
Arsenic triiodide
Arsenic trioxide
Arsenic trisulfide
Indium arsenide antimonide phosphide
Arsenate minerals including:
Aktashite
Adamite
Abernathyite