CN106338533A - Method for determining content of barium in barium carbonate for fireworks and crackers - Google Patents
Method for determining content of barium in barium carbonate for fireworks and crackers Download PDFInfo
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- CN106338533A CN106338533A CN201610776050.8A CN201610776050A CN106338533A CN 106338533 A CN106338533 A CN 106338533A CN 201610776050 A CN201610776050 A CN 201610776050A CN 106338533 A CN106338533 A CN 106338533A
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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
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
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Abstract
The invention discloses a method for determining the content of barium in barium carbonate for fireworks and crackers. The method comprises the following steps: preparing a plurality of parts of barium carbonate working fluid with different concentrations, taking an energy dispersion X-ray fluorescence spectrophotometer as a detecting instrument, assuming a certain sample size, establishing an analysis method through an intensity calibration mathematical calibration method to convert the mass concentrations of Ba in the plurality of parts of prepared barium carbonate working fluid into mass percent concentrations of Ba, recording the fluorescence intensity of Ba injected each time, and establishing a calibration curve; preparing a pyrotechnic composition to be tested into sample fluid, recording the fluorescence intensity of Ba displayed on the instrument, reading out the mass percent concentration value of Ba corresponding to the fluorescence intensity of Ba according to the determined calibration curve, and computing the content of barium in a sample. According to the method, matrix effects among all elements in the sample can be eliminated or basically eliminated by optimizing sample dissolving conditions and all parameter conditions of the X-ray fluorescence spectrophotometer, and the method is simple to operate, short in detection period, good in accuracy and high in precision.
Description
Technical field
The present invention relates to analysis and testing technology field is and in particular to energy dispersion type x-ray fluorescent spectrometry kind measures cigarette
The method of barium content in flower firecracker brium carbonate.
Background technology
In prior art, the detection method of the main constituent barium content in fireworks and firecrackers brium carbonate is based on traditional credit
Analysis method, the method standard commonly used at present is " industrial potassium titanate " (gb 1614-2011).The ultimate principle of this standard method: carbon
Sour barium generates barium chloride with hydrochloric acid reaction, is subsequently adding sulfuric acid solution and generates barium sulfate precipitate, according to the Mass Calculation of barium sulfate
Go out the content of brium carbonate.
This standard methods described has the disadvantage that (1) detection cycle is longer, and general those of skill in the art need 1～2
Working day just can complete one-time detection.In addition, being easy in concrete process of the test because testing crew skilled operation degree is inadequate
Introduce the uncertainty causing measuring result error.(2) operating procedure is cumbersome, successively will through sample dissolution, heated and boiled,
The step such as filter, precipitate, refiltering, drying, weighing.
The method that energy dispersion type x-ray fluorescence spectrophotometer is developed at present is used for the lossless qualitative analyses of sample.Pin
To solid sample sxemiquantitative and quantitative elemental detection, most samples adopt nondestructive determination, powder pressing method and fusion method
Directly measure (such as: " the mensure x-ray fluorescent spectrometry of bullion content " (gb/t 18043-2008) uses lossless inspection
Survey method, " aluminium oxide chemical analysis method and method for measuring physical properties the 30th part x-ray fluorescence spectrum method for measuring element contain
Amount " (gb/t6609.30 2009) use fusion method, and " edxrf method directly measures w-fe-ni-co alloy compound group
Point " (" nuclear electronics and Detection Techniques " 05 phase in 2007) use pressed disc method, " x-ray fluorescent spectrometry quickly measures nitre
Strontium, sodium, calcium, the content of magnesium in sour strontium product " (analytical tool the 6th phase in 2013) use pressed disc method, " electronic and electrical equipment
Middle regulated substance lead, hydrargyrum, the rapid screening x-ray fluorescent spectrometry of chromium, cadmium and bromine " (gb/z 21277-2007) use
Pressed disc method or fusion method).Up to now also there are no the energy dispersion type x based on matrix effect targeting control technology (solwution method)
Ray fluorescence spectrometry detects the open source literature report of barium content in fireworks and firecrackers barium nitrate.
Content of the invention
The technical problem to be solved in the present invention is to provide that a kind of the method is simple to operate, detection cycle is short, and testing result
Accuracy is good, the high method measuring barium content in fireworks and firecrackers barium nitrate of precision.
A kind of method measuring barium content in fireworks and firecrackers brium carbonate, comprises the following steps:
S1, drafting calibration curve
S11, prepare many parts of concentration barium nitrate working solution not etc.；
S12, with energy dispersion type x-ray fluorescence spectrophotometer as detecting instrument, strong using x fluorescence spectrum quantitative analysis
Degree correction mathmetic correction sets up analysis method, and (in this step, selected 2.0g is the sample size being supposed for calibration curve with 2.0g
The sample size that calibration curve supposes, is in the matrix effect considering energy dispersion type x-ray fluorescence spectrophotometer through applicant
On the basis of, carry out what substantial amounts of test determined, changing this numerical value will affect accuracy and the precision of test result)；
In the many parts of barium nitrate working solutions that step s11 is prepared, the mass concentration of ba is converted into the mass percent concentration of ba, then by
One sample introduction, records the fluorescence intensity of each sample introduction, the mass percent concentration of the ba with each working solution as abscissa, with above-mentioned
The corresponding fluorescence intensity of mass percent concentration of ba is vertical coordinate, makes calibration curve；Wherein, by following formula by nitric acid
In barium working solution, the mass concentration of ba is converted into the mass percent concentration of ba:
Wherein, ba% represents the mass percent concentration of ba in barium nitrate working solution, and unit is %；C represents barium nitrate work
Make the mass concentration of ba in liquid, unit is g/l；0.5 represents the volume supposing sample size constant volume, and unit is l；2 represent that calibration is bent
The sample size that line supposes, unit is g；
S2, the quick barium content measuring in fireworks and firecrackers brium carbonate:
S21, preparation test liquid: with fireworks and firecrackers brium carbonate as sample, weigh m gram, with a certain amount of nitric acid and water
Constant volume is configured to the test liquid that volume is v, and ensures the concentration of ba element in the solution after constant volume in calibration curve scope；
S22, by step s12 testing conditions, test liquid is loaded specimen cup it is ensured that sample liquid thickness >=15mm, records energy
The fluorescence intensity of the ba of display in chromatic dispersion quantity type x-ray fluorescence spectrophotometer, bent according to the calibration of above-mentioned determination with this fluorescence intensity
Line reads corresponding ba mass percent concentration value；
The content of barium in s23, calculating sample:
As follows calculate sample in simple substance barium mass percent concentration:
Wherein, ω represents the mass percent concentration of simple substance ba in sample, and unit is %；ω0Represent according to calibration curve
The ba mass percent concentration value reading, unit is %；2 represent the sample size that calibration curve supposes, unit is g；M represents sample
The actual quality weighing, unit is g；V represent constant volume after sample dissolution volume it is ensured that in solution after constant volume ba element dense
In calibration curve scope, unit is ml to degree；500 represent the volume supposing sample size constant volume, and unit is ml.
Further, the mass concentration of the barium nitrate working solution ba of s11 is 0.15g/l～0.73g/l, this concentration range warp
Cross applicant on the basis of the matrix effect considering energy dispersion type x-ray fluorescence spectrophotometer, carry out substantial amounts of test
Determine, changing this numerical value will affect accuracy and the precision of test result.
Further, nitric acid volume described in s11 is 10ml～30ml, and mass percent concentration is 10%～30%.
Further, the testing conditions of s12 are: using the x-ray light pipe collimator for 8.8mm～14mm for the aperture, can
Filter the filter that energy is less than the x-ray of 37.410kev, setting voltage is 45kv～55kv, analysis time is 25s～100s,
Energy range is 0～40kev, and during counting rate is, gaseous environment is air, and electric current is automatic, and matrix effect is not consider.
Preferably, in s12, the testing inspection condition of energy dispersion type x-ray fluorescence spectrophotometer is: using thick cu filter, hole
Footpath is the x-ray light pipe collimator of 8.8mm～14mm, 50kv, and analysis time is 35s, and energy range is 0～40kev.
Further, when preparing test liquid in s21, when weighing sample, it is accurate to 0.1mg, is placed in beaker, add certain
Amount nitric acid, beaker is placed in heating 10min～15min on electric furnace, uses filter paper filtering while hot, filtrate is filtered to volumetric flask, waits to hold
Solution in measuring bottle adds water after being cooled to room temperature and is settled to volume v, obtains test liquid.
Further, in s21 the volume mass of nitric acid and the amount of sample than for 50ml/g～60ml/g, the concentration of nitric acid is
40%～60%.
Preferably, the concentration of nitric acid is 51%.
Preferably, in s22, test liquid thickness is 15mm～30mm.
Further, the span of m is 0.4g～0.6g, and the determination of this interval is to consider through applicant
On the basis of the matrix effect of energy dispersion type x-ray fluorescence spectrophotometer, carry out what substantial amounts of test determined, changed this numerical value
The accuracy of test result will be affected.
The ultimate principle of this assay method: first, for the fireworks and firecrackers feature of firework medicament chemical composition, set up specially
The mathematical model of door, global optimization can directly affect each factor of measurement result, including: the solvent kind of dissolving test portion
Class, chemical composition and volume number, test portion dissolution conditions, test solution constant volume, the matrix effect mathematics for setting up analysis method
Correction method type, for make calibration curve test portion suppose sample size, series standard solution matrix composition, concentration range and
The interval of standard solution point value and the matrix effect phase of the actual sample weighting amount of quantity, test portion and energy dispersion type x fluorescence spectrum instrument
The work in everies such as interaction form, voltage, electric current, the selection of filter, analysis time, counting rate, gaseous environment, energy range are joined
Thickness of test solution etc. in number and specimen cup.Based on the consideration of solvent compositing characteristic, nitric acid is selected to dissolve test portion as solvent, can be by
In the elements such as ba, sr and the ca in test portion and test portion, nitric acid insoluble matter impurity element components are kept completely separate, and be not introduced into except h, n and
Other interference elements outside o element；Secondly, global optimization test portion dissolution conditions, test solution constant volume, be used for setting up analysis method
Matrix effect mathmetic correction type, make calibration curve test portion suppose sample size, series standard solution matrix composition,
The interval of concentration range and standard solution point value and the actual sample weighting amount of quantity, test portion and energy dispersion type x fluorescence spectrum instrument
Matrix effect interaction type, voltage, electric current, the selection of filter, analysis time, counting rate, gaseous environment, energy range etc.
In the work in every parameter such as thickness of test solution and specimen cup in work in every parameter and specimen cup, thickness of test solution etc. directly affects
Each factor of measurement result, by the supposition sample size of global design test portion, the sample size of actual sample, x-ray fluorescence light
Every test parameter of spectrometer, the matrix composition of series standard solution and its concentration span of control etc. for making calibration curve
Crucial Testing factors, set up the calibration curve being specifically designed for ba element determination in fireworks and firecrackers brium carbonate, in this test condition
Under, because in sample test solution, the impurity element concentration such as sr, ca, fe is extremely low, the element such as h, n and o belongs to x-ray fluorescence spectrophotometer
Insensitive light element, and the matrix effect of ba element is negligible in calibration curve standard point interval concentration range, thus
Achieve targeting and control the matrix effect between each element in test solution；Finally, can be according to the difference of fireworks and firecrackers brium carbonate sample
Property determine whether adjust sample size, carry out the quantitative analyses of ba element based on this calibration curve.
Compared with prior art, the having the beneficial effect that of the method for the invention
1st, eliminated using solwution method or substantially eliminate matrix effect, thus can directly use energy dispersion type x-ray fluorescence
Spectrographic method Accurate Determining goes out the barium content in fireworks and firecrackers brium carbonate.Using solwution method eliminate or substantially eliminate matrix effect and
Its advantage is in particular in: (1) liquor sample eliminates the intrinsic inhomogeneities of solid sample and physical-chemical effect, obtains
To analysis result more can represent whole analysis sample；(2) Macrodilution based on solvent, the composition of sample and standard specimen is close to molten
The composition of agent, and solvent is mainly made up of light element, absorption-enhancement effect becomes very little, and matrix effect substantially may not be used
Consider；It is additionally, since x-ray penetration depth deeper, fluorescent radiation absorbs less, so higher absolute sensitivity can be obtained；
(3) if solution made by the sample that standard specimen is difficult to obtain, calibration curve can estimate the factors such as background using standard reagent synthesis
Blank sample be readily made；(4) sample through nitric acid molten after constant volume to certain volume, in test liquid in addition to ba element
The matrix effect very little that the light element such as the impurity elements such as sr, ca and h, o, n produces to ba element, is negligible.
2nd, the method for the invention is simple to operate, and detection cycle is short, and after establishing calibration curve, whole measurement process is only
Including 4 easy steps such as sample weighing, dissolving, transfer constant volume, examination with computers, total time-consuming is less than 2h, and labor intensity is relatively low
And it is less demanding to operator.
3rd, detected using the method for the invention, accuracy is good, precision is high.
Brief description
The calibration curve of the mass percent concentration-fluorescence intensity of the ba that Fig. 1 obtains for inventive embodiments 1, wherein horizontal seat
It is designated as the mass percent concentration of ba in each barium nitrate working solution, unit is %；Vertical coordinate is the mass percent with above-mentioned ba
The corresponding fluorescence intensity of concentration, unit is cps/ma.
Specific embodiment
With specific embodiment, the invention will be further described below, but the invention is not limited in these embodiments.
Embodiment 1: make calibration curve
1) prepare many parts of barium working solutions (require ba in the barium nitrate working solution of gained mass concentration be 0.15g/l～
0.73g/l):
Specific compound method is with reference to as follows:
Accurately weigh 3.0g high pure nitric acid barium (being accurate to 0.1mg), be placed in 300ml beaker, add 100ml～150ml
Water, beaker is placed in heating 10min～15min on electric furnace, uses filter paper filtering while hot, and filtrate is filtered to 500ml volumetric flask, adds
10ml～30ml nitric acid, adds water after the solution in volumetric flask is cooled to room temperature and is settled to scale；Wherein, described nitric acid is
hno3Content is the nitric acid of 10%～30% mass.
Prepare 8 parts of barium nitrate working solutions: pipette respectively the barium nitrate working solution 5ml after above-mentioned constant volume, 10ml, 13ml,
15ml, 20ml, 23ml, 25ml and 30ml, in one group of 100ml volumetric flask, are diluted with water to scale, mix, numbering respectively is work
1st, work 2, work 3, work 4, work 5, work 6, work 7 and work 8, in them, the concentration of ba is shown in Table 1 respectively；
2) draw calibration curve:
2a) with energy dispersion type x-ray fluorescence spectrophotometer (power ＆ light company of the U.S. (thermo electron
Corporation) produce, model quant ' x edxry analyzer) it is detecting instrument, with 2g for calibration curve reference
Sample size, by step 1) mass concentration of ba is become the quality hundred of ba by following formula scales in many parts of barium nitrate working solutions preparing
Divide specific concentration, the results are shown in Table 1；
Wherein, ba% represents the mass percent concentration of ba in barium nitrate working solution, and unit is %；C represents barium nitrate work
Make the mass concentration of ba in liquid, unit is g/l；0.5 represents the volume supposing sample size constant volume, and unit is l；2 represent that calibration is bent
The sample size of line reference, unit is g.
Ba concentration and corresponding fluorescence intensity in table 1 barium nitrate working solution
2b) 8.8mm x-ray light pipe collimator is installed it is ensured that detector in energy dispersion type x-ray fluorescence spectrophotometer
Temperature prepares to set up assay method after being down to 190k；Intensity correction method using x fluorescence spectrum quantitative analysis sets up analysis side
Method, setting filter material is thick cu, and setting voltage is 50kv, and analysis time is 35s, and energy range is 0～40kev, counting rate
For in, gaseous environment is air, and electric current be automatic, and matrix effect is not for considering.Described energy dispersion type x-ray fluorescence spectrophotometer
Each method parameter as shown in table 2；
Table 2 energy dispersion type x-ray fluorescence spectrum instrument parameter
Ba mass percent concentration after 2c) being converted with table 1 is started sample introduction one by one for initial data and adopts spectrum, each sample introduction
Sample liquid thickness be 15mm, record the fluorescence intensity of the ba of each sample introduction, with the mass percent of ba in each barium nitrate working solution
Concentration is abscissa, with fluorescence intensity corresponding with the mass percent concentration of above-mentioned ba as vertical coordinate, makes calibration curve, such as
Shown in Fig. 1.
Embodiment 2: comparison brium carbonate reference material and barium standard solution being measured using the method for the invention
Test
Tested with listed brium carbonate reference material in table 3 and barium standard solution, wherein brium carbonate reference material and
The barium nominal content of barium standard solution is as shown in table 3；When being measured using the method for the invention, reference material presses following sides
Method carries out barium assay after preparing test liquid again.
1) prepare test liquid:
Test liquid is prepared for sample with the reference material of numbering 1, weighs 3 parts of 0.4g～0.6g sample, be accurate to when weighing
0.1mg, the 1st part of sample is placed in 300ml beaker, and the amount according to 50ml/g～60ml/g sample adds nitric acid (in this step, excellent
Choosing adopts hno3Content is the nitric acid of 51% mass), beaker is placed in heating 10min～15min on electric furnace, uses filter paper mistake while hot
Filter, filtrate is filtered to 500ml volumetric flask, is added water and be settled to scale after the solution in volumetric flask is cooled to room temperature, more fixed with water
Hold and obtain the 1st part of test liquid to 500ml；Repeat said method, obtain 3 parts of test liquids of No. 1 reference material.
2) in reference material barium mensure:
By embodiment 1 step 2b) testing conditions, 3 parts of test liquids of the brium carbonate reference material of numbering 1 are entered one by one
Sample, the sample liquid thickness of sample introduction is 15mm, and the fluorescence intensity of the ba of display on grapher, with this fluorescence intensity according to embodiment 1
The calibration curve determining reads corresponding ba mass percent concentration value；
Then as follows calculate numbering 1 reference material in barium mass percent concentration:
Wherein, ω represents the mass percent concentration of barium in sample, and unit is %；ω0Represent and read according to calibration curve
Ba mass percent concentration value, unit be %；The sample size of 2 expression calibration curve references, unit is g；M represents that sample is actual
The quality weighing, unit is g, typically weighs 0.4g～0.6g；V represents the volume of constant volume after sample dissolution, and unit is ml；500
Represent the volume supposing sample size constant volume, unit is ml.
Take wherein three result of calculation values meansigma methodss be numbering 1 reference material barium content, result as indicated at 3, and
Calculate its response rate, the results are shown in Table 3.
By above-mentioned steps 1) and step 2) method, respectively prepare numbering 2 and 3 reference material test liquid, calculate it
Barium content and the response rate, the results are shown in Table 3.
Then directly carry out above-mentioned 2nd) step as the barium standard solution in table 3, each barium titer equally do 3 parts parallel
Sample, takes the barium content as barium standard solution for the meansigma methodss of three result of calculation values, and result as indicated at 3, and calculates its response rate,
The results are shown in Table 3.
Table 3 controlled trial data
As shown in Table 3, the method for the invention is molten to the fireworks and firecrackers brium carbonate of different main contents and serial barium standard
Barium element determination in liquid has good accuracy.
Embodiment 3: using the precision test of the testing result to brium carbonate reference material for the method for the invention
Three different fireworks and firecrackers of main content are separately taken to be that sample is tested with brium carbonate reference material in the present embodiment,
Numbering is respectively 4,5 and 6.
1) prepare test liquid:
Test liquid is prepared for sample with the reference material of numbering 4, weighs 4 parts of 0.4g～0.6g sample, be accurate to when weighing
0.1mg, the 1st part of sample is placed in 300ml beaker, and the amount according to 50ml/g～60ml/g sample adds nitric acid (in this step, excellent
Choosing adopts hno3Content is the nitric acid of 51% mass), beaker is placed in heating 10min～15min on electric furnace, uses filter paper mistake while hot
Filter, filtrate is filtered to 500ml volumetric flask, is added water and be settled to scale after the solution in volumetric flask is cooled to room temperature, more fixed with water
Hold and obtain the 1st part of test liquid to 500ml；Repeat said method, obtain 4 parts of test liquids of No. 4 reference materials.
2) in reference material barium content mensure:
By embodiment 1 step 2b) testing conditions, by 4 parts of test liquid sample introductions one by one of the reference material of numbering 4, every part
Test liquid measures 11 times, and it is 15mm that each sample introduction makes sample liquid thickness, and the fluorescence intensity of display on grapher, with this fluorescence intensity
Corresponding ba mass percent concentration value is read according to the calibration curve that embodiment 1 determines；
Then calculate the mass percent concentration of barium in the reference material of numbering 1 as follows, result is as shown in table 4.
Wherein, ω represents the mass percent concentration of barium in sample, and unit is %；ω0Represent and read according to calibration curve
Ba mass percent concentration value, unit be %；The sample size of 2 expression calibration curve references, unit is g；M represents that sample is actual
The quality weighing, unit is g, typically weighs 0.4g～0.6g；V represents the volume of constant volume after sample dissolution, and unit is ml；500
Represent the volume supposing sample size constant volume, unit is ml.
By above-mentioned steps 1) and step 2) method, prepare the test liquid of the reference material of numbering 5 and 6 respectively, and calculate
Their barium content, the results are shown in Table 4.
Table 4 precision test data
As shown in Table 4, the method for the invention has to the mensure of barium content in different main content fireworks and firecrackers carbonic acid
Good precision, maximum allowable difference is 0.4%.
Embodiment 4: the mensure of barium content in the actually used brium carbonate in fireworks and firecrackers field
1st, for the fireworks and firecrackers brium carbonate of detection:
1#: sample is derived from Guangxi Pubei County fireworks station-service in the brium carbonate producing 36 combination fireworks display effect medicines.
2#: sample is derived from Guangxi Lingshan County fireworks station-service in the brium carbonate producing display shell class product.
2nd, using the method for the invention, above-mentioned fireworks and firecrackers is detected with brium carbonate sample:
Because the calibration curve being determined using embodiment 1, therefore, the step for save drafting calibration curve, is directly carried out
Prepare the step that test liquid carries out upper machine mensure, specific as follows:
2.1) prepare test liquid:
Weigh 1# fireworks and firecrackers brium carbonate sample 0.4g～3 parts of 0.6g sample respectively, when weighing, be accurate to 0.1mg, the 1st
Part sample is placed in 300ml beaker, the amount according to 50ml/g～60ml/g sample add nitric acid (in this step, it is preferred to use
hno3Content is the nitric acid of 51% mass), beaker is placed in heating 10min～15min on electric furnace, uses filter paper filtering, filter while hot
Liquid filters to 500ml volumetric flask, adds water and is settled to scale, then be settled to water after the solution in volumetric flask is cooled to room temperature
500ml obtains the 1st part of test liquid；Repeat said method, obtain 3 parts of test liquids of No. 1 sample.
2) in reference material barium content mensure:
By embodiment 1 step 2b) testing conditions, 3 parts of test liquids of 1# fireworks and firecrackers brium carbonate sample are entered one by one
Sample, the sample path length loading specimen cup is 15mm, and the fluorescence intensity of display on grapher, with this fluorescence intensity according to embodiment
The calibration curve of 1 determination reads corresponding ba mass percent concentration value；
Then the mass percent concentration of 1# fireworks and firecrackers barium in brium carbonate sample, result such as table are calculated as follows
Shown in 5.
Wherein, ω represents the mass percent concentration of barium in sample, and unit is %；ω0Represent and read according to calibration curve
Ba mass percent concentration value, unit be %；The sample size of 2 expression calibration curve references, unit is g；M represents that sample is actual
The quality weighing, unit is g, typically weighs 0.4g～0.6g；V represents the volume of constant volume after sample dissolution, and unit is ml；500
Represent the volume supposing sample size constant volume, unit is ml.
By the compound method of the test liquid of above-mentioned 1# brium carbonate sample, prepare the test liquid of 2# brium carbonate sample respectively, and
Calculate its barium content, the results are shown in Table 5.
The determination data table of barium content in brium carbonate in the actual fireworks and firecrackers of table 5
Claims (9)
1. a kind of method measuring barium content in fireworks and firecrackers brium carbonate is it is characterised in that comprise the following steps:
S1, drafting calibration curve
S11, prepare many parts of concentration barium nitrate working solution not etc., in configuration process, first use water dissolution high pure nitric acid barium, Ran Houjia
Enter a certain amount of nitric acid, then be settled to certain volume with water；
S12, with energy dispersion type x-ray fluorescence spectrophotometer as detecting instrument, the sample size that supposed for calibration curve with 2.0g, adopt
Set up analysis method with the mathmetic correction of intensity correction；The quality of ba in the many parts of barium nitrate working solutions that step s11 is prepared
Concentration conversion becomes the mass percent concentration of ba, then sample introduction one by one, records the fluorescence intensity of the ba of each sample introduction, with each work
In liquid, the mass percent concentration of ba is abscissa, with fluorescence intensity corresponding with the mass percent concentration of above-mentioned ba or calculating
The mass percent concentration of ba afterwards is vertical coordinate, makes calibration curve；Wherein, by following formula by barium nitrate working solution
The mass concentration of ba is converted into the mass percent concentration of ba:
Wherein, ba% represents the mass percent concentration of ba in barium nitrate working solution, and unit is %；C represents barium nitrate working solution
The mass concentration of middle ba, unit is g/l；0.5 represents the volume supposing sample size constant volume, and unit is l；2 represent that calibration curve is false
Fixed sample size, unit is g；
S2, the quick barium content measuring in fireworks and firecrackers brium carbonate:
S21, preparation test liquid: with fireworks and firecrackers brium carbonate as sample, weigh m gram, with a certain amount of nitric acid and water constant volume
It is configured to the test liquid that volume is v, and ensure the concentration of ba element in the solution after constant volume in calibration curve scope；
S22, by step s12 testing conditions, test liquid is loaded specimen cup it is ensured that sample liquid thickness >=15mm, records energy color
The fluorescence intensity of display in scattered type x-ray fluorescence spectrophotometer, with this fluorescence intensity according to the calibration curve of above-mentioned determination read with
Its corresponding ba mass percent concentration value；
The content of barium in s23, calculating sample:
As follows calculate sample in simple substance barium mass percent concentration:
Wherein, ω represents the mass percent concentration of simple substance ba in sample, and unit is %；ω0Represent according to calibration curve reading
Ba mass percent concentration value, unit is %；2 represent the sample size that calibration curve supposes, unit is g；M represents that sample is actual and claims
The quality of amount, unit is g；V represents the volume of constant volume after sample dissolution it is ensured that the solution concentration after constant volume is in calibration curve scope
, unit is ml；500 represent the volume supposing sample size constant volume, and unit is ml.
2. according to claim 1 a kind of measure fireworks and firecrackers brium carbonate in barium content method it is characterised in that
The mass concentration of the barium nitrate working solution ba of s11 is 0.15g/l～0.73g/l, and described nitric acid volume is 10ml～30ml, quality
Percent concentration is 10%～30%.
3. according to claim 2 a kind of measure fireworks and firecrackers brium carbonate in barium content method it is characterised in that
The testing conditions of s12 are: set up analysis method using the mathmetic correction of intensity correction, aperture is the x-ray of 8.8mm～14mm
Light pipe collimator and can filter energy be less than 37.410kev x-ray filter, setting voltage be 45kv～55kv, analyze
Time is 25s～100s, and energy range is 0～40kev, and during counting rate is, gaseous environment is air, and electric current is automatic, matrix
Effect is not consider.
4. according to claim 3 a kind of measure fireworks and firecrackers brium carbonate in barium content method it is characterised in that
In s12, the testing inspection condition of energy dispersion type x-ray fluorescence spectrophotometer is: using thick cu filter, aperture is 8.8mm～14mm
X-ray light pipe collimator, 50kv, analysis time be 35s, energy range be 0～40kev.
5. in a kind of mensure fireworks and firecrackers brium carbonate according to claim 3 or 4 barium content method, its feature exists
In, in s21 prepare test liquid when, when weighing sample, be accurate to 0.1mg, be placed in beaker, add a certain amount of nitric acid, by beaker
It is placed in heating 10min～15min on electric furnace, use filter paper filtering while hot, filtrate is filtered to volumetric flask, treats that the solution in volumetric flask is cold
But add water to room temperature and be settled to volume v, obtain test liquid.
6. according to claim 5 a kind of measure fireworks and firecrackers brium carbonate in barium content method it is characterised in that
In s21, for 50ml/g～60ml/g, the concentration of nitric acid is 40%～60% to the volume mass of nitric acid and the amount of sample ratio.
7. a kind of method measuring barium content in fireworks and firecrackers brium carbonate according to claim 6 is it is characterised in that nitre
The concentration of acid is 51%.
8. according to claim 6 a kind of measure fireworks and firecrackers brium carbonate in barium content method it is characterised in that
In s22, test liquid thickness is 15mm～30mm.
9. a kind of method measuring barium content in fireworks and firecrackers brium carbonate according to claim 8 is it is characterised in that m
Span be 0.4g～0.6g.
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