doom hayes separations, inc. - separationexpert.com.br

Doom Hayes Separations, Inc. Analytical Polymers

POROUS POLYMERSSince the development of porous polymers for use in gas Maximum SurfaceTappedBulk Polarity

chromatography by Hollis and Hayes in the mid 1960's, veryHayeSep®Operating Area Density Polymer (hlowest

little has been done to improve their performance. Commer-Polymer Temp. m2/gram gram/cc Composition" 9=tiighest)

cial polymers such as Porapak" and Chrornasorbv have A 165°C 526 0.356 DVB -7been available since this time for chromatographic use. (high purity)However these commercially available polymers have been EGDMplagued with problems such as batch-to-batch variations, (high purity)incomplete or inadequate cleanup and shrinkage. These B 190°C 608 0.330 DVB/PEI 8variations and inconsistencies in production and handlinghave led to poor performance and reproducibility. C 250°C 442 0.322 DVB/ACN 6

HayeSep® analytical polymers and packed columns are0 290°C 795 0.3311 DVB 1

now available to chromatographers at a reasonable cost.(high purity)

Hayes Separations, Inc. takes pride in providing the N 165°C 405 0.355 DVB/EGDM 9necessary technical assistance to support our users. We

P 250°C 165 0.420 DVB/Styrene 3guarantee that our polymers are better than any other onthe market and we are continuing to develop and test new Q 275°C 582 0.351 DVB 2packings for specific separation problems. R 250°C 344 0.324 DVB/NV2P 5

HayeSep® polymers are thoroughly cleaned and precon- S 250°C 583 0.334 DVB/4VP 4ditioned for twelve hours under oxygen-free nitrogen before T 165°C 250 0.381 EGDM 10packaging. These handling techniques produce polymerswhich are consistently the same, with no shrinkage and

-DVB Divinylbenzene ACN Acrylonitrileminimum bleed. Columns packed with HayeSep® requireminimum conditioning.

EGDM Ethyleneglycoldimethacrylate NV2P N-vinyl-2-pyrollidinonePEl Polyethyleneimine 4VP 4-vinyl-pyridine

HayeSep® A This polymer separates permanent gases (hydrogen, nitrogen, oxygen, argon, carbon monoxide, and nitric oxide) at ambient temperatures.It also exhibits good separation characteristics for the C2's, hydrogen sulphide and water at higher temperatures.

Figure 1PERMANENT GASESColumn: 36' x 1/8" packed

with HayeSep" A80/100 mesh

Column Temp: 25°Detector: PE. 900 T.C. 225 ma

Att. x 2 180°C .Flow: He 23 cc/minSample: 25 microliters Air

plus Hydrogen andCarbon Monoxide

1. Hydrogen5%2. Nitrogen 48.5%3. Oxygen 13%.,4. Argon 0.5%5. Carbon Monoxide33%

t- ,9

5

3

,o

, , ,

Figure 2PERMANENT GASSTANDARD 500 ppmColumn: 25' x 1mm packed

with HayeSep® A170/200 mesh

Column Temp: 23°CFlow: He 15 cc/minSample: 20 microliters

MInutes

1. Neon2. Hydrogen3. Nitrogen4. Oxygen5. Argon6. Carbon Monoxide

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Haye5ep® B Designed to separate the C1 and C2 amines as well as trace levels of ammonia and water, this polymer eliminates the need for causticwashing of material prior to packing.

Figure 3AMINE5 #1Column: 5' x 1/8"

58 packed withHayaSep" B80/100 mesh

Column Temp: 140° up to190°C at16°C/min

Injector Temp: 150°CDetector: RE. 900 TC.

175 maAtl. x 8180°C

Flow: He 30 cclminSample: 0.2 microliters

with on-columninjection

1. Air2. Water3. Methylamine4. Dimethylamine5. Trimethylamine6. Ethylene diamine

1

JIo

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Figure 4AMINE5#2Column: 5' x 1/8" packed

with HayeSep® B80/100 mesh

Column Temp: 140°C up to190°C at 16°C/min

Injector Temp: 150°CDetector: RE. 900 TC.

175 maAtt, x 8 180°C

Flow: He 30 cclminSample: On-column injection

1. Air2. Water3. Ethylamine4. Diethylamine

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HayeSep® C This polymer is designed for polar hydrocarbons such as hydrogen cyanide, ammonia, hydrogen sulphide and water. Haye5ep C® hassimilar separation characteristics to Chrornosorb" 104.

Figure 5AMMONIA INHYDROGEN SULPHIDEColumn: 5' x 1/8" packed

with HayeSep® C80/100 mesh

Column Temp: 70°CInjector Temp: 200°CDetector: RE. 900 TC.

225 maAt!. x 2 180°C

Flow: He 30 cclminSample: 100 microliters

1. Air2. Carbon Dioxide3. Ammonia

Trace 1: approx 15%Trace 2: approx 1.5%

4. Hydrogen Sulphide5. Unknown in

Hydrogen Sulphide6. Unknown in

Hydrogen Sulphide7. Water

1 3 4

5 6I \

, I5 0

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t 3

Figure 6TRACE AMMONIA IN WATERColumn: 5' x 1/8" SS packed

with Haye5ep® C80/100 mesh

Column Temp: 115°CInjector Temp: 140°CDetector: RE. 900 TC.

225maAt!. x 2 180°C

Flow: He 30 cclminSample: 1 microliter

Trace 11. Air2. Carbon Dioxide3. Ammonia

300 ppm4. Water

(balance)

Trace 21. Air2. Carbon Dioxide3. Ammonia

100 ppm4. Water

(balance)

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HayeSep@ N, P,a, R, S, and T These polymers are interchangeable with the Porapak® series for separations of low molecular weight materials containinghalogens, sulphurs, water, alcohols, glycols, free fatty acids, esters, ketones and aldehydes.

Figure 7AMMONIAColumn: S' x 1/S" SS.packed

with HayeS~P60/S0 mesh

Column Temp: SO°CInjector Temp: 1500CManifold Temp: 1S00CDetector: T.C. 175 ma 200°CFlow: He 30 cclminSample: 0.1 microliters of

NH40H with on-column injection

3

1. Air2: Ammonia 35%3. Water65%

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Figure 9TRACE WATER ANALYSISColumn: 9' x 1/8" Ni packed

with HayeSep@ R80/100 mesh

Column Temp: 118°CFlow: He 30 cclminDetector: Varian T.C.

with Bendix On-LineProcess Analyzer

Sample: 10 microlitersEthyl Chloride

1. Air2. Water 12 ppm3. Hydrogen Chloride4. Ethyl Chloride

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I 1 '----J_ '-- L- '--.JL. _b I I I I ! I

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Figure 8SOLVENTSColumn: 8' x 1/8" SS packed

with HayeSep@ P60/80 mesh

Column Temp: 80°C up to180°C at16°C/min

Injector Temp: 150°Manifold Temp: 180°CDetector: 175 ma 200°CFlow: He 30 cclminSample: 0.2 microliters with

on-column injection

1. Air2. Water3. Methanol4. Ethanol5. Acetone6. Chloroform

2 3

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8

Figure 10MAPP GASColumn: 10' x 1/8" SS

packed withHayeSep@ R

Column Temp: 80°Flow: He 30 cclminSample: 15 microliters

1. Air2. Metharie3. Carbon Dioxide4. Ethane5. Propylene6. Propane7. Propadiene8. Methyl Acetylene

\..

6

Figure 11HYDROCARBONS ANDSULPHUR GASESColumn: 8' x 1/8"

packed withHayeSep® Q80/100 mesh

Column Temp: 90°CFlow: He 30 cclmin

e

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1. Air2. Methane3. Carbon Dioxide4. Ethylene5. Acetylene6. Ethane7. Hydrogen Sulfide8. Carbonyl Sulfide 45 8

9. Propylene ,~o10. Propane11. Propadiene \ h

___ t-IUU~H.I ''-' '--J L..J \J " _Io

Figure 13METHANOL INPROPYLENE/PROPANEColumn: 5' x 1/8" SS

packed withHayeSep® T1001120mesh

Column Temp: 1200CInjector Temp: 132°CDetector: p.E. 900 T.C.

225 ma 1500CFlow: He 30 cclmin

1. Air/Methane2. Carbon Dioxide3. Ethane4. Propylene/Propane5. C46. C47. Methanol

23 4

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Figure 12C2'sColumn: 5' x 1/8" SS

packed withHayeSep® T

Column Temp: 32°CDetector: Alt. x 216 180°CFlow: He 30 cclminSample: 50 microliters

1. Air2. Methane3. Carbon Dioxide4. Ethylene5. Ethane6. Acetylene

4

I~~ _ Vl'--_-'

I I I Io 2 4 6

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-...--

Figure 14FORMALDEHYDEColumn: 5' x 1/8" SS packed

with HayeSep® T100/120 mesh

Column Temp: 132°CInjector Temp: 165°Detector: p.E. 900 T.C.

175 MAAlt. x 32 1800CFlow: He 30 cc/minSample: 0.2 microliters

1. Air2. Formaldehyde3. Water4. Methanol

-----l.....Ji lLI I Io 3

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Relative Retention Times

Ethane = 1.00

Columns 6' x 1/8" 55 65°CHe 30 cc/min

Compound QN R 5 T

Hydogen 0.19 .143 0.17 .19 .21Air 0.23 .186 0.2 .21 .25Nitric oxide 0.25 .217 0.21 .23 .33

Methane 0.30 .256 0.28 0.3 .35Carbon dioxide 0.71 0.45 0.50 0.52 0.85Nitrous oxide 0.80 0.57 0.59 0.59

Ethylene 0.83 0.74 0.78 0.78 0.9Acetylene 1.41 0.74 1.0 0.87 2.11Ethane 1.0 1.0 1.0 1.0 1.0

Water 10.1 1.45 0.68 ~J'6 4.12 19.1Hydrogen sulphide 2.1 1.40 1.73 1.87 2.88Hydrogen cyanide 19.3 2.31 15.6 8.26 28.8

Carbonyl sulphide 2.82 2.33 2.46 2.63 3.4Sulphur dioxide 12.0 3.05 9.78 17.8. 19.0/Propylene 4.66 3.20 3.45- 3.65 4.91

Propane 4.66 3.67 3.88 4.1 4.63Propadiene 6.50 4.12 4.39 4.7 7.55Methylacetylene 9.5 4.12 4.84 5.14 11.3

Methyl chloride 7.43 3.93 4.67 4.92 9.2Vinyl chloride 14.9 6.04 9.04 9.7 17.3Ethylene oxide 17.7 6.06 8.78 9.7 23.3

Ethyl chloride 35.0 12.25 19.3 20.7 43.2Carbon disulphide 32.4 40.7

INTRODUCINGA UNIQUENEW PRODUCT Comparison of

D FormulationsHayeSep® D This new polymer made from high puritydivinylbenzene is unavailable anywhere else. It has a highsurface area and higher operating temperatures thancompetitive polymers. Available in four different porositieswith surface areas from 790 to over 800 m2/gram, this range Average Pore Bulk Surfaceallows flexibility, since in water/ethane separations porosity Diameter Density Porosity Areadetermines the order of elution. ~microns) gram/cc % m2/gram

These D formulations exhibit superior separationcharacteristics for light gases. Significant separationabilities include the separation of CO and CO2 from roomair at ambient temperatures and the separation of acetylene Dip .0317 .3283 69.1 774prior to other C2's. HayeSep® D is particularly useful in theseparation and analysis of water and hydrogen sulphide.

Deb .0308 .3311 70.35 803

Dox .0351 .3457 66.1 793

DB .0332 .3834 64.2 781

Figure 15SCOTT MIX 237Column: 20' x 1/8" Ni packed

with HayeSepi!> D100/120 mesh

Column Temp: 25°CInjector Temp: 100°CDetector: P.E. 900 I.C.

225 ma 140°CFlow: He 30 cclminSample: Valco valve

50 microliters vapor(ambient)

1. Nitrogen (balance)2. Oxygen 7% Att.x83. Carbon Monoxide 7% Att.x84. Methane 4.5% Att.x45. Carbon Dioxide 15% Att.x4

u-----' '---- -1

I I I I I I I I I I 1

18Minutes

Figure 16GAS MIXTUREColumn: 10' x 1/8" SS packed

with HayeSepi!> D100/120 mesh

Column Temp: 80°CInjector Temp: 140°CDetector: P.E. 900 I.C.

225maAtt. x 4

Flow: He 30 cclminSample: Valco valve

100 microliters

1. Nitrogen (balance)2. Carbon Dioxide 2%3. Nitrous Oxide 3%4. Water 0.5%5. Hydrogen Sulphide 3%

4

JI I I I

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Figure 17SCOTT MIX 216 (Programmed)Column: 20' x 1/8" Ni packed

with HayeSep® D100/120 mesh

Column Temp: 40°C/2 minprogrammedup to 1100Cat 24OC/min

Injector Temp: 1000CDetector: P.E. 900 T.C.

225 ma 1400CFlow: He 30 cc/minSample: Valco valve

100 microliters(ambient)

1. Nitrogen (balance)2. Carbon Monoxide 1%3. Methane 1%4. Carbon Dioxide 1%5. Acetylene 1%6. Ethylene 1%7. Ethane 1%

Att.x2Att.x2Att.x2Att.x2Att.x2Att.x2

105Minutes

Figure 19C1 - C5 PARAFFINSColumn: 10' x 1/8" SS

packed withHayeSep® D100/120 mesh

Column Temp: 120°Cup to 2000Cat 20OC/min

Detector: 3700 Varian FIDRange: 10-11 Alt. x 16Flow: He 35 cc/minSample: Valco valve

50 microliters

1. Methane 0.1894%2. Ethane 0.0965%3. Propane 0.0989%4. Isobutane 0.1019%5. Butane 0.1019%6. n-Pentane 0.2002%

2 1

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Figure 18C1 - C2'sColumn: 10' x 1/8" SS packed


Column Temp: 80°C IsothermalDetector: 3700 Varian FIDRange: 10-11 Alt. x 16Flow: He 35 cc/min

1. Methane 1%2. Acetylene 1%3. Ethylene 1%4. Ethane 1%

Figure 20TRACE UNSATURATESC2 - C6Column: 10' x 1/8" SS



Detector: 3700 Varian FIDRange: 10-11 Alt. x 16Flow: He 35 cc/min

1. Acetylene 16 ppm2. Ethylene 15 ppm3. Propylene 14.3 ppm4. 1-Butene 15 ppm5. 'l-Penlene 14.75 ppm6. 1-Hexene 16 pprn

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2

1

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Figure 21TRACE ACETALDEHYDEIN AIR 2500 ppmColumn: 3' x 1/8" SS


Column Temp: 100°CInjector Temp: 140°CDetector: PE. 900 rc


100 microliters

1. Air2. Water3. Acetaldehyde

2500 ppm (voL)

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Figure 23TRACE ALCOHOLSIN WATERColumn: 10' x 1/8" packed

with HayeSep® Dox80/100 mesh


Flow: He 33 cclminInjector Temp: 125°CDetector: P.E. 900 rc

225 maAlt. x 1 140°C

Sample: 3 microliters

1. Methanol500 ppm

2. Ethanol200 ppm

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Figure 22TEQUILA HEADSPACEColumn: 3' x 1/8" SS packed

with Haye'Sep" D80/120 mesh

Column Temp: 100°Injector Temp: 140°CDetector: PE. 900 rc.


100 microliters

1. Air2. Carbon Dioxide3. Water4. Methanol5. Acetaldehyde6. Ethanol

All. xlAll. xl

. AII.xlAll. xlAll. xlAII.x8

I 3

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Figure 24HYDROGEN SULPHIDEColumn: 10' x 1/8" Ni packed

with HayeSep'" D100/120 mesh

Column Temp: 60°CInjector Temp: 100°CDetector: PE. 900 rc


50 microliters vapor(ambient)

.

1. Air (balance)2. Carbon Dioxide approx 0.1%3. Water approx 2.5%4. Hydrogen Sulphide approx 2.5%

__ -/,"-' __ J.,,2 __ ---.J ~

5Minutes

COMPARISON OF "0" FORMULATIONS

Retention Time in Minutes

AIR CH4 CO2 C2H2 C2H4 C2H6 H2O

Dip 0.9 1.7 3.1 5.4 5.8 8.3 9.0D* 0.9 1.7 3.1 5.8 6.1 8.4 8.6Dox 1.0 1.8 3.2 5.9 6.3 8.5 8.3DB 0.9 1.6 3.1 6.1 6.6 8.7 8.1*This is our standard D.

Column: 10' x 1/8" SSSO/loo mesh

Column Temp: 45"CDetector: 175 ma Att. x 2 150°Row: He 30 cc/minSample: 50 microliters

Valco valve

12 J

10

Courtesy of John Booker Co.

Figure 25TRACE ETHYLENE OXIDEIN NITROGENColumn: 10' x 1/8" SS packed

with HayeSep® DSO/loo mesh

Column Temp: rso-cInjector Temp: 100°CDetector: Varian 1400 F.I.D.

Att. 10.12x 2 140°CRow: He 30 cc/minSample: 250 microliters

Valco valve

1. Ethylene Oxide 23 ppm.~ --.•...•'~ ...~-

"fI I I I

3 2 1 0

Minutes

Courtesy of John Booker Co.

Figure 27NITROGEN IN OXYGENColumn: 30' x 1/8" SS packed

with HayeSep® DBColumn Temp: 25"CInjector Temp: 25"CDetector: P.E. 900 T. C.

300 maAtt. x 2 140°C

Row: He 30 co/rnln, 90 psigSample: 250 microliters

Valco valve

1. N~rogen 0.4%2. Oxygen· balance

I I I

J 4 5

Minutes

Figure 26HYDROCARBONS/SULFUR GASESColumn: 9'.x 1/8" HayeSep® Dip

100/120 meshColumn Temp: 100°CDetector: P.E. Sigma 300 TCD

Low currentAtt. x 1

Row: He 30 cc/rninSample: 0.5 cc

Valco valve

45 6PEAK RET. AREA CPOTIME %

1. 0.71 31.59 Air2. 0.86 46.88 Methane3. 1.23 5.48 Carbon

Dioxide4. 1.71 2.17 Ace;r.ene5. 1.79 2.72 Ethyene .6. 2.19 3.09 Ethane7. 2.52 0.45 Water8. 2.83 0.19 Hydrogen

Sulfide9. 4.30 0.44 Carbonyl

Sulfide10. 5.82 3.36 Propylene11. 6.57 3.59 Propane

Figure 28SCOTT MIX 234

I I I4 5 6

I I I I

9 10 11 12 13 14

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I

35

Figure 30NITROGEN IN ARGONColumn: 30' x 1/8" SS packed


Column Temp: 2SOCInjector Temp: 2SOCDetector: P.E. 900 T. C.

300 maAtt. x 1 140°C

Flow: He 30 cc/min, 90 psigSample: 250 micrOliters

Valco valve

1. N~rogen 373 ppm2. Argon· balance

Figure 29AIRColumn: 30' x 1/8" SS packed

with HayeSep® DB100/120 mesh


300 maAtt. x 32 140°C

Flow: He 30 cc/rnin, 90 psigSample: 250 microliters

Valco valve

1. N~rogen 78%2. Oxygen 21%3. Argon 0.94%

11

l

I·~

I I3 4 5

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Figure 31ETHYLENE AND SCOTT MIX 216Column: 30' x 1/8" SS packed


Column Temp: 120°CInjector Temp: 120°CDetector: P.E. 900 T. C.

300 maAtt. x 1 140°C

Flow: He 30 cc/rnln, 90 psigSample: 250 microliters

Valco valve

6-

1. Nitrogen18

2. Carbon

Monoxide

/~3. Methane4. Carbon

~

Dioxide5. Acetylene 924 ppm

\6. Ethylene7. Water <;8. Ethane ~ '---....J

I l I I I I I

1 3 6 1 10 " 11 13

Minutes Minutes

Column: 30' x 1/8" SS packedwith HayeSep® DB100/120 mesh


300 ma 140°CFlow: He 30 cc/rnln, 90 psigSample: 250 microliters 5

Valco valve A1. Hydrogen 4% Alt. x 012. Nitrogen 5% Alt. x 323. Carbon

Monoxide 5% Alt. x 324. Methane 4% Alt. x 325. Carbon

Dioxide 5% Alt. x 08

r

r?-I

6

Figure 32NITRIC OXIDE IN NITROGENColumn: 30' x 1/8" SS packed


Column Temp: 22"CInjector Temp: 22"CDetector: P.E. 900 T. C. D.

225 ma 14O"CFlow: 30 cc/minSample: 100 microliters

1. N~rogen Balance

2. Argon3. Nitric Oxide 0.58%

3

2

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Io

Figure 34IMPURITIES IN HYDROGENColumn: 25' x 1/8" SS packed



225maFlow: He 25 cc/minSample: 250 microliters

Valco valve

1. Hydrogen2. Nitrogen3. Oxygen

Balance80 ppm20 ppm

I 1 I I I J

o 5Minutes

2

Figure 33HYDROGEN IN HELIUMColumn: 25' x 1/8" SS packed



150 ma at 140°CFlow: 24 cc/min N2Sample: 50 microliters

Valco valve

1. Helium2. Hydrogen

Balance1%

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2

Io

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2

3

Figure 35AIR IN ARGONColumn: 30' x 1/8" SS packed



225 ma 14O"CFlow: He 30 cc/minSample: 100 microliters

Valco valve

1. Nitrogen

2. Oxygen3. Argon4. Helium

8000 ppm1600 ppm25%Balance

o

~ ---.-J U '-I I

9

Figure 36HYDROGEN/AIR 50/50Column: 25' x 1/8" SS packed


Column Temp: 25°CInjector Temp: 25°CDetector: P.E. 900 T. C. D.

225 ma 140"CAtten x 8

Flow: He 24 cc/mlnSample: 50 microliters

Valco valve

1. Hydrogen2. Nitrogen3. Oxygen4. Argon

Io

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2

3

I6

Figure 3899.995% ARGONColumn: 30' x 1/8" S5 packed



225 ma 140"CFlow: He 30 cc/mlnSample: 100 microliters

Valco valve

1. Nitrogen2. Argon

50 ppmBalance

I I I I I

o

2

...•.

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I I

6

Figure 3799.6% OXYGENColumn: 30' x 1/8" SS packed



225 ma 140"CFlow: He 20 cc/mlnSample: 100 microliters

Valco valve

1. N~rogen2. Oxygen

0.4%

Balance

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I I I I I I I

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Figure 39IMPURITIES IN NITROGEN TRIFLUORIDEColumn: 25' x 1/8" SS packed ~


Column Temp: 25"CInjector Temp: 25°CDetector: P.E. 900 T. C. D.

275 ma 140"CFlow: He 30 cc/min 4

Sample: 250 microlitersValco valve

Chart Speed: 1 crn/rnln

1. N~rogen2. Oxygen3. Carbon Tetrafluoride4. N~rogenTrifluoride

50 ppm250 ppm400 ppmBalance

2

3

2

I I I I

oI I I I I I

'--_---1~U'---_J ~I I I I I

14

Figure 40FAST ANALYSISColumn: 48" x 1/16" x .04" ID SS

packed with HayeSep® DB100/120 mesh


225 ma 140"CFlow: He 16 cc/minSample: 10 microliters

Valco valve

1. Nitrogen 2.7%2. Methane Balance3. Carbon Dioxide3.0%4. Ethane 3.5%

2

3

4

I

1

ULI

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Figure 42SCOTT MIX 234Column: 30' x 1/8" SS packed



225 ma 140"CFlow: He 30 cc/mfnSample: 100 microliters

Valco valve

2I I I I I I I

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Figure 4199.7% CARBON MONOXIDEColumn: 30' x 1/8" SS packed



225 ma 140"CFlow: He 30 cc/rninSample: 100 microliters

Valco valve

1. N~rogen2. Oxygen4. Carbon Monoxide

0.28%0.02%Balance

3

Io

2

1. Helium2. Hydrogen3. Oxygen4. Methane

Balance4%4%4%

4...".I I

10

3

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