CN108802082A - The Quick qualitative detection method of titanium elements in a kind of fireworks and firecrackers pyrotechnic composition - Google Patents
The Quick qualitative detection method of titanium elements in a kind of fireworks and firecrackers pyrotechnic composition Download PDFInfo
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- CN108802082A CN108802082A CN201711445433.8A CN201711445433A CN108802082A CN 108802082 A CN108802082 A CN 108802082A CN 201711445433 A CN201711445433 A CN 201711445433A CN 108802082 A CN108802082 A CN 108802082A
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
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- G01N23/223—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material by irradiating the sample with X-rays or gamma-rays and by measuring X-ray fluorescence
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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Abstract
The invention discloses a kind of Quick qualitative detection methods of titanium elements in fireworks and firecrackers pyrotechnic composition, belong to analysis and testing technology field.Pyrotechnic composition sample is dissected from fireworks and firecrackers product and is come out, grinding, sieving, it is dry, it is cooled to room temperature, using energy dispersion type Xray fluorescence spectrometer as detecting instrument, analysis method is established using intensity method, sample is fitted into instrument sample cup, then sample to be tested is placed in detecting instrument test chamber, the fluorescence intensity level of the titanium elements characteristic spectral line shown on register instrument directly judges whether contain titanium in sample according to this fluorescence intensity level.Titanium elements qualitative analysis is carried out using the method for the invention, accuracy is high, reproducible, easy to operate, efficient, can effectively meet manufacturing enterprise, supervision department and third party laboratory and quickly detect in pyrotechnic composition sample whether contain titanium.
Description
Technical field
The present invention relates to analysis and testing technology fields, and in particular to a kind of energy dispersion type x ray fluorescence spectrometry is quick
The method of titanium elements in qualitative detection fireworks and firecrackers pyrotechnic composition.
Background technology
In the prior art, fireworks and firecrackers is to be based on traditional chemical analysis method with the qualitative checking method of titanium in pyrotechnic composition,
Currently used method standard is《The 4th Partial security of fireworks and firecrackers inspection procedure is exported to examine》（SN/T 0306.4-
2006）.Such standard method have complex for operation step, detection efficiency is low, environmental pollution more using reagent greatly and detection line
It is indefinite to give many deficiencies such as manufacturing enterprise's directive function unobvious.
The method that energy dispersion type X-ray fluorescence spectra technology is developed at present is chiefly used in the lossless qualitative analysis of sample.
It is detected for solid sample sxemiquantitative and quantitative elemental, most samples are directly measured using powder pressing method and fusion method
Such as：《The measurement x ray fluorescence spectrometry of bullion content》(GB/T 18043-2008) using nondestructive determination,《Oxygen
Change titanium chemical analysis method and the 30th partial x-ray fluorescence spectrum method for measuring constituent content of method for measuring physical properties》(GB/
T6609.30-2009) using fusion method,《EDXRF methods directly measure W-Fe-Ni-Co alloy batch components》(《Nuclear power
Son is learned and Detection Techniques》05 phase in 2007) using pressed disc method,《X ray fluorescence spectrometry quickly measures Potassium Chloride Product
The content of middle potassium, sodium, calcium, magnesium》（Analytical instrument the 6th phase in 2013）Using pressed disc method,《It is limited the use of in electronic and electrical equipment
The quick screening x ray fluorescence spectrometry of substance lead, mercury, chromium, cadmium and bromine》(GB/Z 21277-2007) is using pressed disc method
Or fusion method.
Since fireworks and firecrackers pyrotechnic composition has inflammable and explosive property, energy dispersion type X-ray fluorescence spectra skill can not be utilized
Art (EDXRF) directly uses powder pressing method and fusion method to carry out sample treatment.Up to now it also there are no based on energy dispersion
The open source literature report of the method for titanium elements in type X-ray fluorescence spectra technology fast qualitative detection fireworks and firecrackers pyrotechnic composition.
Invention content
It is quickly fixed based on energy dispersion type X-ray fluorescence spectra technology that the technical problem to be solved in the present invention is to provide one kind
Property detection fireworks and firecrackers pyrotechnic composition in titanium elements method.The basic principle of detection：Sample is after by excitation of X-rays, in sample
Different elements can launch different characteristic X-rays, these characteristic spectral lines be identification sample in there are the fingerprints of object element
Information.Pass through the characteristic x-ray fluorescence intensity of object element in determination sample, it is possible to determine that with the presence or absence of titanium member in unknown sample
Element.The fireworks and firecrackers directly upper machine of pyrotechnic composition powder sample is established specific analysis method, according to titanium elements feature by this method
The characteristic x-ray fluorescence intensity value of spectral line come judge in sample whether there is titanium elements.The method is easy to operate, detection cycle
It is short, and testing result accuracy is good, precision is high.
The Quick qualitative detection method of titanium elements, includes the following steps in a kind of fireworks and firecrackers pyrotechnic composition：
1）Prepare sample：Pyrotechnic composition sample is dissected from fireworks and firecrackers product and is come out, takes a small amount of multiple principle by sample
It is placed in mortar made of antistatic material, is carefully ground with antistatic stick, be sieved, sample powder is placed on explosion-proof baking oven
Middle drying is placed in drier is cooled to room temperature after drying, spare；
2) detection method is established：Using energy dispersion type Xray fluorescence spectrometer as detecting instrument, analysis side is established using intensity method
Method；
3）Detect the fluorescence intensity level of titanium elements characteristic spectral line in sample：After sample is fitted into instrument sample cup, sample will be housed
The specimen cup of product is vertically tamped for 3 times or more on the table, then the specimen cup equipped with sample to be tested is placed in detecting instrument test chamber
It is interior, directly measure the fluorescence intensity level of titanium elements characteristic spectral line, the fluorescence intensity level F shown on register instrument；
4）, according to step 3）The F values of acquisition determine whether that there are titaniums：
A, as F >=1000cps/mA, judge to contain titanium in sample；
B, as F < 1000cps/mA, judge not containing titanium in sample.
Further, mortar made of the antistatic material is that preferably copper mortar, the antistatic stick are
Preferably copper rod.
Further, the step 1）It takes total amount to be placed in mortar for 5~10g samples to be ground, crosses 40~100 mesh
Sieve.
Further, the drying time is 4~10 hours, and drying temperature is 50~75 DEG C.
Further, the step 2）The parameter of detecting instrument is set as：Aperture is the X-ray light pipe of 8.8mm~14mm
Collimator and the filter that can filter X-ray of the energy less than 4.508 KeV, setting voltage are 18KV~22kV, analysis time
For >=20s, energy range is 0~40keV, and during counting rate is, gaseous environment is air or vacuum, and electric current is automatic, is not considered
Matrix effect, it is K lines that the line of observation is composed at peak.
Further, the parameter setting of detecting instrument：Filter is aluminium, voltage 20kV, analysis time 30s.
Further, thickness of sample >=3mm in the step 3) specimen cup.
The principle of this method is as follows：The characteristics of for fireworks and firecrackers pyrotechnic composition chemical composition, establish special mathematical modulo
Type, global optimization can directly affect each factor of measurement result, including：Matrix effect number for establishing analysis method
School execute the matrix effect interaction type of type and energy dispersion type X fluorescence spectrum instrument, voltage, electric current, filter and
Compose work in every parameter and the specimen cup pilot scales such as selection, analysis time, counting rate, gaseous environment, the energy range of the line of observation in peak
The thickness etc. of material.Content and titanium elements characteristic spectral line fluorescence intensity based on titanium elements in powder sample are to be positively correlated relationship
And the content of titanium elements and the fluorescence intensity level of titanium elements characteristic spectral line are substantially proportional to example in some titanium elements concentration range
Relationship it is assumed that reasoning out can be to qualitatively judge in sample by detecting the fluorescence intensity of titanium elements characteristic spectral line in sample
The no conclusion containing titanium.
Country variant has different regulations to fireworks and firecrackers unauthorized substances, such as：In APA pyrotechnics association of U.S. relevant criterion
Substance in regulation firework medicament within 0.25% mass percentage is identified as impurity, chinese national standard《Fireworks and firecrackers
Safety and quality》（GB 10631-2013）Substance in middle regulation firework medicament within 0.1% mass percentage is identified as
Impurity, and Holland finds that contained lead element is super in certain kind fireworks from China in an import fireworks sampling inspection result
120mg/kg is crossed, and is notified to.In conjunction with the actual conditions and energy dispersion type X-fluorescence of Chinese fireworks and firecrackers firework medicament
The characteristics of spectral instrument, titanium valve is as one of most common raw material of firework medicament, and the titanium valve as raw material addition is in pyrotechnics
The mass percentage of medicament is generally all 3% or more, and only U.S.'s correlation standard cannot be using diameter less than 100 mesh
（150μm）Titanium valve.In order to solve the practical problem that raw material qualitative detection is often used in fireworks and firecrackers field, this method ginseng conscientiously
APA pyrotechnics association of U.S. relevant criterion content is examined, it is specified that effective detection of titanium elements is limited to 0.25%（Experimental data shows, this
The fluorescence intensity level of bismuth element characteristic spectral line is 1000cps/mA under concentration）.Why the present invention limits effective detection of titanium
It is 0.25%, allows for fireworks and firecrackers produce reality, if Ti content is less than 1%, even if testing result can to have if " detection "
It can be mixed impurity in pyrotechnic composition, and be not the raw material that the producer artificially adds, testing result instructs actual production
It has little significance.If be detected content >=1%, the possibility artificially added is just very big, is only adjusted on formula, substantially
Energy exclusion is the possibility of pyrotechnic composition impurity element.This method is easy to operate, detection cycle is short, and testing result accuracy is good, essence
Density is high.
The present invention takes total amount to be placed in mortar for 5~10g samples and is ground, and crosses 40~100 mesh sieve.Why by sample
Sample size be defined as 5~10g, allow for fireworks and firecrackers with pyrotechnic composition be made of many kinds of substance mechanical mixture it is polynary mixed
Close explosive, sample size too it is small can cause samples taken do not have it is representative and be difficult to meet thickness of sample in specimen cup must be big
In the requirement equal to 3mm, the accuracy of test result will have a direct impact on；And the too big work that can influence sample test of sample size
Efficiency.It places after why the sample after sieving being mixed well and dries in an oven again, also allow for firework medicament composition
Complexity, it is most likely that due to sample inhomogeneities and to test result generate harmful effect.Why sample crossed 40
~100 mesh sieve, and mainly have two aspect reasons：One sieve pore that allows within 40 mesh is too big, be easy to cause screenings particle mistake
It is big and the granular size inhomogeneities of analysis sample is caused to increase, and energy dispersion type X fluorescence spectrometer be to sample surfaces into
Row analysis, the non-uniform sample of granular size very likely generates larger granularity effect, to seriously affect test result
Accuracy.On the other hand, if after pyrotechnic composition sample crosses the sieve of 100 mesh or more, the very little that granularity can become not only influences sample
Screening efficiency as pyrotechnic composition particle is too small and the dust content in environment is caused to increase after sieving, to sample preparation, personnel make
At certain health hazard, more important reason, which is the pyrotechnic composition for being less than 100 mesh sieve pores due to grain size, has height inflammable and explosive
Characteristic, it is easy to be exploded in air by electrostatic or spark initiation, lead to the generation of accident.
Compared with prior art, the method for the invention has the beneficial effect that：
Titanium elements in fireworks and firecrackers pyrotechnic composition are measured based on energy dispersion type X-ray fluorescence spectra technology fast qualitative, it is excellent
Point is in particular in：(1) method is easy to operate, and can be tested call method repeatedly.Newly-built one is only needed before sample test
Secondary test method can recall in different time after method is established and repeat to detect, be required for again without testing every time
Establish test method.After establishing new test method for the first time, entire test process only enters sample including sample preparation, dress sample
Cup and three steps of examination with computer.（2）The method of the invention detection cycle is extremely short, after sample preparation is good, entirely measures
Journey total time-consuming about 5min.（3）The method of the invention labor intensity is very low and of less demanding to operating personnel.（4）Using this hair
Bright the method is detected, and accuracy is good, and precision is high, and False Rate is low.
Specific implementation mode
The present invention program is described in further detail with reference to embodiment, the following description is only intended to explain the invention, and
Its content is not defined.Experimental method used in following embodiments is conventional method unless otherwise specified, following
Material, sample used in embodiment etc., are commercially available unless otherwise specified.
Titanium elements in 1 pyrotechnic composition reference material of embodiment（Low content）The fluorescence intensity level of characteristic spectral line
Using black powder as matrix, ranging from 0~0.5% pyrotechnic composition reference material of Ti content is configured with titanium valve standard substance, is used
Energy dispersion type Xray fluorescence spectrometer measures the characteristic spectral line fluorescence intensity level of different Ti content pyrotechnic compositions, detecting instrument
Parameter is set as：Aperture is the X-ray light pipe collimator of 8.8mm, and setting filter is Al, and setting voltage is 20kV, analysis time
For 30s, energy range is 0~40keV, and during counting rate is, gaseous environment is air, and electric current is automatic, does not consider matrix effect,
It is K lines that the line of observation is composed at peak.It the results are shown in Table 1.
Table 1：Titanium elements in pyrotechnic composition reference material（Low content）The fluorescence intensity level of characteristic spectral line
| Ti content（%） | 0 | 0.05 | 0.15 | 0.20 | 0.25 | 0.30 | 0.35 | 0.40 |
| The fluorescence intensity of titanium elements characteristic spectral line（cps/mA） | 0 | 206 | 609 | 812 | 1008 | 1260 | 1310 | 1490 |
The result shows that：When titanium elements content is below 0.30%, titanium elements characteristic spectral line fluorescence intensity level is the increasing with content
Add and enhance, is positively correlated relationship, and substantially direct proportionality.Particularly, and when Ti content is 0.35%, titanium elements
Characteristic spectral line fluorescence intensity level（1310 cps/mA）Only than titanium elements content, corresponding titanium elements characteristic spectral line is glimmering at 0.30%
Light intensity value（1260 cps/mA）High 50cps/mA, content range decreases the incrementss of fluorescence intensity level than before.It is former
Because mainly as the increase of titanium elements content in sample makes each element in sample that titanium elements are produced with more obvious matrix
Effect, and this matrix effect can make the incrementss of titanium elements characteristic spectral line fluorescence intensity level generate certain random variation, sometimes
It waits fluorescence intensity incrementss and the phenomenon that negative growth occurs, it is strong with the fluorescence of titanium elements within 0.25% to be different from titanium elements content
Degree be substantially proportional to example increase variation, but titanium elements content be 0.25%~0.4% when fluorescence intensity still >=1000cps/mA.
It, can be using its fluorescence intensity >=1000cps/mA as judgment basis when effective detection of titanium elements being therefore limited to 0.25%.
Embodiment 2：Titanium elements in pyrotechnic composition reference material（Constant）Characteristic spectral line fluorescence intensity level
Using black powder as matrix, the pyrotechnic composition reference material for being 1~99.9% with titanium valve standard substance configuration content, with energy color
The fluorescence intensity that type Xray fluorescence spectrometer measures different Ti content pyrotechnic compositions is dissipated, the parameter of detecting instrument is set as：Aperture is
The X-ray light pipe collimator of 8.8mm, setting filter are Al, and setting voltage is 20kV, analysis time 30s, energy range 0
~40keV, during counting rate is, gaseous environment is air, and electric current is automatic, does not consider matrix effect, it is K lines that the line of observation is composed at peak.
It the results are shown in Table 2.
Table 2：The characteristic spectral line fluorescence intensity list of titanium in the pyrotechnic composition of constant Ti content
| Pyrotechnic composition reference material | 1 | 2 | 3 | 4 | 5 | 6 | 7 |
| Content（%） | 0 | 1 | 10 | 30 | 50 | 80 | 99.9 |
| Fluorescence intensity（cps/mA） | 0 | 4120 | 42621 | 123121 | 193561 | 35473 | 405803 |
As shown in Table 2：One, when not containing titanium elements in sample, the characteristic spectral line fluorescence intensity of titanium elements in corresponding method
Also it is 0.Two, take Ti content value difference larger（Such as 1%~99.9%）Point observation, corresponding characteristic spectral line fluorescence intensity be with
It the increase of content and enhances, correlation, but not direct proportionality.The main reason is that due to the content of titanium elements
Increase so that the matrix effect that each element generates titanium elements in sample is further apparent, and directly affecting for matrix effect can make it
It is corresponding can be generated with the increase of characteristic element with titanium elements characteristic spectral line fluorescence intensity incrementss it is certain with
The phenomenon that machine changes, and incrementss will appear negative growth sometimes.
For comprehensive Tables 1 and 2 related data it is found that when titanium elements content >=0.25%, the fluorescence of titanium elements characteristic spectral line is strong
Angle value always >=1000cps/mA.It therefore, can be by titanium elements characteristic spectrum when titanium elements content is in 0~99.9% range
Fluorescence intensity level >=1000cps/mA of line is as judgment basis of the titanium elements in sample containing measurement >=0.25%.
Embodiment 3：The repetitive test of method
The purpose of this repetitive test is that the mass percentage of titanium elements is 0.25% in different type firework medicament to confirm
When corresponding characteristic spectral line fluorescence intensity level titanium valve standard substance is added, configures respectively using different type pyrotechnic composition as matrix
The pyrotechnic composition reference material that titanium elements content is 0.25% is measured, and is detector with energy dispersion type Xray fluorescence spectrometer
Device, measures the fluorescence intensity of different Ti content pyrotechnic compositions, and the parameter of detecting instrument is set as：Aperture is the X-ray light pipe of 8.8mm
Collimator, setting filter are Al, and setting voltage is 20kV, and analysis time 30s, energy range is 0~40keV, and counting rate is
In, gaseous environment is air, and electric current is automatic, does not consider matrix effect, it is K lines that the line of observation is composed at peak.Specific test result is shown in Table
3。
Table 3：The fluorescence intensity level of titanium elements characteristic spectral line in different type pyrotechnic composition sample
By the test data of table 3 it is found that in different pyrotechnic composition samples, when titanium elements content is 0.25%, titanium elements feature is glimmering
Luminous intensity is 1000 cps/mA or so, is differed within ± 10%.
Embodiment 4：
The different-effect combined firework for extracting the production of Beihai, Guangxi enterprise carries out medicament analysis, judges in its pyrotechnic composition used
Whether titanium is contained.
（1）Pyrotechnic composition sample is dissected from combined firework and is come out, takes a small amount of multiple principle that 8g samples will be taken to place
It in copper mortar, is carefully ground with copper rod, crosses 60 mesh sieve, sample powder is placed in explosion-proof baking oven to 4 hours dry, drying
Temperature is 50 DEG C, is placed in drier is cooled to room temperature after drying,
（2）Establish detection method：Using energy dispersion type Xray fluorescence spectrometer as detecting instrument, is established and analyzed using intensity method
Method；The parameter of detecting instrument is set as：Aperture is the X-ray light pipe collimator of 8.8mm, and setting filter is Al, and voltage is arranged
For 20kV, analysis time 50s, energy range is 0~40keV, and during counting rate is, gaseous environment is air, electric current be it is automatic,
Do not consider matrix effect, it is K lines that the line of observation is composed at peak.
（3）Measure fluorescence intensity：Sample is fitted into instrument sample cup, the specimen cup equipped with sample is vertical on the table
Compacting 5 times, the specimen cup equipped with sample to be tested is placed in instrument test cabin, the fluorescence of titanium elements characteristic spectral line is directly determined
Intensity value F.The results are shown in Table 4.
Table 4：The fluorescence intensity level of titanium elements characteristic spectral line in different-effect combined firework pyrotechnic composition
| Sample number into spectrum | 1 | 2 | 3 | 4 | 5 | 6 |
| Fluorescence intensity（cps/mA） | 3 | 5580 | 6523 | 2 | 8485 | 2015 |
（4）It qualitatively judges in sample and whether contains titanium：A, as F >=1000cps/mA, judge to contain titanium in sample；B, as F <
1000cps/mA judges not containing titanium in sample.
By the test result of table 4 it is found that the characteristic spectral line fluorescence intensity level of titanium elements is respectively less than in sample 1 and sample 4
1000 cps/mA, therefore, it is possible to determine that sample 1 and sample 4 not titaniferous, and in sample 2,3,5,6 titanium elements characteristic spectral line
Fluorescence intensity level is all higher than 1000 cps/mA, it is possible to determine that sample 2,3,5,6 contains titanium.
Embodiment 5：
The different-effect spraying decoration class firework product for extracting the production of Hepu of Guangxi enterprise carries out medicament analysis, judges its pyrotechnics used
Whether contain titanium in medicine.
（1）Pyrotechnic composition sample is dissected from combined firework and is come out, takes a small amount of multiple principle that 5g samples will be taken to place
It in copper mortar, is carefully ground with copper rod, crosses 40 mesh sieve, sample powder is placed in explosion-proof baking oven to 5 hours dry, drying
Temperature is 60 DEG C, is placed in drier is cooled to room temperature after drying,
（2）Establish detection method：Using energy dispersion type Xray fluorescence spectrometer as detecting instrument, is established and analyzed using intensity method
Method；The parameter of detecting instrument is set as：Aperture is the X-ray light pipe collimator of 8.8mm, and setting filter is Al, and voltage is arranged
For 20kV, analysis time 50s, energy range is 0~40keV, and during counting rate is, gaseous environment is vacuum, electric current be it is automatic,
Do not consider matrix effect, it is K lines that the line of observation is composed at peak.
（3）Measure fluorescence intensity：Sample is fitted into instrument sample cup, the specimen cup equipped with sample is vertical on the table
Compacting 8 times, the specimen cup equipped with sample to be tested is placed in instrument test cabin, the fluorescence of titanium elements characteristic spectral line is directly determined
Intensity value F.The results are shown in Table 5.
Table 5：The fluorescence intensity level of titanium elements characteristic spectral line in different-effect spraying decoration class product pyrotechnic composition
| Sample number into spectrum | 1 | 2 | 3 | 4 | 5 | 6 |
| Fluorescence intensity（cps/mA） | 3 | 11254 | 8214 | 21562 | 6 | 2 |
（4）It qualitatively judges in sample and whether contains titanium：A, as F >=1000cps/mA, judge to contain titanium in sample；B, as F <
1000cps/mA judges not containing titanium in sample.
By the test result of table 5 it is found that the characteristic spectral line fluorescence intensity level of titanium elements is less than 1000 in sample 1,5 and 6
Cps/mA, the characteristic spectral line fluorescence intensity level of titanium elements is respectively less than 1000 cps/mA in sample 2~4.Therefore, it is possible to determine that sample
Product 2~4 contain titanium, not titaniferous in sample 1,5 and 6.
Embodiment 6：
The different-effect vomit bead fireworks product for extracting the production of liuyang hunan outlet fireworks manufacturing enterprise carries out medicament analysis, sentences
Whether contain titanium in its disconnected pyrotechnic composition used.
（1）Pyrotechnic composition sample is dissected from combined firework and is come out, takes a small amount of multiple principle that 10g samples will be taken to place
It in copper mortar, is carefully ground with copper rod, crosses 80 mesh sieve, sample powder is placed in explosion-proof baking oven to 4 hours dry, drying
Temperature is 75 DEG C, is placed in drier is cooled to room temperature after drying,
（2）Establish detection method：Using energy dispersion type Xray fluorescence spectrometer as detecting instrument, is established and analyzed using intensity method
Method；The parameter of detecting instrument is set as：Aperture is the X-ray light pipe collimator of 8.8mm, and setting filter is Al, and voltage is arranged
For 20kV, analysis time 60s, energy range is 0~40keV, and during counting rate is, gaseous environment is air, electric current be it is automatic,
Do not consider matrix effect, it is K lines that the line of observation is composed at peak.
（3）Measure fluorescence intensity：Sample is fitted into instrument sample cup, the specimen cup equipped with sample is vertical on the table
Compacting 3 times, the specimen cup equipped with sample to be tested is placed in instrument test cabin, the fluorescence of titanium elements characteristic spectral line is directly determined
Intensity value F.The results are shown in Table 6.
Table 6：The fluorescence intensity level of titanium elements characteristic spectral line in different-effect group of spitting out pearl product pyrotechnic composition
| Sample number into spectrum | 1 | 2 | 3 | 4 | 5 | 6 |
| Fluorescence intensity（cps/mA） | 0 | 31652 | 13 | 24 | 0 | 2 |
（4）It qualitatively judges in sample and whether contains titanium：A, as F >=1000cps/mA, judge to contain titanium in sample；B, as F <
1000cps/mA judges not containing titanium in sample.
By the test result of table 6 it is found that the characteristic spectral line fluorescence intensity level of titanium elements is more than 1000 cps/mA in sample 2,
The characteristic spectral line fluorescence intensity level of titanium elements is respectively less than 1000 cps/mA in sample 1,3,4,5,6.Therefore, it is possible to determine that sample
1,3,4,5,6 not titaniferous, 2 titaniferous of sample.
The foregoing is merely the preferred embodiment of the present invention, are not intended to restrict the invention, for those skilled in the art
For member, the invention may be variously modified and varied.Any modification made by all within the spirits and principles of the present invention, etc.
With replacement, improvement etc., should be included within the scope of the present invention.
Claims (7)
1. the Quick qualitative detection method of titanium elements in a kind of fireworks and firecrackers pyrotechnic composition, including prepare sample, establish detection side
Method detects the fluorescence intensity level of titanium elements characteristic spectral line in sample and is judged to whether there is titanium in sample according to F values, and feature exists
In being as follows：
1）Prepare sample：Pyrotechnic composition sample is dissected from fireworks and firecrackers product and is come out, takes a small amount of multiple principle by sample
It is placed in mortar made of antistatic material, is carefully ground with antistatic stick, be sieved, sample powder is placed on explosion-proof baking oven
Middle drying is placed in drier is cooled to room temperature after drying, spare；
2）Establish detection method：Using energy dispersion type Xray fluorescence spectrometer as detecting instrument, analysis side is established using intensity method
Method；
3）Detect the fluorescence intensity level of titanium elements characteristic spectral line in sample：After sample is fitted into instrument sample cup, sample will be housed
The specimen cup of product is vertically tamped for 3 times or more on the table, then the specimen cup equipped with sample to be tested is placed in detecting instrument test chamber
It is interior, the fluorescence intensity level of titanium characteristic spectral line is directly measured, the fluorescence intensity level F of titanium is shown on register instrument；
4）Judged to whether there is titanium in sample according to F values：
A, as F >=1000cps/mA, judge to contain titanium in sample；
B, as F < 1000cps/mA, judge not containing titanium in sample.
2. according to claim 1 in a kind of fireworks and firecrackers pyrotechnic composition titanium elements Quick qualitative detection method, feature
It is, mortar made of the antistatic material is copper mortar, and the antistatic stick is copper rod.
3. according to claim 1 in a kind of fireworks and firecrackers pyrotechnic composition titanium elements Quick qualitative detection method, feature
It is, the step 1）It takes total amount to be placed in mortar for 5~10g samples to be ground, crosses 40~100 mesh sieve.
4. according to claim 1 in a kind of fireworks and firecrackers pyrotechnic composition titanium elements Quick qualitative detection method, feature
It is, the drying time is 4~10 hours, and drying temperature is 50~75 DEG C.
5. according to claim 1 in a kind of fireworks and firecrackers pyrotechnic composition titanium elements Quick qualitative detection method, feature
It is, the step 2）The parameter of detecting instrument is set as：Aperture be 8.8mm~14mm X-ray light pipe collimator and can
The filter of X-ray of the energy less than 4.508 KeV is filtered, setting voltage is 18KV~22kV, and analysis time is >=20s, energy
Ranging from 0~40keV, during counting rate is, gaseous environment is air or vacuum, and electric current is automatic, does not consider matrix effect, peak spectrum
The line of observation is K lines.
6. according to claim 5 in a kind of fireworks and firecrackers pyrotechnic composition titanium elements Quick qualitative detection method, feature
It is, the parameter setting of detecting instrument：Filter is set as aluminium, voltage 20kV, analysis time 30s.
7. according to claim 1 in a kind of fireworks and firecrackers pyrotechnic composition titanium elements Quick qualitative detection method, feature
It is, thickness of sample >=3mm in the step 3) specimen cup.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| TWI685659B (en) * | 2019-05-03 | 2020-02-21 | 國防部軍備局生產製造中心第２０５廠 | Method and device for propellant examination by lapping method |
| TWI687678B (en) * | 2019-05-03 | 2020-03-11 | 國防部軍備局生產製造中心第２０５廠 | Method for propellant examination by optical method |
| CN111855719A (en) * | 2020-07-29 | 2020-10-30 | 河北南玻玻璃有限公司 | Sample preparation method for analyzing chemical components of quartz sandstone by X-ray fluorescence spectrometry |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106093098A (en) * | 2016-08-31 | 2016-11-09 | 吴俊逸 | A kind of measure the method for copper content in fireworks and firecrackers firework medicament |
-
2017
- 2017-12-27 CN CN201711445433.8A patent/CN108802082A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106093098A (en) * | 2016-08-31 | 2016-11-09 | 吴俊逸 | A kind of measure the method for copper content in fireworks and firecrackers firework medicament |
Non-Patent Citations (1)
| Title |
|---|
| 罗立强 等: "《X射线荧光光谱分析》", 31 May 2015, 化学工业出版社 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| TWI685659B (en) * | 2019-05-03 | 2020-02-21 | 國防部軍備局生產製造中心第２０５廠 | Method and device for propellant examination by lapping method |
| TWI687678B (en) * | 2019-05-03 | 2020-03-11 | 國防部軍備局生產製造中心第２０５廠 | Method for propellant examination by optical method |
| CN111855719A (en) * | 2020-07-29 | 2020-10-30 | 河北南玻玻璃有限公司 | Sample preparation method for analyzing chemical components of quartz sandstone by X-ray fluorescence spectrometry |
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