CN105467064A - Method for determining total carbon content of boron-containing propellant primary combustion product - Google Patents
Method for determining total carbon content of boron-containing propellant primary combustion product Download PDFInfo
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- CN105467064A CN105467064A CN201410414284.9A CN201410414284A CN105467064A CN 105467064 A CN105467064 A CN 105467064A CN 201410414284 A CN201410414284 A CN 201410414284A CN 105467064 A CN105467064 A CN 105467064A
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Abstract
The invention provides a method for determining the total carbon content of a boron-containing propellant primary combustion product, used in the field of spaceflight fuels. The method comprises the following steps: grinding the product, sieving the ground product, weighing the product, and preparing a sample; oxidizing-reducing the sample in an automatic detection system, and drying the above obtained carbon dioxide-containing substance; and sending carbon dioxide separated from an adsorption-desorption system to the detection system of an element analyzer, detecting to obtain a carbon content curve, and comparing the carbon content curve with a premade standard sample curve to obtain the total carbon content of the sample. The method has the advantages of simplicity, applicability, strong operability, and good reappearance and high accuracy of a measurement result.
Description
Technical field
The present invention relates to a kind of aerospace fuel products of combustion assay method, specifically total carbon content assay method in a kind of boron-propellant primary combustion product.
Background technology
In boron-propellant primary combustion product, the component of carbon containing has carbon black and B
4c, both are difficult to separately separation and quantitative separately.If the total carbon content in products of combustion can be measured, can to carbon black or B
4when any one is quantitative in C two kinds of materials, just can extrapolate the amount of another kind of carbonaceous material.Therefore, measure the total carbon content in boron-propellant primary combustion product, for the constituent analysis of boron-propellant primary combustion product, have great importance.
Chinese periodical " solid-rocket technology " the 29th volume the 3rd phase in 2006 " boron powder coated and containing the constituent analysis of Boron Coated propellant combustion residue ", the document adopts chemical analysis to analyze the combustion residue fractions containing Boron Coated propellant, and analysis process figure thinks theoretically can record carbon black and B
4total carbon content in C, but do not provide concrete analysis process and analyze data.
The carbon content measuring material can adopt elemental analyser usually, adopts C/H/N measurement pattern, but under this detecting pattern, oxidation furnace temperature is lower, B
4c can not be completely oxidized, and the total carbon content error of mensuration is large, and reappearance is also poor.
Be more than the state of the art of total carbon content assay method in boron-propellant primary combustion product, its major defect existed is: do not have ready-made applicable method can reference, does not have actual operation.
Summary of the invention
The object of the present invention is to provide a kind of easy, workable, total carbon content assay method in the boron-propellant primary combustion product that accuracy is high.
Technical scheme of the present invention is: comprise according to the following steps:
1) using boron-propellant primary combustion product to be determined as sample, grinding after precise, obtain the sample prepared;
2) sample is inserted the automatic sample handling system of elemental analyser, then oxidation reaction and reduction reaction is carried out by the oxidation-reduction system of automatic sample handling system feeding elemental analyser, described oxidation reaction is: obtain oxycarbide adding under oxygen condition and sample and catalyzer are reacted at the temperature of 1000 ~ 1200 DEG C, described reduction reaction is: oxycarbide and reductive agent are reacted at 750 ~ 950 DEG C, the carbonated material desiccant dryness then will obtained;
3) dried carbonated material is sent into the absorption-resolution system of elemental analyser, by carbon dioxide and other separating substances, then the carbon dioxide that separation obtains is sent in the detection system of elemental analyser and detect, what obtain carbon contains discharge curve, comparing this carbon with the standard model curve made in advance containing discharge curve, obtain the total carbon content of sample.
Described catalyzer is tungstic acid.
Described reductive agent is wire copper.
The standard model curve made in advance adopts and is made as standard model containing carbon compound.
The standard model curve made in advance adopts benzene sulfonic acid to be made as standard model.
The purity of described benzene sulfonic acid is greater than 99.5%.
Described detection system is thermal conductivity cell detector.
Described oxidation reaction is carried out at the temperature of 1150 DEG C.
Described reduction reaction is carried out at 850 DEG C.
The invention has the beneficial effects as follows: the present invention can measure total carbon content in boron-propellant primary combustion product, and method is easy, workable, and measurement result favorable reproducibility, accuracy is high.
Embodiment
Below in conjunction with embodiment, the present invention is further described.
Following example is the unrestricted technical scheme of the present invention in order to explanation only, according to actual needs to any modification or partial replacement not departing from spirit and scope of the invention, all should be encompassed in the middle of right of the present invention.
One, instrument condition:
1. instrument is elemental analyser, and uses thermal conductivity cell detector;
2. helium and oxygen pressure are 0.2Mpa, and helium gas flow is 100ml/min;
3. furnace temperature: 1150 DEG C;
4. reduction furnace temperature: 850 DEG C;
5. burning condition: 90 seconds oxygenation time;
6. oxidation tube-oxygenant: tungstic acid;
7. reduction tube-reductive agent: wire copper, purity (massfraction) is not less than 99%;
8. drying agent: phosphorus pentoxide;
9. standard model: select carbon compound benzene sulfonic acid as organic element analysis standard substance, purity is greater than 99.5%;
10. gas: helium purity is not less than 99.995%; Oxygen purity is not less than 99.995%.
Two, the method for the present embodiment comprises the steps:
1, sample preparation
Using boron-propellant primary combustion product to be determined as sample, grind after about 3 minutes and cross 1250 mesh sieves, precise, obtains the sample prepared.
2, the preparation of instrument
Start instrument, the gas circuit of inspection apparatus whole system;
Setting analytical parameters, by operating conditions conditioning instrumentation;
After furnace temperature reaches, do the correction (correcting with organic element analysis standard substance) that blank analysis value repeatedly and sample conditionization run instrument:
Calibration curve (20-30 point): this curve is generally a period of time do once, is kept in workstation;
Day correction coefficient: record on the basis of calibration curve, must take multiple measurements on the same day of test sample.Accurately take 5.0mg standard substance and measure day correction coefficient, general METHOD FOR CONTINUOUS DETERMINATION 2 ~ 5 times, capable coefficient of making even is as day correction coefficient mean value.Often enter 15 ~ 30 samples, do 2-3 standard specimen, with the stability of detection system, and adjust day correction coefficient in time.
The preparation of typical curve:
Accurately take standard model 0.1mg, 0.2mg, 0.3mg, 0.4mg, 0.5mg, 0.75mg, 1.0mg, 1.25mg, 1.5mg, 1.75mg, 1.5mg, 1.75mg, 2.0mg, 3.0mg, 3.5mg, 4.0mg, 4.5mg, 5mg, 6mg, 7mg, 9mg, 11mg in tinfoil paper boat, the sample injection disc that system is stable is put into after good seal, operation method, the data according to gained are set up and preserve newly-built standard model.The same day, correction factor factor exceeded outside 0.9 ~ 1.1 scope, again made curve.
3, the mensuration of total carbon content in boron-propellant primary combustion product
Under the test condition identical with standard model, sample is measured.Accurately take 2mg sample, record sample weighting amount is also in sample weighting amount input service station, tinfoil paper boat is put into the stable sample injection disc of elemental analyser, operation method, that is: sample is inserted the automatic sample handling system of elemental analyser, then sent into by automatic sample handling system in the oxidation-reduction system of elemental analyser and carry out oxidation reaction and reduction reaction, described oxidation reaction is: obtain oxycarbide adding under oxygen condition and sample and catalyzer are reacted at the temperature of 1150 DEG C, described reduction reaction is: oxycarbide and reductive agent are reacted at the temperature of 850 DEG C, then the carbonated material desiccant dryness will obtained, dried carbonated material is sent into the absorption-resolution system of elemental analyser, by carbon dioxide and other separating substances, then the carbon dioxide that separation obtains is sent in the detection system of elemental analyser and detect, what obtain carbon contains discharge curve, comparing this carbon with the standard model curve made in advance containing discharge curve, obtain the total carbon content of sample.
Claims (9)
1. a total carbon content assay method in boron-propellant primary combustion product, is characterized in that, comprises according to the following steps:
1) using boron-propellant primary combustion product to be determined as sample, grinding after precise, obtain the sample prepared;
2) sample is inserted the automatic sample handling system of elemental analyser, then oxidation reaction and reduction reaction is carried out by the oxidation-reduction system of automatic sample handling system feeding elemental analyser, described oxidation reaction is: obtain oxycarbide adding under oxygen condition and sample and catalyzer are reacted at the temperature of 1000 ~ 1200 DEG C, described reduction reaction is: oxycarbide and reductive agent are reacted at 750 ~ 950 DEG C, the carbonated material desiccant dryness then will obtained;
3) dried carbonated material is sent into the absorption-resolution system of elemental analyser, by carbon dioxide and other separating substances, then the carbon dioxide that separation obtains is sent in the detection system of elemental analyser and detect, what obtain carbon contains discharge curve, comparing this carbon with the standard model curve made in advance containing discharge curve, obtain the total carbon content of sample.
2. total carbon content assay method in boron-propellant primary combustion product as claimed in claim 1, is characterized in that: described catalyzer is tungstic acid.
3. total carbon content assay method in boron-propellant primary combustion product as claimed in claim 1, is characterized in that: described reductive agent is wire copper.
4. total carbon content assay method in boron-propellant primary combustion product as claimed in claim 1, is characterized in that: the standard model curve made in advance adopts and is made as standard model containing carbon compound.
5. total carbon content assay method in boron-propellant primary combustion product as claimed in claim 1, is characterized in that: the standard model curve made in advance adopts benzene sulfonic acid to be made as standard model.
6. total carbon content assay method in boron-propellant primary combustion product as claimed in claim 5, is characterized in that: the purity of described benzene sulfonic acid is greater than 99.5%.
7. total carbon content assay method in boron-propellant primary combustion product as claimed in claim 1, is characterized in that: described detection system is thermal conductivity cell detector.
8. total carbon content assay method in boron-propellant primary combustion product as claimed in claim 1, is characterized in that: described oxidation reaction is carried out at the temperature of 1150 DEG C.
9. the determination of elemental analysis method of total carbon in tobacco as claimed in claim 1 and tobacco product, is characterized in that: described reduction reaction is carried out at 850 DEG C.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108281553A (en) * | 2018-01-10 | 2018-07-13 | 苏州大学 | A kind of poly- 3,4- ethene dioxythiophenes cladding tungsten oxide nanometer stick, preparation method and applications |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20020166612A1 (en) * | 2001-02-27 | 2002-11-14 | Chan May L. | Insensitive high energy booster propellant |
| CN102539623A (en) * | 2011-12-26 | 2012-07-04 | 西北工业大学 | Method for accurately and quantitatively analyzing combustion residue of boron-based fuel-rich propellant |
| CN102621294A (en) * | 2012-04-09 | 2012-08-01 | 东北林业大学 | Method for measuring carbon content in wood |
| CN103091353A (en) * | 2011-11-01 | 2013-05-08 | 中国科学院沈阳应用生态研究所 | Determination method of carbon and nitrogen contents in soil |
-
2014
- 2014-08-21 CN CN201410414284.9A patent/CN105467064A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20020166612A1 (en) * | 2001-02-27 | 2002-11-14 | Chan May L. | Insensitive high energy booster propellant |
| CN103091353A (en) * | 2011-11-01 | 2013-05-08 | 中国科学院沈阳应用生态研究所 | Determination method of carbon and nitrogen contents in soil |
| CN102539623A (en) * | 2011-12-26 | 2012-07-04 | 西北工业大学 | Method for accurately and quantitatively analyzing combustion residue of boron-based fuel-rich propellant |
| CN102621294A (en) * | 2012-04-09 | 2012-08-01 | 东北林业大学 | Method for measuring carbon content in wood |
Non-Patent Citations (1)
| Title |
|---|
| 赵鹏等: "含硼固体推进剂燃烧残渣中三氧化二硼和碳含量测定及燃烧机理研究", 《化学推进剂与高分子材料》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108281553A (en) * | 2018-01-10 | 2018-07-13 | 苏州大学 | A kind of poly- 3,4- ethene dioxythiophenes cladding tungsten oxide nanometer stick, preparation method and applications |
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Application publication date: 20160406 |