Additives in Hydrophobic Polymers

Phthalates and alkylbenzenes were analyzed using GPC KF-801 (a column for organic SEC (GPC)).

Sample :
1. DNP (Dinonyl phthalate)
2. DOP (Dioctyl phthalate)
3. DHP (Dihexyl phthalate)
4. DBP (Dibutyl phthalate)
5. DPP (Dipropyl phthalate)
6. DEP (Diethyl phthalate)
7. DMP (Dimethyl phthalate)
8. n-Bu benzene (n-Butylbenzene)
9. n-Pr benzene (n-Propylbenzene)
10. Et benzene (Ethylbenzene)
11. Toluene (Methylbenzene)
12. Benzene

Columns      : Shodex GPC KF-801 (8.0mmID*300mm) x 4
Eluent       : THF
Flow rate    : 1.0mL/min
Detector     : UV(254nm)
Column temp. : Room temp.

Phthalates and alkylbenzenes were analyzed using GPC KF-401HQ (a semi-micro organic SEC (GPC) column).

Sample :
1. Dioctyl phthalate
2. Dibutyl phthalate
3. Dipropyl phthalate
4. Diethyl phthalate
5. Dimethyl phthalate
6. n-Propylbenzene
7. Ethylbenzene
8. Toluene
9. Benzene

Columns      : Shodex GPC KF-401HQ (4.6mmID*250mm) x 2
Eluent       : THF
Flow rate    : 0.3mL/min
Detector     : UV(254nm)(small cell volume)
Column temp. : 40deg-C

Phthalates were analyzed using RSpak DS-613 with different eluents. With THF/H2O eluent, the elution pattern is that of typical reversed phase. With C2H5OH eluent, the pattern is also that of reversed phase but the peak shape is rather broad and the separation is not so good except the separation between DEHP and DBP. With n-hexane/C2H5OH eluent, the elution pattern is that of normal phase.

Sample : 2.5micro-L
(A)0.2% each, 0.4%(DOP)
(B)(C)0.4% each
1. DMP, Dimethyl phthalate
2. DEP, Diethyl phthalate
3. DPP, Dipropyl phthalate
4. DBP, Dibutyl phthalate
5. DHP, Dihexyl phthalate
6. DEHP, Diethylhexyl phthalate
7. DOP, Dioctyl phthalate

Column       : Shodex RSpak DS-613 (6.0mmID*150mm)
Eluent       : (A) THF/H2O=70/30 (Reversed phase)
               (B) C2H5OH (Reversed phase)
               (C) n-Hexane/C2H5OH=95/5 (Normal phase)
Flow rate    : (A)0.5mL/min, (B)(C)0.6mL/min
Detector     : UV(254nm)
Column temp. : (A)(B) 50deg-C, (C)25deg-C

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

Sample :
1. Benzene
2. Toluene
3. Ethylbenzene

Column       : Shodex RSpak RP18-413 (4.6mmID*150mm)
Eluent       : CH3CN/THF/H2O=50/10/40
Flow rate    : 1.0mL/min
Detector     : UV(254nm)
Column temp. : Room temp.

Phthalates were analyzed using GPC KF-802 (a column for organic SEC (GPC)) and effect of flow rate on plate number is shown.

Sample :
Benzene
DMP, Dimethyl phthalate
DBP, Dibutyl phthalate
DOP, Dioctyl phthalate

Column       : Shodex GPC KF-802 (8.0mmID*300mm)
Eluent       : THF
Column temp. : Room temp.

The color of some impurity substance in a resin changed to yellow. And, the substance was fractionated by recycle analysis using GPC H-2001 and the chemical structure was determined.

Sample : Butylated hydroxytoluene, BTH

Columns      : Shodex GPC H-2001 (20.0mmID*500mm) x 2
Eluent       : CHCl3
Flow rate    : 3.0mL/min
Detector     : UV(254nm)
Column temp. : Room temp.

S. Nakamura et al, J. Chromatgr. , 83 (1973) 279

Antioxidant (Irganox1010) in Polystyrene was analyzed with GPC/MS using GPC KF-402HQ (a semi-micro organic SEC (GPC) column). Only a low molecule weight domain can be poured into a mass spectrometer (MS) by using GPC mode. Therefore, it is not necessary to pretreat.
Please refer to Simultaneous Analysis of Various Additives of Polymer in Polystyrene (GPC/MS)

Sample : 1ppm Irganox 1010 in 1000ppm Polystyrene, 5micro-L
1. Polystyren
2. Irganox 1010

(HPLC)
Instrument   : Agilent 1100
Column       : Shodex GPC KF-402HQ (4.6mmID*250mm) x 2
Eluent       : THF
Flow rate    : 0.3mL/min
Detector     : UV(210nm)
Column temp. : 40deg-C
(MS)
Instrument      : Thermo Quest LCQ Advantage
Ionization      : APCI
Capillary temp. : 180deg-C
Vaporizer temp. : 450deg-C
Source voltage  : 6000V
Sheath gas flow : 80L/min

Irganox 1010 in styrene foam cup for instant noodles was analyzed with GPC/MS using KF-402HQ (a semi-micro organic SEC (GPC) column). Only a low molecule weight domain can be poured into a mass spectrometer (MS) by using GPC mode. KF-402HQ can provide the high sensitivity analysis without pretreatment of samples.
Refer to Simultaneous Analysis of Various Additives of Polymer in Polystyrene (GPC/MS).

Sample : 0.1%, 5micro-L
1. Polystyren
2. Irganox 1010

(HPLC)
Instrument   : Agilent 1100
Column       : Shodex GPC KF-402HQ (4.6mmID*250mm) x 2
Eluent       : THF
Flow rate    : 0.3mL/min
Detector     : UV(210nm)
Column temp. : 40deg-C
 
(MS)
Instrument      : Thermo Quest LCQ Advantage
Ionization      : APCI
Capillary temp. : 180deg-C
Vaporizer temp. : 450deg-C
Source voltage  : 6000V
Sheath gas flow : 80L/min

Various additives of polymer in polystyrene were analyzed simultaneously with GPC/MS using GPC KF-402HQ (a semi-micro organic SEC (GPC) column).

Sample : 5micro-L
Irganox 1010
Irganox 1076
Irgafos 168
Tinuvin 234
BHT dimer
BHT

(HPLC)
Instrument   : Agilent 1100
Column       : Shodex GPC KF-402HQ (4.6mmID*250mm) x 2
Eluent       : THF
Flow rate    : 0.3mL/min
Column temp. : 40deg-C
 
(MS)
Instrument      : Thermo Quest LCQ Advantage
Ionization      : APCI
Capillary temp. : 180deg-C
Vaporizer temp. : 450deg-C
Source voltage  : 6000V
Sheath gas flow : 80L/min
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