CN100557414C - A kind of mensuration nitrocotton nitrogen content and the inhomogeneity method of nitrogen amount - Google Patents

Abstract

This technology belongs to polymeric material field, is specifically related to a kind of natural polymer derivant---nitrocotton (NC) nitrogen content and the inhomogeneity mensuration of nitrogen amount.The NC fiber can be similar to regards a kind of uniaxial crystal as, behind the light incident NC fiber birefringence can take place.Birefraction and NC nitrogen content linear dependence.The present invention takes this as a foundation just, adopt polarizing microscope quarter-wave plate method by measuring in one batch (about 100) every NC fiber or more straight one section offset angle on it, and calculate the nitrogen content (numerical relation of offset angle and nitrogen content obtains by the NC compensating fibre angle of measuring some batches of known nitrogen contents) of this NC fiber by offset angle, with the mean value of to be measured batch of all NC fiber nitrogen contents nitrogen content as this batch NC fiber, with the standard variance of this batch NC fiber nitrogen content as weighing the index that this batch NC fiber nitrogen amount distributes.

Description

A kind of mensuration nitrocotton nitrogen content and the inhomogeneity method of nitrogen amount

Technical field

This technology relates to a kind of natural polymer derivant-nitrocotton nitrogen content and the inhomogeneity mensuration of nitrogen amount, belongs to field of polymer material detection.

Background technology

Nitrocotton claims nitrocellulose, cellulose nitrate (Nitrocellulose is called for short NC) again, and its range of application is very extensive.Militarily, nitrocotton is rifle, big gun, rocket and the missile armament principal ingredient with gunpowder and propellant; At civil area, nitrocotton can be used for producing rapid-curing cutback paint, automobile, furniture and other industrial ceramic lacquer, coating, xylonite goods etc.The homogeneity of nitrogen content and nitrogen amount is the main quality index of NC, and the main performance of its restriction and decision NC is as the quality of the height of energy, solubility property and processability etc.And the method for testing the NC nitrogen content is at present managed the average nitrogen content that nitrometer methods, interferometer mode, Di's Grindelwald alloyage etc. can only obtain a collection of NC as five, can not obtain the distribution situation of different N C fiber nitrogen content.The present invention promptly provides a kind of can obtain average nitrogen content of NC and the inhomogeneity method of nitrogen amount simultaneously.

Summary of the invention

The objective of the invention is to adopt polarizing microscope quarter-wave plate method test NC nitrogen content and nitrogen amount homogeneity.

Method of testing is:

1. selection and preparation refractive index are in the immersion liquid of 1.51-1.53, and immersion liquid is mixed by material 1 and material 2 among the present invention, and wherein, material 1 is glycerine, water, naphthalene bromide, and material 2 is kerosene, caryophyllus oil;

2. get dry NC fiber to be measured an amount of (about 100), spreading adds one to two immersion liquid on microslide equably, covered, and drive away issuable bubble;

3. polarizer and the analyzer of adjusting polarizing microscope make both quadratures, insert quarter wave plate, make still to be dark field;

4. ready testing sample is placed on the objective table, focus make more straight on a fiber or the fiber one section clear, rotate objective table, make fibre matting.Rotate 45 ° of objective tables again, make fiber the brightest;

5. the rotation analyzer makes fiber delustring once more, writes down angle (offset angle) β of analyzer rotation ₁

6. repeating step 4 and step 5 are measured an other fiber corresponding compensation angle β ₂

7. according to step 4 and step 5, measure all fibres corresponding compensation angle β ₃, β ₄, β ₅β _n, obtain average offset angle β

$\stackrel{\‾}{\mathrm{\β}}=\underset{i=1}{\overset{n}{\mathrm{\Σ}}}{\mathrm{\β}}_i$

8. measure the average offset angle of the nitrocotton fiber of 5-7 batch known average nitrogen amount with said method, average nitrogen content and the average offset angle data of each batch NC are done linear regression, obtain a standard working curve, curvilinear equation is

N％＝A+Bβ(1)

In the formula, A, B are instrument constant.

9. with the average offset angle β substitution formula (1) of to be measured batch of NC fiber, can obtain the average nitrogen content of this batch NC fiber;

10. the offset angle β that to be measured batch every NC fiber is recorded _iSubstitution formula (1) can be obtained the nitrogen content of every NC fiber; Can obtain the standard deviation D of this batch NC fiber nitrogen content according to formula (2) _ξ, and characterize the homogeneity that this batch NC nitrogen content distributes with this.

$D_{\mathrm{\ξ}}=\frac{\underset{i=1}{\overset{n}{\mathrm{\Σ}}}(\stackrel{\‾}{\mathrm{\β}}-{\mathrm{\β}}_i)}{n-1}---\left(2\right)$

11. the data relative deviation that the NC nitrogen content that obtains according to above-mentioned steps and the interferometer mode that generally adopts now record is in 0.1%.

Embodiment

Embodiment is as follows:

Embodiment 1

Measure 100 NC fibers, obtain its offset angle data and be:

4，6，5，6，4，5，7，6，6，6，4，3，10，5，4，4，7，6，3，5，4，12，2，3，5，6，5，5，7，6，4，2，6，7，6，2，8，4，3，3，7，6，4，3，4，6，3，4，6，4，6，4，6，5，7，5，5，7，4，5，6，5，4，10，4，6，6，6，6，6，5，7，5，3，3，7，6，4，6，6，7，2，4，5，6，2，5，5，5，5，5，5，14，3，6，5，6，2，5，6，5。

Try to achieve average offset angle β ₁=5.2, calculating average nitrogen content is 11.91%, D _ξ=3.677.

The nitrogen content of this batch NC that interferometer mode is measured is 11.9%, and both relative deviations are 0.08%.

Embodiment 2

Measure 100 NC fibers, obtain its offset angle data and be:

1，1，2，0，1，0，3，0，2，3，0，1，3，4，1，2，0，0，1，1，1，0，0，1，0，0，0，4，1，3，1，2，0，0，1，1，0，1，0，3，0，0，0，2，1，0，1，0，1，0，2，2，1，0，0，4，1，2，0，3，2，3，0，1，0，4，2，5，0，2，0，0，1，1，0，0，1，0，3，1，0，0，1，1，0，0，0，1，1，1，0，1，3，1，1，1，1，1，1。

Try to achieve average offset angle β ₁=0.86, calculating average nitrogen content is 12.166%, D _ξ=1.853.

The nitrogen content of this batch NC that interferometer mode is measured is 12.17%, and both relative deviations are 0.03%.

Embodiment 3

Measure 100 NC fibers, obtain its offset angle data and be:

5，1，6，2，3，1，7，2，3，4，6，2，3，4，6，3，3，4，3，3，4，4，5，3，2，3，8，3，2，2，2，3，1，3，3，3，2，3，3，3，2，3，4，3，1，1，5，1，2，3，3，1，5，4，1，4，4，2，1，10，3，2，1，7，4，1，1，1，3，3，1，1，3，3，1，1，2，1，1，1，4，3，1，1，4，3，1，1，2，2，1，1，2，2，2，4，2，3，2，6。

Try to achieve average offset angle β ₁=2.81, calculating average nitrogen content is 12.25%, D _ξ=2.943.

The nitrogen content of this batch NC that interferometer mode is measured is 12.25%, and both relative deviations are 0%.

Embodiment 4

Measure 100 NC fibers, obtain its offset angle data and be:

17，14，15，10，10，16，9，16，11，12，14，12，12，18，12，10，14，14，20，8，10，14，22，12，8，14，10，13，12，10，10，10，16，12，10，20，10，12，10，18，20，12，11，10，10，11，5，16，14，11，12，16，16，14，22，25，16，13，8，10，13，16，22，17，12，17，10，18，12，11，17，12，18，10，15，19，16，12，15，15，12，11，15，15，10，10，15，12，10，9，15，19，10，13，12，17，16，10，12，16。

Try to achieve average offset angle β ₁=13.53, calculating average nitrogen content is 12.71%, D _ξ=14.11.

The nitrogen content of this batch NC that interferometer mode is measured is 12.72%, and both relative deviations are 0.08%.

Claims (1)

1. measure nitrocotton nitrogen content and the inhomogeneity method of nitrogen amount for one kind, the method for testing that it is characterized in that it specifically:

(1) selection and preparation refractive index are in the immersion liquid of 1.51-1.53, and immersion liquid is mixed by material 1 and material 2, and wherein material 1 is glycerine, water, naphthalene bromide, and material 2 is kerosene, caryophyllus oil;

(2) it is an amount of to get dry NC fiber to be measured, and spreading adds one to two immersion liquid on microslide equably, covered, and drive away bubble;

(3) polarizer and the analyzer of adjustment polarizing microscope make both quadratures, insert quarter wave plate, make still to be dark field;

(4) ready testing sample is placed on the objective table, rotate objective table, make fibre matting, rotate 45 ° of objective tables again, make fiber the brightest;

(5) the rotation analyzer makes fiber delustring once more, writes down the angle of analyzer rotation, promptly refers to offset angle β ₁

(6) repeating step 4 and step 5 are measured an other fiber corresponding compensation angle β ₂

(7), measure all fibres corresponding compensation angle β according to step 4 and step 5 ₃, β ₄, β ₅... β _n, obtain average offset angle β,

$\stackrel{\‾}{\mathrm{\β}}=\underset{i=1}{\overset{n}{\mathrm{\Σ}}}{\mathrm{\β}}_i$

(8) measure the average offset angle of the nitrocotton fiber of 5-7 batch known average nitrogen amount with said method, average nitrogen content and the average offset angle data of each batch NC are done linear regression, obtain a standard working curve, curvilinear equation is

N％＝A+Bβ (1)

In the formula, A, B are instrument constant;

(9), can obtain the average nitrogen content of this batch NC fiber with the average offset angle β substitution formula (1) of to be measured batch of NC fiber;

(10) the offset angle β that to be measured batch every NC fiber is recorded _iSubstitution formula (1) can be obtained the nitrogen content of every NC fiber; Can obtain the standard deviation D of this batch NC fiber nitrogen content according to formula (2) _ξ, and characterize the homogeneity that this batch NC nitrogen content distributes with this;

$D_{\mathrm{\ξ}}=\frac{\underset{i=1}{\overset{n}{\mathrm{\Σ}}}(\stackrel{\‾}{\mathrm{\β}}-{\mathrm{\β}}_i)}{n-1}.---\left(2\right)$