Qualitative Analysis of Volatile Components in Cement Retarder
1 Experiments
1.1 Instrument and apparatus
GC-MS3100 gas chromatograph-mass spectrometer
Constant temperature oven or other temperature control device
5mL pipettor
20 mL headspace vial, and its cap, septum, crimper
1 mL disposable medical syringe and 5# needle
1.2 Sample pretreatment
Specified amount of samples were respectively taken and placed in 20 mL headspace vial, capped, placed in oven at 100 °C for 40 min for heating and stabilization. Then, specified amount of headspace gas was collected with 1 mL disposable medical syringe and injected for GC-MS analysis.
1.3 Analysis Conditions
GC conditions: Equity-5 (30m×0.25mm×0.25μm) quartz capillary column, precolumn pressure 30 kPa, split injection, split ratio: 25:1, injection volume: 0.4 mL, vaporization chamber temperature: 150 °C, column temperature program: hold at 35 °C for 4 min, then ramp up to 205 °C at 10 °C/min, hold for 5 min.
MS conditions: EI source, electron energy 70 eV, ion source temperature 150 °C, interface temperature 150 °C, scanning mode: full scan qualitative, scanning range: 25u~280u; solvent peak time: 1.55 min (avoiding air peak), electron multiplier high voltage: 1100V.
1.1 Instrument and apparatus
GC-MS3100 gas chromatograph-mass spectrometer
Constant temperature oven or other temperature control device
5mL pipettor
20 mL headspace vial, and its cap, septum, crimper
1 mL disposable medical syringe and 5# needle
1.2 Sample pretreatment
Specified amount of samples were respectively taken and placed in 20 mL headspace vial, capped, placed in oven at 100 °C for 40 min for heating and stabilization. Then, specified amount of headspace gas was collected with 1 mL disposable medical syringe and injected for GC-MS analysis.
1.3 Analysis Conditions
GC conditions: Equity-5 (30m×0.25mm×0.25μm) quartz capillary column, precolumn pressure 30 kPa, split injection, split ratio: 25:1, injection volume: 0.4 mL, vaporization chamber temperature: 150 °C, column temperature program: hold at 35 °C for 4 min, then ramp up to 205 °C at 10 °C/min, hold for 5 min.
MS conditions: EI source, electron energy 70 eV, ion source temperature 150 °C, interface temperature 150 °C, scanning mode: full scan qualitative, scanning range: 25u~280u; solvent peak time: 1.55 min (avoiding air peak), electron multiplier high voltage: 1100V.
Figure 1 TIC chromatogram of cement retarder
Table 1 Analysis result of volatile components in cement retarder
| Peak No | Compound | CAS No. |
| 1 | A c e t a l d e h y d e | 75-07-0 |
| 2 | E t h a n o l | 64-17-5 |
| 3 | A c e t o n e | 67-64-1 |
| 4 | D i m e t h y l s u l f i d e | 75-18-3 |
| 5 | A c e t i c a c i d , m e t h y l e s t e r | 79-20-9 |
| 6 | P r o p a n a l , 2 - m e t h y l - | 78-84-2 |
| 7 | 2 , 3 - B u t a n e d i o n e | 431-03-8 |
| 8 | E t h y l A c e t a t e | 141-78-6 |
| 9 | 1 - P r o p a n o l , 2 - m e t h y l - | 78-83-1 |
| 10 | B u t a n a l , 3 - m e t h y l - | 590-86-3 |
| 11 | B u t a n a l , 2 - m e t h y l - | 96-17-3 |
| 12 | 1 - B u t a n o l , 3 - m e t h y l - | 123-51-3 |
| 13 | 1 - B u t a n o l , 2 - m e t h y l - | 1565-80-6 |
Figure 2 Mass spectra and search result of peak No. 4
Figure 3 Mass spectra and search result of peak No. 6
Figure 4 Mass spectra and search result of peak No. 8
