CN107796907A - The purity analysis methods of speciality CL 20 - Google Patents
The purity analysis methods of speciality CL 20 Download PDFInfo
- Publication number
- CN107796907A CN107796907A CN201710888811.3A CN201710888811A CN107796907A CN 107796907 A CN107796907 A CN 107796907A CN 201710888811 A CN201710888811 A CN 201710888811A CN 107796907 A CN107796907 A CN 107796907A
- Authority
- CN
- China
- Prior art keywords
- standard
- speciality
- sample
- acetonitrile
- purity analysis
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/89—Inverse chromatography
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/62—Detectors specially adapted therefor
- G01N30/74—Optical detectors
Landscapes
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The present invention relates to explosive purity analysis technology, specially a kind of purity analysis methods of speciality CL 20.Solves the technical problem for lacking a kind of method that can accurately analyze the purity of speciality CL 20 at present.A kind of purity analysis methods of speciality CL 20, are analyzed using calibration curve method, are comprised the following steps：（1）Weigh two parts of 20 standard specimens of CL, 3 standard test solutions to 5 various concentrations are configured to respectively, chromatographic determination is carried out to the standard test solution of above-mentioned various concentrations under prescribed conditions, draw its chromatogram, the standard specimen concentration and standard specimen chromatogram peak height of all standard test solutions are recorded, calibration curve parameter A, B value is calculated according to above-mentioned data；（2）Weigh two parts of 20 samples of CL to be measured, it is respectively placed in volumetric flask, chromatographic determination is carried out under chromatographic condition same with standard test solution, records sample chromatogram peak height, the solution concentrations of CL 20 are calculated, the contents of CL 20 are drawn further according to sample original quality, counter push away of sample solution extension rate.
Description
Technical field
The present invention relates to explosive purity analysis technology, specially a kind of speciality CL-20 purity analysis methods.
Background technology
Speciality CL-20 be using common CL-20 as raw material, by special process obtain in crystal shape, crystalline density, grain
The one kind for having Special Manifestations in the indexs such as degree distribution, product purity can meet particular/special requirement of the bursting work to speciality CL-20.But
It is to lack a kind of method that effectively can accurately analyze speciality CL-20 purity at present.
The content of the invention
The present invention carries to solve to lack a kind of technical problem for the method that can accurately analyze speciality CL-20 purity at present
For a kind of speciality CL-20 purity analysis methods.
The present invention is realized using following technical scheme：A kind of speciality CL-20 purity analysis methods, using calibration curve
Method is analyzed, and the calibration curve method comprises the following steps：
（1）Two parts of CL-20 standard specimens are weighed, are respectively placed in two volumetric flasks, constant volume after being dissolved with appropriate acetonitrile；With acetonitrile by this
Mother liquor dilutes step by step, two parts of standard specimens is configured into 3 standard test solutions to 5 various concentrations respectively, under prescribed conditions
Chromatographic determination is carried out to the standard test solution of above-mentioned various concentrations, its chromatogram is drawn, records all standard test solutions
Standard specimen concentration and standard specimen chromatogram peak height, then by above-mentioned data convolution（1.1）Calibration curve parameter A, B value is calculated, its is linear
Coefficient R value should be not less than 0.995, if linearly dependent coefficient R values are more than 0.995, this time test result is invalid, again
Weigh CL-20 standard specimens；
Cs=A×Hs+B （1.1）
C in formulas--- standard specimen concentration；
Hs--- standard specimen chromatogram peak height；
（2）Sample determines
Two parts of CL-20 samples to be measured are weighed, are respectively placed in volumetric flask, constant volume after being dissolved with appropriate acetonitrile；With standard testing
Chromatographic determination is carried out under the same chromatographic condition of solution, sample chromatogram peak height is recorded, is substituted into and obtained the formula of A, B coefficient
（1.1）In, CL-20 solution concentrations are calculated, CL-20 is drawn further according to sample original quality, counter push away of sample solution extension rate
Content；The arithmetic mean of instantaneous value of parallel result twice is taken as final tested volume, it is allowed to which difference is not more than 2%；If tolerance is more than
2%, then step（2）Sample measurement result is invalid to be measured, it is necessary to weigh sample again.
Further, in addition to normalization method；The normalization method comprises the following steps：CL-20 samples are weighed, it is first molten with acetonitrile
Solution, then by the use of 10 times~15 times of dilution in acetonitrile as solution is determined, by step（1）Methods described carries out chromatographic determination, draws its color
After solvent peak, CL-20 contents are calculated with areas of peak normalization method earlier for spectrogram, rejecting appearance；Determined with parallel chromatography twice
The arithmetic mean of instantaneous value of data is as final result, it is allowed to which difference is not more than 1%, and and step（2）Measured CL-20 purity is carried out
Contrast verification；If tolerance is more than 1%, this time normalization method is invalid, need to re-start measure.
The method of the invention has the advantages of simple, quick, as a result accurate, is highly suitable for speciality CL-20 products
Purity analysis.The precision test result of this method is as follows：
1st, the repeatability of CL-20 purity testings data
In order to examine the error range of CL-20 purity testing data, confirm that it quotes the reliability of data, in the inventive method bar
Under part, 15 purity testings are carried out to a test specimen, measurement result and purity, which calculate, the results are shown in Table 1.
Above-mentioned as shown by data, the result of 15 purity tests of identical product sample, average value 99.27%, arithmetic average is inclined
Difference is 0.03%, and standard deviation 0.36%, when probability coefficent is 0.95, confidence coefficient takes 2.1, repeatability limit 0.63%（2.1*
0.03%）.
This standard provides that the repeatability of purity test data is exactly in same laboratory, is set by same operator using identical
It is standby, carry out testing 15 independent tests of acquisition independently of each other by same test method and in a short time to same measurand
As a result the maximum absolute difference of full test result is not more than repeatability limit 0.63%, when it is parallel test three times when, repeatability limit
For 0.84%（Shown in table 2）
2nd, the repeatability of CL-20 purity testings data
To same sample, different equipment is used by different operators, carries out contrast experiment by identical method of testing, as a result
It is shown in Table 2.
To same CL-20 samples, as shown in upper table, the repeatability limit of the same three parts of sample testing results in laboratory is
0.84%（2.8*0.30）, in different experiments room, the repeatability of three parts of specimen sample test results is limited to 1.15%（2.8*0.41）.
Present invention provide that repeatability, be exactly that distinct device is used by different operators in different experiments room, by identical
The method of testing and maximum absolute difference tested independently of each other same measurand in a short time is not more than repeatability
It is limited to 1.15%.
Embodiment
A kind of speciality CL-20 purity analysis methods, are analyzed using calibration curve method, and the calibration curve method is included such as
Lower step：
（1）Weigh two parts of CL-20 standard specimens（Every part of 0.01g-0.05g, is accurate to 0.0001g）, it is respectively placed in two 25mL capacity
In bottle, constant volume after being dissolved with appropriate acetonitrile；This mother liquor is diluted step by step with acetonitrile, two parts of standard specimens are configured to 3 to 5 respectively
The standard test solution of various concentrations（Concentration is 5 × 10-6g/mL-1~5 × 10-5g/mL-1In the range of）, it is right under prescribed conditions
The standard test solution of above-mentioned various concentrations carries out chromatographic determination, draws its chromatogram spectrogram, records all standard test solutions
Standard specimen concentration and standard specimen chromatogram peak height, then by above-mentioned data convolution（1.1）Calibration curve parameter A, B value is calculated, its is linear
Coefficient R value should be not less than 0.995, if linearly dependent coefficient R values are more than 0.995, this time test result is invalid, again
Weigh CL-20 standard specimens；
Cs=A×Hs+B （1.1）
C in formulas--- standard specimen concentration；
Hs--- standard specimen chromatogram peak height；
（2）Sample determines
Weigh two parts of CL-20 samples to be measured（Every part of 0.01g-0.05g, is accurate to 0.0001g）, it is respectively placed in 25mL volumetric flasks
In, constant volume after being dissolved with appropriate acetonitrile；Chromatographic determination is carried out under chromatographic condition same with standard test solution, records sample color
Spectral peak is high, is substituted into and has obtained the formula of A, B coefficient（1.1）In, CL-20 solution concentrations are calculated, it is original further according to sample
Counter push away of quality, sample solution extension rate draws CL-20 contents；The arithmetic mean of instantaneous value of parallel result twice is taken as final measure
Value, it is allowed to which difference is not more than 2%；If tolerance is more than 2%, step（2）Sample measurement result is invalid, it is necessary to weigh sample again
It is measured.
Also include normalization method；The normalization method comprises the following steps：CL-20 sample 0.01g-0.05g are weighed,（It is accurate to
0.0001g）, first dissolved with 10mL acetonitriles, then by the use of 10 times~15 times of dilution in acetonitrile as solution is determined, by step（1）The side
Method carries out chromatographic determination, draws its chromatogram, and after solvent peak, CL-20 is calculated with areas of peak normalization method earlier for rejecting appearance
Content；Final result is used as using the arithmetic mean of instantaneous value of parallel chromatography determination data twice, it is allowed to which difference is not more than 1%, and and step
（2）Measured CL-20 purity carries out contrast verification；If tolerance is more than 1%, this time normalization method is invalid, need to re-start
Measure.
The liquid chromatography relevant parameter is as follows：
A) chromatographic column：Efficient reverse-phase chromatographic column silica gel bonded C18；
B) mobile phase：60/40 acetonitrile/water；
C) solvent acetonitrile；
D) uv-spectrophotometric detector wavelength：230nm；
E) sampling volume：10μL.
Claims (5)
- A kind of 1. speciality CL-20 purity analysis methods, it is characterised in that analyzed using calibration curve method, the correction is bent Collimation method comprises the following steps：（1）Two parts of CL-20 standard specimens are weighed, are respectively placed in two volumetric flasks, constant volume after being dissolved with appropriate acetonitrile；With acetonitrile by this Mother liquor dilutes step by step, two parts of standard specimens is configured into 3 standard test solutions to 5 various concentrations respectively, under prescribed conditions Chromatographic determination is carried out to the standard test solution of above-mentioned various concentrations, its chromatogram spectrogram is drawn, records all standard test solutions Standard specimen concentration and standard specimen chromatogram peak height, then by above-mentioned data convolution（1.1）Calculate calibration curve parameter A, B value, its line Property coefficient R value should be not less than 0.995, if linearly dependent coefficient R values be more than 0.995, this time test result it is invalid, weigh Newly weigh CL-20 standard specimens；Cs=A×Hs+B （1.1）C in formulas--- standard specimen concentration；Hs--- standard specimen chromatogram peak height；（2）Sample determinesTwo parts of CL-20 samples to be measured are weighed, are respectively placed in volumetric flask, constant volume after being dissolved with appropriate acetonitrile；With standard testing Chromatographic determination is carried out under the same chromatographic condition of solution, sample chromatogram peak height is recorded, is substituted into and obtained the formula of A, B coefficient （1.1）In, CL-20 solution concentrations are calculated, CL-20 is drawn further according to sample original quality, counter push away of sample solution extension rate Content；The arithmetic mean of instantaneous value of parallel result twice is taken as final tested volume, it is allowed to which difference is not more than 2%；If tolerance is more than 2%, then step（2）Sample measurement result is invalid to be measured, it is necessary to weigh sample again.
- 2. speciality CL-20 purity analysis methods as claimed in claim 1, it is characterised in that also including normalization method；The normalizing Method comprises the following steps：CL-20 samples are weighed, are first dissolved with acetonitrile, then by the use of 10 times~15 times of dilution in acetonitrile as measure solution, By step（1）Methods described carries out chromatographic determination, draws its chromatogram, and rejecting appearance after solvent peak, is returned with peak area earlier One, which changes method, calculates CL-20 contents；Final result is used as using the arithmetic mean of instantaneous value of parallel chromatography determination data twice, it is allowed to which difference is less In 1%, and and step（2）Measured CL-20 purity carries out contrast verification；If tolerance be more than 1%, this normalization method without Effect, need to re-start measure.
- 3. speciality CL-20 purity analysis methods as claimed in claim 1 or 2, it is characterised in that the liquid chromatography is related Parameter is as follows：A) chromatographic column：Efficient reverse-phase chromatographic column silica gel bonded C18；B) mobile phase：60/40 acetonitrile/water；C) solvent acetonitrile；D) uv-spectrophotometric detector wavelength：230nm；E) sampling volume：10μL.
- 4. speciality CL-20 purity analysis methods as claimed in claim 1 or 2, it is characterised in that step（1）Middle CL-20 standard specimens Every part of quality is 0.01g-0.05g, is accurate to 0.0001g；The concentration of 3 standard test solutions to 5 various concentrations 5 × 10-6g/mL-1~5 × 10-5g/mL-1In the range of；Step（2）In weigh CL-20 samples 0.01g-0.05g to be measured, be accurate to 0.0001g。
- 5. speciality CL-20 purity analysis methods as claimed in claim 2, it is characterised in that weigh CL-20 in the normalization method Sample 0.01g-0.05g, is accurate to 0.0001g.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710888811.3A CN107796907A (en) | 2017-09-27 | 2017-09-27 | The purity analysis methods of speciality CL 20 |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710888811.3A CN107796907A (en) | 2017-09-27 | 2017-09-27 | The purity analysis methods of speciality CL 20 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107796907A true CN107796907A (en) | 2018-03-13 |
Family
ID=61532530
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710888811.3A Pending CN107796907A (en) | 2017-09-27 | 2017-09-27 | The purity analysis methods of speciality CL 20 |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107796907A (en) |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2000030688A2 (en) * | 1998-11-26 | 2000-06-02 | Bracco International B.V. | Amphipatic polycarboxylic chelates and complexes with paramagnetic metals as mri contrast agents |
| US20030111148A1 (en) * | 2000-03-10 | 2003-06-19 | Cordant Technologies Inc. | Method for recovery of nitramines from aluminized energetic materials |
| CN101624394A (en) * | 2009-08-12 | 2010-01-13 | 北京理工大学 | Sphericized hexanitrohexaazaisowurtzitane (HNIW) crystal and preparation method thereof |
| CN103288839A (en) * | 2013-05-31 | 2013-09-11 | 西安近代化学研究所 | Chromatographic separation method and quantitative detection method of CL-20 (hexaazaisowurtzitane) and three intermediates CL-20 |
| CN106117229A (en) * | 2016-08-31 | 2016-11-16 | 山西北化关铝化工有限公司 | A kind of preparation method of speciality Hexanitrohexaazaisowurtzitane |
-
2017
- 2017-09-27 CN CN201710888811.3A patent/CN107796907A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2000030688A2 (en) * | 1998-11-26 | 2000-06-02 | Bracco International B.V. | Amphipatic polycarboxylic chelates and complexes with paramagnetic metals as mri contrast agents |
| US20030111148A1 (en) * | 2000-03-10 | 2003-06-19 | Cordant Technologies Inc. | Method for recovery of nitramines from aluminized energetic materials |
| CN101624394A (en) * | 2009-08-12 | 2010-01-13 | 北京理工大学 | Sphericized hexanitrohexaazaisowurtzitane (HNIW) crystal and preparation method thereof |
| CN103288839A (en) * | 2013-05-31 | 2013-09-11 | 西安近代化学研究所 | Chromatographic separation method and quantitative detection method of CL-20 (hexaazaisowurtzitane) and three intermediates CL-20 |
| CN106117229A (en) * | 2016-08-31 | 2016-11-16 | 山西北化关铝化工有限公司 | A kind of preparation method of speciality Hexanitrohexaazaisowurtzitane |
Non-Patent Citations (2)
| Title |
|---|
| 董波 等: "离子液体中 CL-20 的高收率低污染硝解方法", 《含能材料》 * |
| 黄志萍 等: "HNIW纯度测定方法研究", 《含能材料》 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103076351B (en) | Method for measuring Mo element in tungstenic ferro-molybdenum alloy through X-ray fluorescence spectrum analysis | |
| CN107543872B (en) | Method for separating and determining edoxaban tosylate hydrate and isomer impurities thereof by chiral high performance liquid chromatography | |
| CN110031573B (en) | Method for measuring vitamin D content by two-dimensional column switching high performance liquid chromatography | |
| CN103293175A (en) | Method for measuring chemical components of liquid sodium silicate | |
| CN105548115B (en) | The assay method of Mercury In Soil | |
| Xie et al. | Determination of total acid content in vinegars by reaction-based headspace gas chromatography | |
| CN106525994B (en) | Method for determining related substances of paracetamol and tramadol capsule | |
| CN110780002B (en) | High-efficiency low-cost detection method for quantifying essential oil components | |
| CN103134863A (en) | Method of determining content of methanol, isobutanol, isoamylol of alcohol | |
| CN111122727A (en) | Method for simultaneously determining concentration of imatinib and imatinib metabolite in human plasma | |
| CN103558174B (en) | A kind of method utilizing cresol content in determined by ultraviolet spectrophotometry Lysol | |
| CN107796907A (en) | The purity analysis methods of speciality CL 20 | |
| CN101581708B (en) | Method for measuring low-concentration methylcyclopentadienyl manganese tricarbonyl by gas chromatography internal standard method | |
| CN107356698B (en) | 2- picoline and method for quantitatively determining while N-serve in a kind of sample | |
| CN109725083A (en) | Based on gas-chromatography-isotopic dilution infrared spectroscopy compounds content mete-wand method | |
| CN111426760B (en) | Method for determining genotoxic impurities in doxofylline raw material medicine | |
| CN112557574B (en) | Method for measuring content of CBZ-AEEA | |
| CN106596750B (en) | Six kinds of content assaying methods in relation to substance in a kind of otoginsenoside preparation of sodium | |
| CN110187021B (en) | Method for simultaneously determining contents of two main drugs in closantel sodium ivermectin injection | |
| CN102507771A (en) | Novel content detection method for sodium hydrogensulfite andrographolide | |
| CN115248260A (en) | HPLC analysis detection method for related substances in cisatracurium besilate bulk drug | |
| CN110441437A (en) | A kind of measuring method of Michaelis acid content | |
| CN112557573B (en) | Method for measuring AEEA-AEEA content | |
| CN105954431B (en) | A kind of method of the HPLC separation determination Ao Pei meter Fen bulk pharmaceutical chemicals in relation to substance | |
| CN106370740A (en) | Method for analyzing residual quantity of residual solvents in atorvastatin calcium intermediate |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20180313 |