* MEMORANDUM REPORT BRL-MR-3720

1938 - Serving the Army for Fifty Years - 1988

ve DENSITY OF HYDROXYLAMMONIUM NITRATE SOLUTIONS

RONALD A. SASSt4 MARK A. DAVIES* ROBERT A. FIFER

MADELYN M. DECKER4A.NTHIONY i. KOT LAR

DECEMBER 1988 DTIC~ELECTEIN

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Aberdeen Proving Ground, MD 21005-5066

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61102A AH43ELEMENT NO. NO. NO. CCESSION NO.

11. TITLE (Include Security Clawiflcation) 6

DENSITY OF HYDROXYLAMMONIUM NITRATE SOLUTIONS

12. PERSONAL AUTHOR(S)R.A. Sasse' , M.A. Davies,* R.A. Fifer, M.M. Decker, A.J. Kotlar

13a. TYPE OF kEPORT 13b. TIME COVERED 14 DATE OF REPORT (Yoar, Month, Day) S. PAGE COUNTFinal FROM Mar 88 TO Sep 88

16. SUPPLEMENTARY NOTATION

*National Research Council Associate

17. COSATI CODES IS. SUBJECT TERMS (Continue on reverie d necessary and identify by block number)

FIELD GROUP SUB-GROUPDensity, Hydroxylammontumi Nitrate, HAN, LP, LPG, dHAN

IL 112

19, ABSTRACT (Continue on reverse if necessary and identify by block number)

Hydroxylammonium nitrate is miscible with water in all proportion% at room temperature. Thedensities of such salt solutions were measured using water and deuterium oxide as solv_!nts.

A second order equation is given to relate density to molar concentratton.-.

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TABLE OF CONTENTS

PageINTRODUCTION .......................... o........... . . . . . . . .5

II. DISCUSSION .......... .... ..... ..... . ...... . .. .. 8

REFERENCES - ... &.......... ........ &......... . . . . . . . . ........ 9

APPENDIX 1 ...... ............. ......... .

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A-,r,

I. INTRODUCTION

Through the long term Liquid Propellant Program at the BRL, there was aneed to measure the density of ingrediei.ts for one or more purposes andapproximate measurements were made to satisfy various requirements as theyexisted at particular times. Measurements were made at varying roomtemperatures during a particular series of days and this generated some usefuldata as opposed to conducting a careful and systematic study. Sasse'l in 1976used an approximate equation for the density, p, in g/cu3 , of hydroxylammoniumnitrate solutions, HAN, derived from data from I to 13 M. The equation was:

p = 1.0000 + 0.0369 M (I)

He made the suggestion that as a first approximation, the ingredients ofHAN based liquid propellants when added one to another acted as independentvolume elements much like "marbles". In this approximation the density ofpure HAN was inferred, by experiments, to be 1.81 g/cm3 and this value wasused later by Freedman and Travis 2 to estimate propellant concentrations anddensities as input to thermodynamic calculations.

The first disclosure that the density/concentration relationship may nutbe linear was offered by Biddle 3 who related hydrometer readings toconcentration. In this work two hydrometers of different radii were used andsurface tension corrections were not made; also, these measurements wereconducted at the room temperature experienced at particular days. Suchreadings were compiled as a practical expedient for establishing productionguides and criteria for maintaining and evaluating evaporation methodology.He showed a single regression line, but not the individual data points,embracing all data from 2.1 to 17.3 M HAN. The equation was given as:

M = 26.04p - 26.38 (2)

which can be transformed to:

p = 1.013 + 0.0384 M (3)

To meet the production goal of 13 M he also made and graphed extensivehydrometer measurements representing the very limited concentration intervalof 11.7 to 14.3 M. lie presented these values in tabular form in units ofpercent concentration. Further, be assumed that he could represent thepercent ('concentration/density data, which is a (curvtng fcsrwton, as a limitedlinear segment, and gavw an equation for that regression line. From his tableof percent concentLations and densities, molarity can he calculated. A linearregression equation of this data was uniquely reported In a physical4properties paper over this limited range as:

p = 1.12292 + 0.03099 M (4)

This .ine is given in Figure 1 of this paper together with Biddle's regressionline representtng all of his data from 2.1 to 17.3 4. The discontinuitybetween the treatment of the entire data set and an extracted subset,Indicates that the density/concentration relationship may he curved; however,fron the limited range of the daLa In the !;uhset .. , not ing the uncertaintiesinv)lved, it Is not clear that the purport-d cui :atcre is sitgnifi('ant. Biddle

used the equivalent of Eq. 4, but In units of percent concentration, in hisevaporation task where the approximations involved did not effect hisobjective. However, he did not explore or discuss the implied curvature.

!

1.1

II

1.4-

1.3

* 1.2

1.1

I U 1 1 1 I I - I I I I I I I I I I I

2 4 a I 10 12 14 Ii s 6 20

CONCENTRATION, moles/liter

Figure 1. Biddle's Data Reference 3. Upper line is the linearregression line of all data and lower line is the linear regression

line of a limited interval.

With the acquisition of temperature controlled density equipment* at theBRL, based on the measurement of the frequency of an oscillator, and theability to make pure crystalline HAN (which was used to make concentratedsolutions), encouraged us to re-examine the relationship between density andconcentration. Further persuasion was offered by the fact that Decker of theBRL was routinely analyzing HAN solutions and navies was preparing deuteratedHAN (noted as dHAN) in D20 for his diamond anvil cell infrared studies.5 Also,Rheingold, et al.,1 determined the density of pure crystalline HAN and dHAN byx-ray methods and Sasse' and Fifer measured the density of pure liquid HAN anddHAN with a pycnometer. Measurements are given in Table I and plotted inFigure 2. Decker titrated all HAN and dHAN solutions with strong base anddetermined the densities of HAN solutions while Davies measured densities ofdHAN solutions made with n20. Both experimenters operated at 20.0C. Fron,measuring the density of pure water, the density determinations are Judged tobe accurate to about 0.14% and the HAN analysis has a precision of 4-5 partsper thousand.

*Mettler/Parr Density Meter, Model DMA 55

6

I

Table 1. Density of HAN and dHAN and Their Solutions

HAN dHAN

Density Concentration Density Concentrationg/cm3 M glcm3 M

0.99963 0.0-pure H20 1.1053 0.0-pure D2 01.02341 0.500 1.1662 1.3361.12533 2.781 1.1904 1.8751.22919 5.232 1.2761 3.936-1.29636 6.858 1.4488 8.3211.37548 8.839 1.6137 12.741.523n6 12.622 1.69694 15.86*1.65569 16.3381.68 17.5** 1.841 .. 1840**1.841 19.17*** 1.916 19.15***

* only value calculated by weight.

** anhydrous melt.*** crystalline value, Reference 6.

1.3 S

elop1.9 .I

M-

U .j

z 1.5-. 1.*aj

1.3 aI..-.' ga•

,U,

I ! I " | I r I I I I -T r--- ! •(4 1.10 1 14 Is I 2

CONCENTRATION, moles /1iter

Figure 2. Second Order Regression Lines for dHAN and IIAN Systems.Upper line is dHAN and lower line is HAN data. Squares are experimentaldata and crosses are calculated regression values. Filled in squares are

crystalline valuject and filled irn circles a re pure melted compounds.

7

II. DISCUSSION

Recognizing the constraints, limitations, and concentration rangesemployed by various investigators the collection of density relationships areall in general agreement. However it is hoped that the present data setreflects the effort of careful temperature control and the curvature noted inFigure 2 is reinforced by the availability of data at high concentrations.Second order least squares and linear regression analyses were performed byKotlar using the data in Table 1 excluding crystalline values. Statisticaldetails are given in the Appendix showing that second order equations betterrepresent the data and the best fit equations are given below:

SHAN 0.9935 + 0.04630 M - 0.0004007 N2 in H20 (5)

PdHAN 1.1045 + 0.04646 M4- 0.0005581 M2 in D2 0 (6)

One would expect tintt tie cur,-•ture noted by the above equations would also bepresent in refracLA-, intrex functions, a parameter that some of us wish todocument.

Some structural information may be deduced by including the crystallineand anhydrous liquid HAN values in the concentration plot given in Figure 1.For instance, if one considers the melting of an ionic crystal, then the meltcontains the maximum number of &. pairs possible, what ever that number mightbe. In the present case, HAN changes density from 1.841 to 1.68 upon meltingand with the addition of increments of wver one would expect the number ofion pairs to decrease until a ditute solution is achieved and only solvationtakes place. If the observed curvature in the density plot is due to sucheffects, then ion pairs have a dominant effect upon this parameter fromsaturated solutions to ca. 8 M. Carrying this concept further, then dilutesolutions would not show ion pairing but just free ions would exist andextrapolation of these data, 0 to 8 M, should intersect the crystallinedensity value. This is indeed the case, and such an extrapolation may be madein Figure 2 for both the HAN and dHAN data sets. The figure is too busy tomake this construction and this task is left to the reader. The argument, ifcorrect, implies that the ion pairs formed would have a greater volume thanthe sum of the volumes of its constituents.

It is the general conclusion of this report that the functionalrelationship between density and molar concentration of HAN solutions, overits entire concentration range, is represented by a second order equation thatis very similar to the equation for the deuterated syutem.

8.

REFERENCES

1. R.A. Sasse', BRL, private communication 1976.

2. E. Freedman and K.E. 'iravis, BRL, private communication 1981.

3. R.A. Biddle, "Concentration of HAN Solution," Mortoa Thiokol Inc., Elkton,MD. Final Contract Report DAAD05-84-M-6657, May 1985.

4. M.M. Decker, N. Klein, E. Freedman, C.S. Leveritt, and J.Q. WoJciechowski,"HAN-Based Liquid Gun Propellants: Physical Properties," BRL Report No.TR-2864, US Army Ballistic Research Laboratories, Aberdeen Proving Ground,MD, 1987.

5. M.A. Davies and R.A. Fifer, "High Pressure FTIR Studies of Aqueous HAN anddHAN Solutions Using Diamond Anvil Cell Techniques," in preparation.

6. A.L. Rheingold, J.T. Cronin, T.B. Brill, and F.K. Ross, "Structure ofHydroxylammonium Nitrate (HAN) and the Deuterium Homolog," Acta Cryst.,Vol. C43, pp. 402-404, 1987.

L

9

APPENDIX

A linear regression line and a second order regression fit was performedon both data sets , dAN and dHAN, given in Table 1. Concentration is in unitsof moles/liter(M) and density (p) is in units of grams/cubic centimeter.Results are:

Table 2. Regression Analyses

Coefficient StandardDeviation

HAN for: P - PI + P2 (M)

P1 = 1.0145 7.690E-3P2 - 3.93OIE-2 7.720E-4

Density 1.4195E-2.

HAN for: P - P1 + P2 (M) + P3 (M2 )

P1 = 0.9935 2.983E-3P2 = 4.6297E-2 8.771E-4P3 -- 4.0066E-4 4.842E-5

Density 4.3519E-3

dhAiv fo': P = t-I + P2 (M)

P1 = 1.1191 8.506E-3P2 = 3.7755E-2 I.003E-3

Density 1 .5086E-2

dHAN for:. p - PI + P2 (M) + P3 (M2 )

PI = 1.1045 3.622F-3P2 = 4.6458E-2 1.392E-3P3 =-5.5811 E-4 8.670E-5

Density 5.0046E-3

It is interesting that the statistics for both the IAN and dIIAN data arecomparable and thus the experiments are of equal percision. This is thedesired result; however, due to "improvements" such an occurrence is not seentoo often.

The standard deviation for density using the quadratic equation is threetimes smaller than given by the linear equation; therefore, the data for HANand dHAN are better represented by the quadratic equations given above. Theseequations are reproduced in the body of the text.

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1. BRL Report Number Date of Report

2. Date Report Received

3. Does this report satisfy a need? (Comment on purpose, related project, orother area of interest for which the report will be used.)

4. How specifically, is the report being used? (Information source, designdata, procedure, source of ideas, etc.)

S. Has the information in this report led to any quantitative savings as faras man-hours or dollars saved, operating costs avoided or efficiencies achieved,etc? If so, please elaborate.

6. General Coments. What do you think should be changed to improve futurereports? (Indicate changes to organization, technical content, format, etc.)

Name

CURRENT OrganizationADDRESS Address

City, State, Zip

7. If indicating a Change of Address or Address Correction, please provide theNew or Correct Address in Block 6 above and the Old or Incorrect address below.

Name

OLD OrganizationADDRESS

Address

City, State, "Zip

(Remove this sheet, fold as indicated, staple or tape closed, and mail.)