Wang Jianlong

The crystal structure of 2,3-dimethyl-1,4-dinitrobenzene – a Z′ = 4 structure, C8H8N2O4

Abstract C8H8N2O4, triclinic, P1̄ (no. 2), a = 9.1093(5) Å, b = 13.2430(8) Å, c = 15.4334(10) Å, α = 106.544(2)°, β = 98.150(2)°, γ = 96.151(2)°, V = 1745.22(18) Å3, Z = 8, Rgt(F) = 0.0508, wRref(F2) = 0.1141, T = 173(2) K.

Crystal structure of 2-(4-chloro-2,6-dinitrophenyl)-1-(4-chloro-3-nitrophenyl)diazene 1-oxide, C12H5Cl2N5O7

*Corresponding author: Wang Jianlong, School of Chemical Engineering and Technology, North University of China, Taiyuan 030051, Shanxi Province, P.R. China, e-mail: 619379961@qq.com Cao Junyan and Chen Lizhen: School of Chemical Engineering and Technology, North University of China, Taiyuan 030051, Shanxi Province, P.R. China Zhang Luyao: Scientific Research Institute, Gansu yinguang Chemical Industry Group, Baiyin 730900, Gansu Province, P.R. China Abstract C12H5Cl2N5O7, triclinic, P1̄ (no. 2), a= 8.2425(8) Å, b= 8.2814(7) Å, c= 12.4713(12) Å, α= 93.370(4)°, β= 101.590(4)°, γ = 118.222(3)°, V = 723.03(12) Å3, Z = 2, Rgt(F)=0.0516, wRref(F)=0.0858, T = 173(2) K.

3, 4-二硝基吡唑纯度的高效液相色谱分析方法

为准确测定3, 4-二硝基吡唑产品的纯度, 建立了3, 4-二硝基吡唑及其合成过程中可能存在的杂质(3-硝基吡唑、1, 3-二硝基吡唑)的高效液相色谱分析方法。讨论了不同流动相体系、流动相比例、流速等条件对3, 4-二硝基吡唑高效液相色谱分离效果的影响。采用外标法进行定量分析。结果表明, 得出最优的色谱条件为: Hypersil ODS2色谱柱(250 mm×4.6 mm, 5 μm), 紫外检测波长260 nm, 流动相为乙腈/0.1%乙酸水=35:65( V/V ), 流速1.0 mL·min -1 , 柱温25 ℃, 进样量10 μL。在上述色谱条件下, 3-硝基吡唑、3, 4-二硝基吡唑和1, 3-二硝基吡唑的保留因子分别为0.41、1.20、1.52, 3-硝基吡唑和3, 4-二硝基吡唑间的分离度为9.42, 3-硝基吡唑和1, 3-二硝基吡唑间的分离度为3.16。3, 4-二硝基吡唑线性范围为5~500 mg·L -1 , 3-硝基吡唑的线性范围为5~250 mg·L -1 , 1, 3-二硝基吡唑的线性范围为5~250 mg·L -1 。在此范围内, 三种化合物的检测限分别为1.19, 0.60, 1.04 mg·L -1 , 相对标准偏差为1.39%~2.08%, 加标回收率为95.29%~103.43%。