iupac-nist solubility data series. 79. alkali and alkaline...

IUPAC-NIST Solubility Data Series. 79. Alkali and Alkaline Earth MetalPseudohalides

Jiri Halaa

Department of Inorganic Chemistry, Masaryk University, Brno, Czech Republic

Contributors *EvaluatorJiri Hala*

Masaryk University, Czech Republic

H. AkaiwaGunma University, Japan

~Received 23 August 2002; accepted 4 November 2002; published online 13 February 2004!

This volume presents solubility data of azides, cyanides, cyanates, and thiocyanates ofalkali metals, alkaline earth metals, and ammonium. Covered are binary and ternarysystems in all solvents. No solubility data have been found for some of the compounds ofalkali metals, alkaline metals, and ammonium. These include beryllium and magnesiumazides, lithium, rubidium cesium, ammonium, and alkaline earth cyanates and cyanides,and beryllium thiocyanate. Likewise, no solubility data seem to exist for selenocyanatesof the mentioned metals and ammonium. The literature has been covered up to the middleof 2001, and there was a great effort to have the literature survey as complete as possible.The few documents which remained unavailable to the editor, and could not be includedin the volume, are listed in the Appendix. For some compounds it was not possible toshow the Chemical Abstracts registry numbers since these have not been assigned. Forthis reason, the registry number index is incomplete. 2004 American Institute ofPhysics. @DOI: 10.1063/1.1563591#

Key words: alkali metals; alkaline earth metals; ammonia; azides; cyanides; cyanates; organic solvents;thiocyanates; solid-liquie equilibrium; solubility; water.

Contents

1. Preface. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 32. Introduction to the Solubility Data Series:

Solubility of Solids in Liquids. . . . . . . . . . . . . . . . . 32.1. The Nature of the Project. . . . . . . . . . . . . . . . . 32.2. Compilations and Evaluations. . . . . . . . . . . . . 3

2.2.1. Compilations. . . . . . . . . . . . . . . . . . . . . . 32.2.2. Evaluations. . . . . . . . . . . . . . . . . . . . . . . 3

2.3. Quantities and Units Used in Compilationand Evaluation of Solubility Data. . . . . . . . . . 52.3.1. Mixtures, Solutions, and Solubilities... 52.3.2. Physicochemical Quantities and

Units. . . . . . . . . . . . . . . . . . . . . . . . . . . . 52.4. References for the Introduction. . . . . . . . . . . . 7

3. The Solubility of Azides. . . . . . . . . . . . . . . . . . . . . 83.1. Lithium Azide. . . . . . . . . . . . . . . . . . . . . . . . . . 83.2. Sodium Azide. . . . . . . . . . . . . . . . . . . . . . . . . . 93.3. Potassium Azide. . . . . . . . . . . . . . . . . . . . . . . . 15

a!Electronic mail: [email protected] 2004 American Institute of Physics.

0047-268920043311176$39.00 1

3.3.1. Evaluation of the KN3 H2OSystem. . . . . . . . . . . . . . . . . . . . . . . . . . . 15

3.4. Rubidium Azide. . . . . . . . . . . . . . . . . . . . . . . . 173.5. Cesium Azide. . . . . . . . . . . . . . . . . . . . . . . . . . 183.6. Ammonium Azide. . . . . . . . . . . . . . . . . . . . . . . 183.7. Calcium Azide. . . . . . . . . . . . . . . . . . . . . . . . . . 203.8. Strontium Azide. . . . . . . . . . . . . . . . . . . . . . . . 21

3.8.1. Evaluation of the Sr~N3)2 H2OSystem. . . . . . . . . . . . . . . . . . . . . . . . . . . 21

3.9. Barium Azide. . . . . . . . . . . . . . . . . . . . . . . . . . 243.9.1. Evaluation of the Ba~N3)2 H2O

System. . . . . . . . . . . . . . . . . . . . . . . . . . . 244. The Solubility of Cyanides. . . . . . . . . . . . . . . . . . . 25

4.1. Lithium Cyanide. . . . . . . . . . . . . . . . . . . . . . . . 254.2. Sodium Cyanide. . . . . . . . . . . . . . . . . . . . . . . . 26

4.2.1. Evaluation of the NaCNH2OSystem. . . . . . . . . . . . . . . . . . . . . . . . . . . 26

4.2.2. Evaluation of the NaCNNaOHH2OSystem. . . . . . . . . . . . . . . . . . . . . . . . . . . 29

4.3. Potassium Cyanide. . . . . . . . . . . . . . . . . . . . . . 334.3.1. Evaluation of the KCNNH3

System. . . . . . . . . . . . . . . . . . . . . . . . . . . 364.3.2. Evaluation of the KCNEthanol

J. Phys. Chem. Ref. Data, Vol. 33, No. 1, 2004

22 IUPAC-NIST SOLUBILITY DATA SERIES

System. . . . . . . . . . . . . . . . . . . . . . . . . . . 375. The Solubility of Cyanates. . . . . . . . . . . . . . . . . . . 46

5.1. Sodium Cyanate. . . . . . . . . . . . . . . . . . . . . . . . 465.1.1. Evaluation of the NaOCNNH3

System. . . . . . . . . . . . . . . . . . . . . . . . . . . 465.2. Potassium Cyanate. . . . . . . . . . . . . . . . . . . . . . 50

6. The Solubility of Thiocyanates. . . . . . . . . . . . . . . . 526.1. Lithium Thiocyanate. . . . . . . . . . . . . . . . . . . . . 52

6.1.1. Evaluation of the LiSCNH2OSystem. . . . . . . . . . . . . . . . . . . . . . . . . . . 52

6.2. Sodium Thiocyanate. . . . . . . . . . . . . . . . . . . . . 596.2.1. Evaluation of the NaSCNH2O

System. . . . . . . . . . . . . . . . . . . . . . . . . . . 596.2.2. Evaluation of the NaSCNEthanol

System. . . . . . . . . . . . . . . . . . . . . . . . . . . 656.2.3. Evaluation of the NaSCNAcetone

System. . . . . . . . . . . . . . . . . . . . . . . . . . . 676.3. Potassium Thiocyanate. . . . . . . . . . . . . . . . . . . 82

6.3.1. Evaluation of the KSCNH2OSystem. . . . . . . . . . . . . . . . . . . . . . . . . . . 82

6.3.2. Evaluation of the KSCNEthanolSystem. . . . . . . . . . . . . . . . . . . . . . . . . . . 90

6.3.3. Evaluation of the KSCNAcetoneSystem. . . . . . . . . . . . . . . . . . . . . . . . . . . 91

6.3.4. Evaluation of the KSCN2-ButanoneSystem. . . . . . . . . . . . . . . . . . . . . . . . . . . 93

6.3.5. Evaluation of the KSCN1-ButanolSystem. . . . . . . . . . . . . . . . . . . . . . . . . . . 94

6.3.6. Evaluation of the KSCNPyridineSystem. . . . . . . . . . . . . . . . . . . . . . . . . . . 95

6.4. Rubidium Thiocyanate. . . . . . . . . . . . . . . . . . . 1196.5. Cesium Thiocyanate. . . . . . . . . . . . . . . . . . . . . 1216.6. Ammonium Thiocyanate. . . . . . . . . . . . . . . . . . 122

6.6.1. Evaluation of the NH4SCNH2OSystem. . . . . . . . . . . . . . . . . . . . . . . . . . . 122

6.7. Magnesium Thiocyanate. . . . . . . . . . . . . . . . . . 1466.8. Calcium Thiocyanate. . . . . . . . . . . . . . . . . . . . . 1486.9. Strontium Thiocyanate. . . . . . . . . . . . . . . . . . . 1546.10. Barium Thiocyanate. . . . . . . . . . . . . . . . . . . . 155

6.10.1. Evaluation of the Ba~SCN)2 H2OSystem. . . . . . . . . . . . . . . . . . . . . . . . . . 155

7. Appendix. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1628. System Index. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1649. Registry Number Index. . . . . . . . . . . . . . . . . . . . . . 16810. Author Index. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 170

List of Tables1. Interconversions between quanties used as

measures of solubilities. . . . . . . . . . . . . . . . . . . . . . 7

List of Figures1. Lithium azidewater system. . . . . . . . . . . . . . . . . . 82. Sodium azidewater system. . . . . . . . . . . . . . . . . . 103. Potassium azidewater system. . . . . . . . . . . . . . . . 164. Ammonium azideammonia system. . . . . . . . . . . . 195. Sodium cyanidesodium hydroxidewater

system. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 31


6. Sodium cyanateammonia system. . . . . . . . . . . . . 467. Sodium cyanatediethylethermethanol

system. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 498. Lithium thiocyanatewater system. . . . . . . . . . . . . 529. Sodium thiocyanatewater system. . . . . . . . . . . . . 6010. Sodium thiocyanateammonia system. . . . . . . . . . 6411. Sodium thiocyanateacetone system. . . . . . . . . . . . 6712. Sodium thiocyanatemethylthiocyanatewater

system. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8013. Potassium thiocyanatewater system. . . . . . . . . . . 8214. Potassium thiocyanatewater system. . . . . . . . . . . 8515. Potassium thiocyanateammonia system. . . . . . . . 8816. Potassium thiocyanatepotassium carbonate

water system. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 10717. Potassium thiocyanateureawater system. . . . . . . 11118. Potassium thiocyanatewateracetone system. . . . 11319. Potassium thiocyanatepolyethylene~1500!

water system. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 11520. Potassium thiocyanatepolyethylene~6000!

water system. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 11621. Potassium thiocyanatemethylthiocyanatewater

system. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 11622. Potassium thiocyanateethylthiocyanatewater

system. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 11723. Ammonium thiocyanatewater system. . . . . . . . . . 12224. Ammonium thiocyanatewater system. . . . . . . . . . 12425. Ammonium thiocyanateammonia system. . . . . . . 12726. Ammonium thiocyanateammonium nitrate

water system. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 13227. Ammonium thiocyanatepotassium thiocyanate

water system. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 13428. Ammonium thiocyanatepotassium thiocyanate

water system. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 13629. Ammonium thiocyanateammonium sulfate

water system. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 13930. Ammonium thiocyanatetriethylaminewater

system. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 14131. Ammonium thiocyanateureawater system. . . . . 14232. Ammonium thiocyanatemethylthiocyanate

water system. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 14333. Ammonium thiocyanateanilinewater system. . . 14434. Calcium thiocyanatesodium thiocyanatewater

system. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 15035. Calcium thiocyanatepotassium thiocyanate

water system. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 15136. Calcium thiocyanateammonium thiocyanate

water system. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 15237. Calcium thiocyanatemethylthiocyanatewater

system. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 15238. Barium thiocyanatesodium thiocyanatewater

system. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 15639. Barium thiocyanatepotassium thiocyanate

water system. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 15740. Barium thiocyanatemethylthiocyanatewater

system. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 159

33JIRI HALA

1. Preface

This volume presents solubility data of azides, cyanides,cyanates, and thiocyanates of alkali metals, alkaline earthmetals, and ammonium. Covered are binary and ternary sys-tems in all solvents. No solubility data have been found forsome of the compounds of alkali metals, alkaline metals, andammonium. These include beryllium and magnesium azides,lithium, rubidium cesium, ammonium, and alkaline earth cy-anates and cyanides, and beryllium thiocyanate. Likewise, nosolubility data seem to exist for selenocyanates of the men-tioned metals and ammonium. The literature has been cov-ered up to the middle of 2001, and there was a great effort tohave the literature survey as complete as possible. The fewdocuments which remained unavailable to the compiler, andcould not be included in the volume are listed in the Appen-dix. For some compounds it was not possible to show theChemical Abstracts registry numbers since these have notbeen assigned. For this reason, the registry number index isincomplete.

In addition to documents that published numerical data,some papers that presented data in graphical form only wereincluded as well. They were considered for the volume eitherif no other data were available for the system, or if the datawere published in difficult to obtain older literature. Thesecriteria led the compiler to include sometimes papers inwhich the authors failed to specify conditions such as tem-perature, equilibrium time, or methods of analysis. Phasediagrams have been included for some of the ternary sys-tems. For binary eutonic systems, phase diagrams were in-cluded only if no numerical data were reported in the origi-nal documents and the diagrams were the sole source ofinformation. Of the many systems covered by the volume,relatively few were studied by more than one laboratory.Thus the opportunity to carry out evaluations has been lim-ited, and only 20 systems have been evaluated. However,because of some uncertainty in most of the evaluated sys-tems, only tentative solubility values could usually be rec-ommended.

Only those published results that report meaningful datawere considered for the volume. Papers that reported quali-tative results with statements like sparingly soluble or in-soluble, etc., were not considered. However, some docu-ments reported solubility data which, although not includedin the volume for one reason or other ~e.g., single values ofuncertain quality without any supporting information,sketches of phase diagrams!, may nevertheless be of someinformative value to the potential user of this volume in casethey represent the only information available for a given sys-tem. For this reason, a list of systems for which only suchdata exist has been included in the Appendix.

The editor wishes to express his thanks to the followingcolleagues from IUPAC for their effort in proving copies ofpublications, which would otherwise not be available to him:Professor H. Akaiwa, Gunma, Japan ~also for translating theJapanese papers!; D. J. J. Counioux, Lyon, France; Dr. P. G.T. Fogg, London, U.K.; Professor Fu Jufu, Beijing, China;

Dr. H. J. M. Grunbauer, Amsterdam, The Netherlands; Dr. A.Maczynski, Warsaw, Poland; Professor P. Paoletti, Florence,Italy; Professor V. M. Valyashko, Moscow, Russia; and Pro-fessor B. A. Wolf, Mainz, Germany. Without their help thevolume would not be complete.

2. Introduction to the Solubility Data Series:Solubility of Solids in Liquids

2.1. The Nature of the Project

The Solubility Data project ~SDP! has as its aim a com-prehensive review of published data for solubilities of gases,liquids, and solids in liquids or solids. Data of suitable pre-cision are compiled for each publication on data sheets in auniform format. The data for each system are evaluated and,where data from independent sources agree sufficiently, rec-ommended values are proposed. The evaluation sheets, rec-ommended values, and compiled data sheets are publishedon consecutive pages.

2.2. Compilations and Evaluations

The formats for the compilations and critical evaluationshave been standardized for all volumes. A description ofthese formats follows.

2.2.1. Compilations

The format used for the compilations is, for the most part,self-explanatory. Normally, a compilation sheet is dividedinto boxes, with detailed contents described below.

Components

Each component is listed according to IUPAC name, for-mula, and Chemical Abstracts ~CA! Registry Number. TheChemical Abstracts name is also included if this differs fromthe IUPAC name, as are trivial names if appropriate. IUPACand common names are cross-referenced to Chemical Ab-stracts names in the System Index.

The formula is given either in terms of the IUPAC or Hill1

system and the choice of formula is governed by what isusual for most current users: i.e., IUPAC for inorganic com-pounds, and Hill system for organic compounds. Compo-nents are ordered on a given compilation sheet according to:

~a! saturating components;~b! non-saturating components;~c! solvents.In each of ~a!, ~b! or ~c!, the components are arranged in

order according to the IUPAC 18-column periodic table withtwo additional rows:

Columns 1 and 2: H, alkali elements, ammonium, alkalineearth elements

Columns 3 to 12: transition elementsColumns 13 to 17: boron, carbon, nitrogen groups; chal-

cogenides, halogensColumn 18: noble gasesRow 1: Ce to Lu



Row 2: Th to the end of the known elements, in order ofatomic number.

The same order is followed in arranging the compilationsheets within a given volume.

Original Measurements

References are abbreviated in the forms given by Chemi-cal Abstracts Service Source Index ~CASSI!. Names origi-nally in other than Roman alphabets are given as transliter-ated by Chemical Abstracts. In the case of multiple entries~for example, translations! an asterisk indicates the publica-tion used for compilation of the data.

Variables

Ranges of temperature, pressure, etc., are indicated here.

Prepared by

The names of all compilers are given here.

Experimental Data

Components are described as ~1!, ~2!, etc., as defined inthe Components box. Data are reported in the units usedin the original publication, with the exception that modernnames for units and quantities are used; e.g., mass percentfor weight percent; mol dm23 for molar; etc. Usually, onlyone type of value ~e.g., mass percent! is found in the originalpaper, and the compiler has added the other type of value~e.g., mole percent! from computer calculations based on1989 atomic weights.2 Temperatures are expressed as t/C,t/F or T/K as in the original; if necessary, conversions toT/K are made, sometimes in the compilations and always inthe critical evaluation. However, the authors units are ex-pressed according to IUPAC recommendations3 as far as pos-sible.

Errors in calculations, fitting equations, etc., are noted, andwhere possible corrected. Material inserted by the compileris identified by the word compiler or by the compilersname in parentheses or in a footnote. In addition, compiler-calculated values of mole or mass fractions are included ifthe original data do not use these units. If densities are re-ported in the original paper, conversions from concentrationsto mole fractions are included, but otherwise this is done inthe evaluation, with the values and sources of the densitiesbeing quoted and referenced.

Details of smoothing equations ~with limits! are includedif they are present in the original publication and if the tem-perature or pressure ranges are wide enough to justify thisprocedure and if the compiler finds that the equations areconsistent with the data.

The precision of the original data is preserved when de-rived quantities are calculated, if necessary by the inclusionof one additional significant figure. In some cases, compilersnote that numerical data have been obtained from publishedgraphs using digitizing techniques. In these cases, the preci-sion of the data can be determined by the quality of the


original graph and the limitations of the digitizing technique.In some cases graphs have been included, either to illustratedata more clearly, or if this is the only information in theoriginal. Full grids are not usually inserted as it is not in-tended that users should read data from the graphs.

Method

The apparatus and procedure are mentioned briefly. Abbre-viations used in Chemical Abstracts are often used here tosave space, reference being made to sources of further detailif these are cited in the original paper.

Source and Purity of Materials

For each component, referred to as ~1!, ~2!, etc., the fol-lowing information ~in this order and in abbreviated form! isprovided if available in the original paper: source and speci-fied method of preparation; properties; degree of purity.

Estimated Error

If estimated errors were omitted by the original authors,and if relevant information is available, the compilers haveattempted to estimate errors ~identified by compiler or thecompilers name in parentheses or in a footnote! from theinternal consistency of data and type of apparatus used.Methods used by the compilers for estimating and reportingerrors are based on Ku and Eisenhart.4

Comments andor Additional Data

Many compilations include this section which providesshort comments relevant to the general nature of the work oradditional experimental and thermodynamic data which arejudged by the compiler to be of value to the reader.

References

The format for these follows the format for the OriginalMeasurements box, except that final page numbers are omit-ted. References ~usually cited in the original paper! are givenwhere relevant to interpretation of the compile data, or wherecross-reference can be made to other compilations.

2.2.2. Evaluations

The evaluators task is to assess the reliability and qualityof the data, to estimate errors where necessary, and to rec-ommend best values. The evaluation takes the form of asummary in which all the data supplied by the compiler havebeen critically reviewed. There are only three boxes on atypical evaluation sheet, and these are described below.

Components

The format is the same as on the Compilation sheets.

55JIRI HALA

Evaluator

The name and affiliation of the evaluator~s! and date up towhich the literature was checked.

Critical Evaluation

~a! Critical text. The evaluator checks that the compileddata are correct, assesses their reliability and quality, esti-mates errors where necessary, and recommends numericalvalues based on all the published data ~including theses, pat-ents and reports! for each given system. Thus, the evaluatorreviews the merits or shortcomings of the various data. Onlypublished data are considered. Documented rejection ofsome published data may occur at this stage, and the corre-sponding compilations may be removed.

The solubility of comparatively few systems is knownwith sufficient accuracy to enable a set of recommended val-ues to be presented. Although many systems have been stud-ied by at least two workers, the range of temperatures isoften sufficiently different to make meaningful comparisonimpossible.

Occasionally, it is not clear why two groups of workersobtained very different but internally consistent sets of re-sults at the same temperature, although both sets of resultswere obtained by reliable methods. In such cases, a definitiveassessment may not be possible. In some cases, two or moresets of data have been classified as tentative even though thesets are mutually inconsistent.

~b! Fitting equations. If the use of a smoothing equation isjustifiable the evaluator may provide an equation represent-ing the solubility as a function of the variables reported onall the compilation sheets, stating the limits within which itshould be used.

~c! Graphical summary. In addition to ~b! above, graphicalsummaries are often given.

~d! Recommended values. Data are recommended if the re-sults of at least two independent groups are available andthey are in good agreement, and if the evaluator has no doubtas to the adequacy and reliability of the applied experimentaland computational procedures. Data are reported as tentativeif only one set of measurements is available, or if the evalu-ator considers some aspect of the computational or experi-mental method as mildly undesirable but estimates that itshould cause only minor error. Data are considered as doubt-ful if the evaluator considers some aspect of the computa-tional or experimental method as undesirable but still consid-ers the data to have some value where the order of magnitudeof the solubility is needed. Data determined by an inadequatemethod or under ill-defined conditions are rejected. How-ever, references to these data are included in the evaluationtogether with a comment by the evaluator as to the reason fortheir rejection.

~e! References. All pertinent references are given here, in-cluding all those publications appearing in the accompanyingcompilation sheets and those which, by virtue of their poorprecision, have been rejected and not compiled.

~f! Units. While the original data may be reported in theunits used by the investigators, the final recommended valuesare reported in SI units3 when the data can be accuratelyconverted.

2.3. Quantities and Units Used in Compilation andEvaluation of Solubility Data

2.3.1. Mixtures, Solutions and Solubilities

A mixture5 describes a gaseous, liquid or solid phase con-taining more than one substance, where the substances are alltreated in the same way.

A solution5 describes a liquid or solid phase containingmore than one substance, when for convenience one of thesubstances, which is called the solvent, and may itself be amixture, is treated differently than the other substances,which are called solutes. If the sum of the mole fractions ofthe solutes is small compared to unity, the solution is calleda dilute solution.

The solubility of a solute 1 ~solid, liquid or gas! is theanalytical composition of a saturated solution, expressed interms of the proportion of the designated solute in a desig-nated solvent.6

Saturated implies equilibrium with respect to the pro-cesses of dissolution and precipitation; the equilibrium maybe stable or metastable. The solubility of a substance inmetastable equilibrium is usually greater than that of thesame substance in stable equilibrium. ~Strictly speaking, it isthe activity of the substance in metastable equilibrium that isgreater.! Care must be taken to distinguish true metastabilityfrom supersaturation, where equilibrium does not exist.

Either point of view, mixture or solution, may be taken indescribing solubility. The two points of view find their ex-pression in the reference states used for definition of activi-ties, activity coefficients and osmotic coefficients.

Note that the composition of a saturated mixture ~or solu-tion! can be described in terms of any suitable set of thermo-dynamic components. Thus, the solubility of a salt hydrate inwater is usually given as the relative proportions of anhy-drous salt in solution, rather then the relative proportions ofhydrated salt and water.

2.3.2. Physicochemical Quantities and Units

Solubilities of solids have been the subject of research fora long time, and have been expressed in a great many ways,as described below. In each case, specification of the tem-perature and either partial or total pressure of the saturatinggaseous component is necessary. The nomenclature and unitsfollow, where possible, IUPAC Green Book.3 A few quanti-ties follow the ISO standards7 or the German standard;8 see areview by Cvitas9 for details.

A Note on Nomenclature

The nomenclature of the IUPAC Green Book3 calls thesolute component B and the solvent component A. In com-pilations and evaluations, the first-named component ~com-



ponent 1! is the solute, and the second ~component 2 for atwo-component system! is the solvent. The reader shouldbear these distinctions in nomenclature in mind when com-paring equations given here with those in the Green Book.

1. Mole fraction of substance 1, x1 or x~1! ~condensedphases!, y1 ~gases!:

x15n1Y (s51

c

ns ~1!

where ns is the amount of substance of s, and c is the numberof distinct substances present ~often the number of thermo-dynamic components in the system!. Mole percent of sub-stance 1 is 100 x1.

2. Ionic mole fractions of salt i, xi1, xi2: For mixture ofs binary salts i, each of which ionizes completely into ni1cations and v i2 anions, with v i5v i11v i2 and a mixture ofp nonelectrolytes k, of which some may be considered assolvent components, a generalization of the definition inRobinson and Stokes10 gives:

x1i5v1ix1i

11(j51

s

~v j21 !x j

, x2i5v2ix1i

v1ii51...s ~2!

xok5x j

11(j51

s

~v j21 !x j

, k5~s11 !. . .c . ~3!

The sum of these mole fractions is unity, so that, with c5s1p ,

(i51

s

~x1i1x2i!1 (i5s11

c

xoi51. ~4!

General conversions to other units in multicomponent sys-tems are complicated. For a three-component system con-taining nonelectrolyte 1, electrolyte 2, and solvent 3,

x15v12xo1

v122~v221 !x12x25

x12v122~v221 !x12

. ~5!

These relations are used in solubility equations for salts, andfor tabulation of salt effects on solubilities of gases.

3. Mass fraction of substance 1, w1 or w~1!:

w15g1Y (s51

c

gs ~6!

where gs is the mass of substance s. Mass percent of sub-stance 1 is 100 w1. The equivalent terms weight fraction,weight percent and g(1)/100g solution are no longer used.

4. Solute mole fraction of substance 1, xv ,1:

xs ,15m1Y (s51

c8

ms5x1Y (s51

c8

xs ~7!

where c8 is the number of solutes in the mixture. Thesequantities are sometimes called Janecke mole ~mass!fractions.11,12 Solute mass fraction of substance 1, ws ,1, isdefined analogously.


5. Solvent mole fraction of substance 1, xv ,1:

xv ,15x1Y (s51

p

xs. ~8!

Here, p is the number of solvent components in the mixture.Solvent mass fraction of substance 1, wv ,1, is defined analo-gously.

6. Molality of solute 1 in a solvent 2, m1:

m15n1/n2M 2 ~9!

SI base units: mol kg21. Here, M 2 is the molar mass of thesolvent.

7. Aquamolality, Solvomolality of substance 1 in a mixedsolvent with components 2, 3,13 m1

(3):

m1~3 !5m1M /M 3 ~10!

SI base units: mol kg21. Here, the average molar mass of thesolvent is

M5xv ,2M 21~12vv ,2!M 3 ~11!

and xv, is the solvent mole fraction of component 2. Thisterm is used most frequently in discussing comparative solu-bilities in water ~component 2! and heavy water ~component3! and in their mixtures.

8. Amount concentration of solute 1 in a solution of vol-ume V, c1:

c15@formula of solute#5n1/V ~12!

SI base units: mol cm23. The symbol c1 is preferred to @for-mula of solute#, but both are used. The old terms molarity,molar and moles per unit volume are no longer used.

9. Mass concentration of solute 1 in a solution of volumeV, r1:

r15g1/V5c1M 1/V ~13!

SI base units: kg m23.

10. Mole ratio, rA,B ~dimensionless!:9

rn ,125n1/n2 . ~14!

Mass ratio, symbol zA,B, may be defined analogously.9

11. Ionic strength, Im ~molality basis!, or Ic ~concentrationbasis!:

Im51

2(i mizi2, Ic5

1

2(i c iz i2 ~15!

where zi is the charge number of ion i. While these quantitiesare not used generally to express solubilities, they are used toexpress the compositions of nonsaturating components. For asingle salt i with ions of charge numbers z1 and z2,

Im5uz1z2uvmi, Ic5uz1z2uvci. ~16!

Mole and mass fractions and mole ratios are appropriate toeither the mixture of the solution point of view. The otherquantities are appropriate to the solution point of view only.Conversions between pairs of these quantities can be carriedout using the equation given in Table 1 at the end of thisIntroduction. Other useful quantities will be defined in theprefaces to individual volumes or on specific data sheets.

77JIRI HALA

TABLE 1. Interconversions between quantities used as measures of solubilities c-component systems containing c-1 solutes i and single solvent c ~rdensityof solution; M imolar masses of i. For relations for two-component systems, set summations to 0.!

xi wi mi ci

xi5 xi

1

11MiMc

H 1wi 21 1 (j1c21 SMcMj 21D wjwi J

1

111

miMc1(

ji

c21mjmi

1

111

McSrci 2MiD 1(ji

c21cjci

S12 MjMcDwi5

1

11McMi

H1xi 211(jic21 SMjMc 21D xjxiJ wi

1

111

miMiS11(

ji

c21

mjMjDciMi

r

mi51

Mc S1xi 21 2(jic21

xjxiD

1

MiS 1wi 212(jic21

wjwiD mi

1

1

ciSr2(

ji

c21

cjMjD 2Mici5

r

Mi1McH1xi 211(jic21 SMjMc 21D xjxiJ

rwiMi

r

1

miS11(

ji

c21

mjMjD1Mj ci

Salt hydrates are generally not considered to be saturatingcomponents since most solubilities are expressed in terms ofthe anhydrous salt. The existence of hydrates or solvates isnoted carefully in the critical evaluation.

Mineralogical names are also quoted, along with their CARegistry Numbers, again usually in the text and CA RegistryNumbers ~where available! are given usually in the criticalevaluation.

In addition to the quantities defined above, the followingare useful in conversions between concentrations and otherquantities.

12. Density, r:

r5g/V5(s51

c

rs ~17!

SI base units: kg m23. Here g is the total mass of the system.

13. Relative density, d5r/r: the ratio of the density of amixture at temperature t, pressure p to the density of a ref-erence substance at temperature t8, pressure p8. For liquidsolutions, the reference substance is often water at 4 ~C!, 1bar. ~In some cases 1 atm is used instead of 1 bar.! The termspecific gravity is no longer used.

Thermodynamics of Solubility

Thermodynamic analysis of solubility phenomena pro-vides a rational basis for the construction of functions torepresent solubility data, and thus aids in evaluation, andsometimes enables thermodynamic quantities to be extracted.Both these aims are often difficult to achieve because of alack of experimental or theoretical activity coefficients.Where thermodynamic quantities can be found, they are notevaluated critically, since this task would involve examina-tion of a large body of data that is not directly relevant tosolubility. Where possible, procedures for evaluation are

based on established thermodynamic methods. Specific pro-cedures used in a particular volume will be described in thePreface to this volume.

2.4 References for the Introduction

1 E. A. Hill, J. Am. Chem. Soc. 22, 478 ~1900!.2 IUPAC Commission on Atomic Weights and Isotopic Abundances, PureAppl. Chem. 63, 975 ~1989!.

3 I. Mills et al., eds. Quantities, Units and Symbols in Physical Chemistry~the Green Book!~Blackwell Scientific Publications, Oxford, U.K., 1993!.

4 H. H. Ku, p. 73; C. Eisenhart, p. 69; in H. H. Ku, ed., Precision Measure-ment and Calibration, NBS Special Publication 300 ~NBS, Washington,1969!, Vol. 1.

5 V. Gold et al., eds., Compendium of Analytical Nomenclature ~the GoldBook! ~Blackwell Scientific Publications, Oxford, U.K., 1987!.

6 H. Freiser and G. H. Nancollas, eds., Compendium of Analytical Nomen-clature ~the Orange Book! ~Blackwell Scientific Publications, Oxford,U.K., 1987!, Sect. 9.1.8.

7 ISO Standards Handbook, Quantities and Units ~International StandardsOrganization, Geneva, 1993!.

8 German Standard, DIN 1310, Zusammensetzung von Mischphasen ~BeuthVerlag, Berlin, 1984!.

9 T. Cvitas, Chem. International 17, 123 ~1995!.10 R. A. Robinson and R. H. Stokes, Electrolyte Solutions, 2nd ed. ~Butter-

worths, London, 1959!.11 E. Janecke, Z. Anorg. Chem. 51, 132 ~1906!.12 H. L. Friedman, J. Chem. Phys. 32, 1351 ~1960!.13 J. W. Lorimer, in Alkali Metal and Ammonium Chlorides in Water and

Heavy Water (Binary Systems), edited by R. Cohen-Adad, and J. W.Lorimer, IUPAC Solubility Data Series, Vol. 47 ~Pergamon, Oxford, U.K.,1991!, p. 495.

This section was written by:R. Cohen-Adad J. W. Lorimer

Villeurbanne, France London, Ontario, CanadaM. Salomon M.-T. Saugier-Cohen Adad

Sea Bright, N.J., USA Villeurbanne, FranceDecember, 1995


Tem

pera

ture

:no

tre

port

ed.

Solu

bilit

y:in

suffi

cien

tda

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ven

toal

low

for

erro

res

timat

e.

Ref

eren

ces:

1 T.

Cur

tius,

Ber

.24

,33

41~1

891!

.

mpo

nent

s:O

rigi

nal

Mea

sure

men

ts:

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ium

azid

e;L

iN3

;@1

9597

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4#W

ater

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2O

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732-

18-5

#A

.P.

Rol

let

and

J.W

ohlg

emut

h,C

ompt

.R

end.

199,

1772

4

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4!.

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dB

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mpe

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mpo

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FIG

.1.

Phas

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poly

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data

from

Cur

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and

Ris

som

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edby

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.


3.T

he

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Azi

des

3.1.

Lit

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e

Com

pone

nts:

Ori

gina

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easu

rem

ents

:

~1!

Lith

ium

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Cur

tius

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Che

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58,

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30

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.

Var

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3

289

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Exp

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wat

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nol

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ent

tem

pera

ture

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Solv

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Tem

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(t/

C)

LiN

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3

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/mol

kg2

1)b

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732-

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#10

36.1

27.

377

15.5

62.0

712

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1666

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13.5

6

Eth

anol

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2H

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;@6

4-17

-5#

1620

.26

4.14

a Sol

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ases

wer

eno

tin

vest

igat

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b Cal

cula

ted

byco

mpi

ler.

Add

ition

alin

form

atio

n:Sa

tura

ted

solu

tions

ofL

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inw

ater

show

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kalin

ere

actio

n.

Aux

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form

atio

n

Met

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App

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roce

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:So

urce

and

Pur

ity

ofM

ater

ials

:

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isot

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alm

etho

dw

asus

ed.

Exc

ess

salt

was

kept

inco

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tw

ithth

eso

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tfo

rse

vera

lw

eeks

unde

roc

casi

onal

stir

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with

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tem

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tw

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wat

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and

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yzed

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for

LiN

3(%

):N

85.6

7

86.0

2/85

.71,

Li

14.0

9

14.1

8/14

.29.

The

bari

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ide

used

was

prep

ared

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ssol

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Ba~

OH

) 2in

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HN

3.

The

latte

rw

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with

dilu

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2SO

4

ofei

ther

Pb~N

3) 2

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urtiu

s.1

Puri

tyof

wat

erno

tsp

ecifi

ed.A

bsol

ute

etha

nol

was

used

.

Est

imat

edE

rror

:

Co

~1!

~2!

Va

Te Sig

a R b C c A


3.2.

So

diu

mA

zid

e

mpo

nent

s:O

rigi

nal

Mea

sure

men

ts:

Sodi

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ide;

NaN

3;

@266

28-2

2-8#

Solv

ents

T.C

urtiu

san

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Ris

som

,J.

Prak

t.C

hem

.58

,26

1

309

~189

8!.

riab

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dB

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K:

283

29

0J.

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a

Exp

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enta

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ata

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bilit

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NaN

3in

wat

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nol

atdi

ffer

ent

tem

pera

ture

sa

Solv

ent

Tem

pera

ture

(t/

C)

NaN

3

(g/1

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solv

ent!

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3

(m1

/mol

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1)b

ater

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178

15.2

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1

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hano

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-5#

160.

3153

0.04

85

olid

phas

esw

ere

not

inve

stig

ated

.al

cula

ted

byco

mpi

ler.

ditio

nal

info

rmat

ion:

Satu

rate

dso

lutio

nsof

NaN

3in

wat

ersh

owed

alka

line

reac

tion.

Aux

iliar

yIn

form

atio

n

etho

dA

ppar

atusP

roce

dure

:So

urce

and

Pur

ity

ofM

ater

ials

:

isot

herm

alm

etho

dw

asus

ed.

Exc

ess

salt

was

kept

innt

act

with

the

solv

ent

for

seve

ral

wee

ksun

der

occa

sion

alrr

ing

ina

room

with

cons

tant

tem

pera

ture

.E

quili

briu

mpe

ratu

rew

asm

easu

red

inth

esa

tura

ted

solu

tions

prio

rth

draw

alof

the

sam

ples

.Aw

eigh

edam

ount

ofth

esa

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ted

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apor

ated

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ied

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until

cons

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was

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ined

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NaN

3w

aspr

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edby

neut

raliz

ing

8%aq

ueou

sso

lutio

nof

HN

3

with

NaO

H.T

heso

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nof

the

acid

was

obta

ined

bydi

still

atio

nw

ithdi

lute

H2SO

4of

eith

erPb

~N3) 2

orN

H4N

3ac

cord

ing

toC

urtiu

s.1

NaN

3w

asre

crys

talli

zed

from

wat

er,

and

drie

dov

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ncen

trat

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2SO

4in

ava

cuum

dess

icat

or.

Ana

lysi

s,fo

und/

calc

ulat

edfo

rN

aN3

~%!:

Na

35.3

1

35.3

5/35

.38.

Puri

tyof

wat

erno

tsp

ecifi

ed.A

bsol

ute

etha

nol

was

used

.

Est

imat

edE

rror

:Te

mpe

ratu

re:

not

repo

rted

.So

lubi

lity:

insu

ffici

ent

data

give

nto

allo

wfo

rer

ror

estim

ate.

Ref

eren

ces:

1 T.

Cur

tius,

Ber

.24

,33

41~1

891!

.

99JIRI HALA

. Phys. Chem. Ref. Data, Vol. 33, No. 1, 2004

Aux

iliar

yIn

form

atio

n

Met

hod

App

arat

usP

roce

dure

:So

urce

and

Pur

ity

ofM

ater

ials

:

Free

zing

curv

ew

asob

tain

edby

poly

ther

mal

met

hod.

The

solu

bilit

ycu

rve

was

obta

ined

byis

othe

rmal

met

hod.

Exc

ess

salt

was

equi

libra

ted

with

wat

erin

ath

erm

osta

tfo

r1

day

incl

osed

vess

els.

Inth

esa

tura

ted

solu

tions

,az

ide

was

prec

ipita

ted

with

AgN

O3

,an

dsu

bseq

uent

lyde

term

ined

grav

imet

rica

llyas

AgC

l,lit

hium

was

dete

rmin

edgr

avim

etri

cally

asL

i 2SO

4.

Coo

ling

curv

esw

ere

obta

ined

bypo

lyth

erm

alm

etho

d,th

etim

ene

cess

ary

tore

ach

equi

libri

umw

asno

tsp

ecifi

ed.

Itw

asst

ated

that

equi

libri

umw

asat

tain

edve

rysl

owly

,an

dth

atth

esy

stem

ssh

owed

cons

ider

able

tend

ency

tosu

pers

atur

atio

nev

enw

hen

inoc

ulat

ed.

No

deta

ilsre

port

ed.

Est

imat

edE

rror

:Te

mpe

ratu

re:

60.

1

0.5

K~a

utho

rs!.

Solu

bilit

y:10

0w

1:6

0.3%

0.

4%~a

utho

rs!.

Ref

eren

ces:

1 T.

Cur

tius

and

J.R

isso

m,

J.Pr

akt.

Che

m.

58,

261

~189

8!.

Co

~1!

~2!

Va

T/ W Et

a S b C Ad

M An

co sti

tem

wi

so de

J

FIG

.2.

Phas

edi

agra

mof

the

NaN

3

H2O

syst

em@~

full

circ

les!

poly

ther

mal

mea

sure

men

ts;

~ope

nci

rcle

s!is

othe

rmal

mea

sure

men

ts;

~tri

angl

es!

data

from

Cur

tius

and

Ris

som

,1in

clud

edby

the

auth

or#.

Aux

iliar

yIn

form

atio

n

etho

dA

ppar

atusP

roce

dure

:So

urce

and

Pur

ity

ofM

ater

ials

:

efr

eezi

ngcu

rve

was

obta

ined

bypo

lyth

erm

alm

etho

d.T

helu

bilit

ycu

rve

was

obta

ined

byis

othe

rmal

met

hod.

Exc

ess

tw

aseq

uilib

rate

dw

ithw

ater

ina

ther

mos

tat

for

1da

yin

sed

vess

els.

Insa

mpl

esof

the

satu

rate

dso

lutio

ns,

azid

ew

asci

pita

ted

with

AgN

O3

,an

dsu

bseq

uent

lyde

term

ined

vim

etri

cally

asA

gCl,

sodi

umw

asde

term

ined

vim

etri

cally

asN

a 2SO

4.

Coo

ling

curv

esw

ere

obta

ined

byly

ther

mal

met

hod.

Equ

ilibr

ium

time

was

not

spec

ified

.

No

deta

ilsre

port

ed.

Est

imat

edE

rror

:In

suffi

cien

tda

tare

port

edto

allo

wfo

rer

ror

estim

ate.

Ref

eren

ces:

1 T.

Cur

tius

and

J.R

isso

m,

J.Pr

akt.

Che

m.

58,

261

~189

8!.


Com

pone

nts:

Ori

gina

lM

easu

rem

ents

:

~1!

Sodi

umaz

ide;

NaN

3;

@266

28-2

2-8#

~2!

Wat

er;

H2O

;@7

732-

18-5

#J.

Woh

lgem

uth,

Com

pt.

Ren

d.19

8,60

1

3~1

934!

.

Var

iabl

es:

Pre

pare

dB

y:

Tem

pera

ture

J.H

ala

Exp

erim

enta

lD

ata

Tem

pera

ture

(t/

C)

NaN

3

(100

w1

/mas

s%

)N

aN3

(m1

/mol

kg2

1)c

Not

e

220

26.8

5.63

met

asta

ble

eute

ctic

poin

t(i

ce1

NaN

3)

215

.121

.64.

24eu

tect

icpo

int

22.

127

.85.

92tr

ansi

tion

poin

t

028

5.98

100

35.6

8.50

a Res

ults

wer

epr

esen

ted

ingr

aphi

cal

form

~Fig

.2!

.N

umer

ical

valu

esw

ere

repo

rted

for

five

sign

ifica

ntpo

ints

inth

eph

ase

diag

ram

.b S

olid

phas

esw

ere

repo

rted

tobe

NaN

33

H2O

,@

#,be

twee

n2

15.1

Can

d2

2.1

C,

and

NaN

3,

@266

28-2

2-8#

,ab

ove

22.

1C

.c C

alcu

late

dby

com

pile

r.

M Th

so sal

clo

pre

gra

gra

po


mpo

nent

s:O

rigi

nal

Mea

sure

men

ts:

Sodi

umaz

ide;

NaN

3;

@266

28-2

2-8#

Eth

anol

;C

2H

6O

;@6

4-17

-5#

J.A

.C

rans

ton

and

A.

Y.

Liv

ings

tone

,J.

Che

m.

Soc.

501

3

~192

6!.

riab

les:

Pre

pare

dB

y:

K:

273

J.H

ala

Exp

erim

enta

lD

ata

The

solu

bilit

yof

NaN

3w

asre

port

edto

be0.

22g

salt

in10

0g

solv

ent

at0

C.

From

this

valu

eth

eco

mpi

ler

calc

ulat

edm

1

0.03

38m

olkg

21.

Add

ition

alin

form

atio

n:T

heau

thor

sal

sore

port

edth

eso

lubi

lity

ofN

aN3

inbo

iling

etha

nol

tobe

0.46

gsa

ltin

100

gso

lven

t.B

oilin

gin

tof

the

satu

rate

dso

lutio

nan

dat

mos

pher

icpr

essu

reat

whi

chth

em

easu

rem

ent

was

cond

ucte

dw

ere

not

repo

rted

.

Aux

iliar

yIn

form

atio

n

etho

dA

ppar

atusP

roce

dure

:So

urce

and

Pur

ity

ofM

ater

ials

:

isot

herm

alm

etho

dw

asus

ed,

deta

ilsw

ere

not

repo

rted

.al

ysis

ofth

esa

tura

ted

solu

tions

was

carr

ied

out

bytit

ratin

gid

e1in

wei

ghed

sam

ples

.

No

info

rmat

ion

onN

aN3

repo

rted

.E

than

olus

edha

dde

nsity

of0.

799

gcm

23

at17

C.

Est

imat

edE

rror

:Te

mpe

ratu

re:

prec

isio

nno

tre

port

ed.

Solu

bilit

y:in

suffi

cien

tda

tare

port

edto

allo

wfo

rer

ror

estim

ate.

Ref

eren

ces:

1 F.

Ras

chig

,C

hem

.Z

tg.

1203

~190

8!.

1111JIRI HALA


Com

pone

nts:

Ori

gina

lM

easu

rem

ents

:

~1!

Sodi

umaz

ide;

NaN

3;

@266

28-2

2-8#

~2!

Eth

anol

;C

2H

6O

;@6

4-17

-5#

~3!

Wat

er;

H2O

;@7

732-

18-5

#

E.

Lie

ber,

C.

N.

R.

Rao

,H

.E

.D

ingl

e,an

dJ.

Teet

sow

,J.

Che

m.

Eng

.D

ata

11,

105

~196

6!.

Var

iabl

es:

Pre

pare

dB

y:

T/K

:29

8C

once

ntra

tion

ofet

hano

l/%~v

/v!:

0

95.5

J.H

ala

Exp

erim

enta

lD

ata

Solu

bilit

yat

25C

ofN

aN3

inw

ater

et

hano

lso

lutio

nsa

C2H

6O

~%,v

/v!

NaN

3

(g/1

00g

solv

ent!

NaN

3

(m1

/mol

kg2

1)d

043

.60b

6.70

7

4017

.95b

18.1

9c

6011

.17b

10.4

8c

804.

21c

95.5

0.81

b1.

05c

a Sol

idph

ases

wer

eno

tin

vest

igat

ed.

b Syn

thet

icm

etho

d.c I

soth

erm

alm

etho

d.d C

alcu

late

dby

com

pile

r.

Aux

iliar

yIn

form

atio

n

Met

hod

App

arat

usP

roce

dure

:So

urce

and

Pur

ity

ofM

ater

ials

:

The

solu

bilit

ies

wer

ede

term

ined

bysy

nthe

tican

dis

othe

rmal

met

hods

.In

the

synt

hetic

met

hod,

1th

eso

lutio

nsof

know

nco

mpo

sitio

nsw

ere

prep

ared

,an

dth

eir

satu

ratio

npo

ints

wer

ede

term

ined

byva

ryin

gth

ete

mpe

ratu

re.

Inth

eis

othe

rmal

met

hod,

sam

ples

ofth

esa

tura

ted

solu

tions

wer

eev

apor

ated

,an

dth

ere

sidu

ew

asdr

ied

and

wei

ghed

.T

heau

thor

sco

nsid

ered

the

resu

ltsob

tain

edby

isot

herm

alm

etho

das

mor

eac

cura

tean

dre

liabl

e.

No

deta

ilsre

port

ed.

Est

imat

edE

rror

:Te

mpe

ratu

re:

prec

isio

nno

tre

port

ed.

Solu

bilit

y:in

suffi

cien

tda

tare

port

edto

allo

wfo

rer

ror

estim

ate.

Ref

eren

ces:

1 O.F

lasc

hner

and

B.M

acE

wen

,J.C

hem

.Soc

.93,

1000

~190

8!.

Co

~1!

~2!

Va

T/

5 po M An

An

az

J

mpo

nent

s:O

rigi

nal

Mea

sure

men

ts:

Sodi

umaz

ide;

NaN

3;

@266

28-2

2-8#

Solv

ents

R.A

lexa

nder

,E

.C

.F.

Ko,

Y.

C.

Mac

,an

dA

.J.

Park

er,

J.A

m.

Che

m.

Soc.

89,

3703

12

~196

7!.

riab

les:

Pre

pare

dB

y:

K:

273

or29

8J.

Hal

a

Exp

erim

enta

lD

ata

Solu

bilit

ypr

oduc

tof

NaN

3in

thre

eso

lven

tsa

Solv

ent

Tem

pera

ture

(t/

C)

Ksp

bN

aN3

(c1

/mol

dm2

3)c

Met

hano

l;C

H4O

;@6

7-56

-1#

010

20.

90.

355

ulfin

yl-b

ism

etha

ne;d

C2H

6O

S;@6

7-68

-5#

2510

20.

640.

479

N-d

imet

hylf

orm

amid

e;C

3H

7N

O;

@68-

12-2

#25

102

1.9

0.11

2

olid

phas

ew

asN

aN3

,@2

6628

-22-

8#,

inal

lso

lven

ts.

sp5

@Na1

#@N

32#

alcu

late

dby

com

pile

r.im

ethy

lsul

foxi

de.

Aux

iliar

yIn

form

atio

n

etho

dA

ppar

atusP

roce

dure

:So

urce

and

Pur

ity

ofM

ater

ials

:

isot

herm

alm

etho

dw

asus

ed.

Satu

rate

dso

lutio

nsw

ere

pare

dby

shak

ing

the

solid

with

the

solv

ent

ina

stop

pere

dsk

at35

Cfo

r24

h,an

dth

enfo

rfu

rthe

r24

hat

0C

etha

nol!

orat

25C

~oth

ertw

oso

lven

ts!.

The

liqui

dph

ases

rean

alyz

edby

pote

ntio

met

ric

titra

tion

with

AgN

O3

.T

helid

phas

esw

ere

anal

yzed

afte

rdr

ying

at1

mm

Hg

for

48h

room

tem

pera

ture

.

NaN

3,A

nala

rgr

ade

prod

uct,

sour

ceno

tspe

cifie

d.M

etha

nolw

aspu

rifie

dac

cord

ing

toC

lare

etal

.1D

imet

hyls

ulfo

xide

was

apr

oduc

tof

Cro

wn

Zel

lerb

ach

Cor

p.N

,N-d

imet

hylf

orm

amid

e~s

ourc

eno

tsp

ecifi

ed!

was

drie

dw

ithty

pe4A

mol

ecul

arsi

eve,

and

frac

tiona

ted

twic

eun

der

redu

ced

pres

sure

ofdr

yni

trog

en.

Est

imat

edE

rror

:Te

mpe

ratu

re:

prec

isio

nno

tre

port

ed.

Solu

bilit

y:in

suffi

cien

tda

tagi

ven

toal

low

for

erro

res

timat

e.

Ref

eren

ces:

1.B

.W.C

lare

,D.C

ook,

E.C

.F.K

o,Y

.C.M

ac,a

ndA

.J.P

arke

r,J.

Am

.C

hem

.So

c.88

,19

11~1

966!

.


Com

pone

nts:

Ori

gina

lM

easu

rem

ents

:

~1!

Sodi

umaz

ide;

NaN

3;

@266

28-2

2-8#

~2!

Met

hano

l;C

H4O

;@6

7-56

-1#

F.H

udsw

ell,

J.S.

Nai

rn,

and

K.

R.

Gad

sby,

J.A

ppl.

Che

m.,

Supp

l.Is

sue.

No.

2,S1

37

8~1

951!

.

Var

iabl

es:

Pre

pare

dB

y:

T/K

:29

8J.

Hal

a

Exp

erim

enta

lD

ata

The

solu

bilit

yof

NaN

3w

asre

port

edto

be2.

491

or2.

486

gsa

ltin

100

cm3

ofth

esa

tura

ted

solu

tion

at25

C,

asde

term

ined

from

wei

ght

ofth

ere

sidu

eor

titra

tion,

resp

ectiv

ely.

Usi

ngth

eso

lubi

lity

ofN

aN3

inw

ater

of40

.8g

salt

per

100

gw

ater

at20

C,1

and

the

dens

ityof

the

satu

rate

dso

lutio

nof

NaN

3in

met

hano

lof

0.80

83g

cm2

3 ,th

eau

thor

sco

rrec

ted

the

expe

rim

enta

llyde

term

ined

solu

bilit

yin

met

hano

lfo

rth

eco

ntri

butio

nfr

om0.

035

mas

s%

wat

erin

met

hano

lus

ed,

and

obta

ined

the

solu

bilit

yof

NaN

3as

3.16

60.

01g

NaN

3

in10

0g

anhy

drou

sm

etha

nol,

or2.

48N

aN3

in10

0cm

3of

the

satu

rate

dso

lutio

n.Fr

omth

efo

rmer

valu

eth

eco

mpi

ler

obta

ined

m1

50.

486

mol

kg2

1.

Aux

iliar

yIn

form

atio

n

Met

hod

App

arat

usP

roce

dure

:So

urce

and

Pur

ity

ofM

ater

ials

:

An

isot

herm

alm

etho

dw

asus

ed.

Exc

ess

solid

was

shak

enm

echa

nica

llyw

ithth

eso

lven

tfo

r5

min

,an

dth

enke

ptin

ath

erm

osta

tfo

r1

h.T

his

proc

edur

ew

asre

peat

edth

ree

times

whi

chw

assu

ffici

ent

tore

ach

equi

libri

um.

Twen

tym

Lof

the

satu

rate

dso

lutio

nw

asw

ithdr

awn

with

api

pette

thro

ugh

asi

nter

ed/g

lass

filte

r,an

dth

eso

lven

tw

asev

apor

ated

belo

w50

Cin

aw

eigh

edbe

aker

.T

here

sidu

ew

asdr

ied

at50

Cto

cons

tant

wei

ght,

and

corr

ecte

dfo

rbl

ank

expe

rim

ent.

The

resi

due

was

then

anal

yzed

for

NaN

3by

reac

ting

itw

ithex

cess

(NH

4) 2

Ce~

NO

3) 6

and

back

-titr

atin

gex

cess

Ce~

IV!

with

FeSO

4

usin

gth

eo-

phen

anth

rolin

eFe

~II!

com

plex

asin

dica

tor.

NaN

3,

sour

ceno

tspe

cifie

d,co

ntai

ned

99.9

%N

aN3

afte

rdr

ying

toco

nsta

ntw

eigh

tat

50C

.It

was

used

with

out

furt

her

puri

ficat

ion.

Met

hano

l,bo

iling

poin

t65

C,

was

ofhi

gh-g

rade

puri

ty.

Itco

ntai

ned

0.03

5m

ass

%w

ater

.

Est

imat

edE

rror

:Te

mpe

ratu

re:

prec

isio

nno

tre

port

ed.

Solu

bilit

y:6

0.2%

~aut

hors

,ba

sed

onth

ree

mea

sure

men

ts;

indi

vidu

alre

sults

not

repo

rted

!.

Ref

eren

ces:

1 T.

Cur

tius

and

J.R

isso

m,

J.Pr

akt.

Che

m.

58,

261

~189

8!.

Co

~1!

~2!

Va

T/ S

N,

a S b K c C d D M An

pre

fla ~m we

so at


mpo

nent

s:O

rigi

nal

Mea

sure

men

ts:

Sodi

umaz

ide;

NaN

3;

@266

28-2

2-8#

Sodi

umam

ide;

NaN

H2

;@7

782-

92-5

#A

mm

onia

;N

H3

;@7

664-

41-7

#

T.K

awak

ami

and

S.M

orot

o,N

agoy

aK

ogyo

Giju

tsu

Shke

nsho

Hok

oku

8,79

3

8~1

959!

.

riab

les:

Pre

pare

dB

y:

K:

273

30

3/m

olkg

21:

0

0.13

H.A

kaiw

aan

dJ.

Hal

a

Exp

erim

enta

lD

ata

Solu

bilit

yin

the

NaN

3

NaN

H2

liqui

dam

mon

iasy

stem

mpe

ratu

re(t

/C

)N

aNH

2

(g/1

00g

NH

3)

NaN

H2

(m2

/mol

kg2

1)b

NaN

3

(g/1

00g

NH

3)

NaN

3

(m1

/mol

kg2

1)b

Solid

phas

ea

00.

910.

0233

50.5

7.77

A

0.92

0.02

3148

.57.

46A

2.69

0.06

9051

.47.

91A

1B

2.32

0.05

9543

.46.

68B

1.98

0.05

0834

.45.

29B

1.70

0.04

3634

.75.

34B

1.24

0.03

1822

.13.

40B

0.78

0.02

0012

.61.

94B

0.77

0.01

9711

.41.

75B

100

048

.67.

48A

1.51

0.03

8748

.57.

46A

3.10

0.07

9549

.17.

55A

1B

3.16

0.08

1050

.17.

71A

1B

2.73

0.07

0042

.56.

54B

2.11

0.05

4131

.54.

85B

1.58

0.04

0522

.33.

43B

0.98

0.02

5112

.31.

89B

200.

800.

0205

48.1

7.40

A

2.31

0.05

0949

.57.

62A

3.68

0.09

4348

.47.

45A

1B

2.70

0.06

9235

.85.

51B

2.48

0.06

3631

.24.

80B

1.97

0.05

0525

.73.

95B

1.87

0.04

7923

.13.

55B

1.51

0.03

8719

.93.

06B

1.52

0.03

9019

.32.

97B

1.11

0.02

8512

.41.

91B

0.74

0.01

907.

571.

16B

0.51

0.01

315.

050.

777

B

301.

590.

0408

47.2

7.26

A

3.39

0.08

6948

.67.

48A

1B

5.07

0.13

046

.07.

08B

4.40

0.11

339

.86.

12B

3.44

0.08

8231

.94.

91B

2.72

0.06

9724

.83.

82B

2.32

0.05

9521

.13.

25B

a A:

NaN

3,

@266

628-

22-8

#;B

:N

aNH

2,

@778

2-92

-5#.

b Cal

cula

ted

byco

mpi

ler

~J.H

.!.

1313JIRI HALA


Com

pone

nts:

Ori

gina

lM

easu

rem

ents

:

~1!

Sodi

umaz

ide;

NaN

3;

@266

28-2

2-8#

~2!

Am

mon

ia;

NH

3;

@766

4-41

-7#

T.K

awak

ami

and

S.M

orot

o,N

agoy

aK

ogyo

Giju

tsu

Shke

nsho

Hok

oku

8,79

3

8~1

959!

.

Var

iabl

es:

Pre

pare

dB

y:

T/K

:23

1.7

26

3.9

H.A

kaiw

aan

dJ.

Hal

a

Exp

erim

enta

lD

ata

Solu

bilit

yof

NaN

3in

liqui

dam

mon

iaas

afu

nctio

nof

tem

pera

ture

Tem

pera

ture

(t/

C)

NaN

3

(g/1

00g

NH

3)

NaN

3

(m1

/mol

kg2

1)a

Solid

phas

eb

29.

351

.45

7.91

A

218

.052

.51

8.08

A

227

.952

.23

8.03

c

228

.950

.40

7.75

c

232

.844

.69

6.78

c

236

.039

.25

6.03

B

237

.038

.60

5.94

B

241

.532

.14

4.94

B

a Cal

cula

ted

byco

mpi

ler

~J.H

.!.

b A:

NaN

3;

@266

28-2

2-8#

;B

:N

aN36

NH

3,

@#.

c Not

repo

rted

.

Aux

iliar

yIn

form

atio

n

Met

hod

App

arat

usP

roce

dure

:So

urce

and

Pur

ity

ofM

ater

ials

:

Dri

edN

aN3

~2.9

84g!

and

exce

ssof

drie

dliq

uid

amm

onia

wer

ein

trod

uced

into

apr

essu

rebo

ttle.

The

mix

ture

was

tran

sfer

red

into

aD

ewar

flask

and

cool

edw

ithac

eton

e/dr

yic

eco

olan

t.T

heso

lubi

lity

ofN

aN3

was

dete

rmin

edby

the

clou

dm

etho

d.A

tte

mpe

ratu

res

belo

w2

35C

the

solu

tions

show

eda

tend

ency

tow

ard

supe

rsat

urat

ion.

NaN

3,

com

mer

cial

lyav

aila

ble

prod

uct

~sou

rce

not

spec

ified

!,w

asre

crys

talli

zed

from

liqui

dam

mon

ia.

Est

imat

edE

rror

:Te

mpe

ratu

re:

60.

2K

~aut

hors

!.So

lubi

lity:

prec

isio

nno

tre

port

ed.

Co

~1!

~2!

~3!

Va

T/

m2

Te

J

mpo

nent

s:O

rigi

nal

Mea

sure

men

ts:

Sodi

umaz

ide;

NaN

3;

@266

28-2

2-8#

6,7,

9,10

,17,

18,2

0,21

-oct

ahyd

ro-d

iben

zo@b

,k#

4,7,

10,1

3,16

#hex

aoxa

cycl

ooct

adec

in;

0H24

O6

;@1

4187

-32-

7#~1

8-di

benz

o-cr

own-

6!So

lven

ts

L.

N.

Yas

treb

ov,

T.M

.Sh

uvae

va,

and

L.

N.

Kra

vche

nko,

Zh.

Prik

l.K

him

.50

,21

07

8~1

977!

.

riab

les:

Pre

pare

dB

y:

/mol

dm2

3:

0

0.15

J.H

ala

Exp

erim

enta

lD

ata

Solu

bilit

yof

NaN

3in

vari

ous

solv

ents

asa

func

tion

of18

-dib

enzo

-cro

wn-

6co

ncen

trat

ion

Solv

ent

Tem

pera

ture

(t/

C)

C20

H24

O6

(c2

/mol

dm2

3)

NaN

3

(c1

/mol

dm2

3)

ulfin

yl-b

is~m

etha

ne!;

aC

2H

6O

S;@6

7-68

-5#

800

1.1

0.05

1.1

0.10

1.19

0.15

1.66

N-d

imet

hylf

orm

amid

e;C

3H

6N

O;

@68-

12-2

#80

00.

18

0.05

0.19

0.10

0.21

0.15

0.26

Eth

anol

;C

2H

6O

;@6

4-17

-5#

750

0.11

0.05

0.12

0.10

0.17

0.15

0.31

Ace

tone

;C

3H

6O

;@6

7-64

-1#

550

0.00

24

0.05

0.00

58

0.10

0.01

04

0.15

0.01

39

2-B

utan

one;

C4H

8O

;@7

8-93

-3#

750

0.00

19

0.05

0.00

28

0.10

0.00

70

0.15

0.01

15

Cyc

lohe

xano

ne;

C6H

10O

;@1

08-9

4-1#

800.

150.

0038

Ace

toni

trile

;C

2H

3N

;@7

5-05

-8#

800.

150.

0092

a Dim

ethy

lsul

foxi

de.

Aux

iliar

yIn

form

atio

n

Met

hod

App

arat

usP

roce

dure

:So

urce

and

Pur

ity

ofM

ater

ials

:

No

info

rmat

ion

repo

rted

.N

oin

form

atio

nre

port

ed.

Est

imat

edE

rror

:Te

mpe

ratu

re:

prec

isio

nno

tre

port

ed.

Solu

bilit

y:in

suffi

cien

tda

tagi

ven

toal

low

for

erro

res

timat

e.


Aux

iliar

yIn

form

atio

n

Met

hod

App

arat

usP

roce

dure

:So

urce

and

Pur

ity

ofM

ater

ials

:

An

isot

herm

alm

etho

dw

asus

ed.

Exc

ess

ofso

lids

wer

eeq

uilib

rate

dw

ithliq

uid

amm

onia

atth

ede

sire

dte

mpe

ratu

rein

apr

essu

rebo

ttle

imm

erse

din

ath

erm

osta

ted

Dew

arfla

sk.

Insa

mpl

esof

the

satu

rate

dso

lutio

ns,

amm

onia

was

dete

rmin

edfr

omw

eigh

tlo

ssaf

ter

allo

win

git

toev

apor

ate

from

aw

eigh

edsa

mpl

e.T

heco

nten

tof

NaN

H2

inth

ere

sidu

ew

asde

term

ined

alka

limet

rica

llyaf

ter

deco

mpo

sing

the

amid

eby

addi

ngca

rbon

ate-

free

wat

er.

The

NH

3lib

erat

edw

asab

sorb

edin

exce

ssst

anda

rdH

2SO

4so

lutio

n,an

dex

cess

acid

was

back

-titr

ated

agai

nst

NaO

Hso

lutio

n.T

hem

etho

dfo

rN

aN3

dete

rmin

atio

nw

asno

tre

port

ed.

NaN

3,

sour

ceno

tsp

ecifi

ed,

was

apr

oduc

tof

99.4

5%

99.6

5%pu

rity

.NaN

H2

was

prep

ared

byre

duct

ion

ofN

aN3

with

sodi

umm

etal

inliq

uid

amm

onia

,usi

ngir

onpo

wde

ras

aca

taly

st.P

urity

ofth

epr

oduc

tw

asno

tre

port

ed.

Est

imat

edE

rror

:Te

mpe

ratu

re:

prec

isio

n6

0.2

K~a

utho

rs!.

Solu

bilit

y:in

suffi

cien

tda

tagi

ven

toal

low

for

erro

res

timat

e.

Co

~1!

~2!

@1,

C2

~3!

Va

c 2 S N,


Tetr

ahyd

rofu

rane

;C

4H

8O

;@1

09-9

9-9#

650.

153

0.00

21

1,4-

Dio

xane

;C

4H

8O

2;

@123

-91-

1#80

0.15

30.

0042

Ben

zene

;C

6H

6;

@71-

43-2

#80

0.15

30.

0064

a Dim

ethy

lsul

foxi

de.

b Bas

edon

the

effe

ctof

met

hano

lon

the

solu

bilit

yof

NaN

3,

the

com

pile

ras

sum

edth

isfig

ure

coul

dbe

am

ispr

int.

The

corr

ectv

alue

coul

dbe

eith

er0.

15or

0.05

.

Aux

iliar

yIn

form

atio

n

Met

hod

App

arat

usP

roce

dure

:So

urce

and

Pur

ity

ofM

ater

ials

:

Not

hing

spec

ified

.N

othi

ngsp

ecifi

ed.

Est

imat

edE

rror

:So

lubi

lity:

insu

ffici

ent

data

give

nto

allo

wfo

rer

ror

estim

ate.

3.3.

Po

tass

ium

Azi

de

3.3.

1.E

valu

atio

no

fth

eK

N3

H2O

Sys

tem

mpo

nent

s:E

valu

ator

:

Pota

ssiu

maz

ide;

KN

3;

@207

62-6

0-1#

Wat

er;

H2O

;@7

732-

18-5

#J.

Hal

a,D

epar

tmen

tof

Inor

gani

cC

hem

istr

y,M

asar

ykU

nive

rsity

,61

137

Brn

o,C

zech

Rep

ublic

,Ju

ne20

01

Cri

tica

lE

valu

atio

nT

heso

lubi

lity

ofK

N3

inw

ater

was

mea

sure

dby

isot

herm

alm

etho

din

two

docu

men

ts.

Cur

tius

and

Ris

som

1re

port

edth

ree

valu

estw

een

283.

6an

d29

0.1

K,w

hile

Woh

lgem

uth2

repo

rted

the

phas

edi

agra

mof

the

KN

3

H2O

syst

em,a

ndnu

mer

ical

data

only

at27

3.1

d37

3.1

K.

Alth

ough

the

two

sets

ofda

taw

ere

obta

ined

unde

rdi

ffer

ent

equi

libra

tion

cond

ition

san

dw

ithun

know

npr

ecis

ion

ofpe

ratu

rem

easu

rem

ent

the

data

seem

tobe

ingo

odag

reem

ent

sinc

eth

eyfa

llon

ast

raig

htlin

e.L

east

squa

retr

eatm

ent

ofth

eda

tatw

een

273.

1an

d29

0.1

Kyi

elde

dan

equa

tion

for

the

solu

bilit

yof

KN

3in

wat

eras

afu

nctio

nof

tem

pera

ture

asm

1/m

olkg

215

0.05

94T

211

.11,

ich

can

beus

edto

obta

inte

ntat

ive

solu

bilit

ies

inth

em

entio

ned

tem

pera

ture

rang

e.

fere

nces

:

.C

urtiu

san

dJ.

Ris

som

,J.

Prak

t.C

hem

.58

,26

1~1

898!

.

Woh

lgem

uth,

Com

pt.

Ren

d.19

8,60

1~1

934!

.

1515JIRI HALA


Com

pone

nts:

Ori

gina

lM

easu

rem

ents

:

~1!

Sodi

umaz

ide;

NaN

3;

@266

28-2

2-8#

~2!

6,7,

9,10

,17,

18,2

0,21

-oct

ahyd

ro-d

iben

zo@b

,k#

@1,4

,7,1

0,13

,16#

hexa

oxac

yclo

octa

deci

n;C

20H

24O

6;

@141

87-3

27#

~18-

dibe

nzo-

crow

n-6!

~3!

Met

hano

l;C

H4O

;@6

7-56

-1#

~4!

Solv

ents

L.

N.

Yas

treb

ov,

T.M

.Sh

uvae

va,

and

L.

N.

Kra

vche

nko,

Zh.

Prik

l.K

him

.50

,21

07

8~1

977!

.

Var

iabl

es:

Pre

pare

dB

y:

Con

cent

ratio

nof

CH

4O

/v/v

%:

1

3Fo

rea

chso

lven

tm

easu

rem

ents

wer

eca

rrie

dou

tat

one

tem

pera

ture

and

one

18-d

iben

zo-C

row

n-6

conc

entr

atio

n.

J.H

ala

Exp

erim

enta

lD

ata

Solu

bilit

yof

NaN

3in

vari

ous

solv

ents

inth

epr

esen

ceof

18-d

iben

zo-c

row

n-6

asa

func

tion

ofm

etha

nol

conc

entr

atio

n

Solv

ent

Tem

pera

ture

(t/

C)

C20

H24

O6

(c2

/mol

dm2

3)

Met

h

iupac-nist solubility data series. 79. alkali and alkaline...

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