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Method for determining iron soap content in emulsion

A measurement method and emulsion technology, applied in the direction of weighing by removing certain components, can solve problems such as iron soap is not easy to separate

Inactive Publication Date: 2017-05-17
QUAKER CHEM CHINA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The purpose of the invention is to overcome the deficiencies in the prior art, provide a kind of assay method of iron soap content in the emulsion, solve the problem that iron soap is not easy to separate with other emulsion components; analyze iron soap content fast, accurately, analysis error Meet the error requirements of conventional chemical analysis methods

Method used

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  • Method for determining iron soap content in emulsion
  • Method for determining iron soap content in emulsion
  • Method for determining iron soap content in emulsion

Examples

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no. 1 example

[0050] The first embodiment: the normal phase solid phase extraction column used in this embodiment is: HF Mega BE-Si, 5 gm, 20 ml (Agilent, Part No: 14256026).

[0051] Sample dehydration step: Accurately weigh 200.00g of the emulsion sample, heat it for 2 hours with a rotary evaporator at a vacuum degree greater than or equal to 0.09Mpa, and a water bath of 60°C to obtain a dehydrated sample, and collect it in a 50ml small beaker.

[0052] Purification step: place the 50ml small beaker on the magnetite for 30min.

[0053] Iron soap enrichment step, sample the test sample of 1.0000g gram from the top of the dehydrated sample, dissolve it with 10ml chloroform to obtain the chloroform aqueous solution of the test sample, add the normal phase solid phase extraction column activated with 20ml chloroform in advance, Control the chloroform aqueous solution of the test sample to pass through the normal phase solid phase extraction column at a speed of 1ml / min, and wash the normal ph...

no. 2 example

[0057] The second embodiment: the normal phase solid phase extraction column used in this embodiment is: HF Mega BE-Si, 5 gm, 20 ml (Agilent, Part No: 14256026).

[0058] Sample dehydration step: Accurately weigh 400.00g of the emulsion sample, heat it for 2 hours with a rotary evaporator at a vacuum degree greater than or equal to 0.09Mpa, and a water bath at 70°C to obtain a dehydrated sample, and collect it in a 50ml small beaker.

[0059] Purification step: place the 50ml small beaker on the magnetite for 30min.

[0060] Iron soap enrichment step, sample the test sample of 5.0000g gram from the top of the dehydrated sample, dissolve it with 20ml chloroform to obtain the chloroform aqueous solution of the test sample, add the normal phase solid phase extraction column activated with 60ml chloroform in advance, Control the chloroform aqueous solution of the test sample to pass through the normal phase solid phase extraction column at a speed of 1ml / min, and wash the normal p...

no. 3 example

[0064] The third embodiment: the normal phase solid phase extraction column used in this embodiment is: CNWBOND SI SPE2G, 10ML (Anpel, Part No: SBEQ-CA1358)

[0065] Sample dehydration step: Accurately weigh 100.00g of the emulsion sample, heat it for 1 hour with a rotary evaporator at a vacuum degree greater than or equal to 0.09Mpa, and a water bath of 60°C to obtain a dehydrated sample, and collect it in a 50ml small beaker.

[0066] Purification step: place the 50ml small beaker on the magnetite for 30min.

[0067] Iron soap enrichment step, sample 0,5000g of test sample from the top of the dehydrated sample, dissolve it with 10ml of chloroform to get the chloroform aqueous solution of the test sample, add it to the normal phase solid phase extraction column activated in advance with 10ml of chloroform , the chloroform aqueous solution of the test sample is controlled to pass through the normal phase solid phase extraction column at a speed of 1ml / min, and the normal phase...

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Abstract

The invention discloses a method for determining the iron soap content in an emulsion. The method comprises the following steps: weighing an emulsion sample having a weight Ws, adding into a round-bottom flask having a weight W1, and performing vacuum dewatering to obtain a dewatered sample in the round-bottom flask, wherein the total weight after dewatering is W2; adsorbing iron powder in the dewatered sample by means of a magnet; taking a test sample having a weight W3 from the top of the dewatered sample, preparing a test sample trichloromethane solution, passing the solution through a normal solid-phase extraction column at a rate of 1-2 ml / min, and sequentially eluting the normal solid-phase extraction column with trichloromethane and isopropanol; passing a 2-10wt.% hydrochloric acid isopropanol solution through the normal solid-phase extraction column at a rate of 1 ml / min or below to obtain a separation eluate, collecting the obtained separation eluate by means of a beaker having a weight W4, evaporating the solvent of the separation eluate, and cooling to obtain a collection; removing impurities in the collection, wherein the total weight of the impurity-removed collection and the beaker is W5; and determining the iron soap content W% according to a computing formula shown in the specification.

Description

technical field [0001] The invention relates to a method for measuring iron soap content in emulsion. Background technique [0002] During the cold rolling process of strip steel, due to the high temperature and high pressure in the rolling deformation zone in the roll gap area, a large amount of iron powder with a diameter of micron is produced by the wear between the strip steel and the roll, and a large part of these iron powder is recycled. The system enters the emulsion system. These iron powders are active iron powders with a large amount of charge. Because the emulsion of cold-rolled steel contains a certain amount of fatty acid, the rolling oil droplets of these active iron powders in the emulsion attract each other to form iron soap, which has a large viscosity. When the iron soap value reaches a certain level, many problems will arise. When it is sprayed onto the rolling mill, it is easy to adhere to the rolls and the rolling mill, causing a large amount of sludg...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N5/04
CPCG01N5/04
Inventor 谭芳
Owner QUAKER CHEM CHINA
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