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D-A148 324 CHARACTERIZATION AND SELECTION OF POLYMER MATERIALS FOR i/lI BINARY MUNITIONS..(U) ARMY MATERILS AND MECHANICSI RESEARCH CENTER WATERTOWdN MA C R DESPER JUL 84
UNCLA7SIFIED AMMRC-TR-84-28-PT-2 F/O 19/1 N
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AMMRC TR 84-28 JAD
CHARACTERIZATION AND SELECTION
OF POLYMER MATEALS,-N3 -_
BINARY MUI 'J .
PART 2: -ARACTERIZATION OF LLD INSIle
00~' C. RICHARD DESPER (,-~ MATERIALS CHARACTERIZATION DIVISION
/
July 1984
': DTIC ':1113 Approved for public release; distribution unlimited. -E_"DEC 7 1984UCL.
ARMY MATERIALS AND MECHANICS RESEARCH CENTER D ::D::::'L Watertown, Massachusetts 02172-0001
84 11 29 055
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tia S
The findings in this report are not to be construed as an officialDepartment of the Army position, unless so designated by otherauthorize~d documents.
Mention of any trade names or manufacturers in this reportshall not be construed as advertising noi as an official
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UNCLASSIFIED119CuRITy CLASSIFICATION OF Tisl PAGE (When Data Entered) __________________
REPRTDO METAIO PGEREAD INSTRUCTIONS 1REPOR DOCMENTTIONPAGEBEFORE COMPLETING FORM JIREPORT mumSE GOVT ACCESSION NO. 3. RECIPIENT'S CATALOG NMB~ER 1
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CHARACTERIZATION AND SELECTION OF POLYMERMATERIALS FOR BINARY MUNITIONS STORAGE - Final ReportPART 2: CHARACTERIZATION OF LLDPE RESINS GPERFORMING ORG. REPORT HUU1SER
7. AUTI4OR(sj S. CONTRACT OR GRANT NUMIERI'e)
C. Richard Desper
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Army Materials and Mechanics Research Center 5/A Project: 1L162622A554Watertown, Massachusetts 02172-0001 kMS Code: 6126225540AI1DRXMR-OM
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U.S. Army Materiel Command July 1984Alexandria, Virginia 22333 13 NUMBER Of PAGES
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If SUPPLEMENTARY NOTES
It K EY WORDS (Conlin... on I...... . It n. a.~ nd Ode-Illy Ill telnyb .. etl,')
Polyethylene CrystallizationStress corrosion Cracking (fracturihg)Life tests CopolymersMolecular weight
20 ABSTRAC T (ConPitn.0e- rere,ee j1.1 It no,de...erend Ideent.I, y h block nurmbew)
(SEE REVERSE SIDE)
DD, AN ~j1473 EDITION OF 1 NO0V 6SIS OSSOI Fr UNLSSFESECIURITY CLASSIFICATION OF THIS PAGE (Wten 1e 11010e~a
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UNCLASSIFIEDSECUEITY CLASSIPICATION OF THIS PAGR flaml Det Enwod)
Block No. 20
ABSTRACT
;This work is aimed at determining the materials properties required for*storage of DF (methyiphosphonic difluoride) over extended periods of time
at temperatures as high as 70"C. Earlier studies showed the most likelymode of failure to be environmental stress cracking of the polyolefin con-tainer, rather than chemical or oxidative attack. The most promising candi-dates in terms of resistance to environmental stress cracking are ethylenecopolymers with a small alpha-olefin comonomer content. The comonomer,typically butene-l or hexene-1, introduces short side chain branches whichdisrupt the regularity of the crystal morphology, presumably leading to agreater proportion of intercrystalline ties. An X-ray diffraction methodwas developed for measuring the amount of short chain branching which offersgreater accuracy than the previous infrared absorption method. Character-ization of short chain branching by such a method, along with molecularweight characterization by gel permeation chromatography and crystallinitydetermination by density, were deemed essential to quality control of resinsfor the intended application. A
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CONTENTS
Page
INTRODUCTION ............ ......................... 1
EXPERIMENTAL 0
X-Ray Diffraction Procedures ...... .............. 1
Density Determination ........ .................. 6
GPC Determinations ......... ................... 6
SAMPLES ............. ........................... 6
RESULTS AND DISCUSSION
Molecular Weight Determinations ...... ............. 7
Characterization of Branch Content ..... .......... 9
Crystallinity ........ ...................... .... 12
CONCLUSIONS ......... ......................... .... 14
ACKNOWLEDGMENTS ........ ....................... .... 15
APPENDIX.......... ............................... 17
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INTRODUCTION
The present work is a continuation of previously reported workI having the goalof determining the materials properties required for storage of DF (methylphosphonic ..difluoride) over extended periods of time at elevated temperatures. Attention has .been focused on thermoplastic polyolefins, which, in some instances, appear to offerthe requisite chemical resistance and long term stability. However, the performanceof the current polyethylene container material and possible replacement materials mustbe critically assessed, particularly in view of new requirements for enduring more ..... .
severe storage conditions.
The previous work' identified environmental stress cracking as the major factorcontributing to premature failure in DF containers. This conclusion is in accordwith the results of earlier screening studies by White and co-workers.2 The litera-ture on environmental stress cracking has been surveyed (see Appendix) and resindensity, molecular weight, and applied stress are key factors influencing environ-mental stress cracking. As suggested in the previous work,1 medium density is .preferred to high density, since the greater crystallite perfection associated withhigh density in polyethylene would lead to a higher degree of regular chain foldinginstead of the more desirable intercrystalline links. Medium density is generallyachieved by deliberate incorporation of a controlled amount of side chain branchesin the polyethylene molecule by copolymerization with a small amount of an alpha-olefin (such as butene-l) which results in a short linear aliphatic side chain.High molecular weight is also desirable for better resistance to environmentalstress cracking. The present work addresses itself to following up several recom-mendations from the previous work.1
1. Development of a method for determination of side chain content from measure- ..ment of crystal lattice parameters,
2. Characterization of alternate of polyethylene resins as a possible replace-ment for the Marlex M407MQ used in the past, and
3. Development of a method for measurement of long chain branching for morecomplete resin characterization. The previous work also singled out residual stress,introduced by prccessing, as an aggravating factor leading to premature failure byenvironmental stress cracking. However, this factor shall be dealt with elsewhere asa processing problem and will not be addressed here, where the focus is on materialsproblems.
EXPERIMENTAL
X-Ray Diffraction Procedures
Data were obtained using a Xentronics Corporation XD10 area-imaging proportionalcounter mounted on a Picker four-circle goniometer.3 The primary X-ray beam is mono-chromated by reflection from a highly oriented pyrolytic graphite crystal and collimated .
1. DESPER, C. R. Characterization and Selection of Polymer Materials for Binary Munitions Storage. Army Materials and MechanicsResearch Center, AMMRC TR 83-45, August 1983.
2. WHITE, S. S., LEEP, D. A., FIELDER, D., and DUNNE, L. P. The Permeation of the Chemical Components of Binary G-MunitionThrough Polyethylenes. Edgewood Arsenal Technical Report EC-TR-74080, AD-C000378, Aberdeen Proving Ground, Maryland, November 1974.
3. DESPER, C. R., and BURNS, R. An Area-Imaging Proportional Counter for X-Ray Diffraction. Adv. X-Ray Anal., v. 24, 1981, p. 161.
.: -. . . .. ... . ..-. . ... .
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by a 0.5-mm circular pinhole aperture a distance of 225-mm from the X-ray source. Thepolymer film samples were placed in a special sample holder4 designed to hold a specimenin the reflection position as in a conventional Bragg-Brentano Powder Diffractometer.The area detector, placed at a distance of 290-mm from the specimen, covered a maximumangular range of 160 in both the horizontal and vertical directions.
The area detector rests on a detector arm which moves in a horizontal plane (see!Figure 1), positioned to intercept the Bragg angle range of interest, chosen to be20 = 140 to 290 in the present instance. Data for this entire angular range wereobtained simultaneously using the area detector in conjunction with a Wicat 150 mini-computer. Data for each pattern were stored in arrays of dimensionality 256 X 256. -Two modes of data acquisition were used: (a) wide-range patterns ("Zoom I) were
obtained covering the range 20 = 140 to 290 with a vertical divergence range of 170(see Figure 2), and (b) more detailed patterns ("Zoom I") were obtained covering therange 29 = 200 to 270 (see Figure 3) with a vertical divergence range of ±3.50. In
both instances the instrument resolution was approximately 0.20, but the data pointswere spaced at 0.0540 and 0.0270 intervals, respectively. The Zoom I patterns showedthe entire range of interest, including the tails of the polyethylene amorphous peak,while the Zoom II patterns showed the shapes of the (110) and (200) crystalline linesin greater detail. The latter patterns were used for precise measurement of dspacings.
RI
B
r• r
Figure 1. Polyethylene folded chain crystalshowing intercrystal line links (I) resultingfrom a chain branch (B); also showingregular folds (R).
4. DESPER. C. R. A Comluter-Controled X-Ray Diffwctometer for Texture Studes of Polycrytallfine Mhternkl. Adv. X-Ray Anal., 5v. 12, 1969, p. 404.
2
.. .. . . .... . .. . . ...-.-. . . ii ... .
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25 - -- n r .. - r r r - --- -0-f r- - .
240.
224.
1744
128 -
112
96
so
64
48'
32
16'
10 20 30 40 50 60 70 80 90 100
Figure 2. Diffraction pattern of M445 at Zoom 1. Channel 128:polyethylene (110) reflection; channel 170: polyethylene (200)reflection; channel 218: graphite (002) reflection._
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240
224
208
192
176
160
128:
112
96
64
48
32
10 20 303 40 50 60 70 80 90 100
Figure 3. Diffraction pattern of M445 at Zoom 11. Channel 60:polythylene (110) reflection; channel 142.5: polyethylene (200)reflection; channel 237.5: graphite (002) reflection.
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Since the area detector method recorded all the data in a pattern simultaneously,only one to three minutes were required to obtain a pattern, compared to a typicaldata acquisition time of six hours per sample using the older angular scanning method.
Angular calibration was accomplished by measuring the primary beam (suitably -attenuated by transmission through copper foils) at intervals of 1.000 on eitherside of and including the 20 = 0.000 position in a single pattern. The calibrationthus established at the 0 position of the detector arm is transferred to any otherrange by simply adding the new angular position of the detector arm to the calibra- .-tion curve. In addition, for increased precision in the determination of d spacings,the polyethylene film samples were coated with a thin layer of graphite (as previously Sdescribed) to provide an internal reference, the (002) line at 20 = 26.620.
Finally, to obtain a curve of intensity as a function of 20, it is necessary toreduce the two-dimensional data from the detector to a single dimension. However,the diffraction pattern of the randomly oriented polyethylene crystallites appearsas a series of arcs on the detector face. In the long run, it would be possible to Suse all of the information in these arcs by transforming the data from cartesian toangular coordinates. For the present, however, the required intensity curve wasobtained by vertically suming the data along a long, narrow strip following thehorizontal center line of the pattern. By using only the data on a narrow strip,the effect of the arc curvature may be neglected and the Bragg angle 20 may beidentified with the horizontal cartesian coordinate axis. In the parlance of powder -diffractometry, this procedure is equivalent to using a Soller slit system of limitedvertical divergence 6 as described by Eastabrook.5 The effective vertical divergenceused in obtaining the present intensity curves was 6 = 2.20 for the "Zoom I" data and6 1.10 for the "Zoom II" data.
The d spacings of the (110) and (200) planes were calculated from the peakdiffraction angles using Bragg's well-known equation. The a and b lattice parameters
were then calculated using the following equations:
a = 2 d20 0 (1)
and .
b - 2 = d - 2 - a - 2 (2)110
which are appropriate for the orthorhombic unit cell of polyethylene.
To determine crystallinity from the "Zoom I" data, the intensity curves weremathematically resolved into separate polyethylene amorphous, (110), and (200), andgraphite (002) components.6 The calculation of crystallinity XC from the relativeareas of the Gaussian polyethylene components followed the method of Gopalan andMandelkern:
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XC (All 0 + A 200 )/(A1 1 0 + A20 0 + Aamorph). (3)
5. EASTABROOK, J. N. Effect of Vertical Divergence on the Displacement and Breadth of X-Ray Powder Diffraction Lines. Brit. J.Appl. Phys., v. 3, 1952, p. 349. ...
6. DESPER, C. R. Computer Programs for Reduction of X-Ray Diffraction Data for Oriented Polycrystallme Specimens. Army Materialsand Mechanics Research Center, AMMRC TR 72-34, November 1972.
7. GOPALAN, M. R., and MANDELKERN, L. Degree of Crystallinity of Linear Polyethylene From ide-Angle X-Ray Diffraction. -Polymer Letters, v. 5, 1967, p. 925.
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Use of this equation, however, ignores the effect of the clear lacquer and graphitecoating on the specimen surface. This point will be discussed later in greaterdetail.
Density Determination
Densities were determined in a density gradient column made from water andisopropanol at 230, using glass beads of known density for calibration. To obtaincrystallinity values, limiting values of amorphous and crystalline specific volumesVA and VC of 1.170 and 0.999 cm3/g were used based on the data of Gopalan andMandelkern. 7 The resulting formula for crystallinity XC is: 0
XC = (VA - I/0)/(VA - VC). (4)
GPC Determinations
Molecular weight characterization was accomplished using the Waters Model 150-C 9Gel Permeation Chromatograph. The polymer specimens were dissolved in trichloro-benzene (TCB) and run at 1350C. Two chromatograms were obtained for each samplesolution. Data were analyzed against known calibration standards using an on-lin,microprocessor.
SAMPLES
Samples of DF container material which were studied in previously reported work1
were available for comparative characterization. Using the terminology of the earlierreport, these samples were denoted by both their history and nominal thickness in mm.In terms of history, the samples fall into three classes:
1. OLD sheets stocked from 1973 production runs;
2. NEW - sheets stocked from 1977 production runs; and
3. EXPOSED - two cannisters which were fabricated in 1973, filled with DF liquidfrom that date to 1981, then drained and rinsed with water.
Samples are also designated by nominal thickness, either 1.5 nm or 6 mm for differentparts of the cannister, although the same polymer resin was used in each instance forboth thicknesses.
The above samles were fabricated from the same resin grade (Marlex M407MQ,Philips Petroleum Co.), reportedly a copolymer of ethylene and butene-l, the ethylenebeing the major constituent. Presumably the butene-I constituent polymerizes to leaveethyl side groups pendent on a largely linear polyethylene molecule. However, thisresin grade has recently been superseded by a new grade, Marlex M445, reportedly acopolymer of ethylene and hexene-l having quite similar properties. For the M445these short-chain branching deliberately introduced by incorporation of the comonomerwould consist of butyl groups rather than ethyl groups. Both resins fall in ageneral class of polyolefins described as "Linear Low Density Polyethylenes," orLLDPE's. In actual fact, these resins are of medium density, around 0.94 g/cm 3 , com- .fpared to density values around 0.92 for low density polyethylenes (LDPE's) containingextensive long-chain branching, or to values around 0.96 for high density polyeth-ylenes (HDPE's) which are essentially free of branching of either the short- or long-chain type.
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A series of standard samples of varying branch content were also available forcalibration purposes. The polymer resins were extensively characterized using methodsdescribed by Billmeyer8 ,9 and WilliamsI0 and made available to the polymer sciencescience community in the 1960's by the Plastics Department of E. I. DuPont de Nemours& Co., Inc., Wilmington, Delaware. These samples are labeled "University ContactPolyethylene" and are numbered PE-75, -76, -78, -79, -80, -81, -82. and -85. Charac-terization data is available in the work of Bodily and Wunderlich.I The last resinof this series, PE-85, is an essentially linear polymer. Two other linear polyeth-ylenes, Marlex 6007 and Chemplex 6109, were also incorporated into the study. All ofthe standard samples were available as pellets which were compression molded at 1700to films of 0.2-mm thickness.
In this study, the DF container samples, which were available as thick sheets,were prepared for X-ray studies by microtoming a section of 0.2-mm thickness, whichwas subsequently heat-relaxed by melting briefly on a glass slide resting on a hotplate at 1700. This treatment was necessary to relieve the residual stresses pre-viously reported1 in these materials.
The samples were further prepared for X-ray diffraction studies by applying athin coating of graphite to one side. The graphite was applied by first spraying thesurface with a clear lacquer (Illinois Bronze, Federal Stock No. 8010-515-2487), thendusting with graphite powder and spreading the powder evenly with a cotton-tippedapplicator.
RESULTS AND DISCUSSION
Molecular Weight Determinations
The gel permeation chromatograms for the three resins are shown in Figure 4, andthe computed results are given in Table I. The results for two of the resins, the1977 version of M407MQ and the replacement grade M445, are remarkably similar in termsof Mn and Mw . There is some difference in the Mz values but probably not enough inrelative terms (roughly 350,000 compared to 370,000) to be a cause for concern. Com- Spared to the earlier resin, M407MQ vintage 1973, both resins are somewhat lower inmolecular weight in terms of Mn and Mw . The most significant difference in the data,
Table 1. POLYETHYLENE MOLECULAR WEIGHT CHARACTERIZATION
BY GEL PERMEATION CHROMATOGRAPHY
Designation Resin Mn Aw Mz Mw/Mn
OLD - 6 mm M407MQ (1973) 29,300 172,300 369,000 5.8830,500 174,100 377,000 5.71
NEW - 6 mm M407MQ (1977) 20,500 156,700 348,000 7.6422,100 160,300 351,000 7.25
M445 M445 (1982) 22,200 163,400 370,000 7.3623,100 161,700 367,000 7.00
8. BILLMEYER, F. W., Jr. Characterization of Molecular Weight Distributions in High Polvmers. J. Polym. Sci., C8, 1965, p. 161.9. BILLMEYER, F. W., Jr. Testbook of Polymer Science. Wiley Intcrscience. New York, Ch. 3, 1971.
10. WILLIAMS, D. J. Polymer Science and Engineering. Prentice-lall, Englewood Cliffs, New Jersey, Ch. 1, 1971.II. BODILY, D., and WUNDERLICH, B. Thermodynamics of Crvstalline Linear High Polymers. IV. The Effect of Ethyl, Acetate. and
Ifvdroxyl Side (; ups on the Noperties of Polyethylene. J. Polym. Sci.: Part A-2, v. 4, 1966, p. 25.
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in fact, is the high Mn value of 29,900 for the earliest resin, compared to values of21,300 and 22,700 for the two later resins. Thib difference is large enough to be ofconcern in terms of its possible effect on physical properties and long-term storagebehavior as a DF container material. The prime concern would be in terms of resis- -tance to environmental stress cracking, since low molecular weight is known, ingeneral, to have an adverse effect. The literature does not, however, contain infor-mation of sufficient detail to permit drawing conclusions about the effect of differ- -.-ences in the molecular weight distribution. We are therefore forced to rely on theresults of exposure tests for each particular resin grade. However, the close simi-larity in molecular weight values between the M407MQ 1977 resin and the M445 resin -leads us to predict that, barring significant differences in other parameters, thesetwo grades will perform in similar manner.
Increasing Molecular Size
Ni LO N- CO 0'-
C4 Cn• LO ,- o
•~N ... . . .. "
o Co (q 0 CN- M o CO0 N- -
Figure 4. Gel permeation chromatograms: (a) M407MQ (1973); AD(b) M407MQ (1977); (c) M445.
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Characterization of Branch Content
The apparent branch content (CH3 /IOOC) from infrared measurements is correlatedfor the standard samples with the lattice parameters a and b, and with the plane ,spacing dll 0 in Figure 5. Least squares straig, lines drawn through the data yield 0the equations:
(CH3/100C) 30.17 (a - ao), (5)
(CH31100C) = 103.03 (b - bo), and (6)
(CH3/100C) = 91.80 (dll 0 - dll 0,0 ) (7)
where the constants ao, bo, and dll, 0 are the intercepts corresponding to the X-rayparameters of a linear polyethylene. The values of the three constants are 7.404,4.935, and 4.107 X, respectively. 4
The X-ray data for the three resins of unknown branch content are used with thecorrelations of Figure 5 and equations 5 through 7 to calculate their branch contents.The results are given in Table 2.
Data for several of the samples were replicated, allowing an estimate of theprecision of the lattice parameter determination. It was found that dll 0 is deter-mined to a standard deviation (a) of 0.001 A, while the standard deviation of an aor b determination is 0.004 . However, when these values are used in conjunctionwith the slopes of equations 5 through 7, as summarized in Table 3, the standarddeviations of the branch content are found to be nearly equal for the a and dll0correlations, but much higher for the b correlation. The key factor is the fact thatthe a correlation has the lowest slope (equation 5), reflecting the fact that the adimension of the unit cell expands over three times more rapidly than b with increas-ing branch content. Thus, although a and b are determined to about the same preci-
sion, about three times as much error propagates into the branch content value when
Table 2. BRANCH CONTENT FROM LATTICE PARAMETER MEASUREMENTS 0 4Estd. Estd. Estd.
Resin a, A (CH3/100C) b, A (CH3/OOC) dll O , A (CH3/100C)
M407MQ (1973) 7.432 0.85 4.943 0.78 4.116 0.86
M407MQ (1977) 7.434 0.91 4.946 1.09 4.118 1.04
M445 (1982) 7.432 0.85 4.945 0.99 4.117 0.95
Table 3. PROPAGATION OF ERROR, LATTICE PARAMETER/BRANCHCONTENT CORRELATION
Slope of 0Ordinate Abscissa o (Abscissa)* Correlation a (Ordinate)*
0 0
(CH3/100C) a 0.004 A 30.17%/A 0.12%0
0
(CH3/lOOC) b >O.OCI A 103.03%/A 0.41%0
0(CH3/1OOC) dll 0 0.001 A 91.80%/A 0.09%
*Standard deviation values are absolute, not relative.
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a. _ diretion expansion x
3.0
(04 31IOOC) 30.11 IS-4)X
2.0
X
1.0 - UnknOwns
WIVI/MO 977'1 M4W7ao .4 MIQ 41973.M4
00 -- . ! I ! l !1.400 7.410 7.420 1.430 7.440 7.450 7.460 7.470 7.490) .4 7.5M 1.510
bdireion expansion
(04lo /1,C) 1DID I
CHCI3 C)1) XI_)
3.0
ICH./lOOC) • !- oY"
1. CH3) 10C) X
x
2.0 xx
Unknw .5mo M 1917)
1.0 MM5
MIO&(3 (19"3)bo 4.935
0.0
91 b (
4 934 4.940 4.950 4.940 4.970
c. dilo direction expansion X
3.0 ICH 31IOC)
x
2.0 X
%i)CH3 IODC) • 91.90 W1o x
";""1 X
Unknowns:
1.0 - M4OM (1977"
M407M0 (1973)
0.0 t_,-: I d 110
4.100 4.110 4.120 4.130 4.140
Figure 5. Lattice expansion versus side-chain content in polyethylene.
10
." .. . -..
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using the b correlation in place of the a correlation. On the other hand, the param-eter d1 l0 is also much less sensitive to branch content than is a, but d11 0 is deter-mined to greater precision, since the reflection is the sharpest and most intense ofthe polyethylene diffraction lines. The two effects tend to cancel out, resulting - -in comparable precision, on the order of 0.1%, for the branch content when determined 0
from either the a or dJl 0 correlations.
At this point it is appropriate to examine the results for the three unknown resinsand ask whether there are significant differences between them in branch content. Theresults, shown in Table 4, are most instructive. Using the a correlation, the averagebranch content for the three unknown resins is 0.87 with a standard deviation of 0.03 . .CH3/IOOC. However, in Table 3 the estimated precision of such a determination is 0.12CH3 /IOOC; in other words, the three unknowns agree with each other to a precisionbetter than the predicted precision of the determination. The same pattern is seenfor the results (Table 4) of the b and dll 0 correlations. This could be fortuitous,but a better explanation may be offered by the data in Table 5, in which parameterscharacterizing the sharpness of the diffraction lines and the signal/noise ratio of •the diffraction peaks are listed. The low density resins (PE-75 through PE-80) showbroad diffraction lines and low signal/noise ratios, while the linear high-densityresins (PE-85, 6007, and 6109) give sharp lines and higher signal/noise ratios. The
Table 4. STANDARD DEVIATIONS* OF BRANCH CONTENT SDETERMINATION OF UNKNOWNS
AverageOrdinate Abscissa Ordinate a (Ordinate)
(CH3/lOOC) a 0.87% 0.03% -
(CH3/lOOC) b 0.95% 0.13% 5 •
_
(CH3/JOOC) d1l0 0.95% 0.07%
*Comparing correlation line results for thethree resins of unknown branch Lontent.
Table 5. FACTORS INFLUENCING PRECISION OFDIFFRACTION SPACING MEASUREMENT
Peak Width at Half Intensity Peak Signal/Noise Ratio
Sample (110) (200) (110) (200)
PE-75 0.5820 0.7620 4.2 1.1 .
PE-76 0.508 0.716 5.1 1.3
PE-79 0.528 0.722 5.2 1.2
PE-80 0.522 0.704 5.9 2.7
PE-85 0.338 0.390 23.2 4.5
6007 0.334 0.382 17.5 5.7 •
6109 0.302 0.384 15.1 3.8
M407MQ:
(1973) 0.408 0.460 10.8 4.1
(1977) 0.390 0.434 14.3 7.3
M445 0.402 0.440 13.7 4.6
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three medium density unknowns fall in between, but closer to the high density valuesof line breadth and signal/noise ratio. The precision of a lattice parameter measure-ment will be influenced by both factors, with smaller line breadth and higher signal/noise ratio favoring greater precision in a lattice parameter value and in the result-ing branch content value. Thus, the precision of a determination is not uniform overthe entire range of branch content values. Low density resins will give less preciseresults, while medium and high density resins will give more precise results. Theexcellent agreement in Table 4 for the results on the three unknowns is not fortui-tous, but reflects the greater precision inherent in the method at lower branchcontent values.
The lattice parameter method for determining branch content thus becomes moreprecise in the range where the infrared method (ASTM D2238-68) becomes less precise.For comparison, the relative precision of the a lattice parameter correlation is 4%at 3 (CH3/IOOC) and 3% at 0.87 (CH3/IOOC), whiTe the ASTM standard for the infraredmethod gives an estimated precision of 2% at 3 (CH3/IOOC) and 5% at 0.3 (CH3/lOOC).
The accuracy of the two methods must be considered as well as the precision.Precision refers to the reproducibility of a measurement and, generally, takes intoaccount random errors in the measurement. Accuracy refers to the error between thedetermined result and the true value, and thus includes systematic error as well.There evidently can be a great deal of systematic error in the infrared method, since, -although good precision is obtained within a single laborat,:ry, the ASTM standardreports a coefficient of variability of 13% to 30% when results from differentlaboratories are compared.
The measurement of polyethylene lattice parameters by X-ray diffraction is alsosubject to the possibility of systemati... error arising from errors in instrumentalignment. For example, Table 6 lists literature values for the a parameter of lin-ear polyethylene which range from 7.385 to 7.45. In the present work, however, stepshave been taken to eliminate the effect of such systematic error on the branch contentdetermination. First, the use of the position-sensitive detector, which records data .-.for all angle values simultaneously rather than sequentially, means that any drift inthe instrumentation affects the entire pattern rather than skewing a portion of thepattern. Second, the use of the graphite internal standard diffraction line minimizesthe effect of instrumental variables between determinations for different samples.Third, the use of standard polyethylene samples run under the same conditions as theunknowns means that absolute accuracy is not required in the determination of latticeparameters. The diffraction spacings measured here could be in error in absoluteterms, but the correlation with branch content is still valid to the precision of theexperiment.
The most significant area for improvement in the method is in the standard sam-ples. A wider range of branch content values in the standard samples, as well as moreaccurately known branch contents would be valuable for improving the correlation co-efficient of the least squares fit and for checking for curvature in the correlation.
Crystallinity
The crystallinity values for the three unknowns and for the standard samples, asdetermined bv density and by X-ray diffraction, are listed in Table 7. Serious dis-crepancies are evident between the density and X-ray crystallinities, and are believedto have their origin in the graphite and lacquer coating applied to the surface tofurnish an internal reference line tor precise measurement of lattice parameters.
12...............•
-
Table 6. LITERATURE VALUES, A PARAMETEROF LINEAR POLYETHYLENE
Author Date a
.-alter & Reding'' 1956 7.385 90
Cole & Holmes' 1960 7.40
Swan"4 1962 7.417
Wunderlich & Poland's 1963 7.40, 7.45
Bodily & Wunderlich" 1966 74Zugenmaler & Can tow16 1969 7.41 8Kavesh & Schult' 1970 7.388Wunderlich'5 1973 7.426This Work 1983 7.404
Table 7. CRYSTALLINITY VALUES BYDENSITY AND X-RAY DIFFRACTION
Densty ~ Crystallinity, XcSample (g/cm3) From p X-Ray*
M4407MQ:
(1973) 0.9395 0.618 0.50
(1977) 0.9420 0.624 0.54
M445 0.9409 0.627 0.55
PE-75 0.9143 0,446 0.37
PE-76 0.9211 0.493 0.40
PE-78 0.9203 0.488 0.44
PE-79 0.9219 0.499 0.39
PE-80 0.9213 0.495 0.42
PE-81 0.9189 0.478 0.40
PE-82 0.917 1 0.466 0.42
PE-85 0.9512 0.694 0.69
6007 0.9532 0.707 0.77
6109 0.9620 0.763 0.60
*Specimens coated witi clear lacqer andgraphite. Density values of Xc arepreferred.
12. WALTER, E. R., and RE.DING, F. P. Variations in Unit Cell Dimensions in Pclythylene. J1. Polym. Sci., Y. 21, 1956, p. 561.13. COLE, E, A., and HOLMES, D. R. Crystal Lattice Parameters and the 7Termal Expansion of Linear Paraffin Hydrocarbons, Including
Polyethylenes. J1. Polym. Sci., v. 46, 1960, p. 245.14. SWAN, P. R. Polyethylene Unit Cell Variations with Branching. J. Polym. Sci., v. 56, 1962, p. 409.15. WUNDERLICH, B., and POLAND, D. Thermodynamics of Crystalline Linear High Polymers. II. 7The influence of Copolymer Units
on the T7hermodynamic Properties of Polyethylene. J. Polym. Sci. A, v. 1, 1963, p. 357.
16. ZIJGENMAIER, P., and CANTOW, H. J. Indication of X-Ray Wide Angle Reflexes of Substances of (rthorhombwr Unit Celli Mea-surements on Polyethylene and Ethylene-P'opylene Copolymers. Kolioid-Z. Z. Polym., v. 230, 1969. p. 229.
17. ICAVESH, S., and SCHULTZ, J. M. Lamellar and Interlamellar Structure in Melt-Crystallized Polyethylene. L. Degree of Crystalinity,Atomic Positions, Particle Size, and Lattice Disorder of the F~rst and Second Kinds. J. Polym. Sci.: Part A-2, v. 8. 1970, p. 243.0
18. WUNDERLICH, B. Macromolecular Phzysics. Academic Press, New York, v. 1, 1973, p. I L 3-154.
13
-
1 .. 7 7-7. .
This coating evidently contributes diffuse intensity (in addition to the sharp graphiteline, whose intensity is accounted for) in the region of the amorphous polyethylenemaximum, invalidating the X-ray crystallinity values by making them generally lowerthan the true crystallinities. 0
For comparison, Table 8 lists crystallinity values determined by both the densityand X-ray methods for six DF container samples previously studied. 1 The two sets ofcrystallinities are essentially in agreement, even though the X-ray method suffersfrom greater scatter. The average crystallinity of the six samples is 0.627 ± 0.01 bydensity, and 0.62 ± 0.03 by X-ray diffraction. The scatter in the X-ray crystallin-ities is believed to lie in errors associated with: (a) separation of the broad, lowamorphous intensity curve from baseline intensity, and (b) separation of the (110) and(200) diffraction peaks from the amorphous peak. Obviously, the X-ray method, basedon the calibration of Goalan and Mandelkern7 is valid, but the density method ofdetermining crystallinity is preferred.
SO.
Table 8. COMPARISON OF DENSITY AND X-RAY VALUESOF CRYSTALLINITY, DF CONTAINER SPECIMENS
Density p Crystallinity, XcSample (g/cm ) From p X-Ray*
OLD - 1.5 mm 0.9396 0.618 0.60 0
OLD - 6 mm 0.9394 0.617 0.67
NEW - 1.5 mm 0.9411 0.628 0.63NEW - 6 Fn 0.9430 0.641 0.59
EXPOSED - 1.5 mm 0.9420 0.634 0.62
EXPOSED - 6 mm 0.9402 0.622 0.58
Average 0.9409 0.627 0.62
Standard Deviation 0.0013 0.01 0.03
*Reflection method, no coating.
The density values listed in Tables 7 and 8 for the 1973 and 1977 vintages sam-ples of container material, and for the replacement resin M445, all lie within therange 0.939 to 0.943 g/cm3 given in the specification MIL-P-51431 (EA) for these con-tainer resins. In fact, the small differences observed between the six samples ofTable 8 may not be particularly significant compared to experimental uncertainty. Thesix vary by a standard deviation of 0.0013 g/cm3, while replicate determinations ofdifferent specimens of a single independent sample yielded a standard deviation of0.0006 g/cm . Thus the difference between the six samples of Table 8 is only twicethe experimental uncertainty. For all practical purposes, the six container samplesof Table 8, and the replacement resin M445, have identical density values.
CONCLUSIONS
The three resin grades studied - M407MQ vintage 1973, M4O7MQ vintage 1977, andM445 vintage 1982 - proved to be remarkably similar materials in terms of molecularweight and branch (comonomer) content. Although this is evidence of product con-sistency on the part of the vendor, a clear need remains for close monitoring ofmaterials parameters to meet the requirements for DF containers. The determination
14
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-
of molecular weight distribution by gel permeation chromatography is a far betterguide than the melt flow index and is recommended for inclusion in a materials speci-fication. Precision determination of lattice parameters appears to offer the possi-bility for more accurate measurement of side chain content, particularly at thelevel of approximately I CH3 /IOOC, or 0.5% comonomer content, which is of interest 0for the ethylene/butene-I and ethylene/hexene-I copolymers in the LLDPE class of . y.polyolefins. The X-ray lattice parameter method has the potential for bettercharacterization of these materials for branch content than the presently used in-frared method. However, characterization of crystallinity by the establisheddensity method is the best choice for this purpose.
Once these three parameters (molecular weight distribution, branch contents, anddensity) are established, the properties of the polyolefin material (aside from pro-cessing effects) are fairly well defined. The question of long-chain branching hasnot been addressed here since this parameter is difficult to assess experimentally.However, the LLDPE class of polyolefins is generally believed to be essentiallybelieved to be essentially free of long-chain branching, as are HDPE's, by thenature of the polymerization reactions used. Only LDPE's, polymerized by the high-pressure free radical mechanism are believed to contain significant amounts oflong-chain branches, which have strong effects on the physical, mechanical, andrheological properties. The density specification, however, is judged to coverany possibility of long-chain branching. A polyethylene with a significant levelof long-chain branch content will always have a density considerably lower than 0the specification range of 0.939 g/cm 3 to 0.943 g/cm 3 .
In terms of resin performance, characterization of the three resins indicatesthat all are in the range of molecular weight, density (crystallinity), and branchcontent for optimum resistance to environmental stress cracking. The two laterresins, M407MQ (1977) and M445, are somewhat lower in number average molecularweight Mn than the original M407MQ of 1973. Whether this will have a significanteffect on environmental stress cracking in DF containers is best determined byexposure tests which are in progress at the Chemical Systems Laboratory.
ACKNOWLEDGMENTS -
1.. author wishes to gratefully acknowledge the contributions ofDr. Gary L. Hagnauer and Mr. David A. Dunn, who provided the GPC data, andMs. Judy Brodkin, who provided the densitv data.
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DISTRIBUTION LIST
No. ofCopies To
1 Office of the Under Secretary of Defense for Research and Engineering,The Pentagon, Washington, DC 20301
2 Commander, Defense Technical Information Center, Cameron Station, Building 5,5010 Duke Street, Alexandria, VA 22314
1 Metals and Ceramics Information Center, Battelle Columbus Laboratories,
505 King Avenue, Columbus, OH 43201
Commander, Army Research Office, P.O. Box 12211, Rese