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双波长和三波长分光光度法同时测定乙醛酸和乙二醛 总被引:10,自引:0,他引:10
利用醛基的成肟反应,用双波长法,三波长法同时测定乙醛酸、乙二醛的含量。它们的回收率分别为100.9%-102.3%(n=6)和96.8%-103.0%(n=11)。 相似文献
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离子对高效液相色谱法分析注射用新灭菌 总被引:1,自引:1,他引:1
建立了离子对高效液相色谱法分离与测定复方制剂(新灭菌)中的羟氨苄青霉素及氟氯青霉素含量法。采用C8.10μm,4.6×200mm柱(大连化物所Spherisorb),以含1.4%十六烷基三甲基溴化铵的pH6.5磷酸盐缓冲液-乙腈(68+32)为流动相,在紫外检测器254nm波长处检测,线性范围为0.25~2mg/mL,r=0.9999(n=5),羟氨苄青霉素及氟氯青霉素平均回收率分别为99.5%及100.7%(n=5)。精密度:羟氨苄青霉素及氟氯青霉素日内(4h)平均RSD(相对标准偏差)均为0.8%(n=15),日间(2h)平均RSD分别为0.6%和0.7%(n=3)。 相似文献
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烟草中Fe,Co一阶导数分光光度法同时测定的研究 总被引:4,自引:0,他引:4
本文研究了在pH4.0时,meso-四(4-磺酸基苯基)卟啉与铁、钴同时络合显色的反应条件以及一阶导数光谱行为。此体系一阶导数的灵敏度比零阶导数灵敏度高。Fe ̄(3+)~0.18μg/mL、Co ̄(2+)0~0.24μg/ml,范围内符合比耳定律;检测限为:Fe ̄(3+)=0.48ng/mL,Co ̄(2+)=0.2ng/mL。回收率为:Fe98.5%~100.8%,Co99.2%~101.3%。此方法用于烟草中痕量Fe、Co测定,与AAS值相比较,结果令人满意。 相似文献
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铜(Ⅰ)—苯骈三氮唑络合吸附波的极谱研究与应用 总被引:4,自引:0,他引:4
本文在0.6mol/L NH3-NH4Cl缓冲溶液(pH=9.8)中,Cu(Ⅱ)在滴汞电极上还原生成Cu(Ⅰ),可与苯骈三氮唑(BTA)络合,产生一灵敏的络合吸附波,Ep=-0.73V(us,SCE)。苯骈三氮唑的浓度在0.40-10.0mg/L范围内与极谱波峰高呈线性关系,检测下限为0.40mg/L,相对标准偏差为1.4%-3.2%;回收率为97.5%-101.5%。 相似文献
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病人血样中痕量锗,锶的石墨炉原子吸收光谱法测定 总被引:2,自引:1,他引:2
本文运用石墨炉AAS法加基体改进技术,测定了50岁以上病人血清及环境水样中锗和锶的含量。用0.01mol/LHNO3-0.1%TritonX-100稀释血清,测定精度可与火焰法媲美。锗,锶的特征量分别为28pg和18pg;线性范围为0-250ng/mL和-35.0ng/mL;相对标准偏差(n=10)4.10%和2.49%;回收率分别为92.2%-99.0%和92.0%102%。方法快速准确,结果满 相似文献
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本文研究了阴离子交换树脂从铂系金属混合溶液中使Ph与Pt,Pd,Ir达到定量分离。合适的分离条件是0.5mol.dm^-^3NaCl,pH=2,通Cl2气。Rh的回收率=(100±2)%。 相似文献
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丙烯酸-β-羟乙酯和甲基丙烯酸正丁酯共聚合参数的测定与研究 总被引:1,自引:0,他引:1
用^1H-NMR分析法测定了丙烯酸-β-羟乙酯(M1)和甲基丙烯酸正丁酯(M2)的共聚物组成,用Mayo-Lewis模型的误差变量法计算出不同温度下该体系的溶液聚合的竞聚率,分别为r1=0.63,r2=1.17(60℃);r1=0.61,r2=1.01(80℃);r1=0.61,r2=0.97(100℃);r1=0.70,r2=1.03(120℃);r1=0.68,r2=0.88(140℃)和r1=0.66,r2=0.86(160℃)。根据Arrhenius方程计算获得了体系均聚、共聚反应频率因子之比Aii/Aij和活化能之差Eii-Eij,并讨论了溶剂、氢键对共聚合单体活性的影响。 相似文献
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毛细管气相色谱法测定速效伤风胶囊中对乙酰氨基酚、咖啡因、马来酸氯苯那敏的含量 总被引:3,自引:0,他引:3
用5%Ph-Me-Silicone毛细管色谱柱,FID,二阶程序升温,以正十六烷作为内标物测定速效伤风胶囊中对乙酰氨基酚、咖啡因、马来酸氯苯那敏的含量。浓度线性范围:对乙酰氨基酚4~20g/L,咖啡因0.084~0.42g/L,马来酸氯苯那敏0.15~0.75g/L。平均回收率(n=5):对乙酰氨基酚99.62%(RSD=0.44%)咖啡因96.46%(RSD=1.32%),马来酸氯苯那敏98.55%(RSD=0.65%)。 相似文献
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研究了用HPLC 测定兔眼玻璃体和房水中维拉帕米含量的方法。用丙咪嗪为内标, 采用Spherical C18色谱柱分离, 以甲醇- 0 .04 mol/L 醋酸铵- 乙腈- 二乙胺( 体积比1 ∶1 ∶0 .5 ∶0 .02) 为流动相, 检测波长为278nm 。样品用正己烷- 异丁醇提取后进样, 分析速度快。 样品及内标的保留时间分别为4 .63 min 及9 .23 min ; 线性范围为2 .5 ~100 mg/L, 相关系数r 为0 .999 7 。方法的回收率为100 .3 % ( n = 5) ,RSD 为3 .63% , 日内RSD 为0 .5 % ~3 .61 % , 日间RSD 为3 .75 % ~4 .80 % , 最低检测质量浓度为0.25 mg/ L。 应用该法测定了创伤家兔玻璃体和房水中维拉帕米浓度的变化。 相似文献
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Reactions in droplets in microfluidic channels 总被引:5,自引:0,他引:5
Fundamental and applied research in chemistry and biology benefits from opportunities provided by droplet-based microfluidic systems. These systems enable the miniaturization of reactions by compartmentalizing reactions in droplets of femoliter to microliter volumes. Compartmentalization in droplets provides rapid mixing of reagents, control of the timing of reactions on timescales from milliseconds to months, control of interfacial properties, and the ability to synthesize and transport solid reagents and products. Droplet-based microfluidics can help to enhance and accelerate chemical and biochemical screening, protein crystallization, enzymatic kinetics, and assays. Moreover, the control provided by droplets in microfluidic devices can lead to new scientific methods and insights. 相似文献
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The toxicity of inorganic trivalent arsenic for living organisms is reduced by in vivo methylation of the element. In man, this biotransformation leads to the synthesis of monomethylarsonic (MMA) and dimethylarsinic (DMA) acids, which are efficiently eliminated in urine along with the unchanged form (Asi). In order to document the methylation process in humans, the kinetics of Asi, MMA and DMA elimination were studied in volunteers given a single dose of one of these three arsenicals or repeated doses of Asi. The arsenic methylation efficiency was also assessed in subjects acutely intoxicated with arsenic trioxide (As2O3) and in patients with liver diseases. Several observations in humans can be explained by the properties of the enzymic systems involved in the methylation process which we have characterized in vitro and in vivo in rats as follows: (1) production of Asi metabolites is catalyzed by an enzymic system whose activity is highest in liver cytosol; (2) different enzymic activities, using the same methyl group donor (S-adenosylmethionine), lead to the production of mono- and di-methylated derivatives which are excreted in urine as MMA and DMA; (3) dimethylating activity is highly sensitive to inhibition by excess of inorganic arsenic; (4) reduced glutathione concentration in liver moderates the arsenic methylation process through several mechanisms, e.g. stimulation of the first methylation reaction leading to MMA, facilitation of Asi uptake by hepatocytes, stimulation of the biliary excretion of the element, reduction of pentavalent forms before methylation, and protection of a reducing environment in the cells necessary to maintain the activity of the enzymic systems. 相似文献
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Electrochemistry is one of the most advanced techniques for monitoring neurochemical activities in the living brain because electrochemical approaches bear the advantageous features of high spatial and temporal resolutions, which facilitate its tremendous potential in investigating the highly spatially heterogeneous brain system and the fast dynamics of neurochemical activities. On the other hand, since brain is the most complicated organ in the sense of its numerous kinds of neurochemical species, high selectivity is always required for any analytical methods that approach the brain. In this review, we will discuss various electrochemical methodologies to achieve selective detection of neurochemicals in mammalian brain and the strategies developed mainly by our group towards selective monitoring of both electrochemically active and inactive neurochemicals. At the end, we will discuss possible solutions towards brain mapping of neurochemical species and combination of neurochemical detection strategy with electrophysiology as the direction of future development of electroanalysis in living brain. 相似文献
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G. den Boef 《Fresenius' Journal of Analytical Chemistry》1981,305(2):127-129
Summary At the session of the WPAC of Fechem on education in analytical chemistry it was concluded that it is now essential to include chemometrics and basic knowledge of computers in all courses on analytical chemistry.
Tendenzen in der analytisch-chemischen Ausbildung
Zusammenfassung Bei einer Tagung der WPAC über die Lehre auf dem Gebiet der analytischen Chemie wurde bei der Betrachtung neuer Aspekte festgestellt, daß vor allem Chemometrie und Grundkenntnisse in Computertechnik in die Ausbildung aufgenommen werden sollten.相似文献
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Ke Min Wojciech Jakubowski Krzysztof Matyjaszewski 《Macromolecular rapid communications》2006,27(8):594-598
Summary: The recently developed initiation system, activators generated by electron transfer (AGET), is used in atom transfer radical polymerization (ATRP) in the presence of a limited amount of air. Ascorbic acid and tin(II ) 2‐ethylhexanoate are used as reducing agents in miniemulsion and bulk, respectively. An excess of reducing agent consumes the oxygen present in the system and, therefore, provides a deoxygenated environment for ATRP. ATRP of butyl acrylate is successfully carried out in miniemulsion and in the presence of air. During polymerization the radical concentration remains constant. The polymerization reaches over 60% monomer conversion after 6 h, which results in polymers with a predetermined molecular weight = 14 000 g · mol−1 and a low polydispersity ( = 1.23). AGET ATRP of styrene is also successful in bulk in the presence of air, as evidenced by linear semi‐logarithmic kinetics, which leads to polystyrene with an of 13 400 g · mol−1 and a low polydispersity index ( = 1.14).