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A Study of Phosphites a Thesis Presented to The A STUDY OF PHOSPHITES A THESIS PRESENTED TO THE UNIVERSITY OF GLASGOW IN PART FULFILMENT OF THE REQUIREMENTS FOR THE DEGREE OF DOCTOR OF PHILOSOPHY. ProQuest Number: 13849308 All rights reserved INFORMATION TO ALL USERS The quality of this reproduction is dependent upon the quality of the copy submitted. In the unlikely event that the author did not send a com plete manuscript and there are missing pages, these will be noted. Also, if material had to be removed, a note will indicate the deletion. uest ProQuest 13849308 Published by ProQuest LLC(2019). Copyright of the Dissertation is held by the Author. All rights reserved. This work is protected against unauthorized copying under Title 17, United States C ode Microform Edition © ProQuest LLC. ProQuest LLC. 789 East Eisenhower Parkway P.O. Box 1346 Ann Arbor, Ml 48106- 1346 •The work described in this thesis is the original work of the author and has not been presented for any degree at this or any other University. ACKNOWLEDGMENTS The author would like to express sincere gratitude to Dr. D.S.Payne for his untiring supervision and provocative interest in the work described in this thesis. Many fruitful discussions and arguments have been held. Thanks are also due to Dr. Nancollas, Dr. Eglinton and Dr. Porte, and the staffs of their laboratories for polarographic, infra-red and nuclear magnetic resonance data, and the interpretation of the data. A generous maintenance grant was provided by Albright and Wilson Ltd. INDEX Page General 1_2 Nomenclature 3.5 Historical Introduction 6-46 a) The early period 6-16 b) The modern period 17-46 (II) The Complexing of Pyrophosphite 47-81 with Metal Ions Compared with the Complexing of Pyrophosphate Experiments on the Solubility of 47.50 Pyrophosphates and Pyrophosphites as a Function of the Metal and Pyro- Anion Concentration Quantitative Investigation of the 50-81 Complexing of Metal Ions by Pyro­ phosphite, using Polarographic Methods a) Theoretical Introduction 50-52 b) Experimental Section 54-76 c) Discussion of Results 77-81 --- z 7 Complexing of Cd2+ by Pyrophosphite 5 4 -5 8 it tt tt tt Phosphite 9 , 5 8 -5 9 Discussion of Results for the Cd ion 5 9 -6 0 Complexing of Cu(ll), Pyrophosphite 6 1 -6 3 tt tt tt Phosphite 6 3 -6 4 Discussion of the Results for the Cu(ll) ion 6 4 -6 5 Complexing of Ni(H), Pyrophosphite 6 5 -6 7 tt tt tt Pb(ll), 68 tt tt tt Co(ll), 68-69 tt tt tt Ba2+ , 6 9 -7 0 tt tt tt Cr(III), 7 0 -7 1 tt tt tt T1|l) , 71 tt tt tt u ° r 7 2 -7 6 Page (ill) Thermogravimetric and Derived 8 2 -2 1 9 Experiments a) Some Experiments on Pyrophosph- orous Acid and Pyrophosphites 8 2 -9 9 (i) The Hydrolysis of the Pyro­ phosphite Anion 82-90 3 3 (ii) The Formation of P-O-P Bonds 9 1 -9 9 b) Some Experiments on Phosphorous Acid and Phosphites 100-119 (i) Vacuum Pyrolysis of Phosphor­ ous Acid 1 0 0 -1 0 6 (ii) Pyrolysis of Phosphorous Acid at Atmospheric Pressure 107-112 (iii) Some Salts of Phosphorous Acid, (Phosphites) 1 1 2 -1 1 9 c) General Discussion 1 2 0 -1 2 4 Experimental Section 1 2 5 -2 1 9 a) (i) The Hydrolysis of the Pyropho­ sphite Anion 1 2 5 -1 3 0 ( The Uptake of Water by Pyrophosphorous Acid 1 3 0 -1 3 1 Dehydration of the Hydrate 1 3 1 -1 3 3 The Crystals obtained by the Auger Reaction 1 3 4 -1 3 6 ) a) (ii) 3 3 The Formation of P-O-P Bonds 1 3 7 -1 5 6 ( NaH(HPO )2.5H 0 1 3 7 -1 4 2 LiH(HPOo) 143 KH(HP03> 143 RbH(HP0 3 ) 1 4 3 -1 4 4 CsH(HP0 3 )H2 0 1 4 4 -1 4 5 NH4H(HP03) 1 4 6 -1 5 0 T1H(HP03)0.25H20 150 BeH2 (HPO3 )xH20 151-152 M g H 2 (HPO3 )2x H20 1 5 2 -1 5 3 CaH2 (HPO3 )6H20 1 5 3 -1 5 4 SrH 2 (HP03 ) 2 1 5 4 -1 5 5 BaH2 (HPO3 )2 1 .5H20 1 5 5 -1 5 6 (Ill), cont., Page b) (i) Vacuum Pyrolysis of Phosphorous Acid 157-172 ( Infra-Red Spectral Study of some of the Products obtained from the Pyrolysis of Phosphorous Acid 167-170 Analytical Data on the Sub­ limate 170-172 ) b) (ii) Pyrolysis of Phosphorous Acid at Atmospheric Pressure 173-191 ( Analytical Data on the Products of Pyrolysis of Phosphorous Acid at Atmospheric Pressure 181-191 Volumetric Analyses 181-182 Paper Chromatography of the Product 183-191 Discussion of the Chromato­ graphic Results 189-191 ) b) (iii) Some Salts of Phosphorous Acid, (Phosphites) 192-219 ( Normal Phosphites 192-217 Li2HP032H20 192-193 N a 2 HP0 3 5 H 2 0 193-195 K 2 HPO 3 O .67H20 195-196 Rb 2 HP03 196-197 CsHP03 2.5 H 2 0 198-200 BeHP0 3 H 2 0 200-202 MgHP035H20 202-203 CaHP03H20 203-205 SrHP03H20 205-206 BaHP03x H20 207 T12HP03 208-209 (NH4 )2 HP03H20 209-210 CdHP03 210-212 ZnHP032H20 212 PbHP03 212-213 SnHP03 214 MnHP030.66H20 214-215 FeHP03l0H20 215 C0 HPO 3 I .5H20 215-216 (Ill), cont., b), (iii), cont., Page NiHP032 .5H20 216 (Hg(l)2 )HP03 216-217 ) Acid Phosphites NaH3 (HPO3 )2 Na2H4(HP03)3 KH3 (HP03 )2 K2H4 (HP03)2 218-219 Appendix (I) The Hydrolysis of SrH2 (HP03 )2 220-221 \ Appendix (II) The Question of Acetyl Phosphite 222-224 SUMMARY OF FINDINGS 1) The pyrophosphite anion is greatly modified as compared to the pyrophosphate anion as regards its tendency to form metal complexes in solution; pyrophosphite is a relatively weak ligand, (p. 57-81). 2) The P-O-P bond in the pyrophosphite unit will not tolerate further attachment of P-O-P bonds as in the condensed phosphates, (c.f.p. 100-119). 3) The P-H bond in the phosphite ion undergoes two types of reaction leading to formation of higher oxy-acids of phosphorus, namely breakdown to gaseous phosphine, this occurs where there are P-OH groups attached to the phosphorus, or to gaseous hydrogen, where there are no P-OH groups present, in this latter case the formation of P-P bonds is favoured in the reaction product, (c.f.112-119). 4) The kinetics of the oxidative breakdown of phosphorous acid have been elucidated in terms of a radical chain reaction, (c.f.p 107-112). 5) During the study of pyrolysis of metal phosphites numerous compounds have been prepared, simple and more complex salts of phosphorous acid which have not been described before. The properties of several salts which have been described in the literature have been more thoroughly investigated than heretofore. 6) Two types of hydrates of pyrophosphorous acid seem to be obtained best described as H- (c.f.p. 87). + HO 0*h 6h and types based on the P-Q H^O structure, (c.f.p 85). 7) For the series of alkali metal hydrogen phosphites and the corresponding alkaline earth salts the ease of P-O-P bond formation on heating is related in a simple way to the sizes of the cations, (c.f.p.91-99). Oxidative breakdown of the P-H bonds in these compounds and others are related to the same function of cations size, cross relationships between the ease of reaction and infra-red spectral data are also found particularly with the cases of P-H reactions, (c.f.96). 8) Shblimation of phosphorous acid has been investigated. The maximum amount of sublimation occurs when the pressure over the acid is such as to allow sublimation but retard the formation of pyrophosphorous acid, (c.f. p. 100-106). 9) An unknown spot has been obtained on the acid chromatograms of products from the pyrolysis of phosphorous acid. It appears in advance of pyrophosphate in acid elutions, and probably corresponds to an unknown phosphorous oxy- anion, (c.f.p 183-191). 1 0 ) Pyrolysis of Rb^HPO^ leads to a product containing most of the original oxidation-reduction equivalent of the original product but no P-H bonds are detectable by infra­ red spectroscopy (c.f.p.196-197). INTRODUCTION The following pages are devoted to the study of phosphites and related compounds. The work described was carried out in the Inorganic Department of Glasgow University under the supervision of Dr. D.S. Payne, as part of the requirements for the degree of Doctor of Philosophy of Glasgow University. Investigations were carried out from September 1959 to March I9625 preliminary work was done as part of the requirement for the degree of Bachelor of Science with Honours in Chemi­ stry during January to March in 1959* The work is presented in three main sections, the histori al section, the complexing ability of pyrophosphite for a number of metal ions and the results and tabulation of thermo- gravimetric experiments on a variety of phosphites and related compounds. This last section comprises the bulk of the work presented. It is given in two sub-sections, the first being a general account of the experiments and the second being a more detailed experimental section. 9 This work is a continuation of the work of Dr.D.S.Payne on the lower oxy-acids of phosphorus, and much of the experi­ mental data given here was obtained by repeating and extending the work of previous investigators of this school.
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