CN104181265B - Determination of fatty acid method in propellant heat insulation layer - Google Patents
Determination of fatty acid method in propellant heat insulation layer Download PDFInfo
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- CN104181265B CN104181265B CN201310194344.6A CN201310194344A CN104181265B CN 104181265 B CN104181265 B CN 104181265B CN 201310194344 A CN201310194344 A CN 201310194344A CN 104181265 B CN104181265 B CN 104181265B
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Abstract
The present invention is a kind of for determination of fatty acid method in the propellant heat insulation layer of space flight high polymer chemistry fuel Physico-chemical tests.Comprise five steps: determine detected object, preparation detects sample, selects testing conditions, makes calibration curve, forms data list.With the fatty acid extract of propellant different substrate materials rubber elastomer heat insulation layer for detected object; Prepare detect sample time, the preparation of test samples extract adopt analyze pure acetone as Extraction solvent, heat ultrasonic extraction 60 minutes at 40 DEG C and cooling leaves standstill mode; When selecting testing conditions, mobile phase is acetonitrile/water.It with butyronitrile, butyl and Ethylene Propylene Terpolymer three kinds of heat insulation layers for detected object, utilize high performance liquid chromatography, by described step, realization to determination of fatty acid in different substrate materials rubber elastomer heat insulation layer, and has sample preparation cycle time, testing efficiency is high, low testing cost, experimental technique are reproducible, detect the high advantage of data accuracy.
Description
Technical field
The present invention relates to a kind of red, orange, green, blue, yellow (ROGBY) of aerospace fuel chemical field, specifically a kind of determination of fatty acid method in propellant heat insulation layer.
Background technology
In document, so far there are no relates to stearic acid in the different substrate materials such as butyronitrile, butyl rubber elastomer heat insulation layer and palmitic acid massfraction assay method report.Be stearic acid Extraction and enrichment wherein about in rubber, stearic acid massfraction mensuration is also rarely seen, and be derivatized to methyl stearate, can after instantaneous vaporization, adopt gas chromatography determination, the stearic acid massfraction in fact at present in food or industrial raw materials measures and adopts said method more.Before liquid chromatography for measuring stearic acid massfraction many employings post of bibliographical information or post-column derivation method, to reduce its reserve capability on a column, or adopt derivatization method to make it bring corresponding functional group, be convenient to UV-detector or fluorescence detector detects.
Chinese patent application 201310086431.X proposes the detection method of moving content of fatty acid between the bonding system internal layer of a kind of solid propellant, and its detected object is Ethylene Propylene Terpolymer heat insulation layer and the stearic acid moved in fourth hydroxyl lining thereof and palmitic acid in the bonding system of propellant; When detecting sample preparation, employing be that acetone soaks more than 48 hours as Extraction solvent, and shift, wash, constant volume is in 50ml volumetric flask; Select acetonitrile/methanol/water as mobile phase in testing conditions.The defect of this method is: specific detected object should not be applicable to the detection of other formulated adhesive heat insulation layer, the sample preparation cycle is long, operation steps is many, the expense cost of test process is high, and the reappearance of experimental technique is limited, and the accuracy rate detecting data is easily disturbed.
Summary of the invention
The object of the invention is to provide a kind of determination of fatty acid method in propellant heat insulation layer, it can adapt to multiple detected object effectively, greatly simplifies and detects Sample Preparation Procedure, reliably improves the reappearance of experimental technique and detects the accuracy rate of data.
Technical scheme of the present invention is:
Design a kind of determination of fatty acid method in propellant heat insulation layer, comprise following five steps: determine detected object, preparation detects sample, select testing conditions, make calibration curve, form data list, it is characterized in that: determining in detected object process, fatty acid extract in the heat insulation layer being base material with the different bonding agent of propellant, for detected object, comprises, butyronitrile heat insulation layer, butyl heat insulation layer and Ethylene Propylene Terpolymer heat insulation layer; Detect in sample in preparation, the preparation of test samples extract adopt analyze pure acetone as Extraction solvent, heat ultrasonic extraction 60 minutes at 40 DEG C and cooling leaves standstill mode; In selection testing conditions process, the mobile phase of selection is acetonitrile/water.
The invention has the beneficial effects as follows: owing to determining in detected object process, the fatty acid extract that have selected in different substrate materials rubber elastomer heat insulation layer is detected object, thus adapts to the fatyy acids needs in other base material heat insulation layers preferably.Simultaneously due to the preparation of test samples extract have employed 40 DEG C at heat ultrasonic extraction 60 minutes and cooling leaves standstill mode, thus highly shortened Sample Preparation Procedure, simplify experimental procedure.Be mobile phase owing to have selected acetonitrile/water targetedly in addition, thus optimize testing conditions.The present invention also has that method is simple, easy to operate, experimental technique favorable reproducibility and detect the high advantage of data accuracy.
Embodiment
The present invention is further described to divide three groups below in conjunction with embodiment.
First group, the assay method of stearic acid and palmitic acid massfraction in propellant butyronitrile heat insulation layer.
Step one, determines detected object: detected object is stearic acid and palmitic acid massfraction in propellant butyronitrile heat insulation layer.
Step 2, preparation detects sample: obtain butyronitrile heat insulation layer, be cut into particulate, take weight 0.30 ~ 2.0g in sample bottle, accurately add 40ml and analyze pure acetone, at 40 DEG C, heat ultrasonic extraction 60 minutes with ultrasonic cleaner, cooling leaves standstill, and forms fatty acid extract.
Step 3, selects testing conditions: checkout equipment is high performance liquid chromatography (HPLC), and separation condition is C18 chromatographic column, mobile phase is acetonitrile/water, and evaporative light-scattering detector detects.
Step 4, makes calibration curve: adopt external standard calibration curve standard measure, take a certain amount of stearic acid and palmitic acid, be mixed with the solution of known actual concentrations.According to the liquid phase chromatogram condition that step 2 is selected, be depicted as calibration curve.According to calibration curve, obtain the stearic acid in butyronitrile heat insulation layer and palmitic acid massfraction.
Detect sample with high effective liquid chromatography for measuring, adopt the liquid phase chromatogram condition of acetonitrile/water, evaporative light-scattering detector detects, and according to calibration curve, obtains the stearic acid in butyronitrile heat insulation layer and palmitic acid massfraction.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 40 is sample solution volume number ml.
Step 5, forms data list: will detect data creating data list, detects data according to the stearic acid in butyronitrile heat insulation layer or palmitic acid massfraction, makes list display and detects precision and accuracy in detection.
Table 1 measures the method precision (%) of butyronitrile heat insulation layer stearic acid and palmitic acid massfraction for HPLC method.
Table 2 is the method accuracy of stearic acid and palmitic acid massfraction in HPLC method mensuration butyronitrile heat insulation layer.
Table 1HPLC method measures the method precision (%) of butyronitrile heat insulation layer stearic acid and palmitic acid massfraction
Table 2HPLC method measures the method accuracy of stearic acid and palmitic acid massfraction in butyronitrile heat insulation layer
Second group, the assay method of stearic acid and palmitic acid massfraction in propellant butyl heat insulation layer.
Step one, determines detected object: detected object is stearic acid and palmitic acid massfraction in propellant butyl heat insulation layer.
Step 2, preparation detects sample: obtain butyl heat insulation layer, be cut into particulate, take weight 0.30 ~ 2.0g in sample bottle, accurately add 40ml and analyze pure acetone, at 40 DEG C, heat ultrasonic extraction 60 minutes with ultrasonic cleaner, cooling leaves standstill, and forms fatty acid extract.
Step 3, selects testing conditions: checkout equipment is high performance liquid chromatography (HPLC), and separation condition is C18 chromatographic column, mobile phase is acetonitrile/water, and evaporative light-scattering detector detects.
Step 4, makes calibration curve: adopt external standard calibration curve standard measure, take a certain amount of stearic acid and palmitic acid, be mixed with the solution of known actual concentrations.According to the liquid phase chromatogram condition that step 2 is selected, be depicted as calibration curve.According to calibration curve, obtain the stearic acid in butyl heat insulation layer and palmitic acid massfraction.
Detect sample with high effective liquid chromatography for measuring, adopt the liquid phase chromatogram condition of acetonitrile/water, evaporative light-scattering detector detects, and according to calibration curve, obtains the stearic acid in butyl heat insulation layer and palmitic acid massfraction.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 40 is sample solution volume number ml.
Step 5, forms data list: will detect data creating data list, detects data according to the stearic acid in butyl heat insulation layer or palmitic acid massfraction, makes list display and detects precision and accuracy in detection.
Table 3 is the method precision (%) of stearic acid and palmitic acid massfraction in HPLC method mensuration butyl heat insulation layer.
Table 4 is the method accuracy of stearic acid and palmitic acid massfraction in HPLC method mensuration butyl heat insulation layer.
Table 3HPLC method measures the method precision (%) of stearic acid and palmitic acid massfraction in butyl heat insulation layer
Table 4HPLC method measures the method accuracy of stearic acid and palmitic acid massfraction in butyl heat insulation layer
3rd group, the assay method of stearic acid and palmitic acid massfraction in propellant Ethylene Propylene Terpolymer heat insulation layer.
Step one, determines detected object: detected object is stearic acid and palmitic acid massfraction in propellant Ethylene Propylene Terpolymer heat insulation layer.
Step 2, preparation detects sample: obtain Ethylene Propylene Terpolymer heat insulation layer, be cut into particulate, take weight 0.30 ~ 2.0g in sample bottle, accurately add 40ml and analyze pure acetone, at 40 DEG C, heat ultrasonic extraction 60 minutes with ultrasonic cleaner, cooling leaves standstill, and forms fatty acid extract.
Step 3, selects testing conditions: checkout equipment is high performance liquid chromatography (HPLC), and separation condition is C18 chromatographic column, mobile phase is acetonitrile/water, and evaporative light-scattering detector detects.
Step 4, makes calibration curve: adopt external standard calibration curve standard measure, take a certain amount of stearic acid and palmitic acid, be mixed with the solution of known actual concentrations.According to the liquid phase chromatogram condition that step 2 is selected, be depicted as calibration curve.According to calibration curve, obtain the stearic acid in Ethylene Propylene Terpolymer heat insulation layer and palmitic acid massfraction.
Detect sample with high effective liquid chromatography for measuring, adopt the liquid phase chromatogram condition of acetonitrile/water, evaporative light-scattering detector detects, and according to calibration curve, obtains the stearic acid in Ethylene Propylene Terpolymer heat insulation layer and palmitic acid massfraction.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 40 is sample solution volume number ml.
Step 5, forms data list: will detect data creating data list, detects data according to the stearic acid in Ethylene Propylene Terpolymer heat insulation layer or palmitic acid massfraction, makes list display and detects precision and accuracy in detection.
Table 5 is the method precision (%) of stearic acid and palmitic acid massfraction in HPLC method mensuration Ethylene Propylene Terpolymer heat insulation layer.
Table 6 is the method accuracy of stearic acid and palmitic acid massfraction in HPLC method mensuration Ethylene Propylene Terpolymer heat insulation layer.
Table 5HPLC method measures the method precision (%) of stearic acid and palmitic acid massfraction in Ethylene Propylene Terpolymer heat insulation layer
Table 6HPLC method measures the method accuracy of stearic acid and palmitic acid massfraction in Ethylene Propylene Terpolymer heat insulation layer
Claims (1)
1. determination of fatty acid method in a propellant heat insulation layer, comprise following five steps: determine detected object, preparation detects sample, select testing conditions, make calibration curve, form data list, it is characterized in that: determining in detected object process, with the fatty acid extract in propellant different substrate materials rubber heat-insulating layer for detected object, comprise, butyronitrile heat insulation layer, butyl heat insulation layer and Ethylene Propylene Terpolymer heat insulation layer;
The preparation detecting test samples extract in sample in preparation adopts analyzes pure acetone as Extraction solvent, detected object is cut into particulate, adds at analyzing pure acetone 40 DEG C and at 40 DEG C, heats ultrasonic extraction 60 minutes and the standing mode of cooling with ultrasonic cleaner;
In selection testing conditions process, the mobile phase of selection is acetonitrile/water, checkout equipment is high performance liquid chromatography (HPLC), and separation condition is C18 chromatographic column, evaporative light-scattering detector detects;
In making calibration curve process: adopt external standard calibration curve standard measure, take a certain amount of stearic acid and palmitic acid, be mixed with the solution of known actual concentrations;
According to the liquid phase chromatogram condition that step 2 is selected, be depicted as calibration curve;
According to calibration curve, obtain the stearic acid in detected object and palmitic acid massfraction; Detect sample with high effective liquid chromatography for measuring, adopt the liquid phase chromatogram condition of acetonitrile/water, evaporative light-scattering detector detects, and according to calibration curve, obtains the stearic acid in detected object and palmitic acid massfraction; Computing formula is as follows:
.................................（1）
In formula,
mfor detecting the massfraction (%) of stearic acid or palmitic acid in sample,
c ifor detecting the concentration g/ml of stearic acid or palmitic acid in sample,
mfor detecting the quality g of sample, 40 is sample solution volume number ml;
Form data list: data creating data list will be detected, detect data according to the stearic acid in butyronitrile heat insulation layer or palmitic acid massfraction, make list display and detect precision and accuracy in detection.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1758060A (en) * | 2004-10-09 | 2006-04-12 | 中国药品生物制品检定所 | Determination method of effective component in aliphatic oil |
| CN101975714A (en) * | 2010-10-27 | 2011-02-16 | 武汉工程大学 | Method for measuring adsorption quantity of fatty acid collector on mineral surface |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1758060A (en) * | 2004-10-09 | 2006-04-12 | 中国药品生物制品检定所 | Determination method of effective component in aliphatic oil |
| CN101975714A (en) * | 2010-10-27 | 2011-02-16 | 武汉工程大学 | Method for measuring adsorption quantity of fatty acid collector on mineral surface |
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