CN104062387B - The detection method of content of fatty acid is moved between the bonding system internal layer of solid propellant - Google Patents
The detection method of content of fatty acid is moved between the bonding system internal layer of solid propellant Download PDFInfo
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- CN104062387B CN104062387B CN201310086431.XA CN201310086431A CN104062387B CN 104062387 B CN104062387 B CN 104062387B CN 201310086431 A CN201310086431 A CN 201310086431A CN 104062387 B CN104062387 B CN 104062387B
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Abstract
The present invention is the detection method of moving content of fatty acid between the bonding system internal layer of a kind of solid propellant.It comprises five steps: determine detected object, and preparation detects sample, selects testing conditions, makes calibration curve, forms data list.Stearic acid in the bonding system that its detected object is made up of EPDM rubber insulation, end hydroxy butadiene lining and nitrate ester plasticized polyether propellant and palmitic acid.It utilizes high performance liquid chromatography, by detecting the detecting step such as sample preparation, calibration curve making, data list display, realize the detection of stearic acid in the heat insulation layer to heat insulation layer/bonding system of lining/propellant and between heat insulation layer and lining and palmitic acid migration amount.It is widely used in the adhesive property and mechanical property of evaluating rocket solid propellant bonding system, and have that detection method is simple, experimentation is conveniently promoted, detect the good and data processing accurately reliable advantage of data redundancy.
Description
Art
The present invention relates to a kind of red, orange, green, blue, yellow (ROGBY) of space flight high polymer chemistry fuel, specifically between the bonding system internal layer of a kind of solid propellant, move the detection method of content of fatty acid.
Background technology
At space flight high polymer chemistry fuel area, usual employing is the bonding system of nitrate plasticising polyethers NEPE propellant, wherein, heat insulation layer is ethylene-propylene-diene rubber EPDM, bonding lining is end hydroxy butadiene HTPB prepolymer, there is the migration of stearic acid and palmitic acid between heat insulation layer and bonding lining, the interlayer fatty acid that namely there is the bonding system heat insulation layer of propellant and lining moves.In order to ensure storage adhesive property and the storage mechanical property of the bonding system of propellant, ensureing the q&r of propellant, being necessary the interlayer fatty acid migration amount understanding the bonding system heat insulation layer of propellant and lining.
In prior art, the interlayer fatty acid not relating to the bonding system heat insulation layer of propellant and lining moves quantity measuring method, and be generally used for the stearic acid of food industry and rubber industry and palmitic acid content and detect and all have many defects, comprise sample preparation complexity, testing cost higher, detect that reappearance is low and detection accuracy is poor.
Summary of the invention
The object of the invention is to provide the detection method of moving content of fatty acid between the bonding system internal layer of a kind of solid propellant, it can simplify the processing procedure and reduction testing cost that detect sample effectively, greatly improves and detects reappearance and detection accuracy.
Technical scheme of the present invention is: design the detection method of moving content of fatty acid between the bonding system internal layer of a kind of solid propellant, comprise following five steps:
Step one, determines detected object: detected object is stearic acid and palmitic acid in the bonding system of ethylene-propylene-diene rubber EPDM heat insulation layer, end hydroxy butadiene HTPB lining and nitrate plasticising polyethers NEPE propellant composition;
Step 2, preparation detects sample: the bonding test specimen obtaining ethylene-propylene-diene rubber EPDM heat insulation layer, end hydroxy butadiene HTPB lining and nitrate plasticising polyethers NEPE propellant composition, block is become to peel off bonding heat insulation layer and bonding lining, stripping block is cut into particulate, to chop up a quantitative weighing, form acetone and soak extract, undertaken quantitatively by external standard method;
Step 3, selects testing conditions: checkout equipment is HPLC ELSD detecting device, and chromatographic separation condition is C18 chromatographic column, and mobile phase is acetonitrile/methanol/water;
Step 4, make calibration curve: adopt external standard calibration curve standard measure, take a certain amount of stearic acid and palmitic acid, be placed in volumetric flask, with acetone solution, dilution and constant volume, be mixed with the solution of known actual concentrations, with reference to testing conditions, draw calibration curve, calculate the content of the bonding system internal insulation of propellant and lining stearic acid and palmitic acid;
Step 5, forms data list: detect data according to stearic acid and palmitic acid content, makes list display and detects precision and accuracy in detection.
The invention has the beneficial effects as follows: have employed the immersion of analysis pure acetone owing to detecting sample preparation steps, the testing conditions selected is: checkout equipment is HPLC ELSD detecting device, chromatographic separation condition is C18 chromatographic column, mobile phase is acetonitrile/methanol/water, thus reduces testing cost, simplifies process of the test.Have employed into owing to detecting sample preparation steps the processing procedure that block is peeled off, pelletizing is weighed and acetone soaks, thus for the detection of migration component provides best test specimen simultaneously.In addition owing to can calculate stearic acid and the palmitic acid content of the bonding system internal insulation of propellant and lining by making calibration curve, and the preci-sion and accuracy of detection method can be shown by making data list, thus ensure that the feasibility of detection method, for the quality control of the bonding system of propellant of propellant/lining/heat insulation layer/composition provides technical support.The present invention also has that detection method is simple, experimentation is conveniently promoted, detect the good and data processing accurately reliable advantage of data reappearance.
Embodiment
The present invention is further described to divide two groups below in conjunction with embodiment.
First group, the assay method of stearic acid and palmitic acid content in heat insulation layer in heat insulation layer/bonding system of lining/propellant.
Step one, determines detected object: detected object is stearic acid in the bonding system of ethylene-propylene-diene rubber EPDM heat insulation layer, end hydroxy butadiene HTPB lining and nitrate plasticising polyethers NEPE propellant composition in ethylene-propylene-diene rubber EPDM heat insulation layer and palmitic acid.
Step 2, preparation detects sample: the bonding test specimen obtaining ethylene-propylene-diene rubber EPDM heat insulation layer, end hydroxy butadiene HTPB lining and nitrate plasticising polyethers NEPE propellant composition, block is become to peel off heat insulation layer, stripping block is cut into the particulate that specification is 1mm × 1mm × 1mm, by 0.5 – 2.0g standard, quantitative weighing is carried out to chopped up grain, put into 50ml tool plug triangular flask, add and analyze pure acetone 20ml, soak more than 48h, formed and soak extract, washing is transferred to 50ml volumetric flask constant volume, adopts external standard method to carry out quantitatively.
Step 3, selects testing conditions: checkout equipment is HPLC ELSD detecting device, and chromatographic separation condition is C18 chromatographic column, and mobile phase is acetonitrile/methanol/water.
Step 4, make calibration curve: adopt external standard calibration curve standard measure, take a certain amount of stearic acid and palmitic acid, be placed in 50ml volumetric flask, with acetone solution, dilution and constant volume, be mixed with the solution of known actual concentrations, with reference to selected testing conditions, draw calibration curve, according to calibration curve, obtain the stearic acid in heat insulation layer and palmitic acid content respectively.
Detect sample with high effective liquid chromatography for measuring, adopt the liquid phase chromatogram condition of acetonitrile/methanol/water, evaporative light-scattering detector detects, external standard calibration curve standard measure.Computing formula is as follows:
In formula, M is the massfraction (%) detecting stearic acid or palmitic acid in sample, C
ifor detecting the concentration g/ml of stearic acid or palmitic acid in sample, m is the quality g detecting sample, and 50 is constant volume number ml.
Step 5, forms data list: detect data according to stearic acid or palmitic acid content, makes list display and detects precision and accuracy in detection.
Table 1 surveys by high performance liquid chromatography the method precision (%) of stearic acid and palmitic acid content in bonding heat insulation layer.
Table 2 surveys by high performance liquid chromatography the method accuracy of stearic acid and palmitic acid content in bonding heat insulation layer.
Table 1: the method precision (%) of high effective liquid chromatography for measuring bonding heat insulation layer stearic acid and palmitic acid content
Table 2: the method accuracy of stearic acid and palmitic acid content in high effective liquid chromatography for measuring bonding heat insulation layer
Second group, in heat insulation layer/bonding system of lining/propellant, heat insulation layer moves to the mensuration of stearic acid in lining and palmitic acid content.
Step one, determines detected object: the stearic acid in the end hydroxy butadiene HTPB bonding lining in the bonding system that detected object is made up of ethylene-propylene-diene rubber EPDM heat insulation layer, end hydroxy butadiene HTPB bonding lining and nitrate plasticising polyethers NEPE propellant and palmitic acid;
Step 2, preparation detects sample: obtain ethylene-propylene-diene rubber EPDM heat insulation layer, end hydroxy butadiene HTPB bonds lining and the bonding test specimen of nitrate plasticising polyethers NEPE propellant composition, become block release liner, stripping block is cut into the particulate that specification is 1mm × 1mm × 1mm, by 0.5 – 2.0g standard, quantitative weighing is carried out to chopped up grain, put into 50ml tool plug triangular flask, add and analyze pure acetone 20ml, soak more than 48h, formed and soak extract, washing is transferred to 50ml volumetric flask constant volume, adopts external standard method to carry out quantitatively.
Step 3, selects testing conditions: checkout equipment is HPLC ELSD detecting device, and chromatographic separation condition is C18 chromatographic column, and mobile phase is acetonitrile/methanol/water.
Step 4, make calibration curve: adopt external standard calibration curve standard measure, take a certain amount of stearic acid and palmitic acid, be placed in 50ml volumetric flask, with acetone solution, dilution and constant volume, be mixed with the solution of known actual concentrations, with reference to selected testing conditions, draw calibration curve, according to calibration curve, obtain heat insulation layer in heat insulation layer/bonding system of lining/propellant respectively and move to stearic acid in lining and palmitic acid content.
Detect sample with high effective liquid chromatography for measuring, adopt the liquid phase chromatogram condition of acetonitrile/methanol/water, evaporative light-scattering detector detects, external standard calibration curve standard measure.Computing formula is as follows:
In formula, M is the massfraction (%) detecting stearic acid and palmitic acid in sample, C
ifor detecting the concentration g/ml of stearic acid and palmitic acid in sample, m is the quality g detecting sample, and 50 is constant volume number ml.
Step 5, forms data list: detect data according to stearic acid or palmitic acid content, makes list display and detects precision and accuracy in detection.
Table 3 is the method precision (%) of stearic acid and palmitic acid content in high effective liquid chromatography for measuring lining.
Table 4 is the method accuracy of stearic acid and palmitic acid content in high effective liquid chromatography for measuring lining.
Table 3: the method precision (%) of stearic acid and palmitic acid content in high effective liquid chromatography for measuring lining
Table 4: the method accuracy of high effective liquid chromatography for measuring lining stearic acid and palmitic acid content
Claims (2)
1. move a detection method for content of fatty acid between the bonding system internal layer of solid propellant, it is characterized in that comprising following five steps:
Step one, determines detected object: the stearic acid in the bonding system that detected object is made up of ethylene-propylene-diene rubber EPDM heat insulation layer, end hydroxy butadiene HTPB lining and nitrate plasticising polyethers NEPE propellant and palmitic acid;
Step 2, preparation detects sample: obtain propellant bonding system test specimen, becomes block to peel off bonding heat insulation layer and lining, strippings block is cut into particulate, to chop up a quantitative weighing, form acetone immersion extract, undertaken quantitatively by external standard method;
Step 3, selects testing conditions: checkout equipment is HPLC ELSD detecting device, and chromatographic separation condition is C18 chromatographic column, mobile phase is acetonitrile/methanol/water;
Step 4, make calibration curve: adopt external standard calibration curve standard measure, take a certain amount of stearic acid and palmitic acid, be placed in volumetric flask, with acetone solution, dilution and constant volume, be mixed with the solution of known actual concentrations, with reference to testing conditions, draw calibration curve, calculate stearic acid and the palmitic acid content of bonding heat insulation layer and lining in the bonding system of propellant;
Step 5, forms data list: detect data according to stearic acid and palmitic acid content, makes list display and detects precision and accuracy in detection.
2. between the bonding system internal layer of solid propellant according to claim 1, move the detection method of content of fatty acid, it is characterized in that: when preparation detects sample, a specification that chops up is 1mm × 1mm × 1mm, the weight quantitatively taken is 0.5 – 2.0g, adopts analysis pure acetone 20 – 30ml to produce immersion extract.
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