Designation: D 6474 – 99 An American National Standard

Standard Test Method for

Determining Molecular Weight Distribution and Molecular
Weight Averages of Polyolefins by High Temperature Gel
Permeation Chromatography1
This standard is issued under the fixed designation D 6474; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (e) indicates an editorial change since the last revision or reapproval.

1. Scope Detectors Used in Liquid Chromatography5

1.1 This test method covers the determination of molecular E 691 Practice for Conducting an Interlaboratory Study to
weight distributions and molecular weight averages of linear Determine the Precision of a Test Method5
polyolefins by high temperature gel permeation chromatogra- IEEE/ASTM S1-10 Standard for Use of the International
phy (GPC). This test method uses commercially available System of Units (SI): The Modern System (replaces ASTM
polystyrene standards and equipment and is applicable to E 380 and ANSI/IEEE Standard 268-1992)6
polyethylenes (excluding high pressure low density polyethyl- 3. Terminology
ene–LDPE) and polypropylenes soluble in 1,2,4-
trichlorobenzene (TCB) at 140°C. This test method is not 3.1 Definitions—Definitions of terms applying to plastics
absolute and requires calibration. appear in Terminology D 883.
3.2 Definition of Term Specific to This Standard:
NOTE 1—Size exclusion chromatography (SEC) often is used as an 3.2.1 polyolefin, n—used in this context, refers to PE
alternative name for gel permeation chromatography (GPC).
(except LDPE) and PP thermoplastics.
NOTE 2—Specific methods and capabilities of users may vary with
differences in columns, instrumentation, applications software, and prac- 4. Summary of Test Method
tices between laboratories.
NOTE 3—One general method is outlined herein; alternative analytical 4.1 In this test method, a polyolefin sample is dissolved in a
practices can be followed and are attached in notes where appropriate. solvent and injected onto a chromatographic column(s) packed
NOTE 4—There is no similar or equivalent ISO standard. with a solid substrate, which separates the molecules according
1.2 The values stated in SI units, based on IEEE/ASTM to their size in solution. The separated molecules are detected
S1-10, are to be regarded as the standard. and recorded as they elute from the column according to
1.3 This standard does not purport to address all of the concentration. Through calibration, retention times are con-
safety concerns, if any, associated with its use. It is the verted to molecular weights. Average molecular weight param-
responsibility of the user of this standard to establish appro- eters and molecular weight distribution are determined from
priate safety and health practices and determine the applica- the molecular weight concentration data.
bility of regulatory limitations prior to use.
5. Significance and Use
2. Referenced Documents 5.1 This test method measures the molecular weight distri-
2.1 ASTM Standards: bution and molecular weight averages of polyethylene (except
D 883 Terminology Relating to Plastics2 LDPE) and polypropylene resins. Differences in molecular
D 1898 Practice for Sampling of Plastics2 weight and molecular weight distribution significantly affect
D 3016 Practice for Use of Liquid Exclusion Chromatogra- physical properties, such as morphology, strength, melt flow
phy Terms and Relationships3 etc., and as a result, the final properties of products made from
D 5296 Test Method for Molecular Weight Averages and these resins.
Molecular Weight Distribution of Polystyrene by High
6. Interferences
Performance Size-Exclusion Chromatography4
E 685 Practice for Testing Fixed-Wavelength Photometric 6.1 A major interference is the presence of insoluble, highly
entangled, high molecular weight material that may be linear or
1
This test method is under the jurisdiction of ASTM Committee D-20 on Plastics cross-linked. A successful outcome of the test requires that the
and is the direct responsibility of Subcommitttee D20.70 on Analytical Methods. sample be dissolved completely prior to the chromatographic
Current edition approved Nov. 10, 1999. Published February 2000.
2
separation. The presence of the above-described material often
Annual Book of ASTM Standards, Vol 08.01.
3
Annual Book of ASTM Standards, Vol 08.02.
4
Annual Book of ASTM Standards, Vol 08.03. 5
Annual Book of ASTM Standards, Vol 14.02.
6
Annual Book of ASTM Standards, Vol 14.04.

Copyright © ASTM, 100 Barr Harbor Drive, West Conshohocken, PA 19428-2959, United States.

1
 D 6474
precludes the necessary dissolution step. and shall be of low internal volume so as not to distort the
6.2 A mismatch in the antioxidant level in the dissolved concentration gradient during elution. For this test method, the
sample and that of the TCB eluent (see 8.1). detector cell volume should be 30 µL or less. The most
6.3 The accuracy of the molecular weight results decreases, commonly used concentration detectors for high temperature
that is, they become increasingly underestimated, as the GPC are refractive index or infrared. The former has moderate
a-olefin comonomer content increases in linear low density sensitivity and general utility. When testing detector perfor-
polyethylene (LLDPE). For example, the results for an octene mance, follow the recommendations of the instrument manu-
copolymer containing 30 branches per 1000 carbon atoms will facturer.
be about 6 % low. NOTE 7—For polyolefins, the refractive index (dn/dc) increment is
7. Apparatus essentially constant above molecular weights of 5 000 g/mol. The
response of the components below 5 000 g/mol should be corrected prior
7.1 Essential Components—The essential components of to the molecular weight calculations using a pre-established dn/dc
the instrumentation are a solvent reservoir, a pump, a solvent molecular weight calibration. The principal disadvantage of the differen-
degasser, a sample injection system, packed columns, and a tial refractometer is that the temperature within the detector cell shall be
solute mass detector. controlled to within 0.0001°C.
NOTE 5—Complete high temperature GPC units with a maximum 7.7 Tubing and Fittings—All tubing between the sample
operating temperature of 210°C are commercially available. injector and the detector should be no greater than 0.25 mm
7.2 Solvent Reservoir—The solvent reservoir shall hold (0.01 in.) internal diameter and rated for pressures up to 42
sufficient TCB to ensure consistency of composition for a MPa. Connecting column tubing should be kept as short as
number of runs. The TCB should be protected from exposure possible and all fittings and connectors shall have low dead
to water in the air and the reservoir material shall be inert to the volumes to prevent mixing.
solvent. 7.8 Data Acquisition/Handling System—Means shall be
7.3 Pump—The principal requirement of the pump is pro- provided for determining chromatographic peak heights or
duction of a relatively constant flow, with minimum pulsations, integrated area segments at prescribed time intervals and for
of solvent through the columns. In general, the rate should be handling and reporting data. This is best accomplished using a
adjustable between 0.1 and 5.0 cm3/min and back pressures computer with appropriate software.
should not exceed limits specified by the column manufacturer. NOTE 8—Data acquisition and handling systems for high temperature
Flow rate precision shall be at least 60.3 % as measured under GPC have not been standardized. However, a number of different
the conditions and time interval for a typical analysis. manufacturers provide GPC specific computer software.
7.4 Sample Injection System—The purpose of the injection
system is to introduce the solution containing the sample into 8. Reagents and Materials
the flow stream as a sharply defined zone. Either a six-port 8.1 Solvent—1,2,4-trichlorobenzene (TCB) is recom-
valve with an attached sample loop or a variable volume mended as the solvent for this test method; however, any
injector can be used for this purpose in conjunction with an solvent that has a boiling point higher than the operating
autosampler. Requirements include minimal contribution to temperature, is considered a good solvent for polyolefins, and
band spreading, injector ability to operate at the back pressure is compatible with the GPC components, may be used. With a
generated by the columns, repeatability of injection volume, refractive index detector, the solvent shall have a refractive
and no carryover. index different than that of the polyolefins analyzed. Solvent
7.5 Columns—Stainless steel columns with uniform and purity and consistency shall be considered when choosing a
highly polished inside walls are recommended for high tem- solvent. For example, unless freshly distilled, and subse-
perature GPC. Columns with lengths ranging from 20 to 50 cm quently, kept in a glass container under an inert gas, TCB will
with fittings, frits, and connectors designed to minimize dead react with water to form hydrochloric acid that will attack
volume and mixing are recommended. Generally, the packing tubing walls and degrade column packing. The TCB reservoir
materials, typically styrene divinylbenzene copolymers, have should be protected against exposure to moisture, or be
narrow particle size distributions in the 3 to 20 µm range. replaced frequently with fresh solvent, or both. An antioxidant,
Packing materials are available in a variety of shapes and pore such as 2,6-di-tert-butyl-4-methylphenol (BHT) should be
sizes. Columns may be packed with particles of relatively added to the solvent reservoir at the same concentration, that is,
uniform pore size or with a “mixed bed” of particles to produce about 250 mg/L, as in the solvent used to dissolve the polymer
a broad range of pore sizes. If a set of columns with uniform to minimize any interference due to an antioxidant mismatch
pore size is used, it is recommended that the columns be peak.
connected in order of increasing pore size towards the low NOTE 9—Several laboratories are successfully recycling TCB using
pressure detector side. partial vacuum distillation.
NOTE 6—Packed high temperature GPC columns are available from a 8.2 Polymer Standards—Narrow MWD (MW/Mn < 1.1)
number of manufacturers. polystyrene standards of known molecular weight (available
7.6 Detector—The detector provides a continuous measure from several suppliers) are used for calibration.
of the concentration of solute eluting from the column(s). The 8.3 Other Chemicals—Low MW compounds, such as tolu-
detector shall be sufficiently sensitive and respond linearly to ene or hexadecane, that are used for determining plate count,
the solute concentration, independently of molecular weight, shall be of high purity.

2
 D 6474
9. Hazards ing on the expected breadth of the molecular weight distribu-
9.1 Solvents used in this test method are toxic, or highly tion. Smaller samples should be used when the molecular
flammable, or both. The user is advised to consult literature and weight distribution is narrower, or the molecular weight is
follow recommended procedures pertaining to the safe han- higher, or both. This test method assumes that the mass of the
dling of solvents. injected polymer is low enough for the hydrodynamic volume
of the polymer and the chromatographic separation not to be
10. Sampling mass dependent. If the injected sample mass is too high, the
10.1 Whenever possible, grinding should be used to ensure peak elution volume and the shape of the chromatogram may
a representative sample is analyzed. be affected and lead to erroneous MW values. If in doubt, it is
advisable to rerun an unknown sample or standard at one half
11. Preparation of Apparatus its original concentration to ensure that its elution profile is
11.1 Flow Rate—A flow rate of 1 6 0.1 cm3/min is repeatable. When a change is observed, the analysis should be
suggested. The flow rate should be checked regularly. It is repeated with a lower sample concentration.
recommended that the retention time of the air peak or that of
an added low molecular weight flow rate marker, such as 13. Performance Requirements
toluene, be used to ascertain a flow rate constant to within 13.1 Plate Count Number—The plate count number (N) is a
0.3 %. dimensionless quantity related to column efficiency and pro-
11.2 Detector—Detector performance should be checked vides an indication of the extent of band broadening. Follow
regularly for any deterioration in signal-to-noise ratio. The recommendations of the column manufacturer when initially
calibration mixtures can be used for this purpose. evaluating columns. The plate count number also should be
determined under the same conditions as those used in this test
12. Preparation of Solutions method. For example:
12.1 Polymer Samples: Solvent: TCB
12.1.1 Weigh the polymer samples directly into GPC au- Temperature: 140°C
Flow rate: 1 cm3/min
tosampler vials or into larger heat resistant vials having a cap Test solute: Hexadecane
lined with solvent resistant material. Concentration: ;0.01 % w/v
12.1.2 Add antioxidant containing, that is, about 250 mg /L Injection volume: 300 µL
solvent, preferably siphoned from the solvent reservoir, to give For an approximately Guassian-shaped solute peak, the
a polymer concentration of between 0.05 and 0.2 weight % (see following expression can be used to calculate the number of
12.3). plates (N)/m:
12.1.3 Cap the vials and heat the solutions to about 150°C
for 3 to 6 h to completely dissolve the samples. For polypro- N/L 5 16 3 ~1/L! 3 ~Vr / W!2 (1)
pylene and some high MW polyethylenes, the samples may where:
have to be heated to between 160 and 180°C for complete L = total column length, m,
dissolution. Vr = peak elution volume, mL, or time, min, and
NOTE 10—Magnetic stirring, frequent manual agitation, or a slow W = peak width in units of volume (mL) or time (min) as
rotational arrangement inside an oven is recommended to aid dissolution. determined by measuring the distance between the
Excessive temperatures, prolonged dissolution times, and ultrasonic baseline intercepts of lines drawn tangent to the peak
devices may cause the polymer to degrade. inflection points.
NOTE 11—Filtration of hot polymer solutions to remove or identify the 13.1.1 High temperature GPC columns are expected to
presence of nonvisible gels or other undissolved material is not recom-
exceed 10 000 plates/m. Plate counts should be monitored
mended due to the difficulty involved in filtering at 150°C. Unless
performed very carefully, sample losses may occur due to a drop in regularly and column sets not meeting this performance
temperature during the filtration. Also, most commercial instruments are requirement should be discarded.
or can easily be outfitted with an inline pre-column filter. 13.2 Resolution—The resolution (R) provides an indication
12.2 Polymer Standards—Prepare 3 to 5 “cocktails”, that is, of the component separation and band broadening of a column
mixtures containing 3 to 4 baseline resolved standards, con- set. A GPC specific resolution (Rs) of two standard polymers
taining a total of at least 12 narrow MWD polystyrene differing in molecular weight values by a factor of ten and
standards, as well as some hydrocarbon and polyolefin stan- having polydispersities of less than 1.1 is defined as:7
dards, if available, to give individual concentrations of 0.01 to Rs 5 2~Vr2 – Vr1!/~W1 1 W2! (2)
0.03 weight % (the high molecular weight standards being the
more dilute. The standards should be dissolved at room where:
Vr1, Vr2 = peak elution volume or time of Standards 1 and
temperature (up to three days dissolution time) or at 150°C, as
2, and
described in 12.1, for a few hours. Analyze the standards
within a month of their preparation. Stabilized polystyrene
solutions have been shown to be stable at room temperature for
several months. 7
“Modern Size Exclusion Chromatography—Practice of Gel Permeation and
12.3 Test for Sample Solution Suitability—The mass of the Gel Filtration Chromatography,” W.W. Yau, J.J. Kirkland, and D.D. Bly, John Wiley
polymer injected is typically between 0.05 and 0.5 mg depend- and Sons, 1979.

3
 D 6474

W1, W2 = peak widths of Standards 1 and 2 determined as this is accomplished with a data acquisition software package.
outlined in 13.1. 14.4 Generation of Calibration Curve—Convert the poly-
13.2.1 The two standards should be analyzed at a concen- styrene peak molecular weights to polyolefin molecular
tration of #0.03 % w/v and an injection volume of #300 µL. weights. This is accomplished using the following equation:
This test method requires that the calculated Rs values equal or log10M2 5 $1/~1 1 a2!% 3 log10 ~K1/K2! 1 $~1 1 a1!/~1 1 a2!% 3 log10M1
exceed 2.0. (3)

NOTE 12—General information regarding plate number and resolution where:

can be found in most textbooks on chromatography. M2 = the molecular weight of the polyole-
13.3 Detector Response—Practice E 685 addresses determi- fin,
nation of detector response in Sections 5 and 7. For this test a2, K2 and a1, K1 = Mark-Houwink constants for the
method to be valid, the integrated peak area of the eluted polyolefin and polystyrene, respec-
polymer shall be directly proportional to the mass of polymer tively, and
injected. This can be ascertained by injection of different M1 = molecular weight of the polystyrene.
concentrations of the same polyolefin sample. The above equation is derived from
13.4 Baseline Stability—Practice E 685 classifies deviations the empirical Mark-Houwink equa-
from a perfectly horizontal baseline for a photometric detector tion:
as drift and short-term and long-term noise. These deviations @ h # 5 K 3 Ma (4)
shall be minimized while retaining a high sample response.
Drift, defined as the average slope of the noise envelope over where:
a period of 1 h, is a potential problem when the data handling [h] = intrinsic viscosity and the universal calibration con-
software is unable to correct for it. Without correction, erro- cept8 which states that the product of intrinsic vis-
neous results may be obtained when the drift exceeds 2 % of cosity and molecular weight for any polymer is
the maximum polymer peak signal. Short-term noise, defined proportional to its hydrodynamic volume, which in
as the maximum peak-to-peak amplitude for random variations turn defines the elution volume of the polymer.
of the detector signal with a frequency greater than 1 cycle/ Values for K’s and a’s may be determined with an
min, should not exceed 2 % of the maximum polymer signal. on-line viscometer or obtained from the literature.
Long-term noise, defined as the maximum amplitude for all The following values are recommended for polysty-
random variations of the detector signal of frequencies between rene (PS), polyethylene (PE), and polypropylene (PP)
0.1 and 1 cycles/min, should not exceed 5 % of the maximum in TCB at 140°C:
polymer signal. KPS 5 19 3 1023 mL/g aPS 5 0.655 (5)
13.5 Flow Rate—Small differences (>0.3 %) in the flow rate KPE 5 39 3 1023 mL/g aPE 5 0.725
between the time of calibration and sample analysis will cause KPP 5 19 3 1023 mL/g aPP 5 0.725
significant, systematic errors in MW values calculated. Users
should determine the average flow rate of their system by 14.4.1 Generate the polyolefin GPC calibration curve by
measuring the volume of solvent eluted over a specified time plotting the logarithm of the peak molecular weight values
period. When flow rate variations in excess of 0.3 % are versus the measured peak elution volumes (or times). The
observed, replace or service the pump or correct for flow calibration curve generally assumes an s-shape that asymptoti-
variations by addition of a flow measuring device or use a flow cally approaches total permeation at low MW and total exclu-
rate marker such as for example the air peak or toluene, that is, sion at high MW. It is recommended that a third or fifth order
internal standard. polynomial be used to fit the calibration data. A number of
14. Calibration software packages are available to do this.
14.1 Selection of Polystyrene Standards—Prepare solutions 15. Procedure
of polystyrene calibration standards as outlined in 12.2. A 15.1 Preparation for Analysis—Prepare polymer sample
minimum number of three standards per decade of MW need to solutions as described in Section 12. An internal standard may
be used to adequately define the calibration curve over the MW be added to each sample solution before injection. Alterna-
range covered by the columns. tively, a “stock” solution containing an internal standard for
14.2 Injection of Polystyrene Standards—Make injections monitoring eluent flow rate may be used to prepare the sample
with the instrument autosampler at the same temperature as the solutions. Prepare the apparatus and complete the performance
column oven temperature, that is, typically 140°C. Add the requirements in Section 13.
internal standard, if used, to the solution prior to injection. The 15.2 Injection of Sample Solutions—Following guidelines
injection volumes of all standards shall be identical regardless described in 14.2, the injection volume shall be identical to that
of concentration. The recommended volume is #300 µL for selected for calibration. A sharp increase or “pulse” in back
columns with internal diameters of 0.8 to 1.0 cm. For diameters pressure upon injection indicates a serious problem in the GPC
of <0.8 cm, a smaller volume should be chosen.
14.3 Data Acquisition—Determine the elution peak maxima
and the corresponding elution volumes (or times) for the 8
Z. Grubistic, R. Rempp, and H. Benoit, J. Polym. Sci., Part B, Vol 5, 753
various polystyrene standards (and internal standard). Usually, (1967).

4
 D 6474
system that shall be remedied before continuing. When oper- N

ated unattended, the system should possess the ability to shut Mn 5 ( Ai / (~Ai / Mi!
i51
(7)
down when a specified maximum pressure, for example 250
MPa, is reached. N

15.3 Baseline Determination—Satisfy baseline criteria dis- Mw 5 ( ~Ai 3 Mi!/(Al

i51
(8)
cussed in 13.4. The baseline is assumed to be linear. It is
established by averaging the baseline noise before and after the N
chromatographic envelope and connecting the two with a Mz 5 ( ~Ai 3 Mi2!/(~Ai 3 Mi!
i51
(9)
straight line. If the actual baseline deviates from the generated
line due to drift, shift of excessive noise, the analysis should be 16.2.1 For a constant elution volume interval, DVi, Ai, and
discarded. Mi are the chromatographic peak slice area and polyolefin MW,
respectively associated with the (corrected) elution volume, Vi,
15.4 Integration Limits—The establishment of the low elu-
while N is equal to the number of data points obtained from the
tion volume, that is, high MW end of the chromatogram is
chromatogram between the integration limits (see 15.4). An
usually straightforward. Here, the baseline is not affected by
example of this method of calculating the molecular weight
low MW impurities, and the slope of the polymer response
averages is given in Test Method D 5296. When N is suffi-
tends to be relatively steep.
ciently large, the use of area segments Ai or peak heights Hi
15.4.1 The establishment of the high elution volume, that is,
will yield equivalent results.
low MW is generally more ambiguous and depends largely
16.3 Molecular Weight Distributions/Cumulative Weight
upon the presence of peaks from antioxidants and low MW
Fraction Distribution—Calculate the cumulative distribution
impurities as well as the recovery of a stable baseline. Samples
by integrating the chromatogram to different elution volumes,
frequently exhibit tailing towards low MW’s and it is difficult
that is, molecular weights, using standard numerical integrating
to determine precisely where the chromatogram ends.
procedures, that is, rectangular approximation, and then divid-
15.4.2 It is recommended that the integration limits not fall ing these areas by the total area under the chromatogram. This
outside the elution volumes for the highest and lowest calibra- area ratio is the cumulative weight fraction, Wi, and equals the
tion standards. Integration below a MW of 500 g/mol is not weight fraction of the polymer having retention volumes
recommended due to rapidly changing dn/dc values, poor greater than Vi and molecular weights less than Mi.
definition of the calibration curve and frequent interference 16.4 Molecular Weight Distributions/Differential Molecular
from additive peaks. Weight Distribution—Determine the weight differential distri-
15.5 Data Acquisition—Data systems and computer soft- bution by plotting DW/D(log10M) versus log10M.9 When deter-
ware may handle data acquisition differently. Upon acquisition, mined correctly, plots of the differential distribution functions
data usually is handled in discrete rectangular area segments, versus log10M obtained using different GPC systems to analyze
Ai, or as digitized heights, Hi, by recording the vertical the same sample should be identical. Derivation of differential
displacement between the chromatogram trace and the baseline and cumulative molecular weight distribution functions can be
at elution volumes, Vi, over designated intervals. A minimum found in Test Method D 5296.10
of 40 area segments or heights are required.
15.6 Flow Rate Correction—If the GPC system does not 17. Report
contain a continuous flow rate monitor, then the flow rate shall 17.1 Report the following information:
be within 60.3 % of its value measured at calibration or an 17.1.1 Apparatus:
internal standard should be used. When an internal standard is 17.1.1.1 System type,
used, correct sample elution volumes, Vi’, by the following 17.1.1.2 Column types, dimensions, and manufacturer,
relation: 17.1.1.3 Operating temperature,
corrected Vi 5 Vi’ 3 ~Vis!/~Vis!’ (6) 17.1.1.4 Solvent (plus additives and treatment, if any),
17.1.1.5 Solvent flow rate,
where: 17.1.1.6 Internal standard or flow monitor (if used), or both,
(Vis) and (Vis)’ = the elution volumes of the internal stan- 17.1.1.7 Injection volume, and
dard measured at calibration and for the 17.1.1.8 Polymer sample solution concentration (mg/mL).
sample, respectively. 17.1.2 Plate Count and Resolution:
17.1.2.1 Plate count, N (plates/m),
16. Calculation 17.1.2.2 Test solute for plate count,
16.1 Tabulation of Data—The data acquisition software will 17.1.2.3 Resolution, Rs,
record either area slices or heights of the chromatogram at 17.1.2.4 Standards used for resolution calculation, and
designated elution volume intervals. The appropriate values for 17.1.2.5 Equation used for resolution calculation.
the molecular weight at each elution volume is obtained from 17.1.3 Calibration Standards:
the calibration curve. 17.1.3.1 Polymer standards,
16.2 Calculation of Molecular Weight Averages—The
number-, weight-, and z-average molecular weights (Mn, Mw 9
W.W. Yau and S.W. Fleming, J. Appl. Pol. Sci., Vol 12, 2111 (1968).
and Mz) are calculated using the recorded data and the 10
These distribution functions can be found in “The Elements of Polymer
following expressions: Science and Engineering,” Alfred Rudin, Academic Press, Inc., 1982, as well.

5
 D 6474
17.1.3.2 Molecular weight of polymer standards, and 30 analyses over a period of two months.
17.1.3.3 Peak retention volumes, Vr. 18.2 Table 2 lists repeatability relative standard deviations
17.1.4 Calculated Parameters: for Mn and Mw for two polypropylene materials based on 18
17.1.4.1 Average molecular weights, and analyses over a period of three days.
17.1.4.2 Polydispersity, D = Mw / Mn. 18.3 The reproducibility of this test method is being deter-
mined and will be available on or before January 1, 2004.
18. Precision and Bias
19. Keywords
18.1 Table 1 lists repeatability relative standard deviations
19.1 gel permeation chromatography; molecular weight av-
for Mn and Mw for two linear polyethylene standards based on
erage; molecular weight distribution; polyolefin; size exclusion
chromatography
TABLE 1 Repeatability Relative Standard Deviations (RSD) for TABLE 2 Repeatability Relative Standard Deviations (RSD) for
Linear Polyethylene Polypropylene
Sample PD RSD (Mn) RSD (Mw) Sample PD RSD (Mn) RSD (Mw)
NBS 1475 2.8 4.4 2.0 Homopolymer PP 4.8 10.3 4.5
PE 105K 10.5 5.5 3.5 Copolymer PP 4.8 12.2 4.3

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