Determination of nucleating agents in polypropylene through ultra high performance liquid chromatography

doi:10.19491/j.issn.1001-9278.2023.08.013

Abstract

Abstract:

In this study， five nucleating agents with different properties in polypropylene （PP） were analyzed by using ultra high performance liquid chromatography （UPLC）. The factors affecting the extraction efficiency of sample pretreatment were studied， and the effects of heating extraction， ultrasonic extraction， and microwave⁃assisted extraction （MAE） were investigated. The results indicated that MAE generated a good extraction effect on PP with different properties. In this extraction method， the ACQUITY BEH C18 （50 mm×2.1 mm，1.7 μm） column was used for separation， acetonitrile and water were used as mobile phases， and the UV detection wavelength was set to be 213 nm. The correlation coefficient of external standard curve was >0.995， indicating a good linear relationship between 5 and 300 mg/L. This method presented a recovery ranging from 83.4 % to 113.1 % along with a relative standard deviation （n=9） varying from 0.9 % to 7.9 %. The method developed in this study is suitable for the reliable detection of nucleating agents in PP.

Key words: polypropylene, nucleating agent, pretreatment, liquid chromatography, microwave?assisted extraction

CLC Number:

TQ317.2

ZHANG Panpan, LIU Jing, JIANG Jianzhun, CAO Xuejun. Determination of nucleating agents in polypropylene through ultra high performance liquid chromatography[J]. China Plastics, 2023, 37(8): 93-100.

Figures/Tables 12

References 15

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成核剂	IUPAC 名称	CAS 号	分子式	相对分子质量
M3905	1，3：2，4⁃二苄叉山梨醇	32647⁃67⁃9	C₂₀H₂₂O₆	358.4
HX⁃3	双（3，4⁃二甲基苯亚甲基）山梨醇	135861⁃56⁃2	C₂₂H₃₀O₆	414.5
NX8000	1，2，3⁃三脱氧⁃4，6：5，7⁃双⁃O⁃［（4⁃丙苯基）亚甲基］⁃壬醇	882073⁃43⁃0	C₂₉H₄₀O₆	484.6
SOD BENZOATE	苯甲酸钠	532⁃32⁃1	C₇H₅NaO₂	144.1
NA21	2，2’⁃亚甲基⁃双（4，6⁃二叔丁基苯基磷酸）碱式铝	151841⁃65⁃5	C₅₈H₈₅AlO₉P₂	1 015.2

成核剂	IUPAC 名称	CAS 号	分子式	相对分子质量
M3905	1，3：2，4⁃二苄叉山梨醇	32647⁃67⁃9	C₂₀H₂₂O₆	358.4
HX⁃3	双（3，4⁃二甲基苯亚甲基）山梨醇	135861⁃56⁃2	C₂₂H₃₀O₆	414.5
NX8000	1，2，3⁃三脱氧⁃4，6：5，7⁃双⁃O⁃［（4⁃丙苯基）亚甲基］⁃壬醇	882073⁃43⁃0	C₂₉H₄₀O₆	484.6
SOD BENZOATE	苯甲酸钠	532⁃32⁃1	C₇H₅NaO₂	144.1
NA21	2，2’⁃亚甲基⁃双（4，6⁃二叔丁基苯基磷酸）碱式铝	151841⁃65⁃5	C₅₈H₈₅AlO₉P₂	1 015.2

样品编号	成核剂	标准曲线方程	R²	保留时间/min	LOD/mg·L^-1	LOQ/mg·L^-1
1	SOD BENZOATE	A=5 449.3C-3 617.2	0.995 6	0.49	0.2	0.5
2	M3905	A=4 536.3C-4 088.7	0.999 1	2.56	0.5	1.0
3	NA21	A=7 113.2C-6 306.5	0.999 5	4.31	0.1	0.5
4	HX⁃3	A=6 660.5C-3 015.7	0.998 0	4.84	0.2	0.5
5	NX8000	A=6 867.9C-2 951.6	0.998 8	8.64	0.2	0.5

样品编号	成核剂	标准曲线方程	R²	保留时间/min	LOD/mg·L^-1	LOQ/mg·L^-1
1	SOD BENZOATE	A=5 449.3C-3 617.2	0.995 6	0.49	0.2	0.5
2	M3905	A=4 536.3C-4 088.7	0.999 1	2.56	0.5	1.0
3	NA21	A=7 113.2C-6 306.5	0.999 5	4.31	0.1	0.5
4	HX⁃3	A=6 660.5C-3 015.7	0.998 0	4.84	0.2	0.5
5	NX8000	A=6 867.9C-2 951.6	0.998 8	8.64	0.2	0.5

成核剂	MAE			超声提取			加热回流提取
成核剂	平均质量/mg•g^-1	Range/mg•g^-1	RSD/%	平均质量/mg•g^-1	Range/mg•g^-1	RSD/%	平均质量/mg•g^-1	Range/mg•g^-1	RSD/%
SOD BENZOATE	1.42	0.14	3.5	1.02	0.10	3.2	1.58	0.15	2.4
M3905	1.38	0.25	6.7	1.12	0.12	2.1	1.90	0.07	0.5
NA21	1.30	0.11	2.1	0.88	0.09	1.5	1.86	0.10	1.3
HX⁃3	1.54	0.19	5.6	0.90	0.09	1.6	2.04	0.16	2.5
NX8000	1.34	0.22	4.9	0.82	0.16	2.8	1.94	0.12	1.7