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A HILIC-MS/MS method was developed to determine melamine and its three derivatives, cyanuric acid, ammelide and ammeline in milk and milk powder. The milk sample was directly extracted by acetonitrile with the help of ultrasonic, and milk powder was resolved in water before extraction by acetonitrile.

建立了牛奶和奶粉中三聚氰胺及其3种衍生物(三聚氰酸、三聚氰酸一酰胺、三聚氰酸二酰胺)的亲水色谱-串联质谱检测方法(HILIC-MS/MS)。

After centrifugation, the extracts were separated on HILIC column by using acetonitrile-water as mobile phase. The analytes were identified and quantitated by LC-tandem MS under the positive/negative electrospray ionization and multiple reaction monitormode. The calibration curves showed good linearity in the range of 25-5000 μg/kg for melamine and cyanuric acid, and 50-10000 μg/kg for ammeline and ammelide. The limits of detection and limits of quantification were in the range of 5-20 μg/kg and 50-100 μg/kg, respectively.

牛奶样品直接用乙腈超声波提取;奶粉样品先用水溶解后再加乙腈超声波提取,高速离心后以乙腈-水为流动相,采用亲水作用色谱柱分离这4种化合物,在电喷雾正、负电离切换多反应监测模式下进行定性与定量分析,三聚氰酸一酰胺与三聚氰酸二酰胺含量在50~10000μg/kg之间、三聚氰胺与三聚氰酸在25~5000μg/kg之间,均获得良好的线性。

Ketoheptamethylenimine was prepared by one-pot reaction of cycloheptanone with concentrated sulfuric acid. In this step, oximation and rearrangement occurred .

制备庚内酰胺时,我们采用了&一锅反应&的方法,环庚酮、浓硫酸和硫酸羟胺混合在一起,经过肟化、重排一次得到庚内酰胺

Treatment of dials with N-tert-butanesulfinamide, all biaryl dials were successfully converted into the corresponding bis-imines which were then treated with samarium diiodide to afford diamine products. The absolute configurations of all the intramolecular coupling products were determined by X-ray crystallography.

轴手性二醛与N-叔丁基亚磺酰胺缩合得到相应的亚胺,其为一对非对映异构体。N-叔丁基亚磺酰亚胺在二碘化钐条件下得到的偶联产物,经X-衍射也确定了其立体构型。

The copolycondensation type polyamic acid was synthesized by using 3,3', 4,4'-Benzophenonetetracarboxylic dianhydride as the dianhydride monomer, 4,4'-Diamino diphenylmethane and 4,4'-Oxydianiline as the diamine monomer under microwave irradiation in Dimethylformamide.

在微波辐射条件下,采用3,3',4,4'-二苯酮四羧酸二酐、4,4'-二氨基二苯甲烷和4,4'-二氨基二苯醚为单体,N,N'-二甲基甲酰胺为溶剂,低温合成一种共缩聚聚酰亚胺的前驱体聚酰胺酸,化学亚胺化脱水环化生成BTDA型共缩聚聚酰亚胺。

Firstly, Copolymerization of acrylamide and styrene was carried out in a microemulsion system, in which AM aqueous solution was the continue phase and St was the dispersed phase using ST-80 as surfactants respectively, then hydroxamic functions were prepared with hydroxylamine salt at temperatures of from 60℃ to 90℃.

首先以丙烯酰胺水溶液为连续相,以苯乙烯为分散相,ST-80为乳化剂制成微乳液,在15℃~35℃合成丙烯酰胺与苯乙烯的共聚物;然后采用程序控温方式,在60℃~90℃用硫酸羟胺将共聚物羟肟化合成了一种带有苯环结构的嵌段型氧肟酸类聚合物材料。

At 15-35℃, copolymerization of acrylamide and styene was carried out in a microemulsion system, in which AM aqueous solution was the continuous phase and St was the dispersed phase using ST-80 as surfactants, respectively. Hydroxamic functions were prepared with hydroxylamine salt at temperatures from 60℃ to 90℃.

以丙烯酰胺水溶液为连续相,苯乙烯为分散相,ST-80为乳化剂制成微乳液,在15~35℃下合成丙烯酰胺与苯乙烯的共聚物,采用程序控温方式,在60~90℃下使用硫酸羟胺将共聚物羟肟化得到产物。

In this paper, the third monomer 1,4- benzenediamine was introduced into the system of pyromellitic dianhydride and 4, 4-diamino diphenyl. Polyamic acid was synthesized in N-methyl pyrrolidone by solution polycondensation. The chemical structure of the polymer obtained was characterized by infrared spectrum. The dynamic viscosity and intrinsic viscosity were measured. Studies were mainly focused on the influences of monomer solid contents, monomer adding methods on intrinsic viscosity.

本实验在常用的均苯四酸二酐和4,4'—二氨基二苯醚聚酰亚胺体系中,引入第三单体对苯二胺,采用三元共聚的办法合成出聚酰胺酸溶液,对合成产物进行了分子结构的红外光谱分析以及特性粘数、动力学粘度的测试,并讨论了单体固含量、加入方式等对聚酰胺酸特性粘数的影响。

The glycyrrhizic acid antigen is prepared through the process including following steps: dissolving glycyrrhizic acid in N, N-dimethyl formamide, dioxane or dimethyl sulfoxide, heliophobically adding N-hydroxy succinimide, reacting with dicyclohexylcarbodiimide at 0-10 deg.c for 2-5 hr; and reacting with carrier protein at normal temperature for 4-6 hr to obtain glycyrrhizic acid antigen.

本发明所提供的甘草酸抗体,是用甘草酸抗原免疫动物,然后从被免疫动物的血清中分离得到的;所述甘草酸抗原按如下过程制备:先将甘草酸溶解在N,N-二甲基甲酰胺、二氧六环或二甲基亚砜中,避光加入N-羟基琥珀酰亚胺,然后在0-10℃条件下与二环己基碳二亚胺反应2-5小时;接着与载体蛋白常温反应4-6小时,得到甘草酸抗原。

A plausible process of this reaction is as following: Aldehyde was in equilibrium with the enol form, aldehyde reacted with aniline catalyzed by 2,2,2-trichloroacetic acid to afford imine, the generated imine immediately reacted with enol to form intermediate via intramolecular cyclization.

我们发现一分子芳基叠氮和一分子三苯基磷反应生成一分子磷亚胺,后者与由两分子取代的苯氧乙酰氯原位生成的烯酮反应生成4-亚烷基-β-烷基-内酰胺,其串联过程涉及烯酮亚胺的形成及其与烯酮的[2+2]的环加成反应。

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