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purity
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     ON PURITY OF S-ACTS
     关于S-系的纯性
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     V. of CSD and purity.
     V.值上已优于国外同类产品。
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  purity
Starting with isovanillin, a two-step sequence involving reductive amination and N-benzylation was performed to provide the compounds in good purity.
      
After the crude product is recrystallized from tetrahydrofuran (THF), the final product is obtained with purity above 99%.
      
The polycrystalline materials of SrWO4 were synthesized by means of a solid phase reaction with analytical purity SrCO3 and WO3 at high temperature.
      
The purity of CPS-0 was determined by HPLC and the structure was elucidated by monosaccharide composition analysis, methylation analysis, GC, GC-MS, NMR spectral (1H-NMR, 13C-NMR, HMQC), UV, IR, and elemental analysis.
      
After AACH has been calcined at 1200°C for 2 h, the ultrafine α-Al2O3 with uniform particle size, spherical shape, and more than 99.97% purity is obtained and its powder is well dispersed.
      
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An addition product which is very likely a β-sultone was obtained from the spontaneous reaction between chlorotrifluoroethylene and sulfur trioxide as a distillable colorless liquid (Ia+Ib; b. p. 76.0—76.5°, n_D~(20°) 1.3672, d~(21.8°) 1.71). Its structure was elucidated by elementary analysis, determinations of molecular weight and saponification equivalent, and its infrared spectrum. Preliminary studies of its chemical behavior are also here reported.Similarly, from the reaction of sulfur trioxide with 4,...

An addition product which is very likely a β-sultone was obtained from the spontaneous reaction between chlorotrifluoroethylene and sulfur trioxide as a distillable colorless liquid (Ia+Ib; b. p. 76.0—76.5°, n_D~(20°) 1.3672, d~(21.8°) 1.71). Its structure was elucidated by elementary analysis, determinations of molecular weight and saponification equivalent, and its infrared spectrum. Preliminary studies of its chemical behavior are also here reported.Similarly, from the reaction of sulfur trioxide with 4, 5-dichloroperfluoropentene1 (IV), 4, 6, 7-trichloroperfluoroheptene-1 (V)、4, 6, 8, 9-tetrachloroperfluorononene-1 (VI) and 4, 6, 8, 10, 11-pentachloroperfluoroundecene-1(VII) compounds were also obtained namely; (VIII) (b. p. 79.8—80.0°/63.7mm, n_D~(22.2°) 1.3642)、(IX) (b. p. 56°/0.17 mm, n_D~(20.5°) 1.3800)、(X) (b. p. 81—82°/0.08 mm, n_D~(20°) 1.3893)、 and (XI) (b. p. 115—116°/0.40 mm, n_D~(20°) 1.3949). The yields ranged between 70% and 80%.The addition of sulfur trioxide to 4, 4-dichloropernuorobutene-1 and 2,3-dichloroperfiuorobutene-2 yielded products of lesser purity. From the same reactions, the formation of products which possibly were the carbyl sulfates of these two butenes were noted. The products obtained from the reaction of sulfur trioxide with 1, 2-dichloroperfluoroethene and perfluoropropene were mixtures.

本文报告三氧化硫和氯三氟乙烯的加合反应,以及由此而得的一衍生物。各种定量分析、化学反应和光谱结果指示最合理结构是一个四员杂环的β-磺内酯(Ia+Ib)。对于这一个衍化物的化学性能,也作了初步的研究。同样的,从液体三氧化硫与4,5-二氯全氟戊烯-1、4,6,7-三氯全氟庚烯-1、4,6,8,9-四氯全氟壬烯-1、4,6,8,10,11-五氯全氟十一烯-1的加合反应产物内,经分馏后也可以得到颇为纯粹的同类衍化物(β-磺内酯),产率为70—80%。4,4-二氯全氟丁烯-1以及2,3-二氯全氟丁烯-2与三氧化硫反应后所得的产物则不甚纯净;1,2-二氯二氟乙烯以及全氟丙烯与三氧化硫的反应产物则更不纯净。

In the presesnt paper, two methods for the determination of rare earth impu-rities ia "purified" cerium are described. (1) The sample to be analyzed is converted into chlorides (concentration 10mg CeO_2/ml and acidity 1: 19 HCl). Transfer a drop of the prepared solution tothe flat top of graphite electrode previously treated with liquid paraffin. The elec-trodes are dried on a hot plate and then excited in an A. C. arc (220 V, 5 Amp).Spectrograph, ISP--51 (with UF-85 autocollimating camera tube). Slit, 0.01...

In the presesnt paper, two methods for the determination of rare earth impu-rities ia "purified" cerium are described. (1) The sample to be analyzed is converted into chlorides (concentration 10mg CeO_2/ml and acidity 1: 19 HCl). Transfer a drop of the prepared solution tothe flat top of graphite electrode previously treated with liquid paraffin. The elec-trodes are dried on a hot plate and then excited in an A. C. arc (220 V, 5 Amp).Spectrograph, ISP--51 (with UF-85 autocollimating camera tube). Slit, 0.01 mm.Photographic plate, NIKFI Ⅱ. Using the line pairs (La 4333.74)/(Ce 4330.90'), (Pr 4225.33)/(Ce 4229.63'), (Nd 4061.09)/(Ce 4057.30) and (Y 4374.94)/(Ce 4376.88')La, Pr, Nd & Y can be determined quantitatively in the concentration ranges0.055--0.62%, 0.089--1.29%, 0.052%--0.59% and 0.025--0.40% respectively. Theroot mean square deviations of single determination amount to ±4.7%, ±10.8%,±7.0% and ±7.0% respectively. (2) For cerium samples of high purity, ether extraction is used to removemost of the cerium so that the rare-earth impurities can be concentrated. Becauseof its relatively simple spectrum, the element Y has been used as carrier and in-ternal standard. The concentrate, also in the form of chloride solution (concentration1 mg rare-earth oxides/ml), is excited and photographed by the same method asmentioned in (1) The line pairs used are: (La 4238.38)/(Y 4235.73'), (La 3988.52)/(Y 3951.60'), (Pr 4222.98)/(Y 4235.73) and (Nd 4232.38)/(Y 4235.73')With a sample of 100 mg (1 mg Y_2O_3 added as internal standard), the analyticalsensitivities reach 0.01%, 0.025% and 0.028% for La, Pr and Nd respectively. Theerror of the method amounts to about ±10%.

本工作报告铈中杂质镧、镨,钕及钇的两种光谱测定方法。(1)将试样的氯化物溶液滴于经液体石腊处理过的碳电极上,干燥后以交流电弧激发进行摄谱。采用线对 La 4333.74/Ce 43330.90,Pr 4225.33/Ce4229.63,Nd 4061.09/Ce 4057.30及Y 4374.94/Ce 4376.88时测定灵敏度分别可达0.055%,0.089%,0.052%,0.025%。单次摄谱的均方误差分别为±4.7%,±10.8%,±7.0%及±7.0%。 (2)对于较纯的铈,则采用乙醚萃取先行分离,以浓缩其中所含的杂质,并采用谱线较少的元素钇作内标及载体,以补偿分离过程中损失。浓缩物仍以氯化物溶液状态用上述的激发方法进行摄谱。采用下列线对: La 4238.38/Y 4235.73,La 3988.52/Y 3951.60,Pr 4222.98/Y 4235.73,Nd 4232.38/Y 4235.73取样100毫克时,镧、镨及钕的测定灵敏度分别可达0,01%;0.025%及0.028%。一般误差约在±10%左右。

Design data for high purity toluene recovery from platformate by extractive distillation with phenol, were obtained by a pilot plant study. The extractive distillalations column, 200mm in diameter, possessed 44 bubble cap plates and had a Capacity o?processing 250 kilograms of feed per day. The platformate was first prefractionated to 70-117℃, which contained 0.8% benzene and 48% toluene by weight. The heart cut was then used as the feed for the extractive distillation. The recommended operating conditions...

Design data for high purity toluene recovery from platformate by extractive distillation with phenol, were obtained by a pilot plant study. The extractive distillalations column, 200mm in diameter, possessed 44 bubble cap plates and had a Capacity o?processing 250 kilograms of feed per day. The platformate was first prefractionated to 70-117℃, which contained 0.8% benzene and 48% toluene by weight. The heart cut was then used as the feed for the extractive distillation. The recommended operating conditions were as follows: phenol/feed ratio, 4; reflux ratio, 4-5; feed temperature, 120℃; phenol inlet temperature, 130℃. The actual plates of rectifying, stripping and phenol recovery section were 19, 20 and 5 respectively. The recovery of nitration grade toluene from the feed was 97-98%. When losses in prefractionation, acid washing and redistillation were included, the net recovery of toluene from the platformate was 93%. The result of this study gave the data for designing of full scale production plants.

为了提供以苯酚为溶剂用抽提蒸馏法从铂重整生成油中抽取纯甲苯的工业装置设计依据和操作条件,进行了日处理量为250公斤的中型试验。抽提蒸馏塔为一直径200毫米,拥有44个塔盘的泡帽塔。铂重整生成油先经预分馏切割成70—119℃馏份,其中苯含量为0.8%(重量),甲苯含量为48%(重量)。然后将该馏分进行抽提蒸馏,合理操作条件为酚油比4:1(体积比);回流比4.5;油进口温度120℃;酚进口温度130℃。精馏段塔盘数为19,汽提段塔盘数为20,酚回收段塔盘数为5。产品经酸碱洗涤和再蒸馏后为硝化级纯度的甲苯,抽提蒸馏的甲苯收率可达97—98%(重量)。如包括预分馏损失,则甲苯的收率为96%(重量)。酸碱洗涤和再蒸馏损失一般可按3%计,因此,纯甲苯净收率为93%(重量)。试验结果提供了工业装置的设计数据。

 
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