2 1 MS 300 TRT MS JDI-800 2 g MS Py MS GC Py-GC Py GC 50 Py MS MS Py GC PY-GC 2 JDI-800 MS JDI-800 QP 2000 QP 1000 QP 2000 Fig 1 QP 1000 CI PEG 300 600 423 MS EI CI MS PEG 3 10 g Fig.1 300 600 MS
3 JDI-800 JMS AX 505 MS JMS AX 505 AX 505WA AX 505HA JDI-800 EI CI 10KV Fig 2 AX 505 EI C60 C70 MS m z 720 z 840 C60 z 360 C60 2 z 697 z 673 z 649 Fig 3 -MMA 445 3 MS MS 1ng Fig 3 Py GC
ORIGINAL RESEACH REPORT 190-12 208 Development of a Curie-Point pyrolyzer for mass spectrometry and application to Synthetic polymer analysis Naoki Oguri Akira Onishi and Sigeki Uchino Japan Analytical Industry Co., Ltd. 208 Musashi, Mizuho, Nishitama, Tokyo 190-12, Japan ABSTRACT A Curie-Point direct injection probe that can be used as an injector for mass Spectrometry is described The probe consists of an injection probe and a radio frequency power supply 48 W 10 MHz. The pyrolysis part of the injection Probe is made from ceramic and metals without using organic material around The Curie-Point heating area for decreasing a signal noise. The induction period for reaching constant temperature and the heating period of the probe are 0.2 sec and 0.1-10 sec respectively The detail of the construction and its evaluation of the proposed injection probe are described Pyrolysis mass Spectrometry by using this device is applied for the discrimination between a blended polymer the corresponding a grafted polymer of polypropylene Polystyrene and polypropylene Styrene grafted polymer Keywords Curie Point direct injection probe mass spectrometry Pyrolysis Copolymer blend polymer graft polymer MS 10 MHz 48 W 0.2 0.1 10 - MS Py MS 1 2 3 4 Py-MS Chromatography 14 1993 1R 10R ISSN 0917 3048
GC Py GC Py-GC 50 Py-MS MS Py-GC Py-GC 5 MS 300 TRT Py MS 6 10 m z 200 m z 200 JDI-800 1 5 12 17 JDI-800 Fig.1 JDI 800 12.7mm 280mm MS Fig.1 Schematic view of the Curie-point direct injection probe.
0.3mm 15 2mm 9mm 2 g 0.1 vol wt 1 l 80 12 17 10MHz 48W 0.1 10 0.05 mm 335 11 445 JDI-800 TRT 0 2 160 1,040 1.0 JDI-800 QP 2000A MS EI 70 ev 250 2 St MMA PSMMA St 70 MMA 30 ABS Py GC 10 30 St 60 PP PP PS Pressure Chemical Mn 110,000 BR cis 1,4 BR ER0l SBR Py GC St 43 % w w PS BR B PSBR St 43 % BR 57 % 100 2 PP PS B PPPS 9 1 0 G PPS 9 St 1 1 Fig 2 445 3 Py MS 0 MS 1.15 TIC Curve 1 m z 44(CO2 Curve 4 m z 32 O2 Curve3 m z 28 N2 Curve 2 SIM Selected Ion Monitering
TIC 55.5 0.5 44 % Py MS 10 2 Py MS EI 70eV 16 70eV
Fig 3 764 3 1 g PSMMA Py MS MMA m z 69{CH2=C(CH3) -C + O} MMA { M } + m z 100 m z 78{ [M] + } m z 91 [M] + m z 104 PSMMA 2 z 69 104 500 1 g PSMMA 500 3 5 m z 69 104 4 3 Py GC Fig.4. St MMA n 5 3.1 % Py MS Py GC 4.3 Py MS 12 Fig 3 3 Fig 4 30 Py GC 99 Py MS MS Py GC 100 Fig 4 SM SS SSS Fig 3 EI
3 Py MS Py GC Py MS MS 7 Fig.5 JDI 800 ABS 500 5 Py MS ABS AN Bu St Py MS m/z 53, m/z = 54, m/z = 104. St Bu Fig 7 SBR m z 129{ [ CH2=C(Ph)-CH=CH2-1] + AN St m z 156 [C=C CN -C-CPh 1] + } St l AN 2 m z 210 [C=C(CN)-C-C(CN)-C-C-Ph] + 3 AN Bu St AN Bu EI m/z 205 220 2 6 tert 4 BHT BHT ABS 315 lmg ABS MS 10 ABS MS Fig.6 Fig 6 MS BHT [M] + (m/z 220) [M-CH3] + (m/z=205) [M 75] + m/z 145 BHT St m z 104 91 78 Py MS
BHT d i Oguri 7 Py GC Py MS 13 Py MS MS Fig 7 B SBR Py MS PS BR B PSBR Py MS A A St m z 104 m z 77 m z 91 m z 207 m z 312 Py GC 14 4 4 EI B A St m z 104 m z 77 m z 321 m z 207 m z 312 SBR B z 129 z 143 157 z 262 A 4 5 A BR
5 PP PS B PPPS 445 5 Py MS Fig 8A 4 PS St m z 104 m z 77 m z 91 m z 207 m z 312 PP 2 1 M 1 + m z 83 2 4 1 M 1 + m z 12S 2 4 6 1 M CH3 1 m z 153
Fig 8B G PPS A B 4 A m z 312 B St B PPPS PP Py GC PP 2 4-1- 15 PP PP m z 125 I125
St ISt Ist/I125 Ist/I125 12.2 2.0 PP m z 125 St