f ....................

94--_

Overview of
PolyolefinAdditive Analysis
R.C. Nielson - Waters Chromatography Division, Millipore Corporation
A

Waters
Divisionof MILLIPORE

Presentedat the 1989 InternationalGPC Symposium,October 1-4, 1989

 OVERVIEW OF POLYOLEFIN ADDITIVE ANALYSIS

BY: Richard Nielson

Waters Chromatography Division
Milford, MA 01757

ABSTRACT: The extraction and subsequent separation and quantitation of polymer

additives in polyolefins has proven to be a challenge for the analytical chemist. We
have investigated some ways to extract the additives from polyolefins, namely,
microwave oven and ultrasonic bath techniques for high density polyethylene (HDPE)
and polypropylene. We have concentrated on identifying and quantitating recoveries
for typical polyolefin antioxidants, such as Irganox 1010, Irgafos 168, and Cyasorb UV
i 531. The extraction times are typically 20 minutes for the microwave oven and 30-60
minutes for the ultrasonic bath with 90+% recoveries being obtained. Both normal
phase isocratic (used when phosphites are present) and reverse phase gradient LC
techniques are discussed.

INTRODUCTION: The additive packages used for polyolefins can be quite

complicated, containing several antioxidants, both primary (such as hindered phenols),
and secondary (or also called "synergistic') antioxtdants, as well as antistats, slips,
pigments, etc.

The slip agents tend to be long chain aliphatic amides, such as oleamide and
erucamide. These compounds have limited solubility and UV absorption. Reverse
phase LC analysis (using conventional water/aceto or water/methanol C18 methods) is
very difficult due to the limited solubility of the amides. Methylene chloride does an
excellent job at extracting out these materials, but absorbs in the UV region (-205nm)
required. The differential refractometer proves to be a good detector to use, but our
separations with a normal phase (Si02 column) system failed as the slips eluted all
together at the void volume. We will continue to look at other chromatographic modes
of separation, but the analysis of choice at present seems to be a total nitrogen
elemental analysis determination. We will concentrate on the analysis of antioxldants
for this presentation. The following table lists the antioxidants that we have examined
and chromatographed successfully.

TABLE #1 - POLYOLEFIN ANTIOXIDANTS

ADDITIVE CHEMICAL NAME MANUFACTURER*

BHT Butylated Hydroxy Toluene Many

Irgafos 168 Tds (2,4-di-t-butylphenyl. Ciba-Geigy
phosphite)
Irganox 1010 Tetrakis methylene (3,5-di-t Ciba-Geigy
butyl-4-hydroxyhydrocinnamate)
methane
Irganox 1076 Octadecyl 3,5 di-t-butyl-4- Ciba-Geigy
Ultranox 276 hydroxyhydrocinnamate Borg-Warner
Irganox 1330 1,3,5-trimethyl-2,4,6-tris Ciba-Geigy
Goodrite 1339 (3,5-di-t-butyl-4-hydroxybenzyl)- B.F. Goodrich
benzene
Irganox 3114 1,3,5-tris (3,5,dt-t-butyl-4- Ciba-Geigy
hydroxybenzyl)-s-triazine 2,4,6
(t H,3H,5H) trione
Tinuvin 328 2-(2'-hydroxy-3',5'-di-tert- Ciba-Geigy
amylphenyl benzotriazole
Cyasorb UV 531 2-hydroxy-4-n-octobenzophenone American Cyanamid
Ultranox 626 Bis(2.4-di-t-butylphenyl) Borg-Warner
pentaerythriotol diphosphite
AM 340 ? Ferro
* NOTE: There are other manufacturers that also provide many of the above
stabilizers that are not listed.

RESULTS: This paper will be broken up into two sections: the first will deal with the
extraction and chromatographic analysis of three antioxidants compounded into a high
density polyethylene (HDPE), and the second section will discuss the extraction and
chromatographic analysis of antioxidants compounded into five different polypropylene
resins. We obtained a sample of high density polyethylene (HDPE) in pellet form to
which had been compounded 500 ppm each of BHT, Irganox 1010 and Irganox 1076.
Four separate extraction solvents were utilized, the first being a 9:1 mixture of
cyclohexane and isopropanol, (IPA), which was from a proposed ASTM extraction
method. The second choice (which proved to be more efficient) was a 50:50 mixture of
the same two solvents. The third choice was a 75:25 mixture of methylene chlodde
(MeCI2) and cyclohexane, and the fourth choice being a 98:2 methylene chloride/IPA
mixture. Three different methods of extraction were tded using the first solvent
mixture, including Soxhlet, ultrasonic, (conventional laboratory sonic bath) and
microwave oven, (highpowered, explosion proof microwave oven). Only the ultrasonic
and microwave methods were usedwith the 50:50, 75:25 and 98:2 mixtures as the
Soxhlet method proved to be too long and labor intensive.

The HDPE (for all extraction methods) was ground using the Wiley Mill to a 20 mesh,
with 5 grams + or - 0.10 mg. being added to exactly 50 mls of the solvent mixture.
After the desired extraction time pedod, the HDPE is removed by filtration, and the
solvent mixture allowed to evaporate (without any heat applied, however) to dryness.
The additives are resolubilized with acetonltrile, and brought to mark in a volumetdc
flask. The LC analysis consists of a reverse phase gradient with 3:2 water/acetonitdle
to 100% acetonitrile (5 minute linear gradient) over a Nova-Pak C18 column, (15cm).
Figure #1 shows a typical chromatogram of the extracted antioxidants; in this case,
after two hours extraction using the ultrasonic bath. The BHT, Irganox 1010, and
Irganox 1076 (respectively), peaks are observed. UV detection (@ 254nm in this case)
was used for all of the chromatographic analyses. The table below shows the
recoveries at three different time periods for the Soxhlet extraction using the 9:1
mixture:

TABLE #2
SOXHLIET EXTRACTION - HDPE
9:1 CYCLOHEXANE/ISOPROPANOL

ADDITIVES Con_c_=_Lopm) Conc._(ppm) Conc. (ppm) % Recovery

3 hrs. 7 hrs. 24 hrs. (Total)

BHT 406 427 437 87

IRG. 1010 369 429 464 93
IRG. 1076 421 463. 469 94

The table shows that in order to get the majority of the 1010 out, 24 hours of Soxhlet
extraction may be necessary. The BHT levels are a little on the low side, perhaps
because of the tendency of BHT to sublime under excess heating. The next table
shows the recovedes obtained for the ultrasonic bath extraction, again with the 9:1
cyclohexane/IPA mixture.
TABLE #3
ULTRASONIC EXTRACTION - HDPE
9:1 CYCLOHEXANE/ISOPROPANOL

ADDITIVES Conc. (ppm) Conc. (ppm) Conc. (ppm) % Recovery

1hr. 2hrs. 3 hrs. (Total)
'1
BHT 443 450 454 91
IRG.1010 423 440 458 92
IRG. 1076 453 470 477 95
The relative standard deviations for both the Soxhlet and ultrasonic extraction
techniques were -2%, (result lrom six different extractions and subsequent
chromatographic analyses). The microwave oven was also used, heating the HDPE for
60 minutes in the oven. After -40 minutes, however, the polymer completely
dissolved, and formed a thick suspension upon cooling which was impossible to
handle. It appeared as though the HDPE had formed a mass of "gel", which made
sample filtering and reproducible recovedes impossible.

It was next decided to repeat the microwave and ultrasonic extractions on the HDPE
sample, but using a 50:50 mixture of cyclohexane and IPA. This would cut down on
the amount of non-polar solvent, and presumably, decrease the chance of "gelation" of
the polymer. It was found that only a 20 minute heating of the solution in the
microwave oven at 50% power (and vigorous stirring every 5 minutes) was required to
extract out the additives. The HDPE was ground to a 20 mesh with a Willey Mill for this
experiment as well. The 98:2 MeCI2/IPA mixture was also used for the microwave
oven method (20 minutes at 25% power with stirring every 5 minutes). The results for
the microwave extraction are as follows:

TABLE #4
MICROWAVE EXTRACTION RESULTS- HDPE

ADDITIVE Concentration (ppm) Concentration (ppm)

1:1 Cyclohexane/IPA 98:2 MeCI2/IPA

BHT 451 (90%) 455 (91%)

1010 454 (91%) 459 (92%)
1076 480 (95%) 474 (95%)

The 50:50 cyclohexane/IPA and 75:25 MeCI2/Cyclohexane mixturesproved to work

exremely well with the ultrasonic method of-extraction. The groundHDPE was
extracted for just one hour in the sonic bath, with the solution being stirred every 10
minutes vigorously for at least 30 seconds. The extraction was carded out for only 30
minutes using the MeCI2/cyclohexane mixture (again, stirring every 10 minutes). The
table below illustrates the recoveries obtained for each additive:

TABLE 15
ULTRASONIC EXTRACTION RESULTS - HDPE

ADDITIVE Concentration (ppm) Concentration (ppm)

1:1 Cyclohexane/IPA 75:25 MeCI2/
(60 Min) Cyclohexane (30 Min)

aNT 454 (91%) 449 (90%)

1010 457 (91%) 458 (92%)

1076 475 (95%) 481 (96%)

In all cases, the separations were carried out using a 15cm Nova-Pak C18 column, with
a gradient of 60:40 water/acetonitrile to 100% CH.gCN (5 minute linear gradient). For
the first experiment (9:1 solvent ratio), the flow rat_ was 2.0ml/min., an(:l for the 50:50
solvent mixture extractions, the eluent flow rate was 1.5 ml/min. The column temp.
should be held above room temp., such as 40c. We also used a 7.5cm NovaPak
column, which will bring the 1010 and 1076 retention time down significantly. The
shorter column can be used when the additive package is relatively simple (three
components or less, for example), with the same water/acetonltrilegradient. If the
additive package is much more complicated (i.e., contains several additives that elute
very closely), than the 15cm NovaPak should be used. In summary, the 50:50
cyclohexane/IPA mixture works very well with both the ultrasonic bath extraction
method (1 hr. with stirring every 10 minutes), and the microwave oven (only 20 minutes
at 50% power, vigorous stirring every 5 minutes). The stirring is very important, as
agitation will facilitate the extraction of the additives out of the polymer matrix. The
small amount of IPA added to the MeCI 2 mixture for the microwave extraction is
necessary as MeCI 2 alone heats up very slowly in the microwave, and the IPA
(because of the polar OH group), heats up very quickly. The addition of only 2% was
enough to heat up the solution and extract the additives successfully. The 75:25
MeCI2/cyclohexane mixture used with the ultrasonic bath worked very well also. Any
one o-fthese three methods may be used to efficiently extract out the additive package
for HDPE.

The next step was to investigate the ultrasonic and microwave extraction procedures
and determine recoveries for polypropylene. Several polypropylene resvns were
submitted to us that contained a variety of additive packages. The additives were
resent at various levels, with the precision of the compounding being + or - 35 ppm.
he polypropylene formulations consisted of antistats, pigments, fillers, slip agents, and J
antioxidants/UV degradants. For the purposeof this Work, we will concentrate on the "I
extraction, identification and quantitat,on of the antioxidants, including the phosphite
esters. Each of the resins was said to possibly contain an unknown (but low) amount
of Irganox 1076 which was compound into the resin initially. The 1076 can be
observed at times in some of the chromatograms for the resins. In addition to the
usual hindered phenolic type antioxidants such as Irganox 1010, 1076, and 3114, many
of the resins contained phosphite esters such as Irgafos 168 and Ultranox 626. These
phosphite esters are referredto as secondary antioxidants, or synergistic antioxidants.
One of their primary functions is to react with the hyroperoxide (°OOH) group which is
the last step prior to chain scission. Where reverse phase separation techniques
require water as part of the gradient elution scheme, the phosphite esters are prone to
hydrolysis. We, therefore, examined normal phase chromatographic techniques, using
a Resolve silica column (51.1.particle size) when the phosphites were present. Several
solvent combinations were tried, as well as many gradient and isocratic methods. The
best chromatographic system consisted of a 70:30 mixture of n-butyl
chloridemethylene chloride.

The same methylene chloride/IPA, methylene chloride/cyclohexane and

cyclohexane/IPA solvent mixtures that were used for the HDPE extractions were also
investigated for the polypropylene resins.

Both a variable wavelength UV detector (@ 225nm and the photodiode array detector
were used for the analysis. The following additives were chromatographed as part of
the normal phase separation study:

AM 340 Irganox 1330

BHT Irganox 3114
Irgafos 168 (phosphite) Tinuvin 328
Irganox 1010 Cyasorb UV 531
Irganox 1076 Ultranox 626 (phosphlte)

The Irgafos 168, Irganox 1010, 1076 and 3114 can all be separated in under 7 minutes
at a 1.5 ml/min flow rate. The first extraction procedure consisted of a microwave oven
ocedure, heating 5 grams (+ or - .10mg.) of resin that were previously ground in the
iley Mill to 20 mesh in 50 mls. of a 98:2 methylene chloride/2-propanol mixture. The
IPA is added to allow for heating of the mixture in the microwave.The resins were
extracted in the microwave oven for 20 minutes at 25% power, with vigorous stirring
every 5 minutes. After the extraction period, the solutions were allowed to cool, (the
solvent temperature (48c) was above the boiling point of MeCI 2 (-40c) in the sealed
sample containers), then filtered and dnsed with MeCI 2. The additive solutions are
then brought to mark in a volumetric flask, (10 or 25 mE depending on the amount of
additives present in the resin), then chromatographed by the normal phase, isocratic
separation procedure. The normal phase separation is recommended only when a
pbosphlte ester is present in the formulation, or if the formulation is relatively simple. A
complicated formulation containing several antioxidants (but no phosphite) would best
be separated by reverse phase techniques, which will be discussed later on. Figure #2
shows the normal phase isocratic separation of four antioxidant standards: Irgafos
168, Irganox 1076, Irganox 3114, and Irganox 1010. Figure #3 shows the same
chromatogram, but with the photodiode array detector instead of the UV detector. The
chromatogram is a 3-D picture, with retention time (X direction), absorbance (Y
direction) and wavelength (Z direction) all being shown. The table
below lists the recoveries obtained for four o! the resins, two of which contain a
phosphite ester, using the microwave oven and the 98:2 methylene
chlonde/isopropanol mixture (20 minutes):

TABLE #6
MICROWAVE EXTRACTION RESULTS - POLYPROPYLENE
98:2 METHYLENE CHLORIDEJISOPROPANOL

RESIN "D*

Additive Amount Amount % Recovery

Recovered (ppm) Present (ppm)
+ or - 35

Irganox 31 t 4 565 600 94

Cyasorb UV 531 442 500 88

RESIN "E"

Irgafos 168 521 500 100+

Irganox 1010 986 1000 99

RESIN _G"

Ultranox 626 709 800 89

Irganox 3114 635 800 89

RESIN "1"

BHT 513 500 100+

Irganox 1010 931 1000 93

*Note: The "D" resin also contained 2,000 ppm of AM 340, but the normal phase
separation results were not as good as for the reverse phase analysis, to be discussed
later on, for this antioxidant.

The recoveries are excellent for all of the additives except the Irganox 3114, which was
recovered at only 79%. The two phosphites perhaps showed some signs of
degradation, with a minor peak being observed next to the major one. This peak,
however, eluted very closely to where Irganox 1076 elutes, and identification was
impossible. Some of the resins were reported to contain an unknown amount of 1076.
The 1010 was recovered in the two resins at better than 92%, which is very
encouraging. This is one of the more difficult antioxidants to remove, and the resin
must be ground in the Wiley Mill for extraction to be successful. During the grinding
procedure, one must be careful not to force the resin too quickly, as the heat buildup
may cause the polymer to melt. Addition of carbon dioxide or liquid nitrogen will
prevent this from happening. Some of the resins were extracted "as is" (pellets, not
ground), and recoveries were excellent using the microwave technique except for 1010,
which could be extracted at no better than -40% recovery without grinding. The next
step was to microwave extract the "E" resin and perform the chromatographic
separation six times in order to determine the reproducibility of the technique. The
table below shows the results:
 TABLE #7
"E" RESIN EXTRACTION REPRODUCIBILITY STUDY

Extraction # Conc. Irgafos 168 Conc. Irganox 1010

(ppm) (ppm)

1 521 986
2 485 1034
3 509 981
4 476 1019
5 489 978
6 496 970
[R.S.D. -- 3.3%] [R.S.D. = 2.6%]

This results in a value of 496 + or - 16 ppm, or 3.3% for Irgafos 168, and a value of 995
+ or - 26 ppm, or 2.6% for the Irganox 1010 W_ wm,ld expect the Irgafos (phosphite)
to not be quite as good precision-wise, as this material has more of a tendency to
degrade more rapidly, and the peak height/area variance from run to run was greater
than for the 1010.

The next procedure consisted of an ultrasonic extraction of the "E" resin, (again ._round
with the Wiley Mill), using a 75:25 MeCI2/cyclohexane solvent mixture. The first
extraction was done for thirty mlnutes. As the table below indicates, an additional 30
minutes (or one hour total) was required to extract out the 1010 at 98+ % recovery.
Each extraction was done in triplicate, with the results being as follows:

TABLE #8
ULTRASONIC EXTRACTIONS - 75:25 MeG12/CYCLOHEXANE

ADDITIVE Conc. (ppm) Conc. (ppm)

30 min. 60 min.

Irgafos 168-1 522/500 492/500

Irgafos 168-2 494/500 516/500
Irgafos 168-3 513/500 503/500
1010-1 929/1,000 982/1,000
1010-2 882/1,000 998/1,000
1010-3 921/1,000 980/1,000

The above table indicates that all of the Irgafos 168 is extracted in only 30 minutes,
with -88% (worst case) of the 1010 being extracted out. We can "squeeze out" a little
more of the 1010 if we choose to extract in the ultrasonic bath for afull hour. Figures
#4 and #5 show the UV and photodiode array chromatograms, respectively, for the
ultrasonic extract residue trom the "E" polypropylene resin. The small peak just under
two minutes was not quantitated as 1076, as we did not know how much 1076 (if any)
was present in this resin, (as discussed previously). All of the above chromatography
was carried out using the normal phase isocratic separation with the Resolve Si02
column and the 70:30 BuCI2/MeCI 2 mixture. This procedure proved to be excellent for
several of the resins that containei:l the phosphite esters, with no evidence of any
hydrolysis or other severe degradation of the phosphites having taken place.

The last procedure consisted of a reverse phase analysis, using a 3:2 water/acetonitrile
to 100% acetonttrile 5 minute linear gradient across a Nova-Pak C18 column. The
eluent flow rate was 1.5 ml/minute, with column temperature being maintained at 40°c.
The reverse phase separations afford much better selectivity than does the normal
phase separations, but the retention times are longer. Note, however, the excellent
separation power of the mix of the 7 standards, eluting, in order: BHT, Cyasorb UV
531, Irganox 3114, Tinuvin 328, Irganox 1010, Irganox 1330, and Irganox 1076, (see
Figures #6 and #7). The PDA chromatogram (Fig. #7) shows five of the antioxidant
standards for sake of clarity. These are all baseline separated in just about 20
minutes. Three resins (not containing a phosphite) were extracted in both the
microwave oven and in the ultrason!c bath using, a 50:50 mixture of cyclohexane and
2-propanol. The mwcrowave extraction was carried out for lust 20 minutes at 25%
power, with vigorous stirring for 30 seconds at 5 minute intervals. The ultrasonic
extraction was carded out for 1 hour with vigorous stirring every 15 minutes.
The 5 grams of PP resin were ground as usual on the Wiley Mill. Figure #8 shows the
reverse phase gradient chromatogram for resin "D". Just for curiosity's sake, the "E"
resin was also extracted, but the Irgafos 168 could not be detected. The 1010 was
recovered, however. The results are as follows:

TABLE
MICROWAVE EXTRACTIONS; REVERSE PHASE LC
50:50 CYCLOHEXANE/ISOPROPANOL - 20 MIN.

RESIN "D"

ADDITIVE AMOUNT RECOVERED/PRESENT (ppm)

Irganox 3114 604/600 (100%)

Cyasorb UV 531 511/500 (100%)
AM 340 1770/2000 (89%)

RESIN "E"

Irgafos 168 Not Quantitated

Irganox 1010 986/1000 (99%)
RESIN "I"

BHT 484/500 (97%)

1010 947/1000 (95%)

RESIN "K"

BHT 1274/1400 (91%)

1010 961/1000 (96%)

TABLE #10
ULTRASONIC EXTRACTION RECOVERIES
50:50 CYCLOHEXANE/ISOPROPANOL - 60 MIN.

RESIN "D"

Irganox 3114 583/600 (97%)

Cyasorb UV 531 491/500 (98%)
AM 340 1788/2000 (89%)

RESIN "E"

Irgalos 168 Not detected

Irganox 1010 977/1000 (98%)
RESIN "1"

BHT 469/500 (94%)

1010 953/1000 (95%)

RESIN "K"

BHT 1242/1400 (89%)

1010 938/1000 (94%)
The recoveries are obviouslyvery good. The microwave oven provides a very fast
means of extracting the additives from the groundresin. This technique can be done
on unground resins as well, depending upon the components present in the
formulation. If 1010 is present, for example, the resin must be ground, otherwisethe
1010 will not be recovered at better than 50%. The ultrasonic bath provides an
inexpensive and relativelyfast way of extractingthe additives. The Soxhlet method of
extraction was not tried out on these polypropyleneresins, as we would assume that it
would take at lease seven hours to extract out the majodty of the additives, and
perhaps as much as 16 hours to recover 1010, for example.

CONCLUSIONS: There are many other means of extraction of polyolefinadditives

such as "superheating"a solvent mixturein a sealed vial to as much as 30 degrees C
above the boiling point. We have demonstrated two quick ways to extract and
quantitate the levels of typical antioxidants present in high density polyethyleneand
polypropylene. Most analytical laboratoriP__ have At their disposal an ultrasonicbath
cleaner that will work very well at extracting out the antioxidants. The only other
materials required are 250 ml. beakers and watch glasses. The microwaveoven allows
the extraction to be done more quickly,but at a much higher initialcost. Up to twelve
samples can be extracted at once in the oven, and sample handlingis quite easy. Both
techniques afford a great time savings when compared to conventional Soxhlet
extraction. It is difficultto set up more than four Soxhlet condensersin a hood, so the
sample throughputis obviouslymuch lessthan for the othertwo techniques.
 kig, t¢.t

Chromatogram of Ultrasonic Extracted

HDPE
Acquisition method 990 Quantitation method 990
Units System number 1
Channel I Manual injector
Injection 1 Total injections 1
Run time 25.00 min Sample rate 1.00 per sec
Injection volume I00 uL Rode Analysis
Acquisition version 840/6.2 Quantitation version 860/B01.37

484 UV, 254nm

CHARACTERIZATION ACROSS A NOVAPAK C18 COLUMN. GRADIENT

SEPARATION WITH 3:2 H20/CH3CN TO I00% CH3CN AS ELUENT.
DETECTION WITH 484 UV (254 nm) AND 990 PDA.

#i, 2HRS. ULTRASONIC

:3LI2 Hgnu:,l Ir_le,::tJ,=,n ! L-:t,st,t,e] I

I i I
!l:

[111,,_
4=` (9:1 Cyclohexane/Isopropanol)
4c Reverse Phase Gradient
3.', Detection: 484 UV @ 254 nm

c_._

,j.i

_
loI I ......... i .........
_ _! • • ....... | .........
5 I0 15 2A_ __._:'.=;
l'ttr,ut e_
 Fig, #2

Antioxidant Standards

l Normal Phase Separation

II CONDITIONS:
" H ELUENT:
II n-Butyl Chloride/Methylene Clfloride :70/30
II @ 1.50 ml/min, Isocratic
II CoLuMN:
II Resolve Silica 5p Column

#-
c
o II I_ UV DETECTION: @ 225nm

It
XlnuteI
 Fig, #3

PDA of Polyolefin Standards

Separated by Isocratic Normal Phase LC
 Fig, #4

Ultrasonic Extract from Polypropylene Resin "E"

Irgafos 168 (Phosphite)

Irganox 1010 and 1076

CONDITIONS:
Isocractic Normal Phase LC Separation
with 70:30 n-Butyl n-BuCI2/MeCI2 @
1.5 ml/min, over a 51LResolve
_ Silica Column.
U3 DETECTION with UV @ 225 nm
c-
O
(,_
n"

O
O

m ,

i i i , , , i , i | , i .... . , . | , , i''.. 1", , , I , . . I i t . I . _

0 2 4 6 8
Minutes
 Fig, #5

PDA Chromatogram of Ultrasonic Extract from Resin "E"

_,_,4, Waters 990 Three .Jif,,er, slonal Plot _'_+ [ ELILTF:_: S ] 06 -06 --17,$9 12:2-:56
t;,

,4

• 107_ I010 -
I
 Fig, #6

Polyolefin Standards - Reverse Phase Gradient Separation

ELUENT: 3:2 H20/CH3CN- CH3CN

- 5 Minute Gradient at
1.50 ml/min
m
COLUMN: Nova-Pak CI8

DETECTION: 490 UV @ 225nm i_

It'/

- 5
_
m _: _ -
0 -

rr o
- _ ID
0

- i0
-
___-_
0 5
_
t0
Jl .LL
M_nutes
t5
_ - J_
20
- /

25

i
 Fig #7

PDA 3D Chromatogram of 5 Polyolefin Additive Standards

 Fig #8

Microwave Extract from Polypropylene Resin "D"

BOO CONDITIONS: Reverse Phase Gradient: 3:2 H20/CH3CN

to CH3CN @ 1.50 ml/min
COLUMN: Nova-Pak C18
DETECTION: 490 UV @ 225 nm
4O0

3O0

100

8 10 Htnutes 12 14 16
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