影子
第2楼2009/12/22
我记得论坛哪里有的,一时找不到,试试下面的网址吧:
http://www.verycd.com/topics/2753973/
影子
第3楼2009/12/22
附录Ⅵ B 馏程测定法
馏程系指一种液体照下述方法蒸馏,校正到标准压力[101.3kPa(760mmHg)]下,自开始馏出第5滴算起,至供试品仅剩3~4ml或一定比例的容积馏出时的温度范围。
某些液体药品具有一定的馏程,测定馏程可以区别或检查药品的纯杂程度。
仪器装置 如图。用国产19标准磨口蒸馏装置一套。A为蒸馏瓶;B为冷凝管,馏程在130℃以下用水冷却,馏程在130℃以上用空气冷凝管;C为具有0.5ml刻度的25ml量筒;D为分浸型具有0.5℃刻度的温度计,预先经过校正,温度计汞球的上端与蒸馏瓶出口支管的下壁相齐;根据供试品馏程的不同,可选用不同的加热器,通常馏程在80℃以下时用水浴(其液面始终不得超过供试品液面),80℃以上时用直接火焰或其他电热器加热。
测定法 取供试品25ml,经长颈的干燥小漏斗,转移至干燥蒸馏瓶中,加入洁净的无釉小瓷片数片,插上带有磨口的温度计,冷凝管的下端通过接流管接以25ml量筒为接收器。如用直接火焰加热,则将蒸馏瓶置石棉板中心的小圆孔上(石棉板宽12~15cm,厚0.3~0.5cm,孔径2.5~3.0cm),并使蒸馏瓶壁与小圆孔边缘紧密贴合,以免汽化后的蒸气继续受热,然后用直接火焰加热使供试品受热沸腾,调节温度,使每分钟馏出2~3ml,注意检读自冷凝管开始馏出第5滴时与供试品仅剩3~4ml或一定比例的容积馏出时,温度计上所显示的温度范围,即为供试品的馏程。
测定时,如要求供试品在馏程范围内馏出不少于90%以上时,应使用100ml蒸馏瓶,并量取供试品50ml,接收器用50ml量筒。
测定时,气压如在101.3kPa(760mmHg)以上,每高0.36kPa(2.7mmHg),应将测得的温度减去0.1℃;如在101.3kPa (760mmHg)以下,每低0.36kPa (2.7mmHg),应增加0.1℃。
VI B Determination of Distilling Range
The distilling range of a liquid is the temperature range, corrected for a pressure of 101.3 kPa (760mmHg), within which the liquid distils under the following conditions. The lower limit of the range is the temperature at which the fifth dro-p of condensate leaves the tip of the condenser and the upper limit is the temperature at which all the liquid except 3-4ml has been distilled, or when a specified amount of distillate has been collected.
Distilling range is indicative of the identity and purity of the substance being examined.
Apparatus Use a set of distillation apparatus No. 19, with standard ground joint made in China, A, a distillation flask; B, a condenser, for liquids distilling below 130℃, the condenser is cooled by water, for liquids distilling above 130℃, it is cooled by air; C, a 25ml glass cylinder, graduated in 0.5ml increments; D, a partial-immersion thmometer, graduated in 0.5℃ subdivisions and calibrated. The upper end of the mercury bulb is level with the lower wall of the side-tube of distillation flask. According to different distilling range of the substance being examined, select different heater. For liquids of distilling range below 80℃, a water bath is used as the heater; for liquids of distilling range above 80℃, use an open flame of an electric heater.
Procedure Pour 25ml of the substance being examined into the dried distillation flask through a dry funner with a long stem. Add a few enamel-free porcelain fragments and inser* the thermometer with ground joint. Attach an adapter to the lower end of the condenser and put the cylinder under the adapter. If heat with an open flame, place the distillation flask on the hole in the center of an asbestos plate (in the form of a square with sides of 12-15 cm and with a perforation of 2.5-3.0 cm in diameter in the center, 0.3-0.5 cm thick), the bottom of the flask should be fitted tightly into the perforation to avoid the excessive heating of the vapour of the liquid. Heat with an open flame so that the liquid distils at a rate of 2-3ml per minute. Record the temperature at which the fifth dro-p of condensate leaves the tip of the condenser and the temperature at which all the liquid except 3-4 ml has been distilled, or when a specified volume of distillate has been collected. The temperature range exhibited on the thermometer, is the distilling range of the substance being examined. When not less than 90% of the liquid is to be distilled within the distilling range, use a 100ml distillation flask with 50 ml of the substance being examined, and a 50 ml glass cylinder as the receiv-er.
Correct the observed temperature readings for any variation in the barometric pressure from the normal (101.3 kPa or 760mmHg) by subtracting or adding 0.1℃ for every 0.36kPa (2.7mmHg) in-crease or decrease of the pressure.
影子
第4楼2009/12/25
附录Ⅵ D 凝点测定法
凝点系指一种物质照下述方法测定,由液体凝结为固体时,在短时间内停留不变的最高温度。
某些药品具有一定的凝点,纯度变更,凝点亦随之改变。测定凝点可以区别或检查药品的纯杂程度。
仪器装置 如图:(图略)。内管A为内径约25mm、长约170mm的干燥试管,用软木塞固定在内径约40mm、长约160mm的外管B中,管底间距约10mm。内管用一软木塞塞住,通过软木塞插入刻度为0.1℃的温度计C与搅拌器D,温度计汞球的末端距内管底约10mm。搅拌器D为玻璃棒,上端略弯,末端先铸一小圈,直径约为18mm,然后弯成直角。内管连同外管垂直固定于盛有水或其他适宜冷却液的1000ml烧杯中,并使冷却液的液面离烧杯口约20mm。
测定法 取供试品(如为液体,量取15ml;如为固体,称取15~20g,加微温使熔融),置内管中,使迅速冷却,并测定供试品的近似凝点。再将内管置较近似凝点约高5~10℃的水浴中,使凝结物仅剩极微量未熔融。将仪器按上述装妥,烧杯中加入较供试品近似凝点约低5℃的水或其他适宜的冷却液。用搅拌器不断搅拌供试品,每隔30秒钟观察温度1次,至液体开始凝结,停止搅拌并每隔5~10秒钟观察温度1次,至温度计的汞柱在一点能停留约1分钟不变,或微上升至最高温度后停留约1分钟不变,即将该温度作为供试品的凝点。
【附注】 如某些药品在一般冷却条件下不易凝固,需另用少量供试品在较低温度使凝固后,取少量作为母晶加到供试品中,方能测出其凝点。
VI D Determination of Congealing Point
The congealing point of a substance, determined as described below, is the highest temperature, which remains constant for a short time, occuring during the solidification of the liquid. Congealing point is indicative of the identity and purity of the substance being examined.
Apparatus As Fig. 10 a dry test tube (A) about 25mm in internal diameter and 170mm long is suspended by means of a bored cork inside a larger tube (B) about 40mm in internal diameter and 160mm long. The distance between the bottoms of the two tubes is about 10 mm. The inner tube is stoopered by a bored cork which carries a thermometer (C) graduated in 0.1℃ and a stirrer (D) is a glass rod slightly bent at the upper end, the other end is in the form of a loop which is about 18 mm in diameter at right angle to the rod. The whole assembly is placed in a 1000 ml beaker containing water or a suitable cooling liquid and the surface of the cooling liquid is about 20 mm from the mouth of the beaker.
Procedure Place in the inner tube 15 ml of the liquid or 15-20 g of the melted solid substance being examined and determine the approximate congealing point by cooling rapidly. Place the inner tube in a water bath about 5-10℃ above the approximate congealing point until all the solidified substance but the last trace is melted. Fill the beaker with water or other suitable cooling liquid at a temperature about 5℃ below the approximate congealing point and fix the apparatus as described above. Stir the liquefied substance gently and read the temperature every 30 seconds until it begins to solidify. Stop stirring and read the temperature every 5-10 seconds until the temperature remains constant or becomes constant after a slight elevation for about 1 minute. The highest temperature observed is regarded as the congealing point of the substance being examined.
Annotations If the substance being examined does not start to solidify under normal condition, congealation may be induced by adding a small amount of the substance crystallized by cooling to a lower temperature.
影子
第5楼2009/12/25
附录Ⅵ E 旋光度测定法
平面偏振光通过含有某些光学活性的化合物液体或溶液时,能引起旋光现象,使偏振光的平面向左或向右旋转。旋转的度数,称为旋光度。偏振光透过长1dm并每1ml中含有旋光性物质1g的溶液,在一定波长与温度下测得的旋光度称为比旋度。测定比旋度(或旋光度)可以区别或检查某些药品的纯杂程度,亦可用以测定含量。
除另有规定外 本法系用钠光谱的D线(589.3nm)测定旋光度,测定管长度为1dm(如使用其他管长,应进行换算),测定温度为20℃。用读数至0.01°并经过检定的旋光计。
测定旋光度时,将测定管用供试液体或溶液(取固体供试品,按各药品项下的方法制成)冲洗数次,缓缓注入供试液体或溶液适量(注意勿使发生气泡),置于旋光计内检测读数,即得供试液的旋光度。使偏振光向右旋转者(顺时针方向)为右旋,以“+”符号表示;使偏振光向左旋转者(反时针方向)
为左旋,以“-”符号表示。用同法读取旋光度3次,取3次的平均数,照下列公式计算,即得供试品的比旋度。
a
对液体供试品 [a]
ld
100α
对固体供试品 [a]
$$lc
式中 [a]为比旋度;
D为钠光谱的D线;
t为测定时的温度;
l为测定管长度, dm;
α为测得的旋光度;
d为液体的相对密度;
c为每100ml溶液中含有被测物质的重量,g(按干燥品或无水物计算)。
旋光计的检定,可用标准石英旋光管进行,读数误差应符合规定。
【注意事项】 (1) 每次测定前应以溶剂作空白校正,测定后,再校正1
次,以确定在测定时零点有无变动;如第2次校正时发现零点有变动,则应
重新测定旋光度。
(2) 配制溶液及测定时,均应调节温度至20℃±0.5℃(或各药品项下规定的
温度)。
(3)供试的液体或固体物质的溶液充分溶解,供试液应澄清。
(4) 物质的比旋度与测定光源、测定波长、溶剂、浓度和温度等 因素有关。
因此,表示物质的比旋度时应注明测定条件。
VI E Determination of Optical Rotation
The plane of polarized light can be rotated clockwise or counterelockwise when plane polarized light passes through some liquids or solutions of compounds which are optically active. Optical rotation is expressed in degrees by which the plane of polarization is rotated under specified condition. Specific optical rotation is defined as the optical rotation measured under given wavelength and temperature, when polarized light passed through a layer of a solution 1 dm thick containing 1 g of optically active substance per ml. The measurement of specific optical rotation (or optical rotation) may be used as an identification test, a purity test or a method of assay.
Unless otherwise specified, the values of optical rotation cited in this method are measured at 20℃ with sodium D line (589.3nm), in a tube of 1 dm. Conversion factor should be applied if the tube used is not of the appropriate length. Optical rotation is measured with a calibrated polarimeter accurately read to 0.01º. Rinse the polarimeter tube several times with the liquid or solution prepared as described in the individual monograph. Fill the polarimeter tube solwly with the liquid or solution, taking care to avoid creating or leaving air bubbles. Put the tube into the polarimeter and read the degrees of optical rotation. Substances are described as dextrorotatory or levorotatory according to whether the plane of polarization is ratated clockwise or counterclockwise, respectively, as viewed toward the light source. Dextrorotation is designated (+) and levorotation is designated (-). Carry out 3 measurements, take the average and ca$$lculate the specific optical rotation from one of the following equations:
For liquids
[a]tD=a/ld
For solid substances
[a]tD=100a/$$lc
Where: [a] is specific optical rotation;
D is sodium D line;
t is measuring temperature;
l is the length of the polarimeter tube, dm;
a is the observed rotation in angular degrees;
d is the relative density of the liquid;
c is the weight of solute (g) in 100 ml of the solution, ca$$lculated on the dried basis or anhydrous basis.
Standard quartz polarimetric tube may be used to calibrate the polarimeter, the deviation of reading should comply with the requirements.
Announcements
(1) Blank tests should be performed to check the zero point before and after each measurement,. If the deviation of teading does not comply with the requerements after measurement, repeat the measurement.
(2) The temperature of the solution being tested should be kept constant at 20℃±0.5℃ (or at the temperature specified in the individual monograph).
(3) Liquids or solutions of solid substance should be completely dissolved, and the test solution should be clear.
(4) The specific rotation of a liquid or a substance in solution is affected by several factors including light source, wavelength, solvent, concentration and temperature. When describing the specific optical rotation, the measuring condition should be provided.
影子
第6楼2009/12/26
附录Ⅵ F 折光率测定法
光线自一种透明介质进入另一透明介质的时候,由于光线在两种介质中的传播速度不同,使光线在两种介质的平滑界面上发生折射。常用的折光率系指光线在空气中进行的速度与在供试品中进行速度的比值。根据折射定律,折光率是光线入射角的正弦与折射角的正弦的比值,即
sini
n=─────
sinγ
式中 n为折光率;
sini为光线的入射角的正弦;
sinγ为折射角的正弦。
物质的折光率因温度或光线波长的不同而改变,透光物质的温度升高,折光率变小;入射光的波长越短,折光率越大。折光率以n
本法系用钠光谱的D线(589.3nm)测定供试品相对于空气的折光率(如用阿培氏折光计,可用白光光源),除另有规定外,供试品温度为20℃。
测定用的折光计需能读数至0.0001,测量范围1.3~1.7,如用阿培氏折光计或与其相当的仪器,测定时应调节温度至20℃±0.5℃(或各药品项下规定的温度),测量后再重复读数两次,3次读数的平均值即为供试品的折光率。
测定前,折光计读数应用校正用棱镜或水进行校正,水的折光率20℃时为1.3330,25℃时为1.3325,40℃时为1.3305。
VI F Determination of Refractive Index
Refraction takes place when a beam of light is transmitted from a transparent medium into another transparent medium, since the velocity of light changes in medium of different density. The refractive index of a substance is the ratio of the velocity of light in air to its velocity in the substance. The refractive index may also be defined as the ratio of the sine of the angle of incidence to the sine of the angle of refraction:
n=sin i / sin r
Where n is the refractive index;
i is the angle of incidence;
r is the angle of refraction.
The refractive index varies with the temperature of the substance being examined and the wavelength of incident light. It decreases with the increase temperature. The shorter the wavelength of incident light, the larger the refractive index. Refractive indices are usually stated in terms of sodium line D at a temperature of t and symbolized by n’D. The measurement of refractive index is employed to establish the identity of oils and test for purity of the substance being examined.
Unless otherwise specified, the values of refractive index cited in this method are measured at 20℃ with sodium line D (589.3nm) against air (White light may be used if an Abble refractometer is available).
The refractometer should be able to give readings accurate to 0.0001 in the range of 1.3-1.7. If an Abble refractometer or othjer equivalent instrument is used, the measurement should be conducted at 20℃±0.5℃ (or in accordance with the temperature stated under individual monograph). Three readings should be taken and the mean value is used as the refractive index of the substance being examined. The readings of the refractometer should be calibrated before use with a prism of against water. The refractive index of water is 1.3330 at 20℃, 1.3325 at 25℃ and 1.3305 at 40℃.