毛细管气相色谱法定量分析异菌脲

采用气相色谱法,以邻苯二甲酸二戊酯为内标物,选用DB-35毛细管色谱柱,对异菌脲进行定量分析,柱箱采用程序升温,180℃保持1.0min,以20℃/min速率升至270℃,保持5.0min;进样口温度280℃,检测器(FID)温度280℃,气体流速为载气(氮气)10.0 mL/min,燃气(氢气)30 mL/min,助燃气(空气)300 mL/min,分流比10:1.方法的变异系数0.34%,平均回收率99.98%,标准偏差为0.171,线性相关系数为0.9994.     

乙二醇单甲醚合成液的气相色谱分析

用气相色谱法对乙二醇单甲醚合成液进行跟踪分析.采用φ3 mm×1 m[m(改性PEG20M)∶m(酸洗硅烷化201担体)=10∶100]不锈钢柱;升温程序∶60℃(2 min)6℃/min 160℃(20 min),H2=50mL/min,N2=50 mL/min,AIR=400 mL/min;汽化室温度250℃,检测室温度250℃.建立了一种简便,快速,准确的乙二醇单甲醚合成液中各组分的测定方法.该方法各主产物与原料能达到基线分离,难分离物质对达到峰谷分离.多次测定结果的相对误差是0.27%,相对标准偏差是0.82%(以乙二醇单甲醚计),分析时间小于30min,适合于生产中的控制分析.     

茚虫威在蔬菜中残留量的气相色谱法测定

建立了蔬菜中茚虫威残留量定量检测的气相色谱法.对分析方法的适合性测定结果表明,样品经乙腈提取,氧化铝柱层析净化,以DB-1701毛细管柱为色谱柱,氮气为载气,气化室温度240 ℃,检测器温度300℃,柱温150℃(0.2 min)程序升温(20℃/min)至260℃(10 min),外标法定量的条件进行GC-ECD测定.方法在0.01～1.0 mg/L范围内,相关系数(r2)为0.9998;最小检测量为0.01 ng,最低检出质量浓度为0.005 mg/L;平均添加回收率为86.6%～92.2%,相对标准偏差(RSD)为113%～5.9%.     

气相色谱法测定乳康颗粒中乙酸辛酯的含量

建立乳康颗粒中乳香有效成分乙酸辛酯含量的检测方法.运用安捷伦色谱柱DB-WAX(30 mm×0.32 mm×0.50μm)和FID检测器(氢火焰离子化检测器),在检测器温度为300℃,气化室温度为290℃,色谱柱初始温度为50℃,维持1 min,以10℃/min的速率升至200℃,保持8 min,气体流量为氮气30.0...     

毒死蜱和氯氰菊酯的毛细管气相色谱分析

采用毛细管气相色谱法 ,以癸二酸二正丁酯、癸二酸二正辛酯为内标 ,对毒死蜱和氯氰菊酯的复配乳油进行了定量分析。气相色谱条件为 :30m× 0 .32mm (i.d .) ,膜厚0 2 5 μm(SE 5 4固定液 )熔融石英毛细管柱 ,柱温 :初始 2 0 5℃保持 6min ,以 2 5℃ /min速率升至 2 5 5℃保持 7min ,检测器、汽化室温度为 30 0℃ ,载气 (N2 )的流速为 2mL/min ,分流比 1∶5 0 ,尾吹 30mL/min。该方法检测毒死蜱和氯氰菊酯含量 (质量分数 )的标准偏差分别为 0 .2 8和 0 .0 19,平均相对标准偏差 (RSD) (n =5 )分别为 0 .33%和 0 .85 % ,平均回收率 (n =5 )分别为 10 0 %和 10 0 .2 %。该方法操作简便 ,定量准确     

反应条件对煤-油共炼产物性质的影响

以鄂尔多斯煤及加氢后的煤焦油为原料,采用自制的煤载铁系催化剂,在高压釜内进行煤-油共炼反应,考察反应温度(380℃,400℃,420℃,440℃和460℃)、反应时间(20 min,40 min,60 min和80 min)及氢初压(2 MPa,4 MPa,6 MPa和8 MPa)对煤-油共炼液收率、液体产物馏程及半焦...     

高频涡流线圈用高温绝缘抗开裂涂料的研制

研制了一种可用于高频涡流线圈电阻丝(铂金丝)的有机硅高温绝缘抗开裂表面涂料,涂膜的抗开裂性能优异.试验证明,在经过-60℃条件下通电(电源频率:400 Hz,115 V)4min,断电2 min,10个循环后表面完好.通电过程中线圈最高温度可达到400℃,涂料最高可耐600℃,电击穿强度大于50 kV/mm,体积电阻率大于1012(Ω·cm).     

飞灰在热处理过程中汞的逸出特性

采用安大略水法(OHM)对采自广州珠江电厂(1#)和广州石化总厂第一电场、第二电场(2#、3#)的燃煤飞灰在热处理过程中逸出的零价汞(Hg0)和二价汞(Hg2+)进行分析,选取不同温度(200℃、400℃、600℃、800℃、1000℃)、时间(30min、60min、90min、160min)测定Hg2+和Hg0的逸出量。结果表明:每克飞灰在加热过程中Hg2+的逸出量为1.955～669.87ng,Hg0的逸出量为14.53～3501.15ng。在加热60min后,两种形态的汞几乎完全逸出,Hg2+在600℃时逸出量达到最大(3#除外),Hg0在400℃时逸出量达到最大。在飞灰热处理过程中,汞的逸出量与飞灰所含的未燃尽炭量成正比关系。     

退火时间及温度对聚乳酸结晶性能的影响

从制品后期处理方面,对聚乳酸(PLA)制品的退火时间和退火温度进行调控,采用广角X射线衍射仪(WAXD)、差示扫描量热仪(DSC)、偏光显微镜(POM)分析了不同退火条件对PLA结晶性能的影响。结果表明,退火能够促进PLA结晶,且退火温度和退火时间都不会改变PLA的晶型。退火温度在110℃时,PLA晶体的晶核密度及生长速率最大,退火时间对PLA结晶的影响较小。退火时间为30 min时,退火温度在90、100、110、120℃下PLA的结晶度(X_c)比未退火的PLA分别增大了25.05%、27.26%、32.72%、28.69%,在退火温度为110℃时,退火10、30、60 min下PLA的X_c比未退火的PLA分别增大了31.76%、32.72%、34.3%。在110℃下退火30 min的PLA晶体完全熔融耗时3.6 min,比90℃下退火30 min的PLA慢1.2 min.     

SiC晶须的微波加热合成

首先以硅溶胶(w(siO2)=30%,平均粒径为10～20 nm)和活性炭(平均粒径<10um,w(C)=99.5%)为原料,六偏磷酸钠为分散剂,混匀后在真空下于110℃烘干24 h制成反应前驱体,然后将其破碎成不同粒度的细粉,在多模谐振腔微波炉中分别加热至1 300～1 600℃保温15～60 min制备了SiC晶须,研究了热处理温度、保温时间以及反应前驱体的粒度对晶须产率的影响.结果表明:(1)当热处理温度为1 300～1 400℃时,产物主要为方石英及少量β-SiC,SiC晶须的产率较低;温度达到1 500℃以后,产物主要为SiC晶须及少量SiC颗粒,且在1 500℃下保温时间从15 min延长到30 min时,SiC晶须产率显著增加;温度提高到1 600℃时,生成了等轴SiC颗粒及SiC晶须.(2)1 500℃保温30 min为比较适合的微波加热合成条件,晶须产率能达到80%以上.(3)较小的反应前驱体颗粒有利于SiC晶须的生成.     

B.t.β-环糊精包合物的制备及其杀虫效果

制备出苏云金芽孢杆菌（B．t．）β-环糊精包合物,并对包合物进行了差热分析,证明B．t．原粉被β-环糊精包合。室内生物活性测定结果表明,当B．t．原粉与β-环糊精质量比为0．5：2时,包合物对棉铃虫2龄幼虫的杀虫活性最高,确定包合物中B．t．原粉与肛环糊精的最佳质量比为0．5：2。盆栽药效试验结果表明,当B．t．原粉制成环糊精包合物后,与B．t．原粉和B．t．制剂相比,对小菜蛾的防效明显提高。药剂处理后1、3、7d,B．t．环糊精包合物对小菜蛾的防效分别为41．67％、61．54％和60．00％,而B．t．原粉和制剂的防效分别为23．61％、38．46％、32．00％和31．94％、52．31％、46．00％。     

Refractory compounds of basic composition for the monolithin lining of steel-teeming ladles

Conclusions Questions of the method of production of basic ramming compounds at Panteleimonovka Refractory Plant and their use in the monolithic lining of the walls of 160-ton steel-teeming ladles of the No. 2 Converter Shop of Kirvoi Rog Steel Combine are considered.An analysis of the wear of the lining during service showed that it occurs as the result of spalling of the sintered zone and salamandering of the lining. The use of a movable thermally insulated lid made it possible to hold the temperature of the ladle lining within limits of 730–1120°C between heats and to obtain a basic rammed lining life of 21–39 heats as opposed to an average life for the shop of 14.8 heats.A reserve for increasing the ladle basic lining life is optimization of the thermal conditions of its service, including high-temperature heating of the lining before pouring of the metal, the use of thermally insulated lids with the minimum consumption of time for placing of them, an increase in the life of the well refractory to the life of the walls and bottom, and elimination of cooling of the lining between heats.A Discussion: Problems of the Production and Use of Refractories for the Lining of Steel-Teeming Ladles. [For the start of the discussion see No. 8 (1988) and for the continuation Nos. 9–12 (1988) and Nos. 1–3, 5, and 7 (1989).]Deceased.I. I. Glaka, N. F. Drobot, N. V. Kurmaz, B. P. Zinchenko, S. A. Poznyak, I. M. Ryaboshapkin, V. V. Slushko, A. A. Chulkov, Yu. Bormatov, S. I. Vanchyuk, V. I. Dobrovol'skii, B. G. Zhuravel', N. I. Kiyan, L. I. Nekrasov, N. M. Sokolov, P. V. Khomenko, G. A. Nikitenko, S. Dorgobuzov, P. I. Valiev, N. N. Gorbatko, V. I. Kovalenko, and M. I. Lyakhov of Krivoi Rog Steel participated in the preparation and tests of the basic monolithic linings.Translated from Ogneupory, No. 8, pp. 1–4, August, 1989.     

国外生物降解聚合物的种类及主要组分

据１９９６～１９９８年国外有关文献的汇集,由美,日,德等国主要研制,生产的生物降解聚合物种类为：１,单一型生物降解聚合物;（１）合成酯（酸）类;（２）淀粉基材料;（３）天然高分子材料;２、复合型生物降解聚合物;（１）不同种类的烃基互聚物;（２）烃酯（酸）／聚酯（３）脂肪族聚酯／芳香族聚酯共聚物;（３）淀粉基复合型,（５）光／生物降解聚合物;３、可生物降解水溶性聚合物。     

Book Reviews

Physico-Chemical Basis of Formation of Non-Woven Materials, V. 6. Tikhomirov, Legkaya lndustriya Publ. Moscow 1969. 328 pp. Rub. 2.29.

ADHESIVES FOR METALS. THEORY AND TECHNOLOGY, Nicholas J. DeLollis. Industrial Press Inc., New York 1970. 230 pp. $15.00.     

九种致癌染料剥色工艺的优化

针对纺织品上可能存在的九种致癌染料(C.I.酸性红26、C.I.分散橙11、C.I.分散黄3、C.I.分散蓝1、C.I.直接蓝6、C.I.直接黑38、C.I.直接红28、C.I.碱性红9、C.I.碱性紫14),本文研究并比较了不同剥色工艺对不同致癌染料剥色效果的影响.并提出选用加入尿素的甲醇作为剥色剂,使用超声功率为100W的超声波在70℃处理30分钟可以获得比较理想的剥色效果.     

The ruthenium(VIII)-catalysed oxidation of Illinois No. 6 bituminous coal: An application of g.c.-FT-i.r. spectroscopy for structural analysis

The oxidation of Illinois No. 6 coal proceeds readily with ruthenium(VIII) to provide a mixture of aliphatic and aromatic carboxylic acids. The acids were converted into their methyl esters for analysis by g.c.-m.s. and g.c.-FT-i.r. spectroscopy. Mono-, di-, tri- and tetracarboxylic acids are the principal products of the oxidation of this bituminous coal. The g.c.-FT-i.r. approach has enabled the detection of several different lactones that have not been observed previously. The results imply that cyclic ethers are present in low abundance in Illinois coals.     

Analysis of upgraded SRC-11 and H-coal liquid products

Upgraded coal-derived liquids obtained from catalytic hydroprocessing of SRC-11 and H-coal syncrudes have been studied by i.r., p.m.r., g.c.-m.s., and silica gel chromatography. With increase in residence time, nitrogen, oxygen and aromatics decrease, while naphthenes increase substantially. All the upgraded liquids show low viscosity at 298 K (1.3–1.4 mN s m^?2), even though saturate and aromatic fractions varied with processing severity. In the aromatic-1 fraction, 1 -ring aromatics increase, and 3-ring aromatics decrease, with increase in severity of hydroprocessing. G.c.-m.s. analyses indicate a marked qualitative similarity for saturate and aromatic fractions irrespective of syncrude source. Only the heavier end of the aromatic-1 fraction is noticeably different. Tentative identifications based on m.s. and g.c. retention times are made for most of the significant components. 600 M Hz p.m.r. spectra of the upgraded SRC-11 and H-coal liquids appear identical, but the n.m.r. difference technique revealed slight differences between the two liquids in concentrations of certain species.     

Characterization of coals and coal oxidation by magic-angle 13C n.m.r. spectroscopy

Magic-angle ¹³C n.m.r. spectra have been obtained for a series of vitrinite concentrates. Proper modification of the cross-polarization pulse sequence allows separation of protonated and nonprotonated carbon resonances. This technique is used to determine the relative fraction of nonprotonated aromatic carbons for each of the vitrinites, a parameter observed to decrease with increasing rank. Another parameter, related to the aromatic hydrogen content, is also calculated from these data and the results correlate with those from Fourier transform i.r. spectroscopy. The methods used for analysis of the vitrinite concentrates were then applied to the low-temperature oxidation of coal. The fractional aromaticity as determined by n.m.r. increases with longer oxidation times, indicating preferential attack on aliphatic structures. Here the FT-i.r. results are in quantitative agreement with those from n.m.r. Finally, the advantages of using various pulse sequences to extend the range of magic-angle n.m.r. and of combining FT-i.r. and n.m.r. results are discussed in the context of their potential for coal science.     

Mechanical properties of zirconium dioxide single crystals intended for structural applications

Conclusions New structural materials (single crystals obtained from partially stabilized zirconium dioxide) were studied. It was established that their physical and mechanical properties are certainly comparable to those of the other structural materials. We obtained new information regarding the mechanical behavior of the single crystals of zirconium dioxide that would facilitate further development of the technology of these materials and guide the studies on the mechanisms of their resistance to mechanical forces under different loading conditions.Translated from Ogneupory, No. 8, pp. 14–17, 1991.The authors wish to thank V. I. Aleksandrov, M. A. Vishnyakov, Yu. K. Voron'ko, and V. F. Kalabukhov for participating in the research work concerning crystal growth and V. I. Galenko, A. V. Drozdov, A. V. Cheboryukov, and A. I. Fesenko for carrying out mechanical testing.     

NMR- und UV-VIS-Spektroskopische Untersuchungen an Push-pull-Butadienen

N.M.R. and U.V.-VIS Spectroscopic Investigations on Push-pull Butadienes ¹³C-n.m.r., d-n.m.r. and u.v.-vis spectroscopical data show that the push-pull character of the investigated butadienes is lowered by substitution at the carbon atom in 3-position of the butadiene chain.