Handbook for the Chemical Analysis of Plastic and Polymer Additives

Extraction and Analysis 23
Ethanox 310. Several antioxidant additives are based on this type of structure. Without identifying
the molecular ion of the molecule, an analyst can establish the fact that a substituted propionate
type of antioxidant is present in the material. It is this premise which is the basis for the value of
the MS data.
Abundance Average of 18.732 to 18.769 min.: PLAS-AX-086.D
m/z-->
95
90
85
80
75
70
65
60
55
50
45
40
35
30
25
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15
10
5
0
45 51
57
40 50 60 70 80 90 100 110 120 130 140 150 160 170 180 190 200 210 220 230 240 250 260 270 280 290 300
Figure 2-4 Ethanox 310 Propionate Moiety
Instrumental Conditions
All standards and “real-world” samples were chromatographed using a 30 meter, 0.25 mm i.d.,
0.25 micron film MS-5 column (QuadRex Corporation, Bethany, CT).
The additive standards for the MS library were dissolved in a suitable solvent and a sample was
injected into the GC/MS system, or a sample was transferred into an injection port liner as is done
for “real world” samples. Additive standards were run at temperature program rates of 10 °C or 15
°C due to the lack of the necessity for multi-component separation. The actual temperature
program used is listed on each Total Ion Chromatogram (TIC).
GC conditions for all standards:
• Injection port: 220 °C
• Temperature programs: 50-330 or 340 °C
• Temp. program rates: 10 or 15 °C
MS parameters:
• MS transfer line: 310 °C
• MS source temp: 230 °C
• Threshold: 500
• MS mass range: 45-800 daltons
147
161
203
77
91
105
115
128
141
185
193
65
85 97
121
134
153 173
167
209 225
235
249 261
Determining the instrumental conditions for “real world” samples involves some trial-and-error.
As was discussed earlier in this chapter, the injection port temperature is critical for the success of
this extraction technique. The authors have achieved good success for most samples with injection
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