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Comparison of three chemical detection principles for carbon and sulfur analysis (2)
Release time: 2019-12-05 11:54:51 Click: 1378
，分析速度比较慢，但是结果比较准确。 Two methods for analyzing carbon and sulfur were introduced last time. The three methods for measuring carbon and sulfur elements to be introduced this time are non- aqueous carbon determination and potassium iodate volumetric method for sulfur measurement, conductivity method for carbon and sulfur measurement, and coulometric method for measurement. Carbon and sulfur, these methods all use chemical reagent solutions , the analysis speed is relatively slow, but the results are more accurate.
Determination of sulfur by non-aqueous carbon determination and potassium iodate volumetric method
），预热0.5-1min ，通氧燃烧（氧气流量 1-2L/min ）生成 SO2 和 CO2 气体，经除尘管导入硫，碳吸收杯中，当淀粉吸收液中的纯蓝色逐渐变淡时，随机用 KIO3 溶液，碱性非水溶液滴定硫，碳，将近终点时，间断通氧 1-2 次，继续滴定至溶液呈原来的纯蓝色终点。 Put the sample in the porcelain boat, add the appropriate amount of co-solvent, push the porcelain boat into the high temperature area of the combustion furnace (1200-1250 degrees ), preheat 0.5-1min , oxygen combustion (oxygen flow 1-2L / min ) to generate SO2 With CO2 gas, it is introduced into the sulfur through the dust removal tube, and the carbon absorption cup. When the pure blue in the starch absorption solution gradually fades, the sulfur and carbon are titrated randomly with the KIO3 solution and the alkaline non-aqueous solution. 1-2 times, continue to titrate until the solution is the original pure blue end point. KIO3 标准溶液和碱性非水溶液的毫升数及相应标准试样求得的滴定度，求出硫和碳的含量。 According to the consumed KIO3 standard solution and alkaline non-aqueous solution in milliliters and the corresponding standard sample to obtain the titer, find the content of sulfur and carbon. WM3012-87 ）。 Non-aqueous titration method for measuring carbon is the standard method for measuring carbon in carbon steel and high, medium and low alloy steel ( WM3012-87 ).
The potassium iodate volumetric method is the standard method for determining pig iron powder, carbon steel, alloy steel, high temperature alloy, precision alloy, antimony, and sulfur in silver. 20 世纪 70-80 年代该方法在我国广泛应用。 This method was widely used in China in the 1970s and 1980s .
Conductivity measurement of carbon and sulfur
CO2 和 SO2 混合气体首先导入硫的电导吸收池，池中含有酸性氧化剂的硫吸收液（常用氧化剂有 KIO4,H2O2 等）， SO2 氧化并产生 H2SO4, 引起吸收液氢离子浓度增加，其增值与硫含量成正比例，再经电脑处理，可以显示并打印出硫的含量。 Conductance method is used to measure the amount of carbon. The amount of sulfur is to introduce the mixed gas of CO2 and SO2 produced by the combustion method into the conductivity absorption tank of sulfur first. The pool contains sulfur absorption liquid of acid oxidant (common oxidants are KIO4, H2O2, etc.). H2SO4 causes the concentration of hydrogen ions in the absorption liquid to increase, and its added value is proportional to the sulfur content. After being processed by the computer, the sulfur content can be displayed and printed. SO2 的混合气体再导入碳吸收池，吸收池中装有能吸收 CO2 的溶液（如 NaOH,Ba （ OH ） 2 等），当导入 CO2 后，溶液的电导发生变化，并改变值与 CO2 的量成正比，经电脑处理，可数显并打印出碳的含量。 The carbon measurement by conductivity method is to introduce the mixed gas that has absorbed SO2 into the carbon absorption tank. The absorption tank is equipped with a solution that can absorb CO2 (such as NaOH, Ba ( OH ) 2 etc.). When CO2 is introduced , the conductivity of the solution changes , And the change value is proportional to the amount of CO2 . After computer processing, the carbon content can be displayed digitally and printed. 60 秒。 The whole process is completed automatically in 60 seconds.
1X10-6 。 The conductivity method is mostly used for the determination of low carbon and low sulfur, and the lower limit of measurement can reach 1X10-6 . It can be used as a standard method for determining trace sulfur in tungsten powder, tungsten trioxide, tungstic acid, molybdenum powder, molybdenum trioxide, ammonium molybdate, etc.
Coulometric determination of carbon and sulfur
1300 度左右通氧，试样中的碳转化为 CO 2 ，并导入已经 PH 值的 Ba(ClO 4)2 溶液中，反应生成 HClO 4 和 BaCO 3 沉淀，由于氢离子浓度的增加，溶液的 PH 值发生变化，用脉冲电解方法使溶液的 PH 值恢复至原值。 The Coulomb method is to calculate the carbon content of the sample based on the electricity consumed. Weigh the sample with a co-solvent and place it in a porcelain boat. The temperature of the tube furnace rises to about 1300 degrees with oxygen, and the carbon in the sample is converted to CO 2 , and introduced into the Ba (ClO 4) 2 solution with the PH value , the reaction generates HClO 4 and BaCO 3 precipitation, due to the increase in the concentration of hydrogen ions, the pH value of the solution changes, the pulse electrolysis method to restore the PH value of the solution To the original value. 8X10 -3 度的电量，析出的物质为 0.5X10 -6 g 。 In the electrolysis process, each electric pulse is equivalent to 8X10 -3 degrees of electricity, and the precipitated material is 0.5X10 -6 g .