CN107991332A - A kind of method of barium content in rapid semi-quantitative detection blind sample of fireworks and firecrackers pyrotechnic composition - Google Patents
A kind of method of barium content in rapid semi-quantitative detection blind sample of fireworks and firecrackers pyrotechnic composition Download PDFInfo
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- CN107991332A CN107991332A CN201711444398.8A CN201711444398A CN107991332A CN 107991332 A CN107991332 A CN 107991332A CN 201711444398 A CN201711444398 A CN 201711444398A CN 107991332 A CN107991332 A CN 107991332A
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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
Abstract
The method that the present invention discloses barium content in a kind of rapid semi-quantitative detection blind sample of fireworks and firecrackers pyrotechnic composition, belongs 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, sample to be tested is placed in detecting instrument test chamber again, the fluorescence intensity level of the barium elemental characteristic spectral line shown on register instrument, the content of estimation barium element in the sample, further selects appropriate analytical instrument to carry out the barium content in accurate quantitative analysis fireworks and firecrackers pyrotechnic composition.Barium content semi-quantitative analysis is carried out using the method for the invention, it is easy to operate, it is efficient, estimate the content of barium in sample and differ smaller with its actual content, and effectively can provide data foundation for the method for barium content in further selection accurate quantitative analysis sample.
Description
Technical field
The present invention relates to analysis and testing technology field, and in particular to one kind utilizes energy dispersion type Xray fluorescence spectrometer
The method that barium content in the blind sample of fireworks and firecrackers pyrotechnic composition is detected using intensity method rapid semi-quantitative.
Background technology
In the prior art, do not find quick-fried based on energy dispersion type X fluorescence spectrum joint technology rapid semi-quantitative detection fireworks
The method of bamboo barium content in the blind sample of pyrotechnic composition, the quantitative detecting method of rarely seen barium content.And in fireworks and firecrackers firework medicament
The detection method of barium content is to be based on traditional chemical analysis method, at present in fireworks and firecrackers firework medicament barium content measure side
Method is《Fireworks and firecrackers firework medicament part 1:The measure of barium content》（SN/T 1732.1-2014）, such method is all
Quantitative analysis is carried out to the barium in sample based on traditional chemical analysis method.The standard the method has the following disadvantages：(1)
Detection cycle is longer, and general those of skill in the art need 2 working days to complete one-time detection.In addition, tested specifically
It is easy in journey because of the uncertainty of testing crew skilled operation degree measuring result error not enough and caused by introducing.(2) operation step
Rapid relatively complicated, entirely testing needs to undergo sample pretreatment, washing, dissolving, filtering, transfer, precipitation, enrichment and titration etc.
All multi-steps.（3）Method experimenter is required it is high, in operating procedure many places be related to washing, transfer, dissolving, filtering, precipitation,
Enrichment, titration etc. are readily incorporated probabilistic operating procedure, each test operator must significant care and careful, otherwise
It is very easy to introduce artificial uncertainty.
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.
Being detected for solid sample sxemiquantitative and quantitative elemental, most samples are directly measured using powder pressing method and fusion method,
Such as：《The measure x ray fluorescence spectrometry of bullion content》(GB/T 18043-2008) using nondestructive determination,《Oxygen
Change the 30th partial x-ray fluorescence spectrum method for measuring constituent content of aluminum chemistry 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 magnesium》（Analytical instrument the 6th phase in 2013）Using pressed disc method,《Limited the use of in electronic and electrical equipment
Material 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 barium content method in type X-ray fluorescence spectra technology rapid semi-quantitative detection fireworks and firecrackers pyrotechnic composition.
The content of the invention
The technical problem to be solved in the present invention is to provide one kind based on energy dispersion type X-ray fluorescence spectra technology quick half
The method for quantitatively detecting barium content in the blind sample of fireworks and firecrackers pyrotechnic composition, fireworks and firecrackers pyrotechnic composition is analyzed by rapid semi-quantitative
Middle barium content, necessary data base is provided for barium content in the suitable spectral technique accurate quantitative analysis pyrotechnic composition of further selection
Plinth.The basic principle of detection：For pyrotechnic composition sample after by excitation of X-rays, the different elements in sample can launch different feature X
Ray, these characteristic spectral lines are to identify that there are the finger print information of object element in sample.Pass through object element in determination sample
Characteristic x-ray fluorescence intensity size, can be with the number of barium constituent content in semi-quantitative analysis unknown sample.The method of the present invention is by cigarette
The flower firecracker directly upper machine of pyrotechnic composition powder sample, establishes specific analysis method, glimmering according to the X-ray of barium elemental characteristic spectral line
Light intensity value carrys out barium constituent content in semi-quantitative analysis sample.The method is easy to operate, detection cycle is short, detection efficiency is high and smart
Density is high.The present invention seeks to what is be achieved through the following technical solutions：
A kind of method of barium content in rapid semi-quantitative detection blind sample of fireworks and firecrackers pyrotechnic composition, including prepare sample, establish inspection
The selection of survey method, measure fluorescence intensity, half-quantitative detection with calculating barium content and barium content accurate quantitative analysis method, specifically
Step is 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 on made of antistatic material in mortar, is carefully ground with antistatic rod, sieves, 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）Half-quantitative detection is with calculating barium content：After sample is fitted into instrument sample cup, by the specimen cup equipped with sample in table
It is vertical on face to tamp more than 3 times, then the specimen cup equipped with sample to be tested is placed in detecting instrument test chamber, directly determine barium
The fluorescence intensity level of elemental characteristic spectral line, the fluorescence intensity F of barium is shown on register instrument；
The fluorescence intensity level F of measure is calculated into the content of barium in sample as follows：
Wherein, ω represents the mass percentage of barium nitrate in sample, unit %；C represents the quality percentage of barium nitrate in sample
Corresponding characteristic spectral line fluorescence intensity level is C, unit cps/mA when content is 1%；F represents energy dispersion type x-ray fluorescence light
The fluorescence intensity level for the barium elemental characteristic spectral line that spectrometer is measured, unit cps/mA.
Further, the selection of barium content accurate quantitative analysis method is further included：According to step 3）Obtain the result choosing of ω
Select the instrument of further quantitative analysis：
A, as the mass percentage ω ＞ 10% of barium nitrate in firework medicament sample, select energy dispersion type X fluorescence spectrum method into
Barium content of the one step accurate quantitative analysis fireworks and firecrackers in pyrotechnic composition sample；
B, when mass percentage ω≤10% of barium nitrate in firework medicament sample, inductively coupled plasma transmitting light is selected
Barium content of the spectrometry further accurate quantitative analysis fireworks and firecrackers in pyrotechnic composition sample.
Further, the step 1）Antistatic material made of mortar be copper mortar, the antistatic rod is
Copper rod.
Further, the step 1）Take total amount to be placed in mortar for 5~10g samples to be ground, cross 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
The filter of X-ray of the energy less than 32.065 KeV is enough filtered, voltage be 45~50kV, 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 is preferred：To set filter be thick Cu, voltage 48kV, analysis time are
30s。
Further, the step 3）The value of C is 90~105 cps/mA in calculation formula.
Further, the step 3）The value of C preferably 100 cps/mA in calculation formula.
Further, pyrotechnic composition 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 with pyrotechnic composition chemical composition, establish special mathematical modulo
Type, global optimization can directly affect each factor of measurement result, including：For establishing the type and energy of analysis method
Matrix effect interaction type, voltage, electric current, filter and the peak of color dispersion-type X fluorescence spectrum instrument are composed the selection of the line of observation, are divided
Analyse thickness of sample etc. in the work in every parameters such as time, counting rate, gaseous environment, energy range and specimen cup.Based on barium member
Content of the element in powder sample and barium elemental characteristic spectral line fluorescence intensity are the relation that is positively correlated and the content and barium of barium element
The ratio of the fluorescence intensity level of elemental characteristic spectral line is fluctuated in some interval range it is assumed that detection can be passed through by reasoning out
The fluorescence intensity sxemiquantitative of barium elemental characteristic spectral line calculates the conclusion of the barium content in sample in sample.Instrument measuring is barium
The fluorescence intensity level of element total amount, is convenience of calculation since barium nitrate is the most common barium compound form of pyrotechnic composition, barium total amount
In terms of barium nitrate.The method of the present invention is easy to operate, detection cycle is short, detection efficiency is high, and testing result precision is high, is into one
The accurate quantitative analysis method of step selection barium content provides data foundation.
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
Explosive is closed, sample size is too small to be caused samples taken without representativeness and be difficult to meet in specimen cup that thickness of sample 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.Place after why the sample after sieving is fully mixed and dry in an oven again, also allow for firework medicament composition
Complexity, it is most likely that due to sample inhomogeneities and to test result produce harmful effect.Why sample crossed 40
~100 mesh sieves, mainly there is two aspect reasons：One sieve aperture allowed within 40 mesh is too big, be easy to cause screenings particle mistake
Granular size inhomogeneities increase that is big and causing analysis sample, and energy dispersion type X fluorescence spectrometer be to sample surfaces into
Row analysis, the non-uniform sample of granular size very likely produces 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 cause the dust concentration in environment to increase after sieving, to sample preparation, personnel make
Into certain health hazard, more important reason is due to that particle diameter is less than the pyrotechnic composition in 100 mesh sieve holes with highly inflammable and explosive
Characteristic, it is easy to exploded in atmosphere by electrostatic or spark initiation, cause the generation of accident.
Under normal conditions, energy dispersion type X fluorescence spectrometer is mainly used for quantifying when object element content is constant
Analysis, and inductive coupling plasma emission spectrograph be mainly used for micro or object element content it is relatively low when quantitative point
Analysis.In terms of the selection of object element accurate quantitative analysis method, since different elements have different fluorescent characteristics and other
Characteristic, according to barium element self structure characteristic, sends out in conjunction with energy dispersion type X fluorescence spectrum technology and inductively coupled plasma
The respective analysis speciality of spectral technique is penetrated, the critical reference that 10% barium content is set to subsequent quantitation analysis method by the present invention contains
Amount, for can be more quickly in further quantitative analysis sample barium content necessary reference frame is provided.
Compared with prior art, the method for the invention has the beneficial effect that：
Barium content in the blind sample of fireworks and firecrackers pyrotechnic composition is measured based on energy dispersion type X-ray fluorescence spectra technology rapid semi-quantitative
Method, its advantage is in particular in：(1) method is easy to operate, and can be tested call method repeatedly.Before sample test only
Need to create a test method, after method is established, can be recalled in different time and repeat to detect, without test every time
It is required for re-establishing test method.After new test method is established for the first time, whole test process only includes sample preparation, dress
Sample enters three steps of specimen cup and examination with computer.（2）The method of the invention detection cycle is extremely short, after sample preparation is good,
Whole measurement process total time-consuming about 5min.（3）The method of the invention labor intensity is very low and of less demanding to operating personnel.
（4）Further accurate quantitative analysis method primary dcreening operation is carried out using the method for the invention, detection efficiency is high, and precision is high.
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.
Embodiment 1：Barium constituent content is compared with the fluorescence intensity level of barium elemental characteristic spectral line in pyrotechnic composition
Since in the market can not find the pyrotechnic composition standard substance of the accurate definite value of barium constituent content, and because the physics shape of black powder
State is similar with pyrotechnic composition, and therefore, the pyrotechnic composition configured with barium nitrate standard substance using black powder as matrix difference barium content is joined
Material is examined to be tested.By detecting the characteristic spectral line fluorescence corresponding with its barium element of barium content in different pyrotechnic composition reference materials
The correspondence of intensity level carrys out barium content in reasoning firework medicament corresponding characteristic spectral line fluorescence intensity and generally corresponds to close
System.Using energy dispersion type Xray fluorescence spectrometer as detecting instrument, the parameter of detecting instrument is arranged to：Collimator aperture is
8.8mm, sets filter position thickness Cu, and voltage 48kV, analysis time 30s, energy range is 0~40keV, during counting rate is,
Gaseous environment is air, and electric current is that the automatic and peak spectrum line of observation is K lines.Barium member in half-quantitative detection difference pyrotechnic composition reference material
Plain characteristic spectral line fluorescence intensity size, the results are shown in Table 1.
Table 1：The fluorescence intensity level of barium elemental characteristic spectral line and the correspondence numerical tabular of content value when barium content is constant
| Pyrotechnic composition reference material is numbered | 1 | 2 | 3 | 4 | 5 | 6 |
| Barium nitrate content（%） | 0 | 10 | 30 | 50 | 80 | 99.9 |
| The fluorescence intensity level of barium elemental characteristic spectral line（cps/mA） | 0 | 924 | 2856 | 4952 | 8212 | 10379 |
| The ratio of fluorescence intensity level/content | 0 | 92.4 | 95.2 | 99.0 | 102.7 | 103.9 |
As shown in Table 1：First, when the fluorescence intensity level of the characteristic spectral line of barium element in not baric in sample, its corresponding method
For 0.2nd, barium content is taken to differ larger point observation, the fluorescence intensity level of its corresponding characteristic spectral line is with the increasing of barium content
Add and strengthen, be positively correlated relation, but not into stringent proportional relationship.It is primarily due to the content of barium element and increases
Adding makes the matrix effect that each element produces barium element in sample further obvious, and directly affecting for matrix effect can make its correspondence
Can be produced with the incrementss of barium elemental characteristic spectral line fluorescence intensity level with the increase of characteristic element it is certain random
Change.3rd, the mass percentage of barium nitrate in the sample（%）Corresponding barium elemental characteristic spectral line fluorescence intensity level
（cps/mA）Ratio be to be fluctuated in certain interval range（Concrete numerical value is 1：92.4~103.9）And it is positively correlated relation
's.Due to being half-quantitative detection, proportionality coefficient can use integral multiple ratio 1:90~1:105 carry out approximate calculation.Therefore, in sample
Barium content can use formulaCarry out sxemiquantitative calculating, wherein C represent sample in barium element mass percentage be 1% when pair
The fluorescence intensity level for the barium elemental characteristic spectral line answered, the value of unit cps/mA, C are 90~105.
Embodiment 2：The repetitive test of method（Barium content is 10%）
The purpose of method repetitive test be further confirm that barium in different type firework medicament mass percentage be 10% when
Corresponding barium elemental characteristic spectral line fluorescence intensity level.Respectively using different type firework medicament as matrix, configuration barium nitrate contains
Measure and be measured for 10% pyrotechnic composition reference material sample, using energy dispersion type Xray fluorescence spectrometer as detecting instrument, inspection
The parameter for surveying instrument is arranged to：Analysis method, collimator aperture 8.8mm are established using intensity method, setting filter is thickness Cu, electricity
Press as 48 kV, analysis time 30s, energy range is 0~40keV, and during counting rate is, gaseous environment is air, electric current be from
The dynamic and peak spectrum line of observation is K lines, the fluorescence intensity level of barium elemental characteristic spectral line in half-quantitative detection difference pyrotechnic composition reference material
Size, specific test result are shown in Table 2.
Table 2：The fluorescence intensity level of barium elemental characteristic spectral line in the different pyrotechnic composition reference materials that barium nitrate content is 10%
From the test data of table 2, for barium nitrate when the content in using different pyrotechnic composition matrix samples is 10%, its is corresponding
The fluorescence intensity level scope of barium elemental characteristic spectral line is 952~1034 cps/mA, content of the barium nitrate in firework medicament sample
（%）The fluorescence intensity level of corresponding barium elemental characteristic spectral line（cps/mA）Ratio be also positively correlated relation, and certain
Fluctuation in interval range（Concrete numerical value is 1：95.2~103.4）.Due to being half-quantitative detection, this proportionality coefficient can use integral multiple
1:95~1:105 carry out approximate calculation.So barium content can use formula in sampleSxemiquantitative calculating is carried out, wherein C is represented
Corresponding characteristic spectral line fluorescence intensity level when the mass percentage of barium element is 1% in sample, the value of unit cps/mA, C
For 95~105.
Embodiment 3：Sxemiquantitative quickly detects barium content in the blind sample of pyrotechnic composition and selects further accurate quantitative analysis method
（1）Pyrotechnic composition sample is dissected from fireworks and firecrackers product and is come out, takes a small amount of multiple principle that 5g samples will be taken to place
In copper mortar, carefully ground with copper rod, cross 40 mesh sieves, by sample powder be placed in explosion-proof baking oven dry 4 it is small when, it is dry
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, established using intensity method
Analysis method；The parameter of detecting instrument is arranged to：Collimator aperture is 8.8mm, and setting filter is thick Cu, voltage is 48 KV, point
The analysis time is 40s, energy range 40keV, 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 5 times, then the specimen cup equipped with sample to be tested is placed in detecting instrument test chamber, directly determine barium elemental characteristic spectral line
Fluorescence intensity level F.
The fluorescence intensity level F of measure is calculated into the content of barium in sample as follows：
Wherein, ω represents the mass percentage of barium nitrate in sample, unit %；C represents the quality percentage of barium nitrate in sample
Corresponding barium elemental characteristic spectral line fluorescence intensity level is C, unit cps/mA when content is 1%, the value of C is 100；F is represented
Energy dispersion type Xray fluorescence spectrometer measures the fluorescence intensity level of barium elemental characteristic spectral line, unit cps/mA.
Using the above method, then the pyrotechnic composition of other different substrates is taken to be tested, the results are shown in Table 3.
Barium content detection result in the 3 blind sample of fireworks and firecrackers pyrotechnic composition of table
| Firework medicament sample number into spectrum | 1 | 2 | 3 | 4 | 5 | 6 |
| Fluorescence intensity level（cps/mA） | 1248 | 1584 | 396 | 315 | 454 | 582 |
| Barium content（%） | 12.48 | 15.84 | 3.96 | 3.15 | 4.54 | 5.82 |
（3）Barium content quantitative method choice：According to following rule, according to 3 testing result of table, further selection is used for barium accurate quantitative analysis
The instrument of analysis：
A, ω ＞ 10%, can be selected the further accurate quantitative analysis fireworks and firecrackers pyrotechnic composition sample of energy dispersion type X fluorescence spectrum method
Barium content in product；
B, ω≤10%, can be selected the further accurate quantitative analysis fireworks and firecrackers cigarette of inductively coupled plasma emission spectrography
Barium content in gunpowder sample.
Firework medicament sample 1 and sample 2 can select energy dispersion type X fluorescence spectrum method to analyze fireworks and firecrackers pyrotechnic composition
Barium content in sample, it is quick-fried that inductively coupled plasma emission spectrography analysis fireworks can be selected in firework medicament sample 3,4,5 and 6
Barium content of the bamboo in pyrotechnic composition sample.
Embodiment 4：
6 pyrotechnic composition reference material samples of different barium contents are configured using the red effect pyrotechnic composition of not baric element as matrix,
Using energy dispersion type Xray fluorescence spectrometer as detecting instrument, the parameter of detecting instrument is arranged to：Established and analyzed using intensity method
Method, collimator aperture are 8.8 mm, and setting filter is thickness Cu, and voltage is 48 kV, and analysis time is 60 s, energy range 0
~40 keV, during counting rate is, gaseous environment is air, and electric current is that the automatic and peak spectrum line of observation is K lines, and half-quantitative detection is different
Barium elemental characteristic spectral line fluorescence intensity size in pyrotechnic composition reference material, uses the detection of 3 method of embodiment and ordinary chemical analysis
The result of method detection is contrasted, and the results are shown in Table 4.The results show with the barium content that embodiment 3 detects with by common
The barium constituent content value of chemical analysis method detection very close to the detection of, two methods result ratio 84~97%, completely can be with
It is used for the half-quantitative detection of barium content in the blind sample of fireworks and firecrackers pyrotechnic composition with the method for the present invention.
The results contrast of barium content in 4 distinct methods of the table detection blind sample of fireworks and firecrackers pyrotechnic composition
| Firework medicament sample number into spectrum | 1 | 2 | 3 | 4 | 5 | 6 |
| Fluorescence intensity（cps/mA） | 1248 | 1584 | 396 | 315 | 454 | 582 |
| Estimate content（%） | 12.48 | 15.84 | 3.96 | 3.15 | 4.54 | 5.82 |
| Quantitative detection level（%） | 14.25 | 17.14 | 4.36 | 3.26 | 5.36 | 6.58 |
| Estimate content/quantitative detection level（%） | 87.58 | 92.42 | 90.83 | 96.63 | 84.70 | 88.45 |
The foregoing is merely the preferred embodiment of the present invention, is not intended to limit the invention, and comes for those skilled in the art
Say, the invention may be variously modified and varied.Any modification for being made within the spirit and principles of the invention, equally replace
Change, improve, should be included within the scope of the present invention.
Claims (10)
1. a kind of method of barium content in rapid semi-quantitative detection blind sample of fireworks and firecrackers pyrotechnic composition, including prepare sample, establish
Detection method and half-quantitative detection are with calculating barium content, it is characterised in that comprise the following steps that：
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 on made of antistatic material in mortar, is carefully ground with antistatic rod, sieves, placed after sample powder is fully mixed
It is dry in explosion-proof baking oven, it is placed in drier be cooled to room temperature after drying, it is spare；
2）Establish detection method：Using energy dispersion type Xray fluorescence spectrometer as detecting instrument, analysis side is established using intensity method
Method；
3）Half-quantitative detection is with calculating barium content：After sample is fitted into instrument sample cup, by the specimen cup equipped with sample in table
It is vertical on face to tamp more than 3 times, then the specimen cup equipped with sample to be tested is placed in detecting instrument test chamber, directly measure barium member
The fluorescence intensity of plain characteristic spectral line, the fluorescence intensity level F shown on register instrument；
The fluorescence intensity level F of measure is calculated into the content of barium in sample as follows：
Wherein, ω represents the mass percentage of barium nitrate in sample, unit %；C represents the quality percentage of barium nitrate in sample
The fluorescence intensity level of corresponding characteristic spectral line is C, unit cps/mA when content is 1%；F represents energy dispersion type x-ray fluorescence
The barium elemental characteristic spectral line fluorescence intensity level that spectrometer is measured, unit cps/mA.
2. the method that rapid semi-quantitative detects barium content in the blind sample of fireworks and firecrackers pyrotechnic composition according to claim 1, it is special
Sign is, the selection of barium content quantitative analysis method is further included, specially according to step 3）The result selection for obtaining ω is further
The instrument of quantitative analysis：
A, ω ＞ 10%, select the further quantitative analysis fireworks and firecrackers of energy dispersion type X fluorescence spectrum method with pyrotechnic composition sample
Barium content；
B, ω≤10%, selects the further quantitative analysis fireworks and firecrackers pyrotechnic composition sample of inductively coupled plasma emission spectrography
Barium content in product.
3. the method that rapid semi-quantitative detects barium content in the blind sample of fireworks and firecrackers pyrotechnic composition according to claim 1, it is special
Sign is, the step 1）Antistatic material made of mortar be copper mortar, the antistatic rod is copper rod.
4. the method that rapid semi-quantitative detects barium content in the blind sample of fireworks and firecrackers pyrotechnic composition according to claim 1, it is special
Sign is, the step 1）Take total amount to be placed in mortar for 5~10g samples to be ground, cross 40~100 mesh sieves.
5. the method that rapid semi-quantitative detects barium content in the blind sample of fireworks and firecrackers pyrotechnic composition according to claim 1, it is special
Sign is, the step 1）Drying time for 4~10 it is small when, drying temperature be 50~75 DEG C.
6. the method that rapid semi-quantitative detects barium content in the blind sample of fireworks and firecrackers pyrotechnic composition according to claim 1, it is special
Sign is, the step 2）The parameter of detecting instrument is arranged to：Collimator aperture is 8.8~14mm, and setting can filter energy
The filter of X-ray less than 32.065 KeV, voltage are 45~50kV, 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.
7. the method that rapid semi-quantitative detects barium content in the blind sample of fireworks and firecrackers pyrotechnic composition according to claim 6, it is special
Sign is, the parameter setting of detecting instrument：Setting filter is thick Cu, voltage 48kV, analysis time 30s.
8. the method that sxemiquantitative quickly detects barium content in the blind sample of fireworks and firecrackers pyrotechnic composition according to claim 1, it is special
Sign is, the step 3）The value of C is 90~105 cps/mA in calculation formula.
9. the method that rapid semi-quantitative detects barium content in the blind sample of fireworks and firecrackers pyrotechnic composition according to claim 1, it is special
Sign is, the step 3）The value of C is 100 cps/mA in calculation formula.
10. the method that rapid semi-quantitative detects barium content in the blind sample of fireworks and firecrackers pyrotechnic composition according to claim 1, it is special
Sign is, thickness of sample >=3mm in the step 3) specimen cup.
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| FR2137955A1 (en) * | 1971-05-17 | 1972-12-29 | Westinghouse Electric Corp | |
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| CN106324005A (en) * | 2016-08-31 | 2017-01-11 | 吴俊逸 | Method for determining content of Ba in pyrotechnic composition for fireworks and firecrackers |
| CN106338533A (en) * | 2016-08-31 | 2017-01-18 | 吴俊逸 | Method for determining content of barium in barium carbonate for fireworks and crackers |
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| FR2137955A1 (en) * | 1971-05-17 | 1972-12-29 | Westinghouse Electric Corp | |
| CN2927043Y (en) * | 2006-07-25 | 2007-07-25 | 上海英迈吉东影图像设备有限公司 | Apparatus for inspecting explosive by back scattering technology |
| CN106093096A (en) * | 2016-08-31 | 2016-11-09 | 吴俊逸 | A kind of measure the method for barium content in fireworks and firecrackers barium nitrate |
| CN106324005A (en) * | 2016-08-31 | 2017-01-11 | 吴俊逸 | Method for determining content of Ba in pyrotechnic composition for fireworks and firecrackers |
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