Where the monograph specifies that the specimen under test is hygroscopic, use a dry syringe to inject an appropriate volume of methanol, or other suitable solvent, accurately measured, into a tared container, and shake to dissolve the specimen. Using the same syringe, remove the solution from the container and transfer it to a titration vessel prepared as directed for Procedure. Repeat the procedure with a second portion of methanol, or other suitable solvent, accurately measured, add this washing to the titration vessel, and immediately titrate. Determine the water content, in mg, of a portion of solvent of the same total volume as that used to dissolve the specimen and to wash the container and syringe, as directed for Standardization of Water Solution for Residual Titrations, and subtract this value from the water content, in mg, obtained in the titration of the specimen under test. Dry the container and its closure at 100 for 3 hours, allow to cool in a desiccator, and weigh. Determine the weight of specimen tested from the difference in weight from the initial weight 4of the container.
当各论指明样品在测试条件下具有引湿性时，使用一个干燥的注射器注入合适体积的甲醇或其他合适的溶剂，准确测量，至一个去了皮重的容器中，振摇使样品溶解。使用同一注射器，从容器中移取溶液转移至按规程准备的滴定容器中。用第二部分的甲醇或其他合适的溶剂重复上述操作，准确测量，将这一部分洗涤物加至滴定容器中，立即滴定。如回滴定法水试剂的标定所示，测定与溶解样品和清洗容器与注射器相同体积的的溶剂的水的含量，以mg计，然后从待测样品滴定获得的水的含量中扣除掉这部分值，以mg计。在100℃，干燥容器和它的塞子3小时，干燥器中放冷，称重。与容器初始的重量的差值就是测试样品的重量。

Standardization of the Reagent— Place enough methanol or other suitable solvent in the titration vessel to cover the electrodes, and add sufficient Reagent to give the characteristic endpoint color, or 100 ± 50 microamperes of direct current at about 200 mV of applied potential.
卡尔溶剂的标定---将足量体积的甲醇或其他合适溶剂至滴定容器中，覆没电极，加入足量的卡尔试剂至给出特征性的终点颜色，或者在大约200mV的应用电势下达到100+-50微毫安的直流电。
For determination of trace amounts of water (less than 1%), it is preferable to use Reagent with a water equivalency factor of not more than 2.0. Sodium tartrate may be used as a convenient water reference substance. Quickly add 75 to 125 mg of sodium tartrate (C4H4Na2O6•2H2O), accurately weighed by difference, and titrate to the endpoint. The water equivalence factor F, in mg of water per mL of reagent, is given by the formula:
2(18.02/230.08)(W/V)
in which 18.02 and 230.08 are the molecular weights of water and sodium tartrate dihydrate, respectively; W is the weight, in mg, of sodium tartrate dihydrate; and V is the volume, in mL, of the Reagent consumed in the second titration.
为了测定痕量水分（少于1%），最好使用与水的等价因子不超过2.0卡尔试剂。酒石酸钠可以用于作为一种方便的水标准物质。快速加入75~125mg的酒石酸钠，减重法准确称量，滴定至终点。水的等价因子F，以每毫升卡尔试剂消耗水的质量mg计，用以下公式计算：2(18.02/230.08)(W/V)
其中18.02和230.08是水和酒石酸钠的各自分子量，W是二水酒石酸钠的重量，以mg计，V是第二次滴定消耗的卡尔试剂的体积，以毫升计。

不好意思，废话不多说，请大家多指教

For the precise determination of significant amounts of water (1% or more), use Purified Water as the reference substance. Quickly add between 25 and 250 mg of water, accurately weighed by difference, from a weighing pipet or from a precalibrated syringe or micropipet, the amount taken being governed by the reagent strength and the buret size, as referred to under Volumetric Apparatus 31 . Titrate to the endpoint. Calculate the water equivalence factor, F, in mg of water per mL of reagent, by the formula:
W/V
in which W is the weight, in mg, of the water; and V is the volume, in mL, of the reagent required.
为了精密测定水的显著含量（1%或更多），使用纯化水作为标准物质。从一个称量吸管或者一个事先校准的注射器或微量吸管，快速加入25~250mg的水，减重法准确称量，所取数量由卡氏的浓度和滴定管的型号所决定，参考（31）。滴定至终点。计算水的等价因子F，以每毫升试剂消耗的水的质量mg计，通过以下公式计算：W/V。其中W是水的重量，单位mg，V是所需要卡尔试剂的体积，单位ml。
Procedure— Unless otherwise specified, transfer 35 to 40 mL of methanol or other suitable solvent to the titration vessel, and titrate with the Reagent to the electrometric or visual endpoint to consume any moisture that may be present. (Disregard the volume consumed, since it does not enter into the calculations.) Quickly add the Test Preparation, mix, and again titrate with the Reagent to the electrometric or visual endpoint. Calculate the water content of the specimen, in mg, taken by the formula:
SF
in which S is the volume, in mL, of the Reagent consumed in the second titration; and F is the water equivalence factor of the Reagent.
操作---除另有规定外，转移35~40ml的甲醇或其他合适的溶剂至滴定容器中，以永停法或视觉指示终点，用卡尔试剂滴定可能存在的水汽（所消耗体积忽略不计，因为不会代入到公式计算），快速加入测试样本，混匀，然后再次用卡尔试剂滴定到终点。计算样品中的水的质量，单位mg，用以下公式计算：SF。其中S是第二次滴定所消耗的卡尔试剂体积，单位ml；F是卡氏试剂与水的等价因子。

Method Ib (Residual Titration)
Principle— See the information given in the section Principle under Method Ia. In the residual titration, excess Reagent is added to the test specimen, sufficient time is allowed for the reaction to reach completion, and the unconsumed Reagent is titrated with a standard solution of water in a solvent such as methanol. The residual titration procedure is applicable generally and avoids the difficulties that may be encountered in the direct titration of substances from which the bound water is released slowly.
方法Ib（回滴定法）
原理---参考方法Ia下的原理部分所给与的信息。在回滴定法，过量的卡尔试剂加入到待测样品中，给与足够的时间去达到反应完全，未消耗的卡尔试剂用溶于溶剂例如甲醇的标准水溶液去滴定。回滴定方法是普遍适用的，避免了直接滴定样品时可能遇到的困难，比如结合水释放缓慢。
Apparatus, Reagent, and Test Preparation— Use Method Ia.
Standardization of Water Solution for Residual Titration— Prepare a Water Solution by diluting 2 mL of water with methanol or other suitable solvent to 1000 mL. Standardize this solution by titrating 25.0 mL with the Reagent, previously standardized as directed under Standardization of the Reagent. Calculate the water content, in mg per mL, of the Water Solution taken by the formula:
VF/25
in which V is the volume of the Reagent consumed, and F is the water equivalence factor of the Reagent. Determine the water content of the Water Solution weekly, and standardize the Reagent against it periodically as needed.
器具，试剂，测试样本---参考方法Ia。
回滴定法标准水溶液的标定---准备标准水溶液，用甲醇或合适的溶剂稀释2ml水到1000ml。用卡尔试剂滴定25.0ml的上述溶液去标定该溶液，标定参考之前卡氏试剂的标定。使用以下公式计算标准水溶液中水的含量，单位是mg/ml。
VF/25
其中V是消耗的卡尔试剂的体积，F是卡氏试剂与水的等价因子。每周测定标准水溶液中水的含量，按需要周期性的标定卡尔试剂。

Procedure— Where the individual monograph specifies that the water content is to be determined by Method Ib, transfer 35 to 40 mL of methanol or other suitable solvent to the titration vessel, and titrate with the Reagent to the electrometric or visual endpoint. Quickly add the Test Preparation, mix, and add an accurately measured excess of the Reagent. Allow sufficient time for the reaction to reach completion, and titrate the unconsumed Reagent with standardized Water Solution to the electrometric or visual endpoint. Calculate the water content of the specimen, in mg, taken by the formula:
F(X XR)
in which F is the water equivalence factor of the Reagent; X is the volume, in mL, of the Reagent added after introduction of the specimen; X is the volume, in mL, of standardized Water Solution required to neutralize the unconsumed Reagent; and R is the ratio, V/25 (mL Reagent/mL Water Solution), determined from the Standardization of Water Solution for Residual Titration.
规程---当各论规定使用方法Ib测定水的含量时，转移35~40ml的甲醇或者其他合适的溶剂至滴定容器中，用卡尔试剂滴定，以永停法或视觉观察终点。快速加入待测样本，混匀，加入准确测量的过量的卡尔试剂。给与足够的时间达到反应完全，用标准水溶液去滴定未反应的的卡尔试剂，以永停法或视觉观察终点。用以下公式计算样品中水的含量，单位是mg，
F(X XR)
其中F是试剂与水的等价因子；X加入样品后加入的卡尔试剂体积，单位ml；X是标准水溶液中和未反应试剂所消耗的体积，单位ml，R是一个比值，V/25（单位卡尔试剂/单位标准水溶液）。
Method Ic (Coulometric Titration)
Principle— The Karl Fischer reaction is used in the coulometric determination of water. Iodine, however, is not added in the form of a volumetric solution but is produced in an iodide-containing solution by anodic oxidation. The reaction cell usually consists of a large anode compartment and a small cathode compartment that are separated by a diaphragm. Other suitable types of reaction cells (e.g., without diaphragms) may also be used. Each compartment has a platinum electrode that conducts current through the cell. Iodine, which is produced at the anode electrode, immediately reacts with water present in the compartment. When all the water has been consumed, an excess of iodine occurs, which usually is detected electrometrically, thus indicating the endpoint. Moisture is eliminated from the system by pre-electrolysis. Changing the Karl Fischer solution after each determination is not necessary since individual determinations can be carried out in succession in the same reagent solution. A requirement for this method is that each component of the test specimen is compatible with the other components, and no side reactions take place. Samples are usually transferred into the vessel as solutions by means of injection through a septum. Gases can be introduced into the cell by means of a suitable gas inlet tube. Precision in the method is predominantly governed by the extent to which atmospheric moisture is excluded from the system; thus, the introduction of solids into the cell is not recommended, unless elaborate precautions are taken, such as working in a glove-box in an atmosphere of dry inert gas. Control of the system may be monitored by measuring the amount of baseline drift. This method is particularly suited to chemically inert substances like hydrocarbons, alcohols, and ethers. In comparison with the volumetric Karl Fischer titration, coulometry is a micro-method.
方法Ic（库仑滴定法）
原理---卡尔费休反应被用于电量分析测定水分。然而，碘不是以滴定溶液的形式加入，而是通过阳极氧化含有碘化物的溶液生成的。反应池通常由一个很大的阳极室和一个很小的阴极室组成，中间以隔膜分开。也可以使用其他合适类型的反应池（例如无隔膜的）。每一个室有一个铂电极，可以引导电流通过反应池。在阳极生成的碘，立即与腔室里存在的水反应。当所有的水被反应完，生成的过量的碘，可以被永停法检测到，以此指示终点。水汽可以通过预电解从系统中除去。没有必要在每次测定后更换卡尔费休试剂，因为在相同的试剂溶液中，每个测定都能连续的完成。该方法要求待测样品比较均一，没有副反应发生。样品通常以溶液的形式借助注射方式通过隔膜转移到滴定容器中。气体可以借助一个气体入口管进入到反应池中。方法的精密度主要是由大气中的水汽从系统中被排除的程度决定；因此不推荐将固体样品引入到反应池中，除非采取了比较详细的措施，例如在一个大气压的干燥惰性气体中在手套箱中操作。通过测量基线漂移的数值去监视系统的控制。很明显这个方法适合化学惰性物质例如碳氢化合物、乙醇和乙醚。与卡尔费休容量滴定法比较，库仑分析法是微量法。

Apparatus— Any commercially available apparatus consisting of an absolutely tight system fitted with the necessary electrodes and a magnetic stirrer is appropriate. The instrument's microprocessor controls the analytical procedure and displays the results. Calibration of the instrument is not necessary, as the current consumed can be measured absolutely.
仪器---合适的市售仪器包括一个完全密闭的系统，与之匹配的必要的电极和一个合适的磁力搅拌器。这个仪器的微处理器控制着分析程序并能展示结果。仪器的校准不是必须的，因为被消耗的电流完全能被测量。
Reagent— See Reagent under Method Ia.
Test Preparation— Where the specimen is a soluble solid, dissolve an appropriate quantity, accurately weighed, in anhydrous methanol or other suitable solvents. Liquids may be used as such or as accurately prepared solutions in appropriate anhydrous solvents.
Where the specimen is an insoluble solid, the water may be extracted using a suitable anhydrous solvent from which an appropriate quantity, accurately weighed, may be injected into the anolyte solution. Alternatively an evaporation technique may be used in which water is released and evaporated by heating the specimen in a tube in a stream of dry inert gas, this gas being then passed into the cell.
试剂---参见方法Ia卡尔试剂项。
测试样本---当样品是可溶性固体，取适当质量，准确称量，溶解至无水甲醇或其他合适的溶剂中。液体样品也可以像这样操作或者精确的配制溶液至适当的无水溶剂中。
当样品是不溶性固体，水可以被合适的无水溶剂从一合适的准确称量的样品量中提取出来，注入到阳极液中。也可以用一种蒸馏技术，使用惰性的干燥气体流，将管中的样品加热使水释放并蒸发出来，然后将气体传送到反应池中。

Procedure— Using a dry syringe, quickly inject the Test Preparation, accurately measured and estimated to contain 0.5 to 5 mg of water, or as recommended by the instrument manufacturer into the anolyte, mix, and perform the coulometric titration to the electrometric endpoint. Read the water content of the Test Preparation directly from the instrument's display, and calculate the percentage that is present in the substance. Perform a blank determination, and make any necessary corrections.
规程---使用一个干燥的注射器，快速注入测试样本，准确测量并估计大约含有0.5~5mg水，或者按照仪器制造商的推荐至阳极液中，混匀，采用库仑滴定法滴定至电量终点，直接从仪器显示处读取测试样本的水的含量，计算样品中存在的水的百分含量。作一个空白测定，作任何必要的校正。

METHOD II (AZEOTROPIC—TOLUENE DISTILLATION)
Apparatus— Use a 500-mL glass flask A connected by means of a trap B to a reflux condenser C by ground glass joints (see Figure).
方法II(共沸法----甲苯馏出物)
装置---使用一个与500ml的玻璃烧瓶A，与水分测定管B连接，使用磨口玻璃接头与回流冷凝器C连接（见图）

Toluene Moisture Apparatus甲苯蒸馏装置
The critical dimensions of the parts of the apparatus are as follows. The connecting tube D is 9 to 11 mm in internal diameter. The trap is 235 to 240 mm in length. The condenser, if of the straight-tube type, is approximately 400 mm in length and not less than 8 mm in bore diameter. The receiving tube E has a 5-mL capacity, and its cylindrical portion, 146 to 156 mm in length, is graduated in 0.1-mL subdivisions, so that the error of reading is not greater than 0.05 mL for any indicated volume. The source of heat is preferably an electric heater with rheostat control or an oil bath. The upper portion of the flask and the connecting tube may be insulated. Clean the receiving tube and the condenser with chromic acid cleansing mixture, thoroughly rinse with water, and dry in an oven. Prepare the toluene to be used by first shaking with a small quantity of water, separating the excess water, and distilling the toluene.
装置的关键性的尺寸部分如下。连接管D的内径是9~11mm。水分测定管长度是235~240mm。冷凝管如果是直管类型的，长度大约是400mm，内径不小于8mm。接收管E有5ml的容量，并且它的圆筒状的部分长度大约146~156mm，并且而最小刻度是0.1ml，这样对于任何读出的体积的读数误差不得大于0.05ml。热源最好是使用可变电阻电炉或者油浴。烧瓶的上端和连接管最好是绝缘的。用铬酸清洁接收管和冷凝器，彻底用水冲洗，并在烘箱中干燥。将要用的甲苯先与少量的水振摇，将多余的水分离，并蒸馏甲苯。

Procedure— Place in the dry flask a quantity of the substance, weighed accurately to the nearest centi-gram, which is expected to yield 2 to 4 mL of water. If the substance is of a pasty character, weigh it in a boat of metal foil of a size that will just pass through the neck of the flask. If the substance is likely to cause bumping, add enough dry, washed sand to cover the bottom of the flask, or a number of capillary melting-point tubes, about 100 mm in length, sealed at the upper end. Place about 200 mL of toluene in the flask, connect the apparatus, and fill the receiving tube E with toluene poured through the top of the condenser. Heat the flask gently for 15 minutes and, when the toluene begins to boil, distill at the rate of about 2 drops per second until most of the water has passed over, then increase the rate of distillation to about 4 drops per second. When the water has apparently all distilled over, rinse the inside of the condenser tube with toluene while brushing down the tube with a tube brush attached to a copper wire and saturated with toluene. Continue the distillation for 5 minutes, then remove the heat, and allow the receiving tube to cool to room temperature. If any droplets of water adhere to the walls of the receiving tube, scrub them down with a brush consisting of a rubber band wrapped around a copper wire and wetted with toluene. When the water and toluene have separated completely, read the volume of water, and calculate the percentage that was present in the substance.
操作---将一定量的样品，准确称量至mg，希望含有2~4ml的水，置干燥的烧瓶中。如果样品是糊状的，用金属箔制的尺寸刚好能通过烧瓶颈的称量船称量。如果样品可能引起暴沸，加入足量干燥的、已洗净的砂去覆盖烧瓶底部，也可以用许多长度大约100mm长，上端封口的毛细熔点管。将大约200ml甲苯置烧瓶中，连接装置，从冷凝管上端倾入甲苯至装满接收管E。缓缓加热烧瓶15分钟，当甲苯开始沸腾时，以每秒2滴的速度蒸馏直到大多数水已经~~~，然后增加速度至每秒4滴。当水分很明显已经蒸馏完全，用甲苯清洗冷凝管内部，再用用甲苯饱和的带铜丝的试管刷向下刷管子。继续蒸馏5分钟，移走热源，让接收管放冷至室温。如果任何水滴附着在接收管的壁上，将铜丝缠绕橡皮圈的刷子，用甲苯润湿，将之刷下，当水和甲苯已经完全分离，读水的体积数，并计算样品中存在的水分百分含量。