Alcohols / Amino Alcohols / Ketones

Alcohols

Aliphatic alcohols were analyzed using SUGAR SH1011 and SH1821. Comparing the two chromatograms, the peak shapes with SH1011 are better than those with SH1821.

Sample :
1. Methyl alcohol
2. Ethyl alcohol
3. Isopropyl alcohol
4. n-Propyl alcohol
5. tert-Butyl alcohol
6. sec-Butyl alcohol
7. Isobutyl alcohol
8. n-Butyl alcohol
9. Isopentyl alcohol
10. n-Pentyl alcohol

Columns      : (A); Shodex SUGAR SH-G (6.0mmID*50mm) + SH1821 (8.0mmID*300mm)
               (B); Shodex SUGAR SH-G (6.0mmID*50mm) + SH1011 (8.0mmID*300mm)
Eluent       : 5mM H2SO4 aq.
Flow rate    : 1.0mL/min
Detector     : Shodex RI
Column temp. : 80deg-C

Aliphatic alcohols were analyzed using RSpak DE-613 (a column for reversed phase chromatography).

Sample :
1. Ethylene glycol
2. Methyl alcohol
3. Ethyl alcohol
4. Isopropyl alcohol
5. n-Propyl alcohol
6. tert-Butyl alcohol
7. sec-Butyl alcohol
8. n-Butyl alcohol

Column       : Shodex RSpak DE-613 (6.0mmID*150mm)
Eluent       : H2O
Flow rate    : 1.0mL/min
Detector     : Shodex RI
Column temp. : 60deg-C

Aliphatic alcohols were analyzed using Asahipak C4P-50 6D, C8P-50 6D and ODP-50 6D (columns for reversed phase chromatography).

Sample :
1. Ethylene glycol, 2. 1-Butanol, 3. 1-Hexanol, 4. 1-Octanol, 5. 1-Decanol, 6. 1-Dodecanol, 7. 1-Tetradecanol

Columns      : Shodex Asahipak ODP-50 6D, C8P-50 6D, C4P-50 6D (6.0mmID*150mm each)
Eluent       : H2O/CH3OH=20/80
Flow rate    : 0.6mL/min
Detector     : Shodex RI
Column temp. : 30deg-C

Aliphatic alcohols were analyzed using RSpak KC-811.

Sample :
1. Methyl alcohol
2. Ethyl alcohol
3. Isopropyl alcohol
4. tert-Butyl alcohol
5. n-Propyl alcohol
6. Isobutyl alcohol
7. n-Butyl alcohol

Column       : Shodex RSpak KC-811 (8.0mmID*300mm)
Eluent       : H2O
Flow rate    : 1.0mL/min
Detector     : Shodex RI
Column temp. : 60deg-C

Eight kinds of alcohols were analyzed using SUGAR SC1211. The peaks of pentyl alcohols are tailing a little and better peaks can be obtained by SUGAR SH1011.
Please refer to ‘Aliphatic Alcohols (1) (SH1011, SH1821)‘.

Sample :
1. Glycerol
2. Ethyl alcohol
3. n-Propyl alcohol
4. sec-Butyl alcohol
5. Isobutyl alcohol
6. n-Butyl alcohol
7. Isopentyl alcohol
8. n-Pentyl alcohol

Column       : Shodex SUGAR SC1211 (6.0mmID*250mm)
Eluent       : H2O
Flow rate    : 1.0mL/min
Detector     : Shodex RI
Column temp. : 80deg-C

Aliphatic alcohols were analyzed using SUGAR SH1011.

Sample : 0.1% each, 20micro-L
1. Glycerol
2. Ethylene glycol
3. Methanol
4. Ethanol

Column       : Shodex SUGAR SH1011 (8.0mmID*300mm)
Eluent       : 5mM H2SO4 aq.
Flow rate    : 0.6mL/min
Detector     : Shodex RI
Column temp. : 60deg-C

Diols were analyzed using RSpak DE-613 (a column for reversed phase chromatography).

Sample : Glycols
Ethylene glycol, 1,2-Ethanediol
Trimethylene glycol, 1,3-Propanediol
Tetramethylene glycol, 1,4-Butanediol
Pentamethylene glycol, 1,5-Pentanediol
Hexamethylene glycol, 1,6-Hexandiol

Column       : Shodex RSpak DE-613 (6.0mmID*150mm)
Eluent       : H2O
Flow rate    : 1.0mL/min
Detector     : Shodex RI
Column temp. : 60deg-C

Aromatic alcohols were analyzed using RSpak DE-613 (a column for reversed phase chromatography).

Sample :
1. Pyrogallol
2. Hydroquinone
3. Res]orcinol
4. Pyrocatechol
5. Phenol

Column       : Shodex RSpak DE-613 (6.0mmID*150mm)
Eluent       : 0.01M H3PO4 aq./CH3CN=70/30
Flow rate    : 1.0mL/min
Detector     : UV(254nm)
Column temp. : 40deg-C

Alchohols were analyzed using SUGAR SC1211. By increasing acetonitrile concentration in the eluent, the separation of alcohols becomes insufficient.

Sample :
1. Glycerol
2. Ethyl alcohol
3. n-Propyl alcohol
4. sec-Butyl alcohol
5. Isobutyl alcohol
6. n-Butyl alcohol
7. Isopentyl alcohol
8. n-Pentyl alcohol

Column       : Shodex SUGAR SC1211 (6.0mmID*250mm)
Eluent       : (A); H2O, (B); H2O/CH3CN=80/20, (C); H2O/CH3CN=60/40 
Flow rate    : 1.0mL/min
Detector     : Shodex RI
Column temp. : 70deg-C

SUGAR SH1011 was used to analyzed glycerin and glyceric acid.

Sample : 0.1% each, 10micro-L
1. Glyceric acid
2. Glycerin, Glycerol

Column       : Shodex SUGAR SH1011 (8.0mmID*300mm)
Eluent       : 2mM H2SO4 aq.
Flow rate    : 0.6mL/min
Detector     : Shodex RI
Column temp. : 60deg-C

The following alcohols are used in cosmetics as moisturizing agents. The saccharide analysis column SUGAR SC1211 was used here to perform the simultaneous analysis of as many as 5 moisturizing compounds. SC1211 is suitable for the analysis of multivalent alcohols such as sugar alcohols other than erythritol.

Sample : 0.1% each, 20micro-L
1. 1,3-Propanediol, Trimethylene glycol
2. 1,2-Propanediol, Propylene glycol, PG
3. Ethylene glycol, EG
4. Glycerin, Glycerol
5. meso-Erythritol

Column       : Shodex SUGAR SC1211 (6.0mmID*250mm)
Eluent       : H2O/CH3CN=60/40 
Flow rate    : 0.6mL/min
Detector     : Shodex RI
Column temp. : 40deg-C

Amino Alcohols

Amino alcohols were analyzed using GPC KD-802 + KD-801 (columns for GPC separation).

Sample :
1. Triethanolamine
2. Diethanolamine
3. Monoethanolamine

Columns      : Shodex GPC KD-802 + KD-801 (8.0mmID*300mm each)
Eluent       : 10mM LiBr in DMF
Flow rate    : 1.0mL/min
Detector     : Shodex RI
Column temp. : 50deg-C

Ketones

Ketones were analyzed using RSpak RP18-413 (a column for reversed phase chromatography).

Sample :
1. Acetone
2. Methyl ethyl ketone
3. Diethyl ketone
4. Di-n-propyl ketone
5. Di-n-butyl ketone

Column       : Shodex RSpak RP18-413 (4.6mmID*150mm)
Eluent       : CH3CN/THF/H2O=30/30/40
Flow rate    : 0.6mL/min
Detector     : UV(262nm)
Column temp. : Room temp.

RSpak DE-413 is a polymer-based column for reversed phase chromatography and has unique separation characteristics and superior chemical stability. The column can be used under the same conditions as those for ODS columns. Here, ketone standards were separated by DE-413, DE-613 and an ODS column from other manufacturer. The better separation and shorter analysis time are shown with DE-413.

Sample : 5micro-L
1. 0.2% Methyl ethyl ketone
2. 0.2% Diethyl ketone
3. 0.4% Di-n-propyl ketone
4. 0.6% Di-n-butyl ketone

Columns      : (Left, above); Shodex RSpak DE-413 (4.6mmID*150mm)
               (Left, below); Shodex RSpak DE-613 (6.0mmID*150mm)
               (Right); ODS column (4.6mmID*150mm)
Eluent       : CH3CN/H2O=50/50
Flow rate    : 1.0mL/min
Detector     : UV(262nm)
Column temp. : 40deg-C

The production of packing materials for RSpak DE-413 is done in single stage, and, that of ODS columns is done in two stages, production of base material and bonding of C18 group. The simple production process of DE series ensures good reproducibility between production lots.

Sample : 5micro-L
1. 0.2% Methylethyl ketone
2. 0.2% Diethyl ketone
3. 0.4% Di-n-propyl ketone
4. 0.6% Di-n-butyl ketone

Column       : Shodex RSpak DE-413 (4.6mmID*150mm)
Eluent       : CH3CN/H2O=50/50
Flow rate    : 1.0mL/min
Detector     : UV(262nm)
Column temp. : 40deg-C

To realize the best performance of RSpak DE-413 column, we recommend to use the following HPLC system with the column.

Device Recommended specifications and/or setting Example
Pump Flow rate: max. 1mL/min.
Injector Low dead volume type
Sample loop: max. 50micro-microL(5micro-L loop is recommended)
From injector
to column		 0.1 to 0.13mmID, 100mm length piping
From column
to detector		 0.1mmID piping
Detector Detector with a micro cell should be used.
Response should be set to “FAST”.		 Shodex RI-104
(small cell volume)

Sample : (A); 1.5micro-L, (B); 5micro-L
1. Methylethyl ketone 0.2%
2. Diethyl ketone 0.2%
3. Di-n-propyl ketone 0.4%
4. Di-n-butyl ketone 0.6%

Column       : Shodex RSpak DE-413 (4.6mmID*150mm)
Eluent       : CH3CN/H2O=50/50
Flow rate    : 1.0mL/min
Detector     : UV(262nm)
Column temp. : 40deg-C

When di-n-butyl ketone is analyzed using RSpak DE-413 and DE-413L with water/acetonitrile eluent, a decease of theoretical plate number was observed according to an increase of flow rate. The decrease was marked when the flow rate was faster than 1mL/min.

Sample :
(Right); Di-n-butyl ketone
(Center, Left);
1. 0.1% Methylethyl ketone
2. 0.1% Diethyl ketone
3. 0.2% Di-n-propyl ketone
4. 0.3% Di-n-butyl ketone

Columns      : Shodex RSpak DE-413 (4.6mmID*150mm), DE-413L (4.6mmID*250mm)
Eluent       : CH3CN/H2O=50/50
Detector     : UV(262nm)
Column temp. : 40deg-C

Di-n-butyl ketone were analyzed using RSpak DE-413 (a column for reversed phase chromatography). When the sample concentration was constant, a decrease of column efficiency was observed accroding to an icrease of injection volume. The decrease started from 50micro-L and it was marked when the injection volume exceeded 100micro-L. To the contrary, when the injection volume was constant, a decrease of column efficiency was not observed until sample load exceeded 500micro-g.

Sample : Di-n-butyl ketone

Column       : Shodex RSpak DE-413 (4.6mmID*150mm)
Eluent       : CH3CN/H2O=50/50
Flow rate    : 1.0mL/min
Detector     : UV(262nm)
Column temp. : 40deg-C
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