5.1 This test method is suitable for setting specifications on the materials referenced in 1.2 and for use as an internal quality control tool where AMS is produced or is used in a manufacturing process. It may also be used in development or research work involving AMS.
5.2 This test method is useful in determining the purity of AMS with normal impurities present. If extremely high boiling or unusual impurities are present in the AMS, this test method would not necessarily detect them and the purity calculation would be erroneous.
Область применения1.1 This test method covers the determination of the purity of AMS (α-methylstyrene) by gas chromatography. Calibration of the gas chromatography system is done by the external standard calibration technique.
1.2 This test method has been found applicable to the measurement of impurities such as cumene, 3-methyl-2-cyclopentene-1-one, n-propylbenzene, tert-butylbenzene, sec-butylbenzene, cis-2-phenyl-2-butene, acetophenone, 1-phenyl-1-butene, 2-phenyl-2-propanol, trans-2-phenyl-2-butene, m-cymene, p-cymene, and phenol, which are common to the manufacturing process of AMS. The method has also been found applicable for the determination of para-tertiary-butylcatechol typically added as a stabilizer to AMS. The impurities in AMS can be analyzed over a range of 5 to 800 mg/kg by this method. (See Table 1.) The limit of quantitation for these these impurities averages 4 mg/kg, while the limit of detection averages 1.2 mg/kg. (See Table 1.)
TABLE 1 Summary of Precision Data (mg/kg)
Compound
Repeatability (r)
Reproducibility (R)
Range Studied
Acetone
1.61 + 0.035*Acetone
0.47 + 1.10*Acetone
0.5 – 26
Cumene
−0.46 + 0.031*Cumene
7.88 + 0.19*Cumene
45 – 290
nPropylbenzene (NPB)
2.11 + 0.03*NPB
−7.81 + 0.37*NPB
55 – 195
Phenol
1.84
3.65 + 0.58*Phenol
1 – 40
tertButylbenzene (TBB)
−1.22 + 0.035*TBB
3.63 + 0.087*TBB
150 – 650
secButylbenzene (SBB)
4.23 + 0.019*SBB
21.60 + 0.25*SBB
200 – 765
mCymene
0.31 + 0.035*mCymene
2.34 + 0.35*mCymene
2 – 50
oCymene
1.63
8.00
29 – 31
pCymene
5.12
15.79
10 – 18
cis-2-Phenyl-2-Butene (CPB)
0.17 + 0.030*CPB
5.39 + 0.11*CPB
50 – 225
trans-2-Phenyl-2-Butene (TPB)
1.57
0.54 + 0.20*TPB
19 – 70
1-Phenyl-1-Butene (PB)
4.00 + 0.018*PB
0.17 + 0.19*PB
0.2 – 735
Acetophenone (AP)
–1.09 + 0.15*AP
1.17 + 0.63*AP
15 – 115
para-tert-Butylcatechol (PTBC)
2.21
17.82
10 – 19
2-Methylbenzofuran (MBF)
0.33 + 0.76*MBF
0.75 + 0.60*MBF
1 – 2
2-Phenylpropion aldehyde (PPA)
0.59 + 0.11*PPA
0.29 + 0.23*PPA
1.5 – 15
α-Methylstyrene Oxide (AMSO)
4.61
6.51 + 0.23*AMSO
13 – 32
DimethylBenzyl Alcohol (DMBA)
0.38
0.55 + 2.03*DMBA
0.1 – 1
1.3 In determining the conformance of the test results using this method to applicable specifications, results shall be rounded off in accordance with the rounding-off method of Practice E29.
1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.5 This standard does not purport to address all the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. For specific hazard statements, see Section 8.
1.6 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.