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Method for detecting moisture content of cellulose ester

A cellulose ester and moisture technology, applied in the field of analysis, can solve problems such as long time-consuming, large human error, poisonous and harmful, etc., and achieve the effect of simple operation and short time-consuming

Inactive Publication Date: 2014-12-03
SICHUAN NITROCELLULOSE CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method cannot accurately measure the moisture content of alcohol-containing cellulose nitrate, it is only a rough judgment, and the human error is large
[0006] The Karl Fischer moisture detector is currently recognized as a more accurate instrument for detecting moisture. However, this method not only uses iodine, sulfur dioxide, pyridine, methanol and other substances, but also has many types, and is toxic and harmful. At the same time, the method takes time to measure a sample. Long, so not suitable for industrial detection

Method used

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  • Method for detecting moisture content of cellulose ester

Examples

Experimental program
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Effect test

Embodiment 1

[0038] a. Detection of moisture content in standard samples:

[0039] Using the Karl Fischer method, the moisture content of the ethanol / isopropanol coating cellulose nitrate H80 seconds was measured to be 3.38%.

[0040] The specific operation steps are as follows: Weigh 2g of the product containing ethanol / isopropanol coating cellulose nitrate H for 80 seconds, add 35g of butyl acetate to dissolve, after the sample is completely dissolved, weigh 0.4g of the solution, and inject Karl Fischer In the titration cup of the instrument, the automatic titration by the Karl Fischer instrument can determine the moisture content of the standard sample solution; at the same time, weigh 0.7g butyl acetate to measure the blank moisture value of butyl acetate; through the formula: H 2 O%=【(m 标样 +m 丁酯 )*C-(m 丁酯 *C 丁酯 )】 / m 标样 (In the formula, C represents the moisture content of the standard sample, C 丁酯 Indicates the moisture content of butyl acetate) to obtain the moisture content of...

Embodiment 2

[0048] For the determination of the moisture content of the standard sample in this embodiment and the establishment of the standard curve by the area external standard method, see steps a, b and c of Example 1.

[0049] Weigh 5g of ethanol-containing paint cellulose nitrate L1 / 8 seconds, add 25mL of isopropanol, shake for 15min, centrifuge, take 2uL of the supernatant and inject it into the chromatograph, and use the standard curve to establish the standard curve. For example, the moisture content of the coating cellulose nitrate L1 / 8s containing ethanol in the sample to be tested is 6.57%. The gas chromatographic conditions in this embodiment are column temperature 140°C and vaporization temperature 160°C.

Embodiment 3

[0051] For the determination of the moisture content of the standard sample in this embodiment and the establishment of the standard curve by the area external standard method, see steps a, b and c of Example 1.

[0052] Weigh 5g of ethanol-containing coating cellulose nitrate product H for 20 seconds, add 25mL of isopropanol, shake for 15min, centrifuge, take 2uL of the supernatant and inject it into the chromatograph, and use the established standard curve to measure the The moisture content of the ethanol-containing coating cellulose nitrate product H20 seconds in the test sample was 4.51%. The gas chromatographic conditions in this embodiment are column temperature 140°C and vaporization temperature 160°C.

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Abstract

The invention belongs to the technical field of analysis, and in particular relates to a method for detecting the moisture content of cellulose ester. The method comprises the following steps: A, accurately weighing a standard sample with known moisture content, adding leach liquor, leaching, centrifuging, and taking the supernate for later use; performing gas chromatography detection on the supernate so as to obtain the peak area of the moisture; weighing two samples with known moisture content, repeating the steps so as to obtain the peak area of the moisture of each sample, and establishing a standard curve y=ax+b of the peak areas and the moisture content; and B, repeating the steps for a sample to be detected by using an area external standard method, so as to obtain the peak area of the moisture, and calculating the content of the moisture in the sample to be detected according to the standard curve established in the step A. By adopting the method, the moisture content can be accurately detected, the operation time is short, no toxic solvent is adopted, and thus a relatively effective method is provided for detection on moisture content of cellulose ester.

Description

technical field [0001] The invention belongs to the technical field of analysis, and in particular relates to a method for detecting the water content in cellulose ester. Background technique [0002] Cellulose esters include cellulose nitrate, cellulose acetate butyrate, cellulose acetate or cellulose acetate propionate, etc., which contain a certain amount of moisture. If the moisture is too high, it will affect the application of cellulose ester, so the detection of cellulose The moisture content of the ester is very essential. [0003] For example: cellulose nitrate is a white or yellowish solid fibrous material. Alcohol-containing cellulose nitrate is obtained by flooding cellulose nitrate with alcohols. Alcohol-containing cellulose nitrate has a wide range of applications , mainly used in military medicine, civilian paint ink, etc. [0004] The traditional method for detecting moisture in alcohol-containing cellulose nitrate is the Cupley method. This analysis method...

Claims

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Application Information

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IPC IPC(8): G01N30/02
Inventor 夏晓玉程从勇赵利斌张尧石燕
Owner SICHUAN NITROCELLULOSE CORP