检验氢氧化钾中要确定样品的采样单元数。采样器由袋口的一角斜到袋深的3/4处采样,将采出的样品混匀,用四分法缩分到所要检验的样品量。
The number of sampling units of the sample shall be determined in the test of potassium hydroxide. The sampler slants from one corner of the bag mouth to 3/4 of the bag depth for sampling, mixes the collected samples evenly, and reduces them to the amount of samples to be tested by quartering.
因氢氧化钾肥料吸水性强,故在制备样品时动作应迅速。样品制备后,称取5g试样,到0.001g,加入150ml水,然后在不断搅拌下加热,微沸5min,取下冷却到20℃,移入500ml容量瓶,定容过滤后再吸取25.0ml于250.0ml的容量瓶中。这是一个很关键的环节。
Because potassium hydroxide fertilizer has strong water absorption, it should be rapid when preparing samples. After sample preparation, weigh 5g of sample to 0.001g, add 150ml of water, and then heat it under constant stirring, slightly boil it for 5min, take it down and cool it to 20 ℃, transfer it into a 500ml volumetric flask, filter at constant volume, and then suck 25.0ml into a 250.0ml volumetric flask. This is a key link.
有一些检验员为了一时方便,不是在水温达到20℃时定容,而按常温的水温定容,结果是水温高于20℃时,结果偏高;水温低于20℃时,结果偏低。两次定容造成两次误差,所以,准确的检验温度是检验结果准确与否的关键。水温高于20℃的检验结果与20℃时的检验结果比较见表1。
For temporary convenience, some inspectors do not fix the volume when the water temperature reaches 20 ℃, but according to the normal temperature. The result is that when the water temperature is higher than 20 ℃, the result is higher; When the water temperature is lower than 20 ℃, the result is low. Two times of constant volume cause two times of error, so the accurate test temperature is the key to the accuracy of the test results. See Table 1 for the comparison of the test results when the water temperature is higher than 20 ℃ and the test results when the water temperature is 20 ℃.
在弱碱性介质中,四苯硼钠[NaB(C6H5)4]碱性溶液和洗涤液对检验结果有直接影响。因为配制好的四苯硼钠很不稳定,容易产生浑浊。如果使用前发现有混浊,要用中速滤纸过滤后再使用,否则检验结果偏高。用洗涤液洗涤和用蒸馏水洗涤检验,结果也不一样。有些检验员认为配制洗涤液麻烦,用蒸馏水代替洗涤液,检验结果就会偏低。蒸馏水的原始结果与洗涤剂的正确结果相关数据比较见表1。
In weakly alkaline medium, sodium tetraphenylboron [NaB (C6H5) 4] alkaline solution and washing solution have a direct impact on the test results. Because the prepared sodium tetraphenylboron is unstable and easy to produce turbidity. If turbidity is found before use, it should be filtered with medium speed filter paper before use, otherwise the test result is on the high side. The results of washing with detergent and distilled water are also different. Some inspectors think it is troublesome to prepare washing solution. If distilled water is used instead of washing solution, the test result will be low. See Table 1 for the comparison between the original results of distilled water and the correct results of detergent.
检验中,试液过滤后的洗涤步骤存在洗涤终点不够明确的问题。依据GB6549-1996《氢氧化钾》规定,先抽滤上清液,再用洗涤液(即室温下饱和的四苯硼钾溶液)转移沉淀过滤器中,继续用以上洗涤液洗涤沉淀12次左右,每次洗涤液用量约为5ml。
During the test, there was a problem that the washing end point was not clear enough in the washing step after the test solution was filtered. According to the provisions of Potassium Hydroxide (GB6549-1996), the supernatant is filtered first, and then the washing solution (i.e. potassium tetraphenylborate solution saturated at room temperature) is transferred to the filter for precipitation. The above washing solution is used to wash and precipitate for about 12 times, and the amount of washing solution is about 5ml each time.
如果检验员做不够洗涤次数,在干燥后的坩埚上就能清晰见到粉红色的物质,这是未洗涤尽的氢氧化钠与酚酞产生的物质颜色,终将导致钾含量偏高。因此,洗涤次数均不应低于12次。洗涤次数少于12次的原始结果与不少于12次的正确结果比较见表1。
If the inspector does not wash enough, the pink substance can be clearly seen on the dried crucible. This is the color of the substance produced by the unwashed sodium hydroxide and phenolphthalein, which will eventually lead to a high potassium content. Therefore, the washing times should not be less than 12 times. See Table 1 for the comparison between the original results of less than 12 times of washing and the correct results of no less than 12 times.
总结一下在
氢氧化钾产品的主含量氧化钾检验中,对几个关键环节必须给予足够的重视,对可能产生误差的各种因素要加以避免和克服,才能保证检验结果的准确度。
To sum up, in the test of potassium oxide in the main content of potassium hydroxide products, sufficient attention must be paid to several key links, and various factors that may cause errors must be avoided and overcome to ensure the accuracy of the test results.
The above is the details and points for attention of potassium hydroxide detection. I hope my sharing will help you. If you want to know more, please continue to pay attention to our website http://www.jinhao360.com , we will also release more relevant consultation later. Of course, if you don't understand anything, you are welcome to call.