29 1
Appendix
Commercially available silica packing [ 1,2]
LIST OF SUPPLIERS 1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15.
Alltech Associates Altex Scientific Applied Science Laboratories Chromatec E.I. Du Pont de Nemours E. Merck (U.S.A.: MCIB Manufacturing Chemists) Macherey Nagel & Co Perkin-Elmer Phase Separation Ltd. Reeve Angel (Whatman) Rhone-Progil (France) Shandon Varian Associates Waters Associates Woelm Pharma GmbH & Co
ADDITIONAL ABBREVIATIONS = angular particles = spherical particles p. c. = available as prepacked columns b.p. = bulk packing SBET= specific surface are according to BET Vp = specific pore volume D = most frequent pore diameter ds = thickness of the porous layer at pellicular packings SCX = strong cation exchanger WCX = weak cation exchanger SAX = strong anion exchanger WAX = weak anion exchanger = weight capacity of ion exchanger in mequiv./g Q, MW* = exclusion limit for polystyrenes in tetrahydrofuran at 293 K AMW = log-linear calibration range for polystyrenes in tetrahydrofuran at 293 K a s
APPENDIX A TOTALLY POROUS SILICA PACKINGS FOR LIQUID-SOLID AND LIQUID-LIQUID CHROMATOGRAPHY Trade name Biosil A Chroma Sep SL Hi Eff Micro Part Hi-Flosil
Supplier
Particle shape
Particle size b m )
Trade form
Description
b.p. p.c. p.c. b.p.
SBET= 400 m'/g identical with LiChrosorb Si 60 SBET= 250 m'/g silica and magnesia as constituents
b.p.
SBET= 200 m2/g D =lO+3nm SBET= 675 m2/g; Vp = 0.65 ml/g D =4nm SBET= 500 m'lg; Vp = 0.82 ml/g D =6nm
2 4 3 3
a a a a
12
S
LiChroprep Si 40
6
a
40-63
b.p.
LiChroprep Si 60
6
a
5-20; 15-25; 25-40; 40-63
LiChroprep Si 100
6
a
40-63
b.p. p.c. (40-63 only) b.p.
LiChrospher Si 100
6
S
5; 10; 20
LiChrospher Si 300
6
S
5; 10
b.p. p.c. b.p.
LiChrospher Si 500
6
S
10
b.p.
LiChrospher Si 1000
6
S
10
b.p.
LiChrospher Si 4000
6
S
10
b.p.
LiChrosorb Si 60
6
a
5; 7; 10; 30
LiChrosorb Si 100
6
a
5; 7; 10; 30
13
a
5; 10
p. c. b.p. b.p. p.c. p.c.
Hypersil
Micropak Si
2-10 5; 10; 20 5; 10 4 0 ; 50-75; 75-250 5-7
SBET= 300 m'/g; V p = 1.05 ml/g D =1Onm SBET= 256 m'/g; V p = 1.20 ml/g D =12nm[3] SBET= 250 m'/g; Vp = 2.00 ml/g D = 3 0 n m [3] SBET= 45 m'/g; V p = 0.88 ml/g D = 5 0 n m [3] SBET= 19 m'/g; V p = 0.72 rd/g D = l 0 0 n m [3] SBET= 4.7 m2/g; V p = 0.78 ml/g D = 3 8 5 n m [3] SBET= 475 m'/g; Vp = 0.76 ml/g D =6nm[3] SBET= 278 m'/g; V p = 1.02 ml/g D = 1 0 n m [3] identical with LiChrosorb Si 60
Nucleosil 50
I
S
5; 1.5; 10
b.p.
Nucleosil 100
I
S
5; 1.5; 10
b.p.
Nucleosil 100 V
I
S
5; 7.5; 10
b.p.
1, 10
a
5; 10; 20
p
Partisil
p
Porasil
14
a
8-12
b.p. p.c. p.c.
Porasil A
14
S
31-15: 15-125
b.p.
Porasil B
14
S
31-15; 15-125
b.p.
Porasil C
14
S
31-15; 15-125
b.p.
Porasil D
14
S
31-15; 15-125
b.p.
Porasil E
14
S
31-15; 15-125
b.p.
Porasil F
14
S
31-15: 15-125
b.p.
Porasil T
14
S
15-25; 25-31
b.p.
Sil60
I
a
5; 10; 15; 20
b.p.
sil-x-I
8
a
13 5 5
b.p.
Silica A
8
a
1355
b.p.
Silica Woelm
15
a
b.p.
Spherisorb S
9
S
3-6; 1-12; 10-18; 18-32 5 ; 10; 20
11 11
S
5; 10; 20 5; 10
b.p. b.p.
Spherosil XOA 600 Spherosil XOA 800
S
b.p.
P.
SBET= 500 m'/g; V p = 0.80 ml/g D =5nm SBET= 300 m'/g; V p = 1.0 ml/g D =10nm SBET= 430 m'/g; V p = 1.5 ml/g D =10nm SBET= 400 m'/g D =4-5nm SBET= 400 m'/g; V p = 1.0 ml/g D =10nm SBET= 350-500 m'/g; V p = 1.05 ml/g D -10nm SBET= 125-250 m'/g; V p = 0.90 ml/g D -15nm SBET= 50-100 m'/g; V p = 0.10 ml/g D -30nm SBET= 25-45 m'/g; V p = 0.60 ml/g D -60nm SBET= 10-20 m'/g; Vp = 0.40 ml/g D -100nm SBET= 2-6 m'/g; Vp = 0.25 ml/g D >150nm SBET= 300 m'/g D =15nm SBET= 500 m'/g; V p = 0.75 ml/g D -6nm SBET= 400 m'/g D -10nm SBET= 400 m'/g D -10nm SBET= 500-600 m'/g; V p = 0.80 ml/g D -6nm SBET= 183 m2/g; Vp = 0.52 ml/g D = 10.9 nm (31 SBET= 600 m'/g SBET= 830 mZ/g D -3nm
(Continued on p. 294)
h)
W
W
h)
APPENDIX A (continued)
W P
Trade name
Supplier
Particle shape
Particle size (pm)
Trade form
Description
Spherosil XOA 400 (identical with Porasil A) Spherosil XOA 200 (identical with Porasil B) Spherosil XOB 075 (identical with Porasil C) Spherosil XOB 030 (identical with Porasil D) Spherosil XOB 015 (identical with Porasil E) Spherosil XOB 005 (identical with Porasil F) Zorbax Sil
11
s
10
b.p.
11
s
10
b.p.
11
S
10
b.p.
11
s
10
b.p.
11
s
10
b.p.
11
S
10
b.p.
5
s
5-7
P. c
SBET= 350-500 m2/g; Vp = 1.05 ml/g D <10nm SBET=125-250 m2/g; V p = 0.90 ml/g D -15nm SBET= 50-100 m’/g; V p = 0.70 ml/g D -30nm SBET= 25-45 m2/g; V p = 0.60 ml/g D -60nm SBET= 10-20 m’/g; V p = 0.40 mllg D -100nm SBET= 2-6 m2/g; Vp = 0.25 ml/g D >150nm SBET= 300 m’/g D = 7.5 nm
3, 7
S
10
p.c.
Vydac TP Silica
APPENDIX B SUPERFICIALLY POROUS OR PELLICULAR SILICA PACKINGS FOR LIQUID-SOLID AND LIQUID-LIQUID CHROMATOGRAPHY Trade name
Supplier
Particle shape
Particle size(pm)
Trade form
Description
Corasil I
14
S
37-50
b.p.
Corasil I1
14
S
37-50
b.p.
Pellosil HS Pellosil HC Perisorb A
10 10 6
S
37-44 37-44 30-40
b.p. b.p. b.p.
SBET= 15 m'/g; V p = 0.040 ml/g D = 7 n m [4] SBET= 27 m'/g; V p = 0.049 ml/g D =5nm[4] the HC type has a thicker porous layer than the HS type
sil-x-I1 Vydac 101 Si
8 7
S S
35 5 15 30-44
b.p. b.p.
Zipax
5
S
25-37
b.p.
S S
SBET= 14 m'/g; V p = 0.024 ml/g =6nm[4] SBET= 12 m2/g SBET= 12 m'/g D = 6 nm;ds = 1 rm SBET= 0.9 m'/g; Vp = 0.023 ml/g D = 3 8 n m [4]
D
t4
W
ul
APPENDIX C
h)
CHEMICALLY BONDED SILICA PACKINGS (EXCLUDING BONDED SILICA ION EXCHANGERS) Trade name
Supplier
Particle shape
Particle size (rm)
Trade form
Description
8
a
13 * 5
allylphenyl groups
14
a
31-75
14
a
8-12
Bondapak phenyl (Porasil D) Hi Eff Micro Part C 18
14
a
31-15
b.p. p.c. b.p. p.c. b.p. p-c. b.p.
3
a
10
octadecylsilyl groups
Hypersil SAS Hypersil ODS LiChrosorb RP 2
12
S
12 6
S
a
5 -1 5-1 5; I; 10
LiChrosorb RP 8
6
a
5; 7; 10
LiChrosorb RP 18 LiChroprep RP-2 LiChroprep RP-8
6 6 6
a a a
5;I; 10
LiChroprep RP-18 Micropak CH
6 13
a a
25-40 5-20; 25-40; 40-63 25-40 10
7
S
5; 7.5; 10
b.p. p. c. b.p. b.p. b.p. p.c. b.p. p.c. b.p. b.p. b.p. (40-63 only) b.p. b.p. p.c. b.p.
Reversed phase packings (totally porous} Allylphenyl Sil-X-I Bondapak C 18 (Porasil B) p Bondapak C 18
Nucleosil C 8 Nucleosil C 18
I
S
5; 7.5; 10
ODS S1-X-I
8
a
13+5
Partisil ODS
10
a
10
P.c
b.p. p.c. b.p. p.c. b.p. P.C
octadecylsilyl groups octadecylsilyl groups phenylsilyl groups
dimethylsilyl groups octadecylsilyl groups dimethylsilyl groups octylsilyl groups octadecylsilyl groups dimethylsilyl groups octylsilyl groups octadecylsilyl groups octadecylsilyl groups octylsilyl groups octadecylsilyl groups octadecylsilyl groups octadecylsilyl groups
W
OI
phenylsilyl groups
5-1
b.p. p.c. b.p. p.c. b.p. p.c. p.c.
Phenyl Sil-X-I
8
a
13*5
Spherisorb ODs
9
S
10
Vydac TP Reverse Phase
1
a
10
Zorbax ODS
5
S
octadecylsilyl groups octadecylsilyl groups octadecylsilyl groups
Reversed phase packings (superficially porous or pellicular) Bondapak C 18 Corasil Bondapak Phenyl Corasil CO : PELL ODS ODS Sil-X-I1 Perisorb RP 2 Perisorb RP 8 Perisorb RP 18 Phermaphase ODS Vydax 201 RP Zipax HCP
14
S
37-50
b.p.
octadecylsilyl groups
14
S
31-50
b.p.
diphenylsilyl groups
1,lO 8 6
S S S
6 6
S
44-53 35 * 15 30-40 30-40 30-40 25-31 30-44 21-35
b.p. b.p. b.p. 5.p. b.p. b.p. b.p. b.p.
octadecylsilyl groups octadecylsilyl groups dimethylsilyl groups octylsilyl groups octadecylsilyl groups octadecylsilyl groups octadecylsilyl groups Zipax coated with an unpolar saturated hydrocarbon polymer layer
5 7 5
S
S S S
Polar and moderately polar chemically bonded silica packings (totally porous) (s. also silica ion exchangers) Bondapak Carbohydrate p Bondapak CN p
cyano sil-x-I Durapak Carbowax (Porasil C) Durapak OPN (Porasil) FE Sil-X-I
14
a
8-12
14
a
8-12
8
a
13*5
14
a
31-75
b.p. p.c. b.p. p.c. b.p. p.c. b.p.
14
a
31-75
b.p.
8
a
13t5
b.p. p.c.
cyano groups cyano groups Carbowax 400 chemically bonded oxydipropionitrile groups bonded by a Si-0-C bond fluoroether groups N
W
(Continued on p. 298)
4
APPENDIX C (continued] Trade name
Particle shape
Particle size (gm)
Trade form
Description
6
a
5; 10
diol groups
Micropak CN
13
a
10
Nucleosil CN
7
S
5 ; 10
Nucleosil NO,
7
S
5; 10
Partisil PAC
9
a
10
Sil6WN
7 7 7
a a a
5; 10 5; 10 10
b.p. p.c. b.p. p.c. b.p. p.c. b.p. p. c. b.p. p.c. b.p. b.p. b.p.
Lichrosorb DIOL
Sil 6O-NO2 Vydac TP polar
Supplier
alkylnitrile groups cyano groups nitro goups alkylnitrile groups cyano groups nitro groups
alkylnitrile groups
Polar and moderately polar chemically bonded silica pckings (superficinlly porous or pellicuhr) CO : PELL PAC Durapak Carbowax 400 Corasil Permaphase ETH Perisorb PA 6 vydac 501 PP Zipax ANH Zipax PAM
1 14
S
5 6 7 5
S
5
37-53 37-53
b.p. b.p.
nitrile groups Corasil coated with Carbowax 400
S
25-37 30-40 30-44 25-37
b.p. b.p. b.p. b.p.
S
25-37
b.p.
ether groups Perisorb coated with a polyamide propionitrile groups Zipax coated with a cyanoethylsiliwne polymer layer nylon coated Zipax
S
S S
APPENDIX D TOTALLY POROUS CHEMICALLY BONDED SILICA ION EXCHANGERS Trade name
Supplier
Particle shape
Particle size (urn)
Trade form
Description
10
b.p. b.p. b.p. b.p. b.p.
SCX; sulphonic acid groups SCX; sulphonic acid groups SCX; sulphonic acid groups SCX; sulphonic acid groups SCX; sulphonic acid groups
p.c. b.p. p.c. b.p. b.p. b.p. p.c. b.p. p.c. b.p. p-c. b.p. P*C b.p. p. c. b.p. b.p. b.p. b.p. b.p.
WAX; alkyl amino groups WAX; alkyl amino groups
ation exchangers
LiChrosorb KAT Nucleosil SA Partisil SCX Vydac TP Cation Zorbax SCX
6
a
I 10 I 5
S
5 ; 10
a a S
10 10 5-1
8
a a
1325 10
Anion exchangers p
Amino Sil-X-I Bondapak-NH,
14
Hypersil APS LiChrosorb AN LiChrosorb NH,
12 6 6
S
a a
5-1 10 5; 10
Micropak NH,
13
a
10
Nucleosil-N(CHJ
I
S
5; 10
Nucleosil-NH(CH,),
I
S
5; 10
Nucleosil-NH,
I
S
5; 10
Partisil SAX Sil-60 NH, Sil-60 N(CH,), Vydac TP Anion Zorbax SAX
10
I
I 2 5
10 5; 10 5; 10 10 5-1
WAX; y-aminopropyl groups SAX; dimethylaminoethanol groups WAX; alkyl amine groups WAX; alkyl amine groups SAX; quaternary ammonium groups WAX; dimethylamino groups WAX; alkyl amine groups SAX; quaternary ammonium groups WAX; alkyl amine groups WAX; dimethyl amine groups SAX; quaternary ammonium groups SAX; quaternary ammonium groups h)
W W
APPENDIX E
W
0
SUPERFICIALLY POROUS AND PELLICULAR CHEMICALLY BONDED SILICA ION EXCHANGERS Trade name
Supplier
Particle shape
Particle size (pm)
Trade form
Description
14
S
31-50
b.p.
SCX; sulphonic acid groups
6
S
b.p. b.p. b.p.
SCX; sulphonic acid groups SCX; sulphonic acid groups SCX; sulphonic acid groups
Cation exchangers
Bondapak CX Corasil Perisorb KAT Vydac 401 SA Zipax SCX
5
s
30-40 30-44 . 25-31
14
S
31-50
b.p.
SAX; quaternary ammonium groups
6 5
S
b.p. b.p. b.p. b.p. b.p.
SAX; dimethylaminoethanol groups SAX; quaternary ammonium groups SAX; quaternary ammonium groups SAX; polymer layer on Zipax, strong basic functional groups WAX; polymer layer on Zipax, weak basic functional groups
I
S
Anion exchangers Bondapak AX Corasil Perisorb A N Permaphase AAX Vydac 301 SB Zipax SAX
5
S
30-40 25-31 30-44 25-31
5
S
25-31
s
I
Zipax WAX
s
APPENDIX F SILICA PACKINGS FOR SIZE EXCLUSION CHROMATOGRAPHY
This list collects only packings with graduated pore sizes Trade name
Supplier
Particle shape
Particle size (pm)
Trade form
Description
40-63 63-125 40-63 63-125
b.p.
SBET= 150 m’/g; V p = 0.65 ml/g D =20nm SBET= 50 m2/g; V p = 0.65 ml/g D =50nm
Fractosil200
6
a
Fractosil500
6
a
b.p.
0
b.p.
a
40-63 63-125 63-125
6
a
63-125
b.p.
Fractosil 10000
6
a
63-125
b.p.
Fractosil25000
6
a
63-125
b.p.
LiChrospher Si 100
6
S
5; 10; 20
for pore structure data see .4ppendix A aMw= 3*1U3-5*1U4 [ 5 ]
S
5; 10 10 10 10
b.p. p.c. b.p. b.p. b.p. b.p.
37-75 75-125 31-75 75-125 37-75 75-125 31-75 75-125 37-75 75-125 37-75 75-125
b.p.
for pore structure data see Appendix A
7 7 7 7 7 7
b.p. b.p. b.p. b.p. b.p. b. p.
Fractosil 1000
6
a
Fractosil2500
6
Fractosil5000
LiChrospher LiChrospher LiChrospher LiChrospher
Si 300 Si 500 Si 1000 Si 4000
6 6 6 6
S
S
S
Porasil A
14
S
Porasil B
14
S
Porasil C
14
S
Porasil D
14
S
Porasil E
14
S
Porasil F
14
S
Spherosil XOA 400 Spherosil XOA 200 Spherosil XOB 075 Spherosil XOB 030 Spherosii XOB 015 Spherosil XOC 005
11 11 11 11 11 11
S S S
S S S
b.p.
SBET= ZU m’/g; Y p = U.bU ml/g
D = 100nm SBET= 10 m2/g; VP = 0.60 ml/g D =250nm SBET= 3 m’/g; V p = 0.50 mug D =500nm SBE;T = 2 m’/g; V p = 0.50 ml/g D =lOOOnm SBET= 0.8 m’/g; V p = 0.40 ml/g D =2500nm
-
AMW= 1.5e1u4-1.5~105 [51 a M W = 3*1U4-2*1U6 [ 5 ] aMw= 1O5->7*1O6 [ 5 ]
b.p. b.p. b.p. b.p. b.p.
for pore structure data see Appendix A
s
W
302
REFERENCES 1 R.E. Majors,Inrerrz. Lob.. Nov./Dec. (1975) 71. 2 ti. EngeJhardt, HochdncckflilssigchrorPlotogmphie,Springer-Verlag, New York, 1977. 3 Data measured by the author for a given batch. 4 K. Unger, P. Ringe, J. Schick-Kalb and B. Straube, Z. Anal. Chem, 264 (1973) 267. 5 JJ. Kirkland,J. Ommutogr., 125 (1976) 231.
Addendum
A recent survey about commercial packing is given by R.E. Majors, J. Chromutogr. Sci., 15 (1977) 334.