1、EP 8.0 各论：丙酮 01/2008:0872 (中英文）EP 7.001/2008:0872ACETONE 丙酮C3H6O67-64-1 Mr 58.08【定义】Propanone 丙酮。【CHARACTERS 性状】Appearance: volatile, clear, colourless liquid外观：挥发性、澄清，无色液体。Solubility: miscible with water and with ethanol (96% per cent).溶解性：与水和乙醇（96%）互溶。The vapor is flammable.蒸气易燃。【IDENTIFICATION 鉴别
2、】A. Relative density (see Tests)A：比重（见检查项）。B.To 1mL, add 3mL of dilute sodium hydroxide solution R and 0.3mL of a 25g/L solution of sodium nitroprusside R. An intense red colur is produced which becomes violet with the addition of 3.5mL of acetic acid R.B：于 1ml样品中，加3ml稀氢氧化钠溶液（R），0.3ml的25g/L硝普钠（亚硝酰铁氰
3、化钠）（R）溶液。应呈深红色，加3.5ml醋酸（R）后变为紫色。稀氢氧化钠溶液配制方法：Sodium Hydroxide Solution, Dilute An 8.5% w/v solution of sodium hydroxide (about 2M ).硝普钠：Sodium Nitroprusside Sodium pentacyanonitrosylferrate(III) dihydrate; Na2Fe(CN)5(NO),2H2O = 298.0 (13755-38-9) Analytical reagent grade of commerce. Reddish brown po
4、wder or crystals）C. To 10mL of a 0.1 per cent V/V solution of the substance to be examined in ethanol (50 per cent V/V) R, add 1mL of a 10g/L solution of nitrobenzaldehyde R in ethanol (50 per cent V/V) R and 0.5mL of strong sodium hydroxide solution R. Allow to stand for about 2 min and acidify wit
5、h acetic acid R. Agreenish-blue colour is produced.C：取 10ml 的 0.1%（V/V）样品在乙醇中（50%V/V）（R）稀释液，加 1ml的 10mg/L 对硝基苯甲醛（R）乙醇（50%V/V）溶液，加 0.5ml 浓氢氧化钠溶液（R ）。放置约 2 分钟，用醋酸（R）酸化，应显蓝绿色。浓氢氧化钠溶液（R）：Sodium Hydroxide Solution, Strong A 42% w/v solution of sodium hydroxide (about 10M ).【TESTS 检查】Appearance of solutio
6、n. To 10mL add 10mL of water R. The solution is clear (2.2.1) and colourless (2.2.2, Method II).溶液外观：取 10ml 样品，加 10ml 水，溶液应澄清（附录 2.2.1）无色（附录2.2.2，方法）。Acidity or alkalinity. To 5mL add 5mL of carbon dioxide-free water R, 0.15mL of phenolphthalein solution R and 0.5mL of 0.01M sodium hydroxide. The so
7、lution is pink. Add 0.7mL of 0.01M hydrochloric acid and 0.05mL of methyl red solution R. The solution is red or orange.酸碱度：取样品 5ml，加 5ml 无二氧化碳的水（R），0.15mL 酚酞试液（R）与0.5ml 的 0.01M 氢氧化钠，溶液显粉色。加 0.7ml 的 0.01M 盐酸，0.05ml 甲基红指示液（R），溶液显红色或橙色。酚酞试液：Phenolphthalein Solution Dissolve 0.1 g of phenolphthalein R
8、in 80 ml of alcohol R and dilute to 100 ml with water R. Complies with the following test. Test for sensitivity To 0.1 ml of the phenolphthalein solution add 100 ml of carbon dioxide-free water R. The solution is colourless. Not more than 0.2 ml of 0.02 M sodium hydroxide is required to change the c
9、olour to pink. Colour change pH 8.2 (colourless) to pH 10.0 (red) 甲基红试液：Methyl Red Solution Dissolve 50 mg of methyl red in a mixture of 1.86 ml of 0.1M sodium hydroxide and 50 ml of ethanol (96%) and add sufficient water to produce 100 ml. Complies with the following test. Sensitivity A mixture of
10、0.1 ml of the solution, 100 ml of carbon dioxide-free water and 0.05 ml of 0.02M hydrochloric acid VS is red. Not more than 0.1 ml of 0.02M sodium hydroxide VS is required to change the colour of the solution to yellow. Colour change pH 4.4 (red) to pH 6.0 (yellow). Relative density (2.2.5): 0.790 t
11、o 0.793.比重（附录 2.2.25）：0.7900.793Reducing substances. To 30mL add 0.1mL of 0.02M potassium permanganate and allow to stand in the dark for 2h. The mixture is not completely decolorized.还原性物质：取样品 30ml，加 0.1ml 的 0.02m 高锰酸钾，在黑暗中放置 2 小时，混合物不得全褪色。Related substances. Gas chromatography (2.2.28).有关物质：气相（附录
12、2.2.28）Test solution. The substance to be examined.供试液：待检样品Reference solution (a). To 0.5mL of methanol R add 0.5mL of 2-propanol R and dilute to 100.0mLwith the test solution. Dilute 1.0mL of this solution to 10.0mL with the test solution.对照液（a）：取 0.5ml 异丙醇（R）加于 0.5ml 甲醇 （R ）中，用供试液稀释至 100.0ml。移取 1.
13、0ml 用供试液稀释至 10.0ml。Reference solution (b). Dilute 100uL of benzene R to 100.0mL with the test solution. Dilute 0.20mL of this solution to 100.0mL with the test solution.对照液（b）：取 100L 苯（R）于 100.0mL 容量瓶，用供试液稀释至刻度。移取 0.20ml 该溶液用供试液稀释至 100.0ml。Column: 色谱柱：-material: fused silica,色谱柱材料：熔融石英-size: l=50m,
14、D=0.3mm尺寸：l=50m，D= 0.3mm-stationary phase: macrogol 20,000R (film thickness 1um).固定相：聚乙二醇 20000R（膜厚 1m）Carrier gas: helium for chromatography R.载气：高纯氦气（Helium He = 4.003 (7440-59-7) Laboratory cylinder grade of commerce containing not less than 99.995% v/v of He）. Linear velocity: 21cm/s.线速度：21cm/sS
15、plit ration:1:50分流比：1：50Temperature 升温程序Time 时间（min 分钟） Temperature 温度（）Column 柱温 0-11 4510011-20 100Injection port 进样口 150Detector 检测器 250Detection: flame ionization.检测器：FID Injection: 1uL.进样量：1LRetention time: impurity C = about 7.5min保留时间：杂质 C（苯）=约 7.5 分钟System suitability: 系统适用性：-resolution: min
16、imum 5.0 between the peak due to impurity A (2nd peak) and the peak due to impurity B (3rd peak) in the chromatogram obtained with reference solution (a).分离度：对照液（a ）中杂质 A（第 2 个峰）与杂质 B（第 3 个峰）分离度不小于 5.0-signal-to-noise ration: minimum 5 for the peak due to impurity C in the chromatogram obtained with
17、 reference solution (b).信噪比：对照液（b）色谱图中杂质 C（苯）的信噪比不小于 5。Limits: 限度-impurities A, B: for each impurity, not more than the difference between the areas of the corresponding peaks in the chromatogram obtained with reference solution (a) and the areas of the corresponding peaks in the chromatogram obtain
18、ed with the test solution (0.05 per cent V/V).杂质 A，B：各杂质峰面积不大于对照液（a）色谱图中相应峰面积与供试液色谱图中对应峰面积差值（0.05%V/V）-impurity C: not more than the difference between the area of the peak due to impurity C in the chromatogram obtained with reference solution (b) and the area of the corresponding peak in the chroma
19、togram obtained with the test solution (2ppm V/V).杂质 C（苯）：杂质 C 面积不大于对照液（b）色谱图中杂质 C 峰面积与供试液色谱图中杂质 C 面积差值（2ppmV/V）-any other impurity: for each impurity, not more than the difference between the area of the peak due to impurity A in the chromatogram obtained with reference solution (a) and the area of
20、 the corresponding peak in the chromatogram obtained with the test solution (0.05 per cent V/V).-其它单一杂质：各杂质面积不大于对照液（a ）色谱图中杂质 A 峰面积与供试液色谱图中相应峰面积之差值（0.05%V/V）Matter insoluble in water Dilute 1.0mL to 20mL with water R. The solution is clear (2.2.1)水不溶物取 1.0ml 样品，用水稀释至 20ml，溶液应澄清（附录 2.2.1）。Residue on
21、evaporation: maximum 50ppm.蒸发残渣：不得过 50ppmEvaporate 20.0g to dryness on a water-bath and dry at 100-105. The residue weighs a maximum of 1mg.取样品 20.0g，水浴加热至干，100-105干燥，残渣不超过 1mg。Water (2.5.12): maximum 3g/L. determined on 10.0mL. Use 20mL of anhydrous pyridine R as solvent.水分（附录 2.5.12）：不得过 3g/L取样品 10.0ml，用 20ml 无水吡啶（R）为溶剂，滴定。【STORAGE 贮存】Protected from light.避光保存。【IMPURITIES 杂质】A CH3-OH: methanol. 杂质 A：甲醇B. CH3-CHOH-CH3: propan-2-ol (isopropanol) 杂质 B：异丙醇C: C6H6: Benzene. 杂质 C：苯译者注：文中的“（R） ”表示 EP 规定的试剂级别
