非自身标样定量测定DNTF的分析方法
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摘要
为了在标准物质缺乏的情况下能够准确定量3,4-二硝基呋咱基氧化呋咱(DNTF),采用气相色谱-原子发射光谱(GC-AED)联用技术,建立了一种DNTF的非含能非自身标样定量测定方法;通过对比DNTF和5种非含能材料(二苯胺、苯甲酸、乙酰苯胺、DBS、DBP)的C元素标准曲线,选择相对定量响应因子最接近1的非含能材料作外标物定量DNTF的C元素,再结合分子式对DNTF进行定量。结果表明,苯甲酸的相对定量响应因子最接近1,用苯甲酸的C元素标准曲线定量DNTF的C元素,得到DNTF的C元素线性范围为17.43～426.92μg/mL,相关系数(r)为0.9992;以3倍信噪比计算检测限,得到DNTF的C元素方法检测限为0.0096μg/mL;相同条件下,DNTF在线性范围内高、中、低浓度下的加标回收率分别为104.9%,103.7%和109.4%,相对标准偏差分别为3.3%、1.1%和1.5%;该方法具有较好的准确度和精密度,可以实现在自身标准物质缺乏的情况下用非含能材料作外标物对DNTF的准确定量。
To accurately quantify 3, 4-bisnitrofurazanfuroxan(DNTF) in the absence of standard materials, a quantitative method for the determination of non-energetic and non-self standard of DNTF was established by gas chromatography-atomic emission spectroscopy(GC-AED) combined technology. By comparing the carbon element standard curves of DNTF and five non-energetic materials(diphenylamine,benzoic acid,acetanilide,DBS,DBP), the non-energetic material with the relative quantitative response factor closest to 1 was selected as the external standard to quantify the carbon element of DNTF, and then the DNTF was quantified by the molecular formula. The results show that the relative quantitative response factor of benzoic acid is the closest to 1, and the carbon element of DNTF is quantified by the carbon element standard curve of benzoic acid. The linear range of carbon element of DNTF is 17.43-426.92μg/mL, and the correlation coefficient(r) is 0.9992. The detection limit is calculated by three times of the signal-to-noise ratio and the method detection limit of the carbon element of DNTF is 0.0096μg/mL. Under the same conditions, the recoveries of DNTF at high, medium and low concentrations in the linear range are 104.9%,103.7% and 109.4%, and the relative standard deviations are 3.3%,1.1% and 1.5%, respectively. The method has good accuracy and precision, and accurate quantification of DNTF with non-energetic materials as external standards can be achieved in the absence of their own standard materials.
To accurately quantify 3, 4-bisnitrofurazanfuroxan(DNTF) in the absence of standard materials, a quantitative method for the determination of non-energetic and non-self standard of DNTF was established by gas chromatography-atomic emission spectroscopy(GC-AED) combined technology. By comparing the carbon element standard curves of DNTF and five non-energetic materials(diphenylamine,benzoic acid,acetanilide,DBS,DBP), the non-energetic material with the relative quantitative response factor closest to 1 was selected as the external standard to quantify the carbon element of DNTF, and then the DNTF was quantified by the molecular formula. The results show that the relative quantitative response factor of benzoic acid is the closest to 1, and the carbon element of DNTF is quantified by the carbon element standard curve of benzoic acid. The linear range of carbon element of DNTF is 17.43-426.92μg/mL, and the correlation coefficient(r) is 0.9992. The detection limit is calculated by three times of the signal-to-noise ratio and the method detection limit of the carbon element of DNTF is 0.0096μg/mL. Under the same conditions, the recoveries of DNTF at high, medium and low concentrations in the linear range are 104.9%,103.7% and 109.4%, and the relative standard deviations are 3.3%,1.1% and 1.5%, respectively. The method has good accuracy and precision, and accurate quantification of DNTF with non-energetic materials as external standards can be achieved in the absence of their own standard materials.
引文
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[2] 周涛,程淑杰,王辉,等.DNTF基含铝炸药复合装药的驱动特性[J].火炸药学报,2015,38(5):46-50. ZHOU Tao, CHENG Shu-jie, WANG Hui, et al. Research on driving characteristic for compound charge of DNTF-based aluminized explosive[J]. Chinese Journal of Explosives & Propellants(Huozhayao Xuebao), 2015, 38(5): 46-50.
[3] 郑伟,王江宁.3,4-二硝基呋咱基氧化呋咱(DNTF)的研究进展[J].含能材料,2006,14(6):463-466. ZHENG Wei, WANG Jiang-ning. Review on 3, 4-bisnitrofurazanfuroxan(DNTF)[J]. Chinese Journal of Energetic Materials, 2006, 14(6): 463-466.
[4] Zhang Guang-yuan, Jin Shao-hua, Li Li-jie, et al. Thermal stability assessment of 3, 4-bis(3-nitrofurazan-4-yl)furoxan(DNTF)by accelerating rate calorimeter[J]. Journal of Thermal Analysis and Calorimetry, 2016, 126(3): 1185-1190.
[5] 刘红妮,王克勇,杨彩宁,等.高效液相色谱法测定DNTF纯度[J].化学分析计量,2010,19(1):60-62. LIU Hong-ni, WANG Ke-yong, YANG Cai-ning, et al. Determination of DNTF purity by high performance liquid chromatography[J]. Chemical Analysis, 2010, 19(1): 60-62.
[6] 唐虹,汪翼,王延琦,等.工作场空气中3,4-二硝基呋咱基氧化呋咱的高效液相色谱测定方法[J].中国卫生工程学,2010,9(5):366-368. TANG Hong, WANG Yi, WANG Yan-qi, et al. High performance liquid chromatography method for determination of 3, 4-dinitrofurazanfuroxan in workplace air[J]. Chinese Health Engineering, 2010, 9(5): 366-368.
[7] Taegon Kim, Jaewook Ryu, Min-Ji Kim, et al. Characterization and analysis of vanadium and nickel species in atmospheric residues[J]. Fuel, 2014(117): 783-791.
[9] 潘荣荣,曲刚莲,马果花,等.GC-AED的CIC法定量测定神经性毒剂研究[J].化学工程师,2007(2):36-37. PAN Rong-rong, QU Gang-lian, MA Guo-hua, et al. Quantitative determination of neurotoxic agents by CIC method of GC-AED[J]. Chemical Engineer, 2007(2): 36-37.
[9] 周永新,李前远,靳志云,等.用气相色谱-原子发射光谱法检测VX、Bz及其降解产物[J].分析测试学报,2000,19(3):79-81.