Determination of hydroxy terminated polybutadiene in the blends by liquid critical condition chromatography

doi:10.3724/SP.J.1123.2019.03042

Abstract

Abstract:

A method based on liquid critical condition chromatography (LCCC) was established for the quantification of hydroxy-terminated polybutadiene (HTPB) in polymer blends. The critical conditions for HTPB were investigated using a C18 column as the stationary phase, and tetrahydrofuran (THF)-acetonitrile (ACN) or THF-water as the mobile phase. Irrespective of the relative molecular mass, HTPB was eluted under the critical conditions of THF-ACN (70.7:29.3, v/v) or THF-water (92:8, v/v). Under the optimal conditions, the HTPB exhibited satisfactory linearity in the range of 46.7-216.4 mg/L, with a correlation coefficient (r) of 0.997. The limit of detection reached 4.2 mg/L. The recoveries of HTPB from the prepared mixtures of HTPB and mineral oil ranged from 89.2% to 101.1%, with a relative standard derivation of less than 0.66% (n=6). This method was successfully applied to the quantitative analysis of HTPB in a commercial polyurethane adhesive, and 26.6% of HTPB was detected in the product. This LCCC method is simple, convenient, highly selective, and reliable for quality control and failure studies of formulated products.

Key words: liquid critical condition chromatography(LCCC), hydroxy terminated polybutadiene(HTPB), adhesive, quantitative analysis

WANG Mingfang, JIA Qiangqiang, WANG Yuerong, ZHANG Hongyang, ZHANG Min, HU Ping. Determination of hydroxy terminated polybutadiene in the blends by liquid critical condition chromatography[J]. Chinese Journal of Chromatography, 2020, 38(2): 238-243.

Figures/Tables 5

Fig. 1 Retention behavior of narrowly distributed hydroxyl terminated polybutadiene (HTPB) using tetrahydrofuran (THF)-acetonitrile (ACN) and THF-water in different ratios as the mobile phases Peak relative molecular mass (Mp): 13330, 7828, 2595, and 1362 Da.

Fig. 2 Chromatograms of THF blank and broadly distributed HTPB under the critical conditions

Fig. 3 Chromatograms of a mixture of broadly distributed HTPB and mineral oil a. size exclusion chromatography (SEC); b. liquid critical condition chromatography (LCCC).

Table 1 Average spiked recoveries and RSDs of HTPB in the blends of HTPB and mineral oil (n=6)

Sample	Spiked level/ (mg/L)	Recovery/%	RSD/%
Blends of HTPB and oil	9.5	89.2	0.64
Blends of HTPB and oil	30.9	98.5	0.49
	73.7	101.1	0.66

Table 2 Determination of HTPB in the blends of HTPB and mineral oil and an unknown sample by LCCC and 1H nuclear magnetic resonance spectra (1H-NMR) methods(n=3)

Sample	LCCC		Relative error of LCCC and real content/%	¹H-NMR		Relative error of ¹H-NMR and real content/%
Sample	HTPB/%	RSD/%	Relative error of LCCC and real content/%	HTPB/%	RSD/%	Relative error of ¹H-NMR and real content/%
-: the value is not available for unknown sample.
Blends of HTPB and mineral	26.8	1.4	3.1	38.7	1.6	48.8
oil (26:74, v/v)
Unknown sample	26.6	1.2	-	41.8	2.1	-

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