丙二醇甲醚中超痕量金属杂质元素的ICP-MS/MS分析

Parameter	Setting
RF power/W	1 550
Carrier gas flow/(L·min^-1)	1.05
Make up gas flow/(L·min^-1)	0.25
Sampling depth/mm	8
Cell gas	NH₃/He/H₂(10% NH₃ in He)
Cell gas flow rate/(mL·min^-1)	NH₃/He: 2.8; H₂=2.0
ORS bias voltage/V	-18
KED voltage/V	-8

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表 2在不同分析模式下分析元素的背景等效浓度(BEC)

Table2. Background equivalent concentrations (BEC) of analytes in different analysis modes

Isotope	Potential interferences	BEC/(ng·L^-1)
		SQ mode		MS/MS mode
		no gas	He	NH₃/He	NH₃/He/H₂
²⁴Mg	¹²C₂, ²³Na¹H, ⁷Li¹⁷O, ⁴⁸Ti⁺⁺, ⁴⁸Ca⁺⁺	2 970	411	29.8	31.2
²⁷Al	¹²C¹⁵N, ¹²C¹⁴NH	860	202	77.3	75.4
³⁹K	³⁸ArH, ²³Na¹⁶O	189 000	65 300	126	84.3
⁴⁸Ti	³²S¹⁶O, ³⁴S¹⁴N, ³³S¹⁵N, ¹⁴N¹⁶O¹⁸O, ³⁶Ar¹²C	1 560	87.4	21.0	16.7
⁵¹V	³⁵Cl¹⁶O, ³⁶Ar¹⁴NH, ³⁴Ar¹⁶OH, ³⁶Ar¹³C, ³⁶Ar¹⁵N	479	15.3	8.16	5.04
⁵²Cr	⁴⁰Ar¹²C, ³⁵Cl¹⁶OH, ³⁶Ar¹⁶O, ³⁸Ar¹⁴N, ³⁶Ar¹⁵N¹H	2 170	73.6	41.4	35.8
⁵⁶Fe	⁴⁰Ar¹⁶O, ⁴⁰Ca¹⁶O, ⁴⁰Ar¹⁵N¹H, ³⁸Ar¹⁸O, ¹¹²Cd⁺⁺	1 810	425	122	94.1
⁶⁰Ni	²³Na³⁶ArH, ²³Na³⁷Cl, ⁴⁴Ca¹⁶O, ⁵⁹CoH	316	49.7	21.8	17.6
⁶³Cu	²³Na⁴⁰Ar, ²³Na⁴⁰Ca, ¹²C¹⁶O³⁵Cl, ¹²C¹⁴N³⁷Cl, ⁴⁶Ca¹⁶OH	177	51.3	40.5	34.4
⁶⁶Zn	³⁴S¹⁶O₂, ⁴⁸Ti¹⁸O, ⁴⁸Ca¹⁸O, ³²S¹⁷O₂, ³³S¹⁷O¹⁶O, ³²S³⁴S	223	148	116	89.5

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表 3不同模式下用于消除干扰实验的回收率

Table3. Recovery of interference removal experiment in different modes

Analyte	Interference		Recovery/%
Analyte	Added interferent	Interfering ion	No gas mode	NH₃/He/H₂ reaction mode
²⁴Mg	C (Ethanol)	¹² $C_{2}^{+}$	307	101.3
²⁷Al	C (Ethanol)	¹²C¹⁵N⁺, ¹²C¹⁴NH⁺	223	99.1
³⁹K	/	³⁸ArH⁺	851	98.6
⁴⁸Ti	S (S $O_{4}^{2 -}$ )	³²S¹⁶O⁺, ³⁴S¹⁴N⁺	1 260	102.5
⁵¹V	Cl (Cl^-)	³⁵Cl¹⁶O⁺	208	100.7
⁵²Cr	C (Euhanol)	⁴⁰Ar¹²C⁺	715	101.6
⁵⁶Fe	/	⁴⁰Ar¹⁶O⁺	1 070	97.5
⁶⁰Ni	Na (Na⁺)	²³Na³⁶ArH⁺	322	99.1
⁶³Cu	Na (Na⁺)	²³Na⁴⁰Ar⁺	450	103.4
⁶⁶Zn	S (S $O_{4}^{2 -}$ )	³⁴S¹⁶ $O_{2}^{+}$ , ³²S¹⁷ $O_{2}^{+}$	279	98.9

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表 4校准数据与检出限

Table4. Calibration data and instrumental limits of detection (LOD)

Element	Linear range /(μg·L^-1)	Coefficient (r)	LOD /(ng·L^-1)	Element	Linear range /(μg·L^-1)	Coefficient (r)	LOD /(ng·L^-1)
Mg	0~100	0.999 9	15.1	Cr	0~100	1.000 0	2.18
Al	0~100	1.000 0	17.2	Fe	0~100	0.999 8	35.3
K	0~100	0.999 8	61.5	Ni	0~100	1.000 0	9.75
Ti	0~100	0.999 7	3.84	Cu	0~100	0.999 9	5.81
V	0~100	1.000 0	0.52	Zn	0~100	0.999 8	40.6

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表 5方法的准确性和精密度(n=6)

Table5. The accuracy and precisions of method (n=6)

Element	Spiked /(μg·L^-1)	Found by ICP-MS/MS /(μg·L^-1)	RSD /%	Recovery /%	Found by SF-ICP-MS /(μg·L^-1)	t test
Mg	5.00	5.12±0.23	4.5	102.4	5.08±0.19	p=0.37
Al	5.00	4.91±0.11	2.2	98.2	4.85±0.12	p=0.15
K	5.00	4.88±0.10	2.0	97.6	4.94±0.15	p=0.21
Ti	5.00	5.09±0.15	2.9	101.8	5.16±0.21	p=0.26
V	5.00	5.17±0.19	3.7	103.4	5.05±0.24	p=0.18
Cr	5.00	4.83±0.14	2.9	96.6	4.74±0.18	p=0.11
Fe	5.00	5.21±0.20	3.8	104.2	5.13±0.16	p=0.23
Ni	5.00	4.78±0.08	1.7	95.6	4.82±0.12	p=0.26
Cu	5.00	4.81±0.21	4.4	96.2	4.85±0.09	p=0.33
Zn	5.00	5.19±0.14	2.7	103.8	5.07±0.10	p=0.06

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表 6PGME中10个超痕量金属元素的分析结果(ng·g^-1, n=6)

Table6. Analytical results for determination of 10 ultra-trace metal elements in PGME (ng·g^-1, n=6)

Element	Sample 1		Sample 2		Sample 3
Element	ICP-MS/MS	SF-ICP-MS	ICP-MS/MS	SF-ICP-MS	ICP-MS/MS	SF-ICP-MS
Mg	2.56±0.03	2.34±0.04	1.87±0.03	1.92±0.02	2.15±0.04	2.20±0.05
Al	1.36±0.02	1.41±0.02	2.05±0.02	2.09±0.03	3.61±0.05	3.53±0.04
K	2.23±0.01	2.19±0.03	4.59±0.05	4.66±0.08	1.20±0.02	1.31±0.05
Ti	2.80±0.05	3.01±0.07	1.50±0/02	1.43±0.03	1.97±0.03	1.83±0.03
V	1.62±0.03	1.57±0.02	0.75±0.01	0.79±0.01	1.84±0.05	1.68±0.02
Cr	0.93±0.01	1.04±0.03	2.40±0.03	2.31±0.02	2.75±0.03	2.82±0.03
Fe	5.10±0.12	5.23±0.10	3.65±0.05	3.71±0.04	8.06±0.13	7.82±0.16
Ni	1.66±0.02	1.74±0.03	0.69±0.01	0.64±0.01	1.73±0.04	1.81±0.04
Cu	4.77±0.08	4.92±0.09	2.87±0.04	2.82±0.06	3.21±0.03	3.39±0.05
Zn	3.45±0.04	3.36±0.05	1.21±0.01	1.16±0.02	2.27±0.02	2.32±0.02

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李坦平, 李爱阳. 丙二醇甲醚中超痕量金属杂质元素的ICP-MS/MS分析[J]. 光谱学与光谱分析, 2021, 41(2): 618. Tan-ping LI, Ai-yang LI. Analysis of Ultra-Trace Metal Impurity Elements in Proprylene Glycol Monomethyl Ether Using Inductively Coupled Plasma Tandem Mass Spectrometry[J]. Spectroscopy and Spectral Analysis, 2021, 41(2): 618.

丙二醇甲醚中超痕量金属杂质元素的ICP-MS/MS分析

图 1. NH₃/He反应气流速的优化
(a): 原位质量法; (b): 质量转移法

Fig. 1. Optimization of the NH₃/He reaction gas flow rate
(a): On-mass method; (b): Mass shift method

表 1ICP-MS/MS的操作参数

Table1. ICP-MS/MS operating parameters

表 2在不同分析模式下分析元素的背景等效浓度(BEC)

Table2. Background equivalent concentrations (BEC) of analytes in different analysis modes

表 3不同模式下用于消除干扰实验的回收率

Table3. Recovery of interference removal experiment in different modes

表 4校准数据与检出限

Table4. Calibration data and instrumental limits of detection (LOD)

表 5方法的准确性和精密度(n=6)

Table5. The accuracy and precisions of method (n=6)

表 6PGME中10个超痕量金属元素的分析结果(ng·g^-1, n=6)

Table6. Analytical results for determination of 10 ultra-trace metal elements in PGME (ng·g^-1, n=6)

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丙二醇甲醚中超痕量金属杂质元素的ICP-MS/MS分析

图 1. NH3/He反应气流速的优化(a): 原位质量法; (b): 质量转移法

Fig. 1. Optimization of the NH3/He reaction gas flow rate(a): On-mass method; (b): Mass shift method

表 1ICP-MS/MS的操作参数

Table1. ICP-MS/MS operating parameters

表 2在不同分析模式下分析元素的背景等效浓度(BEC)

Table2. Background equivalent concentrations (BEC) of analytes in different analysis modes

表 3不同模式下用于消除干扰实验的回收率

Table3. Recovery of interference removal experiment in different modes

表 4校准数据与检出限

Table4. Calibration data and instrumental limits of detection (LOD)

表 5方法的准确性和精密度(n=6)

Table5. The accuracy and precisions of method (n=6)

表 6PGME中10个超痕量金属元素的分析结果(ng·g-1, n=6)

Table6. Analytical results for determination of 10 ultra-trace metal elements in PGME (ng·g-1, n=6)

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图 1. NH₃/He反应气流速的优化
(a): 原位质量法; (b): 质量转移法

Fig. 1. Optimization of the NH₃/He reaction gas flow rate
(a): On-mass method; (b): Mass shift method

表 6PGME中10个超痕量金属元素的分析结果(ng·g^-1, n=6)

Table6. Analytical results for determination of 10 ultra-trace metal elements in PGME (ng·g^-1, n=6)