CN107991333A - A kind of method of copper content in rapid semi-quantitative detection blind sample of fireworks and firecrackers pyrotechnic composition - Google Patents
A kind of method of copper content in rapid semi-quantitative detection blind sample of fireworks and firecrackers pyrotechnic composition Download PDFInfo
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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
Abstract
The method that the present invention discloses copper 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 copper characteristic spectral line shown on register instrument, the content of estimation copper in the sample, further selects appropriate analytical instrument to carry out the copper content in accurate quantitative analysis fireworks and firecrackers pyrotechnic composition.Copper 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 copper in sample and differ smaller with its actual content, and effectively can provide data foundation for the method for copper 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 copper 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 bamboo method of copper content in the blind sample of pyrotechnic composition, the quantitative detecting method of rarely seen copper content.And in fireworks and firecrackers firework medicament
The detection method of copper content is to be based on traditional chemical analysis method, at present in fireworks and firecrackers firework medicament copper content measure side
Method is《Fireworks and firecrackers the 4th part of firework medicament:The measure of copper content》（SN/T 1732.4-2014）, such method is all
Quantitative analysis is carried out to the copper 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 copper 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 copper content in the blind sample of fireworks and firecrackers pyrotechnic composition, fireworks and firecrackers pyrotechnic composition is analyzed by rapid semi-quantitative
Middle copper content, necessary data base is provided for copper 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 copper coin cellulose content in semi-quantitative analysis unknown sample.This method is quick-fried by fireworks
The bamboo directly upper machine of pyrotechnic composition powder sample, establishes specific part method, according to the x-ray fluorescence intensity of copper characteristic spectral line
Value carrys out copper coin cellulose content in semi-quantitative analysis sample.The method is easy to operate, detection cycle is short, detection efficiency is high and precision
It is high.The present invention seeks to what is be achieved through the following technical solutions：
A kind of method of copper content in rapid semi-quantitative detection blind sample of fireworks and firecrackers pyrotechnic composition, including prepare sample, establish inspection
The selection of survey method, half-quantitative detection with calculating copper content and copper content accurate quantitative analysis method, comprises 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, 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 copper 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 instrument detection test chamber, Direct Determination of Copper 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 copper in sample as follows：
Wherein, ω represents the mass percentage of cupric oxide in sample, unit %；C represents the quality percentage of cupric oxide in sample
Corresponding characteristic spectral line fluorescence intensity level is C when content is 1%, and the value of unit cps/mA, C are 1100~1200；F is represented
Energy dispersion type X-ray fluorescence spectra measures the fluorescence intensity level of copper characteristic spectral line, unit cps/mA.
Instrument measuring be copper total amount fluorescence intensity level, since cupric oxide is the most common copper compound of pyrotechnic composition
Form, is convenience of calculation, copper total amount is in terms of cupric oxide.
Further, the selection of copper 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, ω ＞ 5%, select the further accurate quantitative analysis fireworks and firecrackers pyrotechnic composition sample of energy dispersion type X fluorescence spectrum method
In copper content；
B, ω≤5%, selects the further accurate quantitative analysis fireworks and firecrackers pyrotechnic composition of inductively coupled plasma emission spectrography
Copper content in sample.
Further, mortar made of the antistatic material is copper mortar, and 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, when the drying time is 4~10 small, drying temperature is 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 8.041 KeV is enough filtered, voltage be 18~22kV, 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：It is middle thickness Pd, voltage 20kV, analysis time to set filter
For 30s.
Further, the step 3）The value of C is 1100~1200 cps/mA in calculation formula.
Further, the step 3）The value of C preferably 1150 cps/mA in calculation formula.
Further, the step 3）Pyrotechnic composition thickness of sample >=3mm in 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 copper coin
Content of the element in powder sample and copper characteristic spectral line fluorescence intensity are the relation that is positively correlated and the content and copper of copper
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 copper characteristic spectral line calculates the conclusion of the copper content in sample in sample.This method operation letter
List, detection cycle is short, detection efficiency is high, and testing result precision is high, for the accurate quantitative analysis of further selection copper content
Method 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 copper 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 1% copper content is set to subsequent quantitation analysis method by the present invention contains
Amount, for can be more quickly in further quantitative analysis sample copper content necessary reference frame is provided.
Compared with prior art, the method for the invention has the beneficial effect that：
Copper 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：Copper coin cellulose content is compared with the fluorescence intensity level of copper characteristic spectral line in pyrotechnic composition
Since in the market can not find the pyrotechnic composition standard substance of the accurate definite value of copper coin cellulose content, and because the physics shape of black powder
State is similar with pyrotechnic composition, and therefore, the pyrotechnic composition configured with cupric oxide standard substance using black powder as matrix different Cu content is joined
Material is examined to be tested.Detect copper content characteristic spectral line fluorescence intensity corresponding with its copper in different pyrotechnic composition reference materials
The correspondence of value carrys out the correspondence of the corresponding characteristic spectral line fluorescence intensity of copper content in reasoning firework medicament.With energy
Color dispersion-type Xray fluorescence spectrometer is detecting instrument, and the parameter of detecting instrument is arranged to：Collimator aperture is 8.8mm, sets filter
Mirror position thickness Cu, voltage 48kV, analysis time 30s, energy range is 0~40keV, and during counting rate is, gaseous environment is sky
Gas, electric current are that the automatic and peak spectrum line of observation is K lines.Copper characteristic spectral line is glimmering in half-quantitative detection difference pyrotechnic composition reference material
Luminous intensity size, the results are shown in Table 1.
Table 1：The fluorescence intensity level of copper characteristic spectral line and the correspondence numerical tabular of content value when copper content is constant
| Pyrotechnic composition reference material | 1 | 2 | 3 | 4 | 5 | 6 |
| Aoxidize copper content（%） | 0 | 10 | 30 | 50 | 80 | 99.9 |
| Fluorescence intensity level（cps/mA） | 0 | 11372 | 33676 | 58123 | 88541 | 118487 |
| Fluorescence intensity level/content | 0 | 1137.2 | 1122.5 | 1162.5 | 1106.8 | 1186.1 |
As shown in Table 1：First, when not containing copper in sample, the fluorescence intensity level of copper characteristic spectral line in its corresponding method
For 0.2nd, copper value content is taken to differ larger point observation, the fluorescence intensity level of its corresponding characteristic spectral line is with copper content
Increase and strengthen, be positively correlated relation, but not into stringent proportional relationship.It is primarily due to the content of cupric oxide and increases
Adding makes the matrix effect that each element produces copper in sample further obvious, and directly affecting for matrix effect can make its correspondence
Can be produced with the incrementss of copper characteristic spectral line fluorescence intensity level with the increase of characteristic element it is certain random
Change.3rd, the mass percentage of cupric oxide in the sample（%）The fluorescence intensity level of corresponding copper characteristic spectral line
（cps/mA）Ratio be to be fluctuated in certain interval range（Concrete numerical value is 1：1106~1186）And it is positively correlated relation.
Due to being half-quantitative detection, proportionality coefficient can use integral multiple 1:1100~1:1200 carry out approximate calculation.Therefore, copper contains in sample
Amount can use formulaSxemiquantitative calculating is carried out, wherein C represents corresponding when the mass percentage of copper in sample is 1%
The fluorescence intensity level of copper characteristic spectral line, the value of unit cps/mA, C are 1100~1200.
Embodiment 2：The repetitive test of method（Copper content is 10%）
The purpose of method repetitive test be further confirm that copper in different type firework medicament mass percentage be 10% when
Corresponding copper characteristic spectral line fluorescence intensity level.Respectively using different type pyrotechnic composition as matrix, configuration oxidation copper content
It is measured for 10% pyrotechnic composition reference material sample, using energy dispersion type Xray fluorescence spectrometer as detecting instrument, detection
The parameter of instrument is arranged to：Analysis method, collimator aperture 8.8mm are established using intensity method, setting filter is middle thickness Pd, electricity
Press as 20 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 copper characteristic spectral line in half-quantitative detection difference pyrotechnic composition reference material,
Specific test result is shown in Table 2.
Table 2：The fluorescence intensity level of copper characteristic spectral line in the different pyrotechnic composition reference materials that copper content is 1%
From the test data of table 2, for cupric oxide when the content in using different pyrotechnic composition matrix samples is 10%, its is corresponding
The fluorescence intensity level scope of copper characteristic spectral line is 11064~11754 cps/mA, and cupric oxide is in firework medicament sample
Content（%）Corresponding copper characteristic spectral line fluorescence intensity level（cps/mA）Ratio is also positively correlated relation, and certain
Fluctuation in ratio interval range（Concrete numerical value is 1:1106~1:1176）.Due to being half-quantitative detection, this proportionality coefficient can use
Integral multiple 1:1100~1:1200 carry out approximate calculation.So copper content can use formula in sampleSxemiquantitative calculating is carried out,
Wherein C represents corresponding characteristic spectral line fluorescence intensity level when the mass percentage of copper in sample is 1%, unit cps/
The value of mA, C are 1100~1200.
Embodiment 3：Sxemiquantitative quickly detects copper 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 and analyzed using intensity method
Method；The parameter of detecting instrument is arranged to：Collimator aperture is 8.8mm, and setting filter is middle thickness Pd, voltage is 20 KV, analysis
Time is 40s, energy range 40keV, and during counting rate is, gaseous environment is air, and electric current is that the automatic and peak spectrum line of observation is K
Line.
（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 copper characteristic spectral line
Intensity level.
By the fluorescence intensity level of measureThe mass percentage content of copper in sample is calculated as follows：
Wherein, ω represents the mass percentage of cupric oxide in sample, unit %；C represents the quality percentage of cupric oxide in sample
Corresponding copper characteristic spectral line fluorescence intensity level is C when content is 1%, and the value of unit cps/mA, C are 1150；F is represented
Energy dispersion type Xray fluorescence spectrometer measures the fluorescence intensity level of copper characteristic spectral line, unit cps/mA.
The pyrotechnic composition of other different substrates is taken to be tested using the above method again, the results are shown in Table 3.
The content detection result of cupric oxide 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） | 16892 | 9254 | 5521 | 8864 | 3521 | 7856 |
| Copper content（%） | 14.69 | 8.05 | 4.80 | 7.71 | 3.06 | 6.83 |
（3）Copper content quantitative approach selects：Further select accurately to determine for copper according to the testing result of table 3 according to following rule
Measure the instrument of analysis：
A, ω ＞ 5%, can be selected the further accurate quantitative analysis fireworks and firecrackers pyrotechnic composition sample of energy dispersion type X fluorescence spectrum method
The content of copper in product；
B, ω≤5%, can be selected the further accurate quantitative analysis fireworks and firecrackers pyrotechnics of inductively coupled plasma emission spectrography
The content of copper in medicine sample.
Firework medicament sample 3 and sample 5 can select inductively coupled plasma emission spectrography analysis fireworks and firecrackers to use
Energy dispersion type X fluorescence spectrum method analysis fireworks can be selected in the content of copper in pyrotechnic composition sample, firework medicament sample 1,2,4 and 6
The content of firecracker copper in pyrotechnic composition sample.
Embodiment 4：
6 pyrotechnic composition reference material samples of different Cu content are configured using the red effect pyrotechnic composition without copper 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 middle thickness Pd, and voltage is 20 kV, and analysis time is 60 s, energy range
For 0~40 keV, during counting rate is, gaseous environment is air, and electric current is that to compose the line of observation be K lines at automatic and peak, half-quantitative detection
Copper characteristic spectral line fluorescence intensity size in different pyrotechnic composition reference materials, uses the detection of 3 method of embodiment and general chemistry
The result of analysis method detection is contrasted, and the results are shown in Table 4.The copper coin cellulose content that the results show is detected with embodiment 3 with
By the copper coin cellulose content that ordinary chemical analysis method detects very close to the result ratio of two methods detection is 81~113%.
Therefore, 3 method of example can be used to be used for the half-quantitative detection of copper content in the blind sample of fireworks and firecrackers pyrotechnic composition completely.
The results contrast of copper content in 5 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 level（cps/mA） | 16892 | 9254 | 5521 | 8864 | 3521 | 7856 |
| Estimate copper content（%） | 14.69 | 8.05 | 4.80 | 7.71 | 3.06 | 6.83 |
| Quantitatively detect copper content（%） | 15.69 | 9.21 | 5.67 | 6.84 | 3.74 | 7.95 |
| Estimate content/quantitative detection level（%） | 93.62 | 87.37 | 84.67 | 112.69 | 81.86 | 85.93 |
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 copper 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 copper 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 copper 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, Direct Determination of Copper 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 copper in sample as follows：
Wherein, ω represents the mass percentage of cupric oxide in sample, unit %；C represents the quality percentage of cupric oxide 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 fluorescence intensity level for the copper characteristic spectral line that spectrum is measured, unit cps/mA.
2. the method that rapid semi-quantitative detects copper content in the blind sample of fireworks and firecrackers pyrotechnic composition according to claim 1, it is special
Sign is, the selection of copper 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 ＞ 5%, select energy dispersion type X fluorescence spectrum method further quantitative analysis fireworks and firecrackers copper in pyrotechnic composition sample
Content；
B, ω≤5%, selects the further quantitative analysis fireworks and firecrackers pyrotechnic composition sample of inductively coupled plasma emission spectrography
The content of middle copper.
3. the method that rapid semi-quantitative detects copper content in the blind sample of fireworks and firecrackers pyrotechnic composition according to claim 1, it is special
Sign is that mortar made of the antistatic material is copper mortar, and the antistatic rod is copper rod.
4. the method that rapid semi-quantitative detects copper 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 copper content in the blind sample of fireworks and firecrackers pyrotechnic composition according to claim 1, it is special
Sign is, when the drying time is 4~10 small, drying temperature is 50~75 DEG C.
6. the method that rapid semi-quantitative detects copper 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 8.041 KeV, voltage are 18~22kV, 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.
7. the method that rapid semi-quantitative detects copper 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：It is middle thickness Pd, voltage 20kV, analysis time 30s to set filter.
8. the method that sxemiquantitative quickly detects copper 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 1100~1200 cps/mA in calculation formula.
9. the method that rapid semi-quantitative detects copper 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 1150 cps/mA in calculation formula.
10. the method that rapid semi-quantitative detects copper content in the blind sample of fireworks and firecrackers pyrotechnic composition according to claim 1, it is special
Sign is, the step 3）Thickness of sample >=3mm in specimen cup.
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| CN201711444400.1A Pending CN107991333A (en) | 2017-12-27 | 2017-12-27 | A kind of method of copper content in rapid semi-quantitative detection blind sample of fireworks and firecrackers pyrotechnic composition |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR2137955A1 (en) * | 1971-05-17 | 1972-12-29 | Westinghouse Electric Corp | |
| CN101968552A (en) * | 2010-09-27 | 2011-02-09 | 上海交通大学 | X-ray wavelength dispersion and diffraction based hazardous article detection method |
| 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 |
| CN106226340A (en) * | 2016-08-31 | 2016-12-14 | 广西出入境检验检疫局危险品检测技术中心 | A kind of measure the method for copper content in fireworks and firecrackers copper sulfate |
| CN106324005A (en) * | 2016-08-31 | 2017-01-11 | 吴俊逸 | Method for determining content of Ba in pyrotechnic composition for fireworks and firecrackers |
-
2017
- 2017-12-27 CN CN201711444400.1A patent/CN107991333A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR2137955A1 (en) * | 1971-05-17 | 1972-12-29 | Westinghouse Electric Corp | |
| CN101968552A (en) * | 2010-09-27 | 2011-02-09 | 上海交通大学 | X-ray wavelength dispersion and diffraction based hazardous article detection method |
| 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 |
| CN106226340A (en) * | 2016-08-31 | 2016-12-14 | 广西出入境检验检疫局危险品检测技术中心 | A kind of measure the method for copper content in fireworks and firecrackers copper sulfate |
| CN106324005A (en) * | 2016-08-31 | 2017-01-11 | 吴俊逸 | Method for determining content of Ba in pyrotechnic composition for fireworks and firecrackers |
Non-Patent Citations (3)
| Title |
|---|
| 罗立强等: "《X射线荧光光谱分析》", 31 March 2015 * |
| 蒋国军等: "EDX、XRD 法定性分析混合火药的主要成分", 《刑事技术》 * |
| 黄敏等: "传火药快速检测方法研究", 《国防技术基础》 * |
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