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The direct amperometric titration of amines with sodium tetraphenylborate solution based upon anodic depolarization at a dropping mercury electrode by the use of excess TPB titrant, was systematically investigated. The influence of various factors such as pH, volume of titration mixture, quantity of sample in a definite volume to be titrated were studied. Based upon the above observations, a method is proposed as follows: Pipette 0.5-2.0 ml (at a concentration of about 2×10~(-2)M) of samples of various... The direct amperometric titration of amines with sodium tetraphenylborate solution based upon anodic depolarization at a dropping mercury electrode by the use of excess TPB titrant, was systematically investigated. The influence of various factors such as pH, volume of titration mixture, quantity of sample in a definite volume to be titrated were studied. Based upon the above observations, a method is proposed as follows: Pipette 0.5-2.0 ml (at a concentration of about 2×10~(-2)M) of samples of various amines into a 50 ml beaker and add 1% HAc to make a volume of about 10-20 ml. The dropping mercury electrode serves as the polarographic anode. Titrate the amines with 0.05 M standard Na-TPB solution (pH 8) at 0.18 V using the saturated NaCl bridge and S.C.E. as reference. After each addition, stir for one minute and allow the solution to obtain a steady current value, then record the galvanometric reading. The end point is graphically plotted with current versus milliliters of titrant; sharp breaks are obtained. The Na-TPB solution was standardized volumetrically by the standard mer- curic solution. Organic bases so determined include aniline, methyl aniline, diethylamine, ephedrine hydrochloride, dimethylaniline, trimethylamine hydrochloride, triethylamine hydrochloride, urotropine, and tetraethylammonium iodide. The relative error of this method is 2%. The more soluble salts of aliphatic primary amines such as methylamine, ethyl- amine, n-butylamine, and even in the case of ephedrine hydrochloride could not be ac- curately titrated. The application of this method to titrate the amines depend largely upon the structure of the amines and the solubility of amine-TPB salts. This method was also successfully applied to titrate the nitrogen containing drugs such as chlopromarzine, cinchophene, quinine sulphate, atropine sulphate, antipyrine, aminopyrine, rivanol, and strychnine. 本文研究了用pH8的四苯硼酸钠水溶液对胺类的直接电流滴定法.滴汞为阳极,饱和甘汞为阴极,以3%琼脂的饱和NaCl溶液为盐桥组成电解池.适宜的滴定条件是:外加电压+0.18伏;底液为pH 2-3的HAc-NaAc介质,而以1%HAc更为方便;滴定体积为10-20毫升.可测的浓度范围和胺类的四苯硼酸盐沉淀的溶解度有关:仲胺为1×10~(-3)-2×10~(-2M);叔胺为6×10~(-4)-2×10~(-2)M;季胺为4×10~(-4)×10~(-3)M;伯胺类不能测定.方法的相对误差因沉淀的溶解度而异,一般在2%以下.滴定时沉淀可不必分离,且无需除氧,操作步骤比较简易. In this paper, it is shown that a c oscillopolarographic titration can be applied advantageously to titrate neostigmine methyl sulfate by sodium tetraphenylborate(NaTPB).NaTPB is added to precipitate quantitatively, neostigmine methyl sulfate from aqueous solution. Filter part of the mixture, and the excess of NaTPB in the filtrate is titrated by thallous sulfate standard solution, using the disappearance of the incision of NaTPB on dE/dt—E curve to indicate the end point of titrations. The recovery was... In this paper, it is shown that a c oscillopolarographic titration can be applied advantageously to titrate neostigmine methyl sulfate by sodium tetraphenylborate(NaTPB).NaTPB is added to precipitate quantitatively, neostigmine methyl sulfate from aqueous solution. Filter part of the mixture, and the excess of NaTPB in the filtrate is titrated by thallous sulfate standard solution, using the disappearance of the incision of NaTPB on dE/dt—E curve to indicate the end point of titrations. The recovery was 99.3~100.2%. Ten determinations on the same samplegave a relative standard deviation of ±0.42%. The method is accurate, rapid and Simple, much superior to the official method adopted now. 交流示波极谱滴定可有效地应用于四苯硼钠滴定甲基硫酸新斯的明。先加入四苯硼钠,使之与新斯的明产生沉淀,然后以硫酸亚铊标准溶液滴定多余的四苯硼钠。以dE/dt—E曲线上四苯硼钠切口的消失为终点。用此法测定了注射液中新斯的明含量,回收率为99.3~100.2%,十次测定的相对标准偏差为0.42%。远较药典方法方便、快速。 A PVC membrane sodium ion-selective microelectrode based on a neutral carrier(ETH 1097)has been constructed. The tip diameters of around 2. 5μm as well as the selectivity coefficients in respect to K~+,Mg~(2+)and Ca~(2+)allow the intracellular measurement of sodium ion activities. The response is linear in the range 10~(-3)to 5×10~(-1)M Na~+ giving a slope of 58. 2 mV(25'℃). The performance of electrode plasticized by dibutylsebacate (DBS)has been compared with that of electrode plasticized by dioctylphthalate(DOP).... A PVC membrane sodium ion-selective microelectrode based on a neutral carrier(ETH 1097)has been constructed. The tip diameters of around 2. 5μm as well as the selectivity coefficients in respect to K~+,Mg~(2+)and Ca~(2+)allow the intracellular measurement of sodium ion activities. The response is linear in the range 10~(-3)to 5×10~(-1)M Na~+ giving a slope of 58. 2 mV(25'℃). The performance of electrode plasticized by dibutylsebacate (DBS)has been compared with that of electrode plasticized by dioctylphthalate(DOP). The change in performance caused by adding sodium tetraphenylborate(NaTBP)or NaSCN to membrane has been studied. The sensitive membrane containing DBS and appropriate amount of NaTPB is suitable for intracellular measurements. 研制了以中性载体(ETH1097)为电活性物质的PVC钠离子选择性微电极。电极尖端直径小至2.5μm,线性响应范围10~(-3)-5×10~(-1)MNa~+,检测下限1.2×10~(-4)M,斜率为58.2mV(25℃).对K~+,Mg~(2+)、Ca~(2+)的选择性系数分别为0.050,6.5×10~(-4)及5.5×10~(-3)。该微电极特别适用于细胞内钠离子活度的测量。实验探讨和比较了癸二酸二丁酯(DBS)和邻苯二甲酸二正辛酯(DOP)为增塑剂的钠微电极的性能。研究了四苯硼钠(NaTPB)和硫氰酸钠(NaSCN)加入膜中后,电极性能的变化。为用于细胞内及临床微量试样中钠离子活度测量,电极采用DBS为增塑剂,并加入适量的NaTPB较宜。
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