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1.
采用气固顶空-气相色谱法同时测定纺织品中N,N-二甲基甲酰胺(DMF)和N,N-二甲基乙酰胺(DMAC)的残留量。样品经剪碎后,称取0.5g,在120℃顶空温度下加热30min,顶空气体采用CAM色谱柱分离,以氮磷检测器(NPD)进行检测。以基体匹配校正法消除基质效应,外标法定量。DMF、DMAC的质量在0.2~400μg范围内与峰面积呈线性关系,检出限均为0.1μg·g-1。两种物质的加标回收率在88.4%~95.3%之间,相对标准偏差(n=6)在2.4%~3.5%之间。 相似文献
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针对某制药企业生产过程中产生的高浓度含N,N-二甲基甲酰胺(DMF)料液,在折流板萃取塔内进行连续萃取分离,结合精馏工艺,实现了DMF的分离与回收。对于DMF初始质量分数为38.46%的料液,以氯仿作为萃取剂,采用脉冲折流板萃取塔对料液中的DMF进行萃取,研究了不同油水相比、流量和脉冲条件下在折流板萃取塔中DMF的萃取效果。结果表明,DMF的萃取效率随着脉冲的加入、油水相比的升高和两相流速的增大而增大,在优化的条件下DMF的萃取率最高为99.94%,分离后的萃余相DMF质量分数达到0.5%以下。进一步,对于负载了DMF的氯仿溶液,分别进行了间歇精馏实验和模拟计算,结果显示通过精馏可以实现氯仿和DMF的有效分离回收。 相似文献
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气相色谱法测定水和废水中N,N-二甲基甲酰胺和N,N-二甲基乙酰胺 总被引:7,自引:1,他引:7
N,N-二甲基甲酰胺和N,N-二甲基乙酰胺都是无色液体,重要的化工原料和性能优良的溶剂,广泛应用于聚氨酯、腈纶、医药、农药、染料、电子等行业,N,N-二甲基甲酰胺和N,N-二甲基乙酰胺对人体有毒,对环境有害。由于N,N-二甲基甲酰胺和N,N-二甲基乙酰胺都与水混溶,沸点较高,较难用溶剂或其它方法将其提取,一般都用直接进水样的方法来测定,但存在峰形不佳、柱子易受污染、需用有机溶剂稀释等不足。本法用Tenax TA作色谱固定相,用长2m、内径3mm玻璃柱直接进水样进行气相色谱的分离和测定,具有峰形佳、分离效果好、分析速度快等特点,用于样品的测定,结果满意。 相似文献
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反相高效液相色谱法测定荧光增白剂CBS中N,N-二甲基甲酰胺的残留量 总被引:1,自引:0,他引:1
建立了反相高效液相色谱外标法检测荧光增白剂CBS(即CF-351)中N,N-二甲基甲酰胺(DMF)残留量的方法。使用Accurasil C18(150 mm×4.6 mm,5 μm)反相液相色谱柱,以甲醇-水为流动相梯度洗脱,流速为1.0 mL/min,检测波长为205 nm,柱温为30 ℃,进样量为5 μL。在上述条件下,在DMF质量浓度为0.19~141 mg/L范围内,其峰面积与质量浓度的线性关系良好。在加标水平(用质量分数表示)为0.2344%和0.4678%时,回收率为98.4%~107.3%。本方法最低检出限(LOD)为0.019%(质量分数),峰面积的相对标准偏差(RSD)为1.73%。此方法可快速、准确地测定出荧光增白剂CBS中DMF的残留量。 相似文献
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利用红外光谱研究了NaNO3和NaClO4在N,N-二甲基甲酰胺(DMF)溶剂中发生离子-溶剂和离子-离子的相互作用, 分析结果表明, DMF的OC-N谱带发生了明显的变化. 定量计算了在Na+浓度为0.22~1.24 mol/kg范围内的溶剂化数为1~4. 对谱图中酰胺基上C-N和CO的特征峰强度随Na+浓度变化的对比, 推测离子溶剂化作用导致DMF的酰胺基内部形成共轭键. 利用量子化学方法进行优化及热力学性质计算, 得到C-N键伸缩振动频率及红外光谱强度变化规律. 优化结构与实验结论相符合. 由NaNO3的ν2谱带及NaClO4的ν1谱带的解析得到溶液中阴离子缔合效应的一般规律, 并通过阴离子缔合特征峰与酰胺基上的N-C-N面外振动峰(865 cm-1)的变化情况, 讨论了溶液中的离子溶剂化作用. 相似文献
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二氧化碳(CO2)是大气中主要温室气体之一,也是丰富、安全、可再生的碳一资源。将CO2催化转化为高附加值化学品不仅能改善人类长期依赖化石资源的困境,还能有效减少CO2排放,助力实现“碳达峰、碳中和”这一“双碳”目标。N,N-二甲基甲酰胺(DMF)是一种年产百万吨级的平台化合物,是优良的溶剂以及重要的化工中间体。因此,以CO2作为羰源,通过高效催化体系的构建实现CO2与二甲胺反应合成DMF具有重要意义。本文分别从还原剂、催化体系和反应机理等角度综述了这一领域近年来的研究进展。最后,对CO2合成DMF催化过程中所面临的问题和未来的发展方向进行了探讨和展望。 相似文献
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利用荧光光谱和量子化学计算方法研究了LiCl和MgCl2对N,N-二甲基甲酰胺(DMF)/乙醇双溶剂体系的微观结构变化的影响。通过对DMF的N—C O键以及盐与DMF和乙醇相互作用的研究发现,离子溶剂化作用导致溶剂体系结构变化,生成多种具有荧光属性的团簇,且随浓度的变化而变化。结合具有荧光属性的团簇分子跃迁能和可能的配位构型的优化以及热力学性质计算得到,共轭体系越大的团簇分子受盐的影响越小且其跃迁能越小的规律。比较Li+和Mg2+形成配位构型离子簇的稳定性和荧光强度,说明了离子极化对溶剂化的影响。 相似文献
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钨钼杂多酸及其盐与二甲基甲酰胺加合物的制备和性质研究 总被引:1,自引:0,他引:1
合成了10种钨钼杂多酸及其盐与DMF的加合物,用IR光谱、Raman光谱、UV光谱、1HNMR、TG-DTA和X射线衍射方法研究了加合物的性质。加合物中配体DMF以C=O键的氧作为配位原子,与杂多酸中的质子或杂多酸盐中的金属阳离子配合成键。IR光谱中νc-o的位移可作为配位键成键强度的判据。 相似文献
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《Physics and Chemistry of Liquids》2012,50(3):383-399
Abstract Viscosities of aqueous solutions of formamide, N-methylformamide and N,N-dimethylformamide have been measured at temperatures 303.15, 308.15, 313.15, 318.15 and 323.15 K. For formamide + water system the viscosity increases exponentially with respect to the mole fraction of formamide. In contrast, N-methylformamide+water and N,N-dimethylformamide+water systems exhibit maxima in water-rich region, the maxima of the latter being higher and sharper than those of the former system. The excess viscosities of formamide+water system are positive at 323.15 K, which turn to negative values at 303.15 K, the magnitude of the values being very small irrespective of their sign. On the other hand, N-methylformamide+water and N,N-dimethylformaide+water systems show large positive excess viscosities for the whole range of composition. The viscosities and excess viscosities for the system formamide+water have been explained by assuming some complex formation between the components with the simultaneous disruption of water structures. For N-methylformamide+water and N,N-dimethylformamide+water systems, it has been assumed that cluster-like structure of water is formed around methyl group(s) attached to N-atom of the amides, which influences the viscosity behaviour of these systems strongly. 相似文献
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M. Umadevi R. Regi Poornima 《Spectrochimica acta. Part A, Molecular and biomolecular spectroscopy》2009,73(5):815-822
FTIR spectra of propionic acid (PA), N,N-dimethyl formamide (DMF) and its binary mixtures with varying molefractions of the PA were recorded in the region 500–3500 cm−1, to investigate the formation of hydrogen bonded complexes in a mixed system. The observed features in ν(CO), δ(OC–N) and νas(CN) of DMF, ν(CO) and ν(CO) of PA have been explained in terms of the hydrogen bonding interactions between DMF and PA and dipole–dipole interaction. The intrinsic bandwidth for the vibrational modes νas(CN) and ν(CO) has been elucidated using Bondarev and Mardaeva model. 相似文献
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N,N-二甲基羟胺(DMHA)是用于动力堆乏燃料后处理U与Pu和Np分离的新型无盐还原剂, 本文研究了硝酸对DMHA γ-辐解及液态辐解产物的影响. 研究结果表明: 在U、Pu分离循环和Pu纯化循环的辐照剂量下, 在0.3-1.0 mol·L-1的硝酸溶液中, 0.1 和0.5 mol·L-1 DMHA具有较好的辐照稳定性. 当吸收剂量为5-25kGy时, DMHA硝酸溶液的液态辐解产物主要有单甲基羟胺、甲醛、甲酸和亚硝酸. 有机物的浓度远远高于亚硝酸浓度, 且随着剂量和硝酸浓度的增加而增大. 对于相同的硝酸浓度和剂量, 0.1 mol·L-1 DMHA辐解产生的一甲基羟胺的浓度高于0.5 mol·L-1 DMHA, 但前者辐解产生的甲醛浓度低于后者; 当硝酸浓度较高时, 0.1 mol·L-1 DMHA辐解产生的甲酸浓度高于0.5 mol·L-1 DMHA. 亚硝酸浓度与硝酸浓度及剂量的关系取决于起始DMHA和硝酸浓度. 相似文献
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M. H. Sorouraddin M. Iranifam A. Imani-Nabiyyi 《Central European Journal of Chemistry》2009,7(1):143-147
A simple and selective method for penicillin V potassium (PVK) determination by chemiluminescence (CL) was developed. Oxidation
of PVK by alkaline hydrogen peroxide produces CL, which is greatly enhanced by N, N-dimethyl formamide (DMF) and N-cetyl-N,N,N-trimethylammonium
bromide (CTMAB). Optimum conditions were established using luminometry. There is a linear relationship between the chemiluminescent
peak height and the amount of PVK within the range 0.5–129.5 mg L−1, with a detection limit of 0.2 mg L−1. The coefficient of variation was 1.2% for 40 mg L−1 PVK solution (n = 7). The method is very simple, has high sensitivity and good selectivity, and is usable for process control.
It was successfully utilized for the determination of PVK in pharmaceuticals and spiked human urine.
相似文献
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SYAMALA Vardhana RAJA SEKHAR Damaramadugu SIVA KUMAR Kasibhatta VENKATESWARLU Ponneri 《中国化学》2007,25(1):32-43
Excess volumes (v^E), ultrasonic velocities (u), isentropic compressibility (△Ks) and viscosities (η) for the binary mixtures of dimethyl formamide (DMF) with 1,2-dichlorobenzene, 1,3-dichlorobenzene, 1,2,4-trichlorobenzene, o-chlorotoluene, m-chlorotoluene, p-chlorotoluene, o-nitrotoluene and m-nitrotoluene at 303.15 K were studied. Excess volume data exhibit an inversion in sign for the mixtures of dimethyl formamide with 1,2- and 1,3-dichlorobenzenes and the property is completely positive over the entire composition range for the mixtures of dimethyl formamide with 1,2,4-trichlorobenzene, o-nitrotoluene and m-nitrotoluene. On the other hand, the quantity is negative for the mixtures of dimethyl formamide with chlorotoluenes. Isentropic compressibility (Ks) has been computed for the same systems from precise sound velocity and density data. Further, deviation of isentropic com- pressibility (△Ks) from ideal behavior was also calculated. AKs values are negative over the entire volume fraction range in all the binary mixtures. The experimental sound velocity data were analysed in terms of Free Length Theory (FLT) and Collision Factor Theory (CFT). The viscosity data were analysed on the basis of corresponding state approach. The measured data were discussed on the basis of intermolecular interactions between unlike molecules. 相似文献
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Densities of sodium methylbenzoate (o-, m-, p-) have been measured in dimethyl formamide (DMF)–water mixtures at 298.15 K with an oscillating-tube densimeter. From these densities, apparent molar volumes of sodium methylbenzoates in DMF–H2O mixtures have been calculated and partial molar volumes at infinite dilution have been evaluated. Substituent and solvent effects on the transfer volumes of each isomer from water to DMF–H2O mixed solvents have also been obtained. The results are explained in terms of solvent–solvent and solute–solvent interactions. 相似文献
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设计合成了可用于识别铜离子的化合物N,N-二甲基吡啶苯甲醛缩对二甲氨基苯甲酰腙(1), 通过1H NMR, 13C NMR和MS等对其结构进行了表征; 采用荧光光谱和吸收光谱法研究了化合物1与金属离子间的相互作用. 结果表明, 化合物1对Cu2+ 呈现良好的选择性, Cu2+ 的加入使化合物1的荧光强度增强12.5倍, 加入其它金属离子如Fe3+, Zn2+, Pb2+, Hg2+, Cd2+, Co2+, Ni2+, Li+, K+, Ca2+, Mg2+ 和 Ag+, 仅引起化合物1荧光强度的微降. 采用双倒数线性回归拟合法计算可知, 化合物1与Cu2+ 形成了1: 1型强发光配合物, 结合常数为2.0×107 L/mol. 相似文献
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Zhong Zhou CHENG Ze Hui JIA Yan CHEN Li Ying CHEN Hua LI 《中国化学快报》2006,17(8):1057-1060
Nicorandil [N-(2-hydroxyethyl)-nicotinamide nitrate NIC] is a novel kind of compound in the treatment of angina pectoris. NIC can be degraded easily in storage. The degradation products include N-(2-hydroxyethy) nicotinamide (HN), nitrate ion (NI), and ni… 相似文献