CN108120735A - The Quick qualitative detection method of strontium element in a kind of fireworks and firecrackers pyrotechnic composition - Google Patents
The Quick qualitative detection method of strontium element in a kind of fireworks and firecrackers pyrotechnic composition Download PDFInfo
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- CN108120735A CN108120735A CN201711443340.1A CN201711443340A CN108120735A CN 108120735 A CN108120735 A CN 108120735A CN 201711443340 A CN201711443340 A CN 201711443340A CN 108120735 A CN108120735 A CN 108120735A
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- G—PHYSICS
- G01—MEASURING; TESTING
- 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
- G01N23/22—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
- 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
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2223/00—Investigating materials by wave or particle radiation
- G01N2223/07—Investigating materials by wave or particle radiation secondary emission
- G01N2223/076—X-ray fluorescence
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Abstract
The invention discloses a kind of Quick qualitative detection methods of strontium element in fireworks and firecrackers pyrotechnic composition, belong to analysis and testing technology field.Pyrotechnic composition sample from fireworks and firecrackers product is dissected 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 instrument test cabin, the fluorescence intensity level of the strontium element characteristic spectral line shown on register instrument directly judges whether contain strontium in sample according to this fluorescence intensity level.Strontium element 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 strontium.
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 strontium element in qualitative detection fireworks and firecrackers pyrotechnic composition.
Background technology
In the prior art,《Fireworks and firecrackers pyrotechnic composition ingredient qualitative determination》（GB/T 15814.1-2010）List fireworks
The qualitative detection correlation technique of strontium, method basic principle in firecracker pyrotechnic composition：Sample after suitably pre-processing, with water or
Dissolving with hydrochloric acid, filtering, takes 2 drop filtrates on potassium chromate test paper.After 1 min, rhodizonic acid sodium solution is added dropwise to spot edge, such as
There is salmon pink spot in edge, and adding 1+20 hydrochloric acid (volume fraction), salmon pink spot disappears afterwards, indicates strontium ion.The method is deposited
In following deficiency：(1) detection cycle is longer, and general those of skill in the art need half of working day that could complete one-time detection.(2)
Operating procedure is relatively complicated, and sample will undergo dissolving, filtering, add some row steps such as indicator solution, chromogenic reaction that could obtain successively
Go out conclusion.（3）Method uses a variety of chemical reagent, and waste liquid has environment certain destruction.（4）The detection limit of method is unknown
Really, fireworks and firecrackers operation instruction is acted on little.
The method that energy dispersion type Xray fluorescence spectrometer is developed at present is chiefly used in the lossless qualitative analysis of sample.Pin
Solid sample sxemiquantitative and quantitative elemental are detected, most samples are directly measured such as using powder pressing method and fusion method：
《The measure x ray fluorescence spectrometry of bullion content》(GB/T 18043-2008) using nondestructive determination,《Aluminium oxide
The 30th partial x-ray fluorescence spectrum method for measuring constituent content of chemical analysis method and 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
Middle potassium, sodium, calcium, the content of aluminium》（Analytical instrument the 6th phase in 2013）Using pressed disc method,《It is limited the use of in electronic and electrical equipment
Substance lead, mercury, chromium, cadmium and the quick of bromine screen x ray fluorescence spectrometry》(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 carries out sample treatment using powder pressing method and fusion method.Up to now also there are no based on energy dispersion
The open source literature report of the method for strontium element in type X-ray fluorescence spectra technology fast qualitative detection fireworks and firecrackers pyrotechnic composition.
The content of the invention
It is quickly fixed based on energy dispersion type X-ray fluorescence spectra technology the technical problem to be solved in the present invention is to provide one kind
Property detection fireworks and firecrackers pyrotechnic composition in strontium element 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 identify sample in there are object element fingerprint
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 strontium member in unknown sample
Element.Fireworks and firecrackers pyrotechnic composition powder sample is directly gone up machine by the method for the present invention, specific analysis method is established, according to strontium feature
The characteristic x-ray fluorescence intensity value of spectral line come judge in sample whether there is strontium element.The method of the present invention is easy to operate, detection is all
Phase is short, and testing result accuracy is good, and precision is high.
The Quick qualitative detection method of strontium element, comprises the following steps in a kind of fireworks and firecrackers pyrotechnic composition：
1）Prepare sample：Pyrotechnic composition sample from fireworks and firecrackers product is dissected and is come out, takes a small amount of multiple principle by pyrotechnics
Medicine is placed on made of antistatic material in mortar, is carefully ground with antistatic stick, and sample powder is placed on explosion-proof baking by sieving
It is dry in case, it is placed in drier is cooled to room temperature after drying, it is 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 strontium element characteristic spectral line in sample：Sample is fitted into instrument sample cup, sample will be housed
Specimen cup vertically tamp 3 times or more on the table, sample to be tested is placed in instrument test cabin, show that strontium is first on register instrument
The fluorescence intensity level F of plain characteristic spectral line；
4）According to step 3）The result F selections of acquisition further determine whether that there are strontiums：
A, as F >=1000cps/mA, judge to contain strontium in sample；
B, as F ＜ 1000cps/mA, judge not containing strontium in sample.
Further, the step 1）Antistatic material made of mortar to be preferably copper mortar, it is described anti-quiet
Torch is preferably copper rod.
Further, the step 1）Total amount is taken to be placed in mortar for 5~10g samples to be ground, crosses 40~100 mesh
Sieve.
Further, the step 1）Drying time for 4~10 it is small when, drying temperature be 50~75 DEG C.
Further, the step 2）The parameter of detecting instrument is arranged to：Collimator aperture is 8.8~14mm, sets energy
Enough filter the filter of X-ray of the energy less than 14.142 KeV, voltage is 22~28kV, and analysis time is >=20s, energy range
For 0~40keV, during counting rate is, gaseous environment is air or vacuum, and electric current is that the automatic and peak spectrum line of observation is K lines.
Further, the parameter setting of detecting instrument：Filter is arranged to thick Pd, voltage is 25 kV, analysis time 30
s。
Further, thickness of sample >=3mm in the step 3) specimen cup.
The principle of the method for the present invention is as follows：The characteristics of for fireworks and firecrackers with pyrotechnic composition chemical composition, establish special number
Model is learned, global optimization can directly affect each factor of measurement result, including：For establishing the matrix of analysis method effect
Answer the matrix effect interaction type of mathmetic correction type and energy dispersion type X fluorescence spectrum instrument, voltage, electric current, filter
Work in every parameter and the specimen cups such as selection, analysis time, counting rate, gaseous environment, the energy range of mirror and the peak spectrum line of observation
Thickness of middle sample etc..Content and strontium element characteristic spectral line fluorescence intensity based on strontium element in powder sample are to be positively correlated
The fluorescence intensity level of relation and the content of strontium element and strontium element characteristic spectral line is in some strontium element concentration range substantially into just
Proportionate relationship it is assumed that sample can be qualitatively judged by detecting the fluorescence intensity of strontium element characteristic spectral line in sample by reasoning out
In whether the conclusion containing strontium.
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 percent concentration 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 percent concentration is identified
For impurity, and Holland finds contained lead element in certain kind fireworks from China in an import fireworks sampling inspection result
More than 120mg/kg, and circulated a notice of.Actual conditions and energy dispersion type X with reference to Chinese fireworks and firecrackers firework medicament are glimmering
The characteristics of photothermal spectroscopic analyzer device, strontium carbonate and strontium nitrate as one of common raw material of firework medicament, and due to strontium nitrate place
Easy deliquescence in air, the probability of fireworks enterprise strontium carbonate is relatively high, and strontium carbonate is in the quality hundred of firework medicament
Divide content generally all more than 5%, in order to solve the practical problem that raw material qualitative detection is often used in fireworks and firecrackers field conscientiously,
Effective detection of our law regulation strontium is defined to 1%.Instrument measuring be strontium element fluorescence intensity, since strontium carbonate is pyrotechnics
The most common strontium compound form of medicine is convenience of calculation, and strontium total amount is in terms of strontium carbonate.When Strontium carbonate contents are 1%, fluorescence intensity
For 1000cps/mA.Due in the actual production process, as raw material addition strontium carbonate firework medicament quality percentage
For content generally all more than 5%, why effective detection of strontium element is defined to 1% by the present invention, allows for fireworks and firecrackers life
Production is actual, if strontium element content is less than 1%, even if testing result is " detection ", it is also possible to be mixed miscellaneous in pyrotechnic composition
Matter, and it is not the raw material that the producer artificially adds, testing result is little to actual production directive significance.Contain if be detected
Measure for 1% when, the possibility artificially added is just very big, is simply adjusted on formula, can exclude to be pyrotechnic composition impurity element substantially
Possibility.Experimental data is shown, in different pyrotechnic composition reference materials, when Strontium carbonate contents are 1%, and strontium element feature
The fluorescence intensity level of spectral line is 1000cps/mA（Deviation is within 10%）.The method of the present invention is easy to operate, detection cycle is short, and
Testing result accuracy is good, and precision is high.
The present invention takes total amount to be placed in for 5~10g samples in mortar and is ground, and crosses 40~100 mesh sieves.Why by sample
Sample size be defined as 5~10g, allow for fireworks and firecrackers with pyrotechnic composition be formed by 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 can be directly affected；And the too big work that can influence sample test of sample size
Efficiency.Why will again place after the abundant mixing of sample after sieving and dry in an oven, 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 sieves mainly have two aspect reasons：One sieve pore allowed within 40 mesh is too big, be easy to cause screenings particle mistake
Granular size inhomogeneities that is big and causing analysis sample increases, 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, so as to seriously affect test result
Accuracy.On the other hand, if after pyrotechnic composition sample crosses sieves more than 100 mesh, very little that granularity can become not only influences sample
Screening efficiency as pyrotechnic composition particle is too small and the dust concentration in environment is caused to increase after sieving, to sample preparation, personnel make
Into certain health hazard, more important reason is since pyrotechnic composition of the grain size less than 100 mesh sieve holes is inflammable and explosive with height
Characteristic, it is easy to be exploded in air by electrostatic or spark initiation, cause the generation of accident.
Compared with prior art, the method for the invention has the beneficial effect that：
Strontium element in fireworks and firecrackers pyrotechnic composition is 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 after method is established, can recall in different time and repeat to detect, be required for again without testing every time
Establish test method.After new test method is established for the first time, entire test process only includes sample preparation, dress sample enters 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 embodiment
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.
The fluorescence intensity level of strontium element characteristic spectral line in the different Strontium carbonate contents pyrotechnic compositions of embodiment 1
With strontium carbonate standard substance, using black powder as matrix, the pyrotechnic composition that strontium carbonate mass percentage is 0~99.9% is configured
Reference material measures the strontium element characteristic spectral line of different Strontium carbonate contents pyrotechnic compositions with energy dispersion type Xray fluorescence spectrometer
Fluorescence intensity level, the parameter of detecting instrument are arranged to：Collimator aperture is 8.8mm, and setting filter is thickness Pd, and voltage is 25 kV,
Analysis time is 30s, and energy range is 0~40keV, and during counting rate is, gaseous environment is air, and electric current is seen for automatic and peak spectrum
Survey line is K lines.
It the results are shown in Table 1.
Table 1：The fluorescence intensity level of strontium element characteristic spectral line in different Strontium carbonate contents pyrotechnic compositions
| Content（%） | 0 | 0.1 | 0.2 | 0.4 | 0.6 | 0.8 | 1 | 1.2 | 1.3 |
| Fluorescence intensity（cps/mA） | 0 | 106 | 201 | 412 | 603 | 112 | 1002 | 1260 | 1281 |
| Content（%） | 1.6 | 1.8 | 2.0 | 10 | 30 | 50 | 80 | 99.9 | |
| Fluorescence intensity（cps/mA） | 1668 | 1869 | 2238 | 9854 | 28456 | 49852 | 82512 | 103779 |
The result shows that：When Strontium carbonate contents are in 0~99.9% scope, the fluorescence intensity level of strontium element characteristic spectral line is with carbon
The increase of sour content of strontium and increase, be positively correlated relation, and be substantially proportional to when Strontium carbonate contents are in 0~1.2% scope example pass
System.Particularly, when Strontium carbonate contents are 1.3%, the fluorescence intensity level of strontium element characteristic spectral line（1281cps/mA）Only compare carbonic acid
Content of strontium corresponding strontium element characteristic spectral line fluorescence intensity level at 1.2%（12609cps/mA）High 21 cps/mA, hence it is evident that fluorescence
The growth of intensity value and Strontium carbonate contents are disproportionate.The main reason is that：With the increase of Strontium carbonate contents in sample, sample
Middle each element generates strontium element further apparent matrix effect, this matrix effect can make the fluorescence intensity of strontium element characteristic spectral line
The phenomenon that incrementss of value can generate certain random variation, and incrementss can reduce or even be present with negative growth sometimes.But work as carbon
During sour content of strontium >=1%, the fluorescence intensity level of strontium element characteristic spectral line always >=1000cps/mA.Therefore, when strontium element content
It, can be using fluorescence intensity level >=1000cps/mA of strontium element characteristic spectral line as strontium member in sample when in the range of 0~99.9%
The judgment basis of cellulose content >=1%.
Embodiment 2：The repetitive test of method
The purpose of this repetitive test is that confirmation is corresponding when strontium carbonate mass percentage is 1% in different type pyrotechnic composition
The fluorescence intensity level of strontium element characteristic spectral line.Respectively using different type pyrotechnic composition as matrix, strontium carbonate standard substance, configuration are added in
Go out the pyrotechnic composition reference material sample that strontium carbonate mass percentage is 1% to be measured, with energy dispersion type x-ray fluorescence light
Spectrometer is detecting instrument, and the parameter of detecting instrument is arranged to：Collimator aperture is 8.8mm, setting filter be thickness Pd, voltage 25
KV, analysis time 30s, energy range is 0~40 keV, and during counting rate is, gaseous environment is air, and electric current is automatic and peak
The spectrum line of observation is K lines.
Specific test result is shown in Table 2.
Table 2：The fluorescence intensity level of strontium element characteristic spectral line in different type pyrotechnic composition sample
From the test data of table 2, in different pyrotechnic composition samples, when Strontium carbonate contents are 1%, strontium element characteristic spectral line
Fluorescence intensity level be 1000 cps/mA or so, differ within ± 10%.
Embodiment 3：
The different-effect combined firework for extracting the production of Beihai, Guangxi enterprise carries out medicament analysis, judges in its pyrotechnic composition used
Whether strontium is contained.
（1）Sample from combined firework is dissected and is come out, takes a small amount of multiple principle that 8g pyrotechnic compositions will be taken to be placed on copper
In mortar processed, carefully ground with copper rod, cross 60 mesh sieves, by sample powder be placed in explosion-proof baking oven dry 4 it is small when, drying temperature
For 50 DEG C, it 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, established and analyzed using intensity method
Method；The parameter of detecting instrument is arranged to：Collimator aperture is 8.8 mm, and it is 25 KV to set filter position thickness Pd, voltage, is analyzed
Time is 30s, and energy range is 40 keV, and during counting rate is, gaseous environment is vacuum, and electric current is that the automatic and peak spectrum line of observation is
K lines.
（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, directly determines the fluorescence of strontium element characteristic spectral line
Intensity value F.The results are shown in Table 3.
Table 3：The fluorescence intensity level of strontium element characteristic spectral line in different-effect combined firework pyrotechnic composition
| Sample number into spectrum | 1 | 2 | 3 | 4 | 5 | 6 |
| Fluorescence intensity（cps/mA） | 2 | 1 | 6563 | 5756 | 6042 | 5915 |
（4）It qualitatively judges in sample and whether contains strontium：A, as the cps/mA of F >=1000, judge to contain strontium in sample；B, as F ＜
1000cps/mA judges not containing strontium in sample.
By equal 1000 cps/ of ＜ of fluorescence intensity level of strontium element characteristic spectral line in the results showed that sample 1 and 2 of table 3
MA, therefore, it is possible to determine that sample 1 and 2 be free of strontium, and in sample 3,4,5,6 strontium element characteristic spectral line fluorescence intensity level >=
1000 cps/mA, it is possible to determine that sample 3,4,5,6 contains strontium.
Embodiment 4：
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 strontium in medicine.
（1）Sample from combined firework is dissected and is come out, takes a small amount of multiple principle that 5g pyrotechnic compositions will be taken to be placed on copper
In mortar processed, carefully ground with copper rod, cross 40 mesh sieves, by sample powder be placed in explosion-proof baking oven dry 5 it is small when, drying temperature
For 60 DEG C, it 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, established and analyzed using intensity method
Method；The parameter of detecting instrument is arranged to：Collimator aperture is 8.8 mm, and setting filter is thick Pd, voltage is 25 KV, analysis
Time is 50 s, and energy range is 40 keV, and during counting rate is, gaseous environment is air, and electric current composes the line of observation for automatic and peak
For K lines.
（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, directly determines the fluorescence of strontium element characteristic spectral line
Intensity value F.The results are shown in Table 4.
Table 4：The fluorescence intensity level of strontium element 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） | 0 | 4568 | 8854 | 6968 | 6 | 2 |
（4）It qualitatively judges in sample and whether contains strontium：A, as F >=1000cps/mA, judge to contain strontium in sample；B, as F ＜
1000cps/mA judges not containing strontium in sample.
By 1000 cps/ of fluorescence intensity level ＜ of strontium element characteristic spectral line in the results showed that sample 1,5 and 6 of table 4
MA, the fluorescence intensity level of strontium element characteristic spectral line >=1000 cps/mA in sample 2~4.Therefore, it is possible to determine that sample 2~4
Containing strontium, strontium is free of in sample 1,5 and 6.
Embodiment 5：
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 strontium in its disconnected pyrotechnic composition used.
（1）Sample from combined firework is dissected and is come out, takes a small amount of multiple principle that 10g pyrotechnic compositions will be taken to be placed on copper
In mortar processed, carefully ground with copper rod, cross 80 mesh sieves, by sample powder be placed in explosion-proof baking oven dry 4 it is small when, drying temperature
For 75 DEG C, it 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, established and analyzed using intensity method
Method；The parameter of detecting instrument is arranged to：Collimator aperture is 14mm, sets that filter is thick Pd, voltage is 25 KV, during analysis
Between for 30 s, energy range is 40 keV, and during counting rate is, gaseous environment is air, and electric current is that compose the line of observation be K at automatic and peak
Line.
（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, directly determines the fluorescence of strontium element characteristic spectral line
Intensity value F.The results are shown in Table 5.
Table 5：The fluorescence intensity level of strontium element 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 | 6652 | 13 | 12 | 0 | 2 |
（4）It qualitatively judges in sample and whether contains strontium：A, as F >=1000cps/mA, judge to contain strontium in sample；B, as F ＜
1000cps/mA judges not containing strontium in sample.
By the cps/mA of fluorescence intensity level >=1000 of strontium element characteristic spectral line in the results showed that sample 2 of table 5, sample
Equal 1000 cps/mA of ＜ of the fluorescence intensity level of strontium element characteristic spectral line in product 1,3,4,5,6.Therefore, it is possible to determine that sample 1,3,
4th, 5,6 strontium is free of, sample 2 contains strontium.
The foregoing is merely the preferred embodiment of the present invention, are not intended to limit the invention, for those skilled in the art
For member, the invention may be variously modified and varied.Any modification for being made within the spirit and principles of the invention, etc.
With replacement, improvement etc., should be included within the scope of the present invention.
Claims (7)
1. a kind of Quick qualitative detection method of strontium element in fireworks and firecrackers pyrotechnic composition, including preparing sample, establishing detection side
Method and qualitative detection strontium element, which is characterized in that be as follows：
1）Prepare sample：Pyrotechnic composition sample from fireworks and firecrackers product is dissected and is come out, takes a small amount of multiple principle by pyrotechnics
Medicine is placed on made of antistatic material in mortar, is carefully ground with antistatic stick, and sample powder is placed on explosion-proof baking by sieving
It is dry in case, it is placed in drier is cooled to room temperature after drying, it is 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 strontium element characteristic spectral line in sample：Sample is fitted into instrument sample cup, sample will be housed
Specimen cup vertically tamp 3 times or more on the table, sample to be tested is placed in instrument test cabin, show that strontium is first on register instrument
The fluorescence intensity level F of plain characteristic spectral line；
4）Judged to whether there is strontium in sample according to F values：
A, as F >=1000cps/mA, judge to contain strontium in sample；
B, as F ＜ 1000cps/mA, judge not containing strontium in sample.
2. according to claim 1 in a kind of fireworks and firecrackers pyrotechnic composition strontium element Quick qualitative detection method, feature
It is, the step 1）Antistatic material made of mortar be copper mortar, the antistatic stick be copper rod.
3. according to claim 1 in a kind of fireworks and firecrackers pyrotechnic composition strontium element Quick qualitative detection method, feature
It is, the step 1）Total amount is taken to be placed in mortar for 5~10g samples to be ground, crosses 40~100 mesh sieves.
4. according to claim 1 in a kind of fireworks and firecrackers pyrotechnic composition strontium element Quick qualitative detection method, feature
It is, the step 1）Drying time for 4~10 it is small when, drying temperature be 50~75 DEG C.
5. according to claim 1 in a kind of fireworks and firecrackers pyrotechnic composition strontium element Quick qualitative detection method, feature
It is, the step 2）The parameter of detecting instrument is arranged to：Collimator aperture is 8.8~14mm, and it is small that setting can filter energy
In the filter of the X-ray of 14.142 KeV, voltage is 22~28kV, and analysis time is >=20s, and energy range is 0~40keV,
During counting rate is, gaseous environment is air or vacuum, and electric current is that the automatic and peak spectrum line of observation is K lines.
6. according to claim 5 in a kind of fireworks and firecrackers pyrotechnic composition strontium element Quick qualitative detection method, feature
It is, the parameter setting of detecting instrument：Filter is arranged to thick Pd, voltage is 25 kV, analysis time 30s.
7. according to claim 1 in a kind of fireworks and firecrackers pyrotechnic composition strontium element Quick qualitative detection method, feature
It is, thickness of sample >=3mm in the step 3) specimen cup.
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| CN201711443340.1A Pending CN108120735A (en) | 2017-12-27 | 2017-12-27 | The Quick qualitative detection method of strontium element in a kind of fireworks and firecrackers pyrotechnic composition |
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106093097A (en) * | 2016-08-31 | 2016-11-09 | 吴俊逸 | A kind of measure the method for content of strontium in fireworks and firecrackers firework medicament |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106093097A (en) * | 2016-08-31 | 2016-11-09 | 吴俊逸 | A kind of measure the method for content of strontium 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 * |
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Application publication date: 20180605 |