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A kind of sampling device and sampling method of Karl Fischer titrator

The technology of a sample feeding device and a titrator is applied in the field of equipment for measuring the moisture of a sample by the Karl Fischer method, which can solve the problems such as the measurement result being lower than the actual value, the accuracy of the measurement result being poor, and the economic cost being increased, so as to prevent moisture from entering, Simple operation and low cost effect

Active Publication Date: 2016-01-13
NAT INST OF METROLOGY CHINA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method has the following disadvantages: due to the need to add a set of devices, thereby increasing the economic cost; moreover, because the inert gas may contain a small amount of moisture, there will be a moisture background value, if the moisture content in the measured sample is close to or less than the moisture background value When , the accuracy of the measurement results will be poor; in addition, because the moisture inside the solid sample may not be heated and volatilized, the measurement results will be lower than the actual value
However, for the sake of reality, "airtight first, then import", often leads to complicated device composition

Method used

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  • A kind of sampling device and sampling method of Karl Fischer titrator
  • A kind of sampling device and sampling method of Karl Fischer titrator
  • A kind of sampling device and sampling method of Karl Fischer titrator

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Embodiment

[0040] Step 1: If figure 1 As shown, under a stable indoor environment with a humidity of 20%, weigh the test sample 4 (pteroyl glutamate), and place the test sample 4 (pteroyl glutamate) on a dry and clean tray 5, Take off the bottle cap 2 of the Karl Fischer titrator reaction bottle, use the sealing film 3 to surround the bottle cap 2 and the tray 5, and make the two stick together to achieve a fixed connection, and then put the reaction bottle cap with the tray and the sample stopper to be tested Put it into the reaction bottle and cover it tightly; start the pre-titration, start the magnetic stirrer 8 to rotate continuously, until the instrument shows that the balance is reached, that is, the water in the bottle has been completely consumed by the reaction;

[0041] Step 2: If figure 2 As shown, the clean and dry metal fine needle 9 punctures the plastic gasket 1 sealed at the upper end of the bottle cap 2 of the reaction bottle, and props against the tray 5 bonded at th...

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Abstract

The invention relates to a sampling device of a Karl Fischer titrator and a sampling method thereof. The sampling device provided by the invention comprises a tray, an elastic bonding material and a fine needle, wherein the outer diameter of the tray is not larger than that of the lower end of a flask cover, the tray is bonded to the lower end of the cover of a reaction flask by the elastic bonding material and is positioned above the liquid level in the reaction flask; the fine needle penetrates through a plastic spacer for sealing an opening in the upper end of the flask cover, props against the tray bonded at the lower end of the flask cover and can separate the tray from the flask cover so as to enable the tray to fall into liquid in the reaction flask. The sampling method of the sampling device comprises the following steps that: when closing is implemented firstly, the tray is fixed by the elastic bonding material and then sealed above the liquid level inside the reaction; when the guiding is implemented subsequently, the fine needle penetrates through the plastic spacer for sealing the opening in the upper end of the reaction flask, and then a sample enters a reaction tank together with the tray. Therefore, the problem that a sealing environment is established for the sample in advance, but then the sealing is difficult to overcome can be solved, and the purposes that a measurement method is easy to operate, and that the measurement is accurate can be achieved.

Description

technical field [0001] The invention relates to equipment for measuring moisture in samples by Karl Fischer method, in particular to a sampling device and a sampling method for a Karl Fischer titrator. Background technique [0002] Moisture determination of solid samples is an important detection content in the fields of pharmaceutical analysis, food analysis, organic chemical analysis, and inorganic chemical analysis. Water is a common chemical analysis target, and the most commonly used determination method is the national standard method "GB / T606-2003 General Method for Determination of Moisture in Chemical Reagents Karl Fischer Method". The experimental principle is to use Karl Fischer reagent (a solution composed of iodine, sulfur dioxide, pyridine and methanol or ethylene glycol methyl ether) to quantitatively react with the water in the sample, so as to measure the concentration of water according to the reaction product or the current generated by the reaction. qual...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N5/00
Inventor 黄挺全灿戴新华何亚娟李红梅贡慧杨屹
Owner NAT INST OF METROLOGY CHINA
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