CN108120737A - A kind of method of Ti content in rapid semi-quantitative detection blind sample of fireworks and firecrackers pyrotechnic composition - Google Patents
A kind of method of Ti content in rapid semi-quantitative detection blind sample of fireworks and firecrackers pyrotechnic composition Download PDFInfo
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- 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
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Abstract
The method that the present invention discloses Ti 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 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, sample to be tested is placed in detecting instrument test chamber again, the fluorescence intensity level of the titanium elements characteristic spectral line shown on register instrument, the content of estimation titanium elements in the sample, further selects appropriate analytical instrument to carry out the Ti content in accurate quantitative analysis fireworks and firecrackers pyrotechnic composition.Ti content semi-quantitative analysis is carried out using the method for the invention, it is easy to operate, it is efficient, it estimates the content of titanium in sample and differs smaller with its actual content, and effectively can provide data foundation for the method for Ti content in further selection accurate quantitative analysis sample.
Description
Technical field
The present invention relates to analysis and testing technology fields, and in particular to a kind of to utilize energy dispersion type Xray fluorescence spectrometer
The method that Ti 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 Ti content in the blind sample of pyrotechnic composition, the quantitative detecting method of rarely seen Ti content.And in fireworks and firecrackers firework medicament
The detection method of Ti content be based on traditional chemical analysis method, at present in fireworks and firecrackers firework medicament Ti content measure side
Method is《Fireworks and firecrackers the 5th part of firework medicament：The measure of Ti content》（SN/T 1732.5-2006）, such method is all
Quantitative analysis is carried out to the titanium 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 that could complete one-time detection.In addition, it was tested specifically
It is easy to introduce the uncertainty for causing measuring result error due to testing crew skilled operation degree is inadequate in journey.(2) operation step
Suddenly it is relatively complicated, after sample priority absolute ethyl alcohol and the multiple washing of acetone, with filtering, transfer, collection filter after dilute nitric acid dissolution
Then slag fully dissolves filter residue with hydrochloric acid again, then undergo filtering, trivalent titanium ion is oxidized to titanic by washing, oxidizer
Ion is sheltered tetravalence titanium ion with screening agent, finally with the content of titanium in EDTA residual quantity titration measuring solution.（3）
Method is high to experimenter's requirement, and many places are related to the appearances such as washing, transfer, dissolving, filtering, precipitation, enrichment, titration in operating procedure
Probabilistic operating procedure is easily introduced, each test operator must significant care and careful, otherwise very easy introducing
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.
It 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 titanium 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 magnesium》（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 Ti 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 Ti content in the blind sample of fireworks and firecrackers pyrotechnic composition analyzes fireworks and firecrackers pyrotechnic composition by rapid semi-quantitative
Middle Ti content provides necessary data base for Ti 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 informations of object element in sample.Pass through object element in determination sample
Characteristic x-ray fluorescence intensity size, can be with the number of titanium elements 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 analysis method, strong according to the x-ray fluorescence of titanium elements characteristic spectral line
Angle value carrys out titanium elements 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 Ti content in rapid semi-quantitative detection blind sample of fireworks and firecrackers pyrotechnic composition, including preparing sample, establishing inspection
The selection of survey method, half-quantitative detection with calculating Ti content and Ti content accurate quantitative analysis method, is 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 sample
It is placed on made of antistatic material in mortar, is carefully ground with antistatic stick, sieve, sample powder is placed on explosion-proof baking oven
Middle drying is placed in drier is cooled to room temperature after drying, spare；
2) detection method is established：Using energy dispersion type Xray fluorescence spectrometer as detecting instrument, analysis side is established using intensity method
Method；
3）Half-quantitative detection is with calculating Ti content：After sample is fitted into instrument sample cup, by the specimen cup equipped with sample in table
It is vertically tamped on face 3 times or more, then the specimen cup equipped with sample to be tested is placed in detecting instrument test chamber, directly measure titanium 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 titanium in sample as follows：
Wherein, ω represents the mass percentage of titanium in sample, unit %；C represents the mass percentage of titanium elements in sample
For 0.1% when corresponding characteristic spectral line fluorescence intensity level be C, the value of unit cps/mA, C are 370~430；F represents energy
The fluorescence intensity level for the titanium elements characteristic spectral line that color dispersion-type X-ray fluorescence spectra is measured, unit cps/mA.
Further, the selection of Ti 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 Ti content；
B, ω≤5% selects the further accurate quantitative analysis fireworks and firecrackers pyrotechnic composition of inductively coupled plasma emission spectrography
Ti content in sample.
Further, mortar made of the antistatic material is copper mortar, and the antistatic stick is 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, 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：Aperture is the X-ray light pipe of 8.8mm~14mm
Collimator and can filter energy less than 4.508 KeV X-ray filter, settings voltage be 18KV~22kV, analysis time
For >=20s, energy range is 0~40keV, and during counting rate is, gaseous environment is air or vacuum, electric current be it is automatic, without considering
Matrix effect, the peak spectrum line of observation is K lines.
Further, the parameter setting of detecting instrument is preferred：Filter is arranged to Al, voltage is 20 kV, analysis time is
30s。
Further, the step 3）The value of C is 370~430 cps/mA in calculation formula.
Further, the step 3）The value of C preferably 400 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 of analysis method and energy
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 titanium member
Content of the element in powder sample and titanium elements characteristic spectral line fluorescence intensity are the relation that is positively correlated and the content and titanium of titanium elements
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 titanium elements characteristic spectral line calculates the conclusion of the Ti 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 Ti 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
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.
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 titanium elements self structure characteristic, is sent 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 5% Ti content is set to subsequent quantitation analysis method by the present invention contains
Amount, for can be more quickly in further quantitative analysis sample Ti content necessary reference frame is provided.
Compared with prior art, the method for the invention has the beneficial effect that：
Ti 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, advantage is in particular in：(1) method is easy to operate, and can be tested call method repeatedly.Before sample test only
It needs to create a test method, after method is established, can be recalled in different time and repeat to detect, without testing every time
It is required for re-establishing test method.After new test method is established for the first time, entire 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.
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.
Embodiment 1：Titanium elements content is compared with the fluorescence intensity level of titanium elements characteristic spectral line in pyrotechnic composition
Since the pyrotechnic composition standard substance of the accurate definite value of titanium elements content, and because the physics shape of black powder can not be found in the market
State is similar with pyrotechnic composition, and therefore, the pyrotechnic composition configured with titanium valve standard substance using black powder as matrix difference Ti content refers to
Substance is tested.Detect the correspondence of the characteristic spectral line fluorescence intensity level that Ti content is corresponding in different pyrotechnic composition reference materials
Relation carrys out the correspondence of the corresponding characteristic spectral line fluorescence intensity of Ti content in reasoning firework medicament.With energy dispersion type X
Ray fluorescence spectrometer is detecting instrument, and the parameter of detecting instrument is arranged to：Analysis method, collimator holes are established using intensity method
Footpath is 8.8mm, and setting filter is Al, and voltage is 20 kV, and analysis time 30s, energy range is 0~40keV, and counting rate is
In, gaseous environment is air, and electric current is that compose the line of observation be K lines at automatic and peak, in half-quantitative detection difference pyrotechnic composition reference material
Titanium elements characteristic spectral line fluorescence intensity size, the results are shown in Table 1.
Table 1：The fluorescence intensity level of titanium elements characteristic spectral line and the correspondence numerical tabular of content value when Ti content is constant
| Pyrotechnic composition reference material | 1 | 2 | 3 | 4 | 5 | 6 |
| Ti content（%） | 0 | 10 | 30 | 50 | 80 | 99.9 |
| Fluorescence intensity level（cps/mA） | 0 | 42621 | 123121 | 193561 | 35473 | 405803 |
| The ratio of fluorescence intensity level/content | 0 | 4262.1 | 4104.0 | 3871.2 | 443.4 | 4062.1 |
As shown in Table 1：First, when not containing titanium in sample, the fluorescence intensity level of titanium elements characteristic spectral line in corresponding method
For 0.2nd, Ti content value is taken to differ larger point observation, the fluorescence intensity level of corresponding characteristic spectral line is with Ti content
Increase and enhance, be positively correlated relation, but not into stringent proportional relationship.The main reason is that since the content of titanium elements increases
Adding makes the matrix effect that each element generates titanium elements in sample further apparent, and directly affecting for matrix effect can make its correspondence
Can be generated with the incrementss of titanium elements characteristic spectral line fluorescence intensity level with the increase of characteristic element it is certain random
Variation.3rd, the mass percentage of titanium in the sample（%）The fluorescence intensity level of corresponding titanium elements characteristic spectral line
（cps/mA）Ratio is fluctuated in certain interval range（Concrete numerical value is 1：3871~4262）And it is positively correlated relation.By
Then half-quantitative detection, proportionality coefficient can use integral multiple 1:3800~1:4300 carry out approximate calculation.Therefore, Ti content in sample
Formula can be usedSxemiquantitative calculating is carried out, wherein C represents corresponding when the mass percentage of Tao Yuansu in sample is 0.1%
The fluorescence intensity level of titanium elements characteristic spectral line, the value of unit cps/mA, C are 380~430.
Embodiment 2：The repetitive test of method（Ti content is 10%）
The purpose of method repetitive test be further confirm that titanium in different type firework medicament mass percentage be 10% when
Corresponding titanium elements characteristic spectral line fluorescence intensity level.Respectively using different firework medicaments as matrix, configuration Ti content is 10%
Sample is measured, and using energy dispersion type Xray fluorescence spectrometer as detecting instrument, the parameter of detecting instrument is arranged to：Using
Intensity method establishes analysis method, collimator aperture 8.8mm, and setting filter is Al, and voltage is 20 kV, analysis time 30s,
Energy range is 0~40keV, and during counting rate is, gaseous environment is air, and electric current is that compose the line of observation be K lines at automatic and peak, semidefinite
Amount detects titanium elements characteristic spectral line fluorescence intensity level in different pyrotechnic composition reference materials, and specific test result is shown in Table 2.
Table 2：Titanium elements characteristic spectral line fluorescence intensity level in the different pyrotechnic composition reference material samples that Ti content is 10%
From the test data of table 2, titanium elements are corresponding when using the content in different pyrotechnic composition matrix samples as 10%
The fluorescence intensity level scope of characteristic spectral line be 37485~42147 cps/mA, content of the titanium in firework medicament sample（%）With it
Corresponding titanium elements characteristic spectral line fluorescence intensity level（cps/mA）Ratio is 3748~4214.Content of the titanium in pyrotechnic composition sample
（%）The fluorescence intensity level of corresponding titanium elements characteristic spectral line（cps/mA）Relation is positively correlated, and ratio is in certain section
In the range of fluctuate（Concrete numerical value is 1：3748~4214）.Due to being half-quantitative detection, this proportionality coefficient can use integral multiple 1:
3700~1:4300 carry out approximate calculation.So Ti content can use formula in sampleCarry out sxemiquantitative calculating, wherein C tables
Corresponding characteristic spectral line fluorescence intensity level when the mass percentage of titanium elements is 0.1% in sample product, unit cps/mA, C
Value be 370~430.
Embodiment 3：Sxemiquantitative quickly detects Ti content in the blind sample of pyrotechnic composition and selects further accurate quantitative analysis method
（1）Pyrotechnic composition sample from fireworks and firecrackers product is dissected 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 it is Al to set filter, voltage is 20 KV, analysis time
For 50s, energy range 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.
（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 titanium elements characteristic spectral line
Intensity value F.
By the fluorescence intensity level of measureThe content of titanium in sample is calculated as follows：
Wherein, ω represents the mass percentage of titanium in sample, unit %；C represents the mass percentage of titanium elements in sample
For 0.1% when corresponding characteristic spectral line fluorescence intensity level be C, the value of unit cps/mA, C are 400；F represents energy dispersion
Type X-ray fluorescence spectra measures the fluorescence intensity level of titanium elements 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.
Ti content testing 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） | 4125 | 24512 | 31245 | 61268 | 6687 | 8654 |
| Titanium mass percentage（%） | 1.031 | 6.128 | 7.811 | 15.317 | 1.672 | 2.164 |
（3）Ti content quantitative approach selects：It further selects accurately to determine for titanium according to the testing result of table 3 according to following rule
Measure the instrument of analysis：
A, the further accurate quantitative analysis fireworks and firecrackers pyrotechnic composition sample of energy dispersion type X fluorescence spectrum method can be selected in ω ＞ 5%
Ti content in product；
B, the further accurate quantitative analysis fireworks and firecrackers pyrotechnics of inductively coupled plasma emission spectrography can be selected in ω≤5%
Ti content in medicine sample.
Firework medicament sample 1,5 and 6 can select inductively coupled plasma emission spectrography to analyze fireworks and firecrackers cigarette
Energy dispersion type X fluorescence spectrum method analysis fireworks and firecrackers can be selected in the content of titanium in gunpowder sample, firework medicament sample 2,3 and 4
With the content of titanium in pyrotechnic composition sample.
Embodiment 4：
To be free of 6 pyrotechnic composition reference material samples of the red effect pyrotechnic composition as the different Ti contents of matrix configuration of titanium elements,
Using energy dispersion type Xray fluorescence spectrometer as detecting instrument, the parameter of detecting instrument is arranged to：It is established and analyzed using intensity method
Method, collimator aperture be 8.8 mm, settings filter be Al, voltage be 20 kV, analysis time be 60 s, energy range be 0~
40 keV, during counting rate is, gaseous environment is air, and electric current is that compose the line of observation be K lines at automatic and peak, half-quantitative detection difference cigarette
Titanium elements characteristic spectral line fluorescence intensity size in gunpowder reference material uses the detection of 3 method of embodiment and ordinary chemical analysis side
The result of method detection is compared, and the results are shown in Table 4.The results show with the titanium elements content that embodiment 3 detects with by general
The titanium elements content of logical chemical analysis method detection is very close to the result ratio of two methods detection is 80~95%.Therefore, it is complete
Half-quantitative detection of 4 method of example for Ti content in the blind sample of fireworks and firecrackers pyrotechnic composition can be used entirely.
The results contrast of Ti 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 level（cps/mA） | 4125 | 24512 | 31245 | 61268 | 6687 | 8654 |
| The Ti content of estimation（%） | 1.031 | 6.128 | 7.811 | 15.317 | 1.672 | 2.164 |
| Quantitatively detect Ti content（%） | 1.247 | 6.941 | 8.741 | 16.245 | 1.924 | 2.698 |
| Estimate content/quantitative detection level（%） | 82.70 | 88.29 | 89.36 | 94.29 | 86.89 | 80.19 |
The foregoing is merely the preferred embodiment of the present invention, are not intended to limit the invention, and come for those skilled in the art
It says, the invention may be variously modified and varied.Any modification for being made within the spirit and principles of the invention is equally replaced
It changes, improve, should be included within the scope of the present invention.
Claims (10)
1. a kind of method of Ti content in rapid semi-quantitative detection blind sample of fireworks and firecrackers pyrotechnic composition, including preparing sample, establishing
Detection method and half-quantitative detection are with calculating Ti content, which is characterized in that are 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 sample
It is placed on made of antistatic material in mortar, is carefully ground with antistatic stick, sieve, will be placed after the abundant mixing of sample powder
It is dry in explosion-proof baking oven, 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）Half-quantitative detection is with calculating Ti content：After sample is fitted into instrument sample cup, by the specimen cup equipped with sample in table
It is vertically tamped on face 3 times or more, then the specimen cup equipped with sample to be tested is placed in detecting instrument test chamber, directly measure titanium 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 Ti content in sample as follows：
Wherein, ω represents the mass percentage of titanium in sample, unit %；C represents the mass percentage of titanium elements in sample
For 0.1% when corresponding characteristic spectral line fluorescence intensity level be C, unit cps/mA；F represents energy dispersion type x-ray fluorescence light
Spectrum measures the fluorescence intensity level of titanium elements characteristic spectral line, unit cps/mA.
2. the method that rapid semi-quantitative detects Ti content in the blind sample of fireworks and firecrackers pyrotechnic composition according to claim 1, special
Sign is, the selection of Ti 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 the further quantitative analysis fireworks and firecrackers of energy dispersion type X fluorescence spectrum method in pyrotechnic composition sample
Ti content；
B, ω≤5% selects the further quantitative analysis fireworks and firecrackers pyrotechnic composition sample of inductively coupled plasma emission spectrography
In Ti content.
3. the method that rapid semi-quantitative detects Ti content in the blind sample of fireworks and firecrackers pyrotechnic composition according to claim 1, special
Sign is that mortar made of the antistatic material is copper mortar, and the antistatic stick is copper rod.
4. the method that rapid semi-quantitative detects Ti content in the blind sample of fireworks and firecrackers pyrotechnic composition according to claim 1, special
Sign 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.
5. the method that rapid semi-quantitative detects Ti content in the blind sample of fireworks and firecrackers pyrotechnic composition according to claim 1, 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 Ti content in the blind sample of fireworks and firecrackers pyrotechnic composition according to claim 1, special
Sign is, the step 2）The parameter of detecting instrument is arranged to：Aperture is the X-ray light pipe collimator and energy of 8.8mm~14mm
Enough filter energy less than 4.508 KeV X-ray filter, settings voltage be 18KV~22kV, analysis time be >=20s, energy
Amount scope is 0~40keV, and during counting rate is, gaseous environment is air or vacuum, and electric current is automatic, without considering matrix effect, peak
The spectrum line of observation is K lines.
7. the method that rapid semi-quantitative detects Ti content in the blind sample of fireworks and firecrackers pyrotechnic composition according to claim 6, special
Sign is, the parameter setting of detecting instrument：Filter is arranged to aluminium, voltage 20kV, analysis time 30s.
8. the method that sxemiquantitative quickly detects Ti content in the blind sample of fireworks and firecrackers pyrotechnic composition according to claim 1, special
Sign is, the step 3）The value of C is 370~430 cps/mA in calculation formula.
9. the method that rapid semi-quantitative detects Ti content in the blind sample of fireworks and firecrackers pyrotechnic composition according to claim 1, special
Sign is, the step 3）The value of C is 400 cps/mA in calculation formula.
10. the method that rapid semi-quantitative detects Ti content in the blind sample of fireworks and firecrackers pyrotechnic composition according to claim 1, special
Sign is, the step 3）Thickness of sample >=3mm in specimen cup.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711443382.5A CN108120737A (en) | 2017-12-27 | 2017-12-27 | A kind of method of Ti content in rapid semi-quantitative detection blind sample of fireworks and firecrackers pyrotechnic composition |
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| CN109443868A (en) * | 2018-10-30 | 2019-03-08 | 周守虎 | The method for measuring Ti content in fireworks material |
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