CN106404815A - Method for determination of content of strontium in strontium carbonate for fireworks and firecrackers - Google Patents
Method for determination of content of strontium in strontium carbonate for fireworks and firecrackers Download PDFInfo
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Abstract
The invention discloses a method for determination of the content of strontium (Sr) in strontium carbonate for fireworks and firecrackers, wherein the method comprises the following steps: preparing a plurality of strontium nitrate working liquids, adopting an energy dispersive X ray fluorescence spectrometer as a detection instrument, taking the mass percentage concentrations of Sr in all the strontium nitrate working liquids as abscissas, taking the fluorescence intensity corresponding to the mass percentage concentrations of Sr as ordinates, and drawing a calibration curve; then preparing a sample liquid, introducing the sample, detecting, recording the fluorescence intensity of Sr displayed in the instrument, reading out the mass percentage concentration value of Sr corresponding to the fluorescence intensity according to the determined calibration curve, and then according to a formula, calculating the mass percentage concentration of Sr in the sample. The method has the advantages of simple operation, short detection period, total consumption time of not more than 2 h, relatively low labor intensity, low requirements on operators, good accuracy and high precision.
Description
Technical field
The invention belongs to analysis and testing technology field is and in particular to content of strontium in a kind of mensure fireworks and firecrackers strontium carbonate
Method.
Technical background
In prior art, the detection method of the principal component content in fireworks and firecrackers strontium carbonate is based on traditional chemical analysis
Method, at present commonly use method standard be《Fireworks and firecrackers mensure the 10th part of chemical raw material key index：Strontium carbonate》
(SN/T 3056.10-2011).The general principle of this standard method：The mensure of barium content：Sample, after dissolving, filtering, uses one
Determine the abundant precipitation by barium ions for the potassium chromate solution of concentration, after precipitation is filtered, using the excessive Cr VI of iodometric titrationiodimetry titration
Ion, does blank assay contrast simultaneously, can determine barium content in test solution.The mensure of strontium：After sample dissolving with hydrochloric acid,
Under saturated ammonium sulfate solution effects, strontium, barium generate sulfate precipitation, and precipitation is through filtering, washing, under the conditions of pH=10, uses
EDTA solution will precipitate dissolving, the excessive EDTA of back titration, and subtractive barium amount obtains Strontium carbonate contents.
This standard methods described has the following disadvantages：(1) detection cycle is longer, and general those of skill in the art need 2 works
Make day just to complete one-time detection.In addition, being easy to not draw because of testing crew skilled operation degree in concrete process of the test
Enter to cause the uncertainty of measuring result error.(2) operating procedure is troublesome, and sample will be through dissolving, filtration, precipitation, precipitation
Enrichment, filtration, washing, precipitation dissolving, the process such as test solution pH value and titration that adjusts first draw strontium barium total amount, then sample again
Again pass by the amount that the step measurements such as dissolving, filtration, precipitation, titration go out barium, the amount that last barium strontium total amount deducts barium just draws strontium
Amount.
The method that energy dispersion type Xray fluorescence spectrometer is developed at present is used for the nondestructive analysis of sample.For solid
Body sample sxemiquantitative and quantitative elemental detection, most samples adopt nondestructive determination, powder pressing method and fusion method direct
Measure (such as：《The mensure x ray fluorescence spectrometry of bullion content》(GB/T 18043-2008) uses nondestructive determination,
《Aluminum oxide chemical analysis method and method for measuring physical properties the 30th partial x-ray fluorescence spectrum method for measuring constituent content》(GB/
T6609.30 2009) use fusion method,《EDXRF method directly measures W-Fe-Ni-Co alloy batch component》(《Nuclear power
Son is learned and Detection Techniques》05 phase in 2007) use pressed disc method,《X ray fluorescence spectrometry quickly measures in strontium nitrate product
Strontium, sodium, calcium, the content of magnesium》(analytical instrument the 6th phase in 2013) uses pressed disc method,《Regulated substance in electronic and electrical equipment
The quick screening x ray fluorescence spectrometry of lead, mercury, chromium, cadmium and bromine》(GB/Z 21277-2007) uses pressed disc method or molten
Melt method).Up to now also have no the energy dispersion type X-ray fluorescence spectra targetting control technology (solwution method) based on matrix effect
Method detects the open source literature report of content of strontium in fireworks and firecrackers strontium carbonate.
Content of the invention
It is an object of the invention to provide a kind of method measuring content of strontium in fireworks and firecrackers strontium carbonate, simple to operate,
Detection cycle is short, and the testing result degree of accuracy is good, precision is high.
For achieving the above object, the method measuring content of strontium in fireworks and firecrackers strontium carbonate of the present invention, walks including following
Suddenly：
1) draw calibration curve：
1.1) many parts of strontium working solutions are prepared, the wherein mass concentration of Sr controls in 0.18g/L～1.62g/L scope；
1.2) with energy dispersion type Xray fluorescence spectrometer as detecting instrument, with 2g for the sample size of calibration curve reference,
Intensity correction method using X fluorescence spectrum quantitative analysis sets up analysis method；By step 1.1) many parts of strontium nitrate works preparing
The mass concentration making Sr in liquid is converted into the mass percent concentration of Sr, then sample introduction one by one, record each sample introduction Sr glimmering
Luminous intensity, the mass percent concentration of the Sr with each strontium nitrate working solution as abscissa, with dense with the mass percent of above-mentioned Sr
Spending corresponding fluorescence intensity is ordinate, makes calibration curve；Wherein, by following formula by the matter of Sr in strontium nitrate working solution
Amount concentration conversion becomes the mass percent concentration of Sr：
Wherein, Sr% represents the mass percent concentration of Sr in strontium nitrate working solution, and unit is %；C represents strontium nitrate work
Make the mass concentration of Sr 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；The conversion coefficient of the mass percentage concentration of 1.4338 expression Sr；
2) the quick content of strontium measuring in fireworks and firecrackers strontium carbonate：
2.1) prepare test liquid：With fireworks and firecrackers strontium carbonate as sample, when preparing test liquid, weigh a certain amount of examination
Sample, is accurate to 0.1mg when weighing, and is placed in beaker, adds a certain amount of nitric acid, by beaker be placed on electric furnace heating 10min～
15min, uses Filter paper filtering while hot, and filtrate is filtered to volumetric flask, added water and be settled to after the solution in volumetric flask is cooled to room temperature
Certain volume；
2.2) press step 1.2) testing conditions, test liquid is loaded specimen cup it is ensured that sample liquid thickness >=15mm, recorder
The fluorescence intensity of the Sr of display on device, reads corresponding Sr mass with this fluorescence intensity according to the calibration curve of above-mentioned determination
Percent concentration value；
2.3) calculate the content of strontium in sample：
Calculate the mass percent concentration of simple substance strontium in sample as follows：
Wherein, ω represents the mass percent concentration of simple substance strontium in sample, and unit is %；ω0Represent according to calibration curve
The Sr mass percent concentration value reading, unit is %；The sample size of 2 expression calibration curve references, unit is g；M represents sample
The actual quality weighing, unit is g；V represents the volume of actual constant volume after sample dissolving, and unit is for mL it is ensured that molten after constant volume
In liquid, the concentration of Sr is in calibration curve scope；500 represent the volume supposing sample size constant volume, and unit is mL；1.4338 table
Show the conversion coefficient of the mass percentage concentration of Sr.
Further, described step 1.1) in, the method preparing strontium working solution is：Weigh a certain amount of strontium nitrate reference substance
Matter or other reference materials containing strontium element, add appropriate water to be dissolved, and are settled to after certain volume with nitric acid and water and obtain
To strontium solution, then pipette the strontium solution of different volumes respectively in the volumetric flask of multiple same specifications, obtain strontium with after water constant volume
Working solution；Wherein the mass concentration of Sr controls in 0.18g/L～1.62g/L scope.This concentration range is considering through applicant
On the basis of the matrix effect of energy dispersion type Xray fluorescence spectrometer, carry out what substantial amounts of test determined, changed this number
Value will affect the degree of accuracy of test result.
Preferably, the volume adding nitric acid is 10mL～20mL, and mass percent concentration is 10%～30%.
Further, described step 1.2) in, testing conditions are：Accurate using the X-ray light pipe for 8.8mm～14mm for the aperture
Straight device, can filter the filter that energy is less than the X-ray of 16.106KeV, and setting voltage is 25kV～35kV, and analysis time is
30s～100s, energy range is 0～40keV, and during counting rate is, gaseous environment is air, and electric current is automatic, and matrix effect is
Do not consider.
Preferably, described step 1.2) in, testing conditions are：Using the X-ray light pipe collimater of aperture 8.8mm, adopt
Fiber filter, setting voltage is 30kV, and analysis time is 35s, and energy range is 0～40keV.
Preferably, described step 2.1) in, the amount of weighing of sample is 1.2g～1.4g.This range of weighing exists through applicant
On the basis of considering the matrix effect of energy dispersion type Xray fluorescence spectrometer, carry out what substantial amounts of test determined, changed
This numerical value will affect the degree of accuracy of test result.
Preferably, described step 2.1) in, the amount that nitric acid presses 40mL～50mL/g sample adds, the mass percent of nitric acid
Concentration is 40%～60%.
Preferably, described step 2.1) in, the mass percent concentration of nitric acid is 51%.
Preferably, described step 2.2) in, sample liquid thickness is 15mm～30mm.
The substantive distinguishing features of the present invention and progress are：
The general principle of the inventive method：For the fireworks and firecrackers feature of strontium carbonate chemical composition, set up special number
Learn model, global optimization can directly affect each factor of measurement result, including：The solvent species of dissolving test portion, chemistry
Composition and volume number, test portion dissolution conditions, test solution constant volume, the matrix effect mathmetic correction class for setting up analysis method
Type, test portion supposition sample size, the matrix composition of series standard solution, concentration range and standard liquid for making calibration curve
The matrix effect interaction shape of the interval of point value and the actual sample weighting amount of quantity, test portion and energy dispersion type X fluorescence spectrum instrument
Work in every parameter and the samples such as formula, voltage, electric current, the selection of filter, analysis time, counting rate, gaseous environment, energy range
Thickness of test solution etc. in cup.First, the consideration based on solvent compositing characteristic, selects nitric acid to dissolve test portion as solvent, can will try
Sr element in material is kept completely separate with nitric acid insoluble matter impurity element components in test portion, and is not introduced into its in addition to H, N and O element
His interference element；Secondly, global optimization test portion dissolution conditions, test solution constant volume, the matrix effect for setting up analysis method
Mathmetic correction type, make calibration curve test portion suppose sample size, series standard solution matrix composition, concentration range and
The interval of standard liquid 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
In the work in every parameter such as thickness of test solution and specimen cup in number and specimen cup, thickness of test solution etc. directly affects measurement result
Each factor, sets up the calibration curve being specifically designed for Sr element determination in fireworks and firecrackers strontium carbonate, in this test condition, by
In sample test solution, the impurity element concentration such as Ba, Ca, Fe is extremely low, and it is unwise that the element such as H, N and O belongs to Xray fluorescence spectrometer
The light element of sense, and the matrix effect of Sr element is negligible in calibration curve standard point interval concentration range, thus realizing
Targeting controls the matrix effect in test solution between each element；Finally, can be true according to the otherness of fireworks and firecrackers strontium carbonate sample
Determine whether adjust sample size, carry out the quantitative analysis of Sr element based on this calibration curve.The method profit is simple to operate, detection cycle
Short, and the testing result degree of accuracy is good, precision is high.
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 XRF
Spectroscopic methodology Accurate Determining goes out the content of strontium in fireworks and firecrackers strontium 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 Sr element
The matrix effect very little that the light element such as the impurity elements such as Ba, Ca, Fe and H, O, N produces to Sr 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 labour intensity is relatively low
And it is less demanding to operating personnel.
3rd, detected using the method for the invention, the degree of accuracy is good, precision is high.
Brief description
Fig. 1 is the calibration curve of the mass percent concentration fluorescence intensity of the Sr that inventive embodiments 1 obtain, wherein horizontal seat
It is designated as the mass percent concentration of Sr in each strontium nitrate working solution, unit is %；Ordinate is the mass percent with above-mentioned Sr
The corresponding fluorescence intensity of concentration, unit is cps/mA.
Specific embodiment
Further illustrate technical scheme below by specific embodiment, but the invention is not limited in that these are real
Apply example.
Embodiment 1
Make calibration curve：
1) (mass concentration requiring Sr in the strontium working solution of gained is 0.18g/L～1.62g/ to prepare many parts of strontium working solutions
L)：
Specific compound method is with reference to as follows：
Accurately weigh 3.0g high-purity strontium nitrate (being accurate to 0.1mg), be placed in 300mL beaker, add 100mL～150mL
Water, beaker is placed in heating 10min～15min on electric furnace, is cooled to after room temperature after solution and is transferred to 500mL volumetric flask, add
10mL～20mL nitric acid, is settled to scale with water.Wherein, the mass percent concentration of nitric acid is 10%～30%.
Prepare 8 parts of strontium nitrate working solutions：Pipette respectively the strontium nitrate working solution 5mL after above-mentioned constant volume, 10mL, 15mL,
20mL, 25mL, 30mL, 40mL and 45mL, 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 Sr is shown in Table 1 respectively.
2) draw calibration curve：
2a) with energy dispersion type Xray fluorescence spectrometer (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 Sr is become the quality hundred of Sr by following formula scales in many parts of strontium nitrate working solutions preparing
Divide specific concentration, the results are shown in Table 1.
Wherein, Sr% represents the mass percent concentration of Sr in strontium nitrate working solution, and unit is %；C expression nitric acid
The mass concentration of Sr in strontium working solution, unit is g/L；0.5 represents the volume supposing sample size constant volume, and unit is L；2 expression schools
The sample size of directrix curve reference, unit is g；The conversion coefficient of the mass percentage concentration of 1.4338 expression Sr.
Table 1：
2b) in energy dispersion type Xray fluorescence spectrometer, 8.8mm X-ray light pipe standard is installed and puts device it is ensured that detector
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, and using thick Pd filter, setting voltage is 30kV, analysis time is 35s, and energy range is 0～40keV, during counting rate is,
Gaseous environment is air, and electric current is automatic, and matrix effect is not consider.The each method of energy dispersion type Xray fluorescence spectrometer
Parameter is as shown in table 2.
Table 2：
Sr 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 each sample introduction, with the mass percent concentration of Sr in each strontium nitrate working solution
For abscissa, with fluorescence intensity corresponding with the mass percent concentration of above-mentioned Sr as ordinate, make calibration curve, such as Fig. 1
Shown.
Embodiment 2
Check experiment strontium carbonate reference material or standard liquid being measured using the method for the invention：
Tested with listed strontium carbonate reference material in table 3 and strontium standard liquid, wherein strontium carbonate reference material and
The strontium nominal content of strontium standard liquid is as shown in table 3；When being measured using the method for the invention, reference material presses following sides
Method carries out content of strontium mensure 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 1.2g～1.4g sample, be accurate to when weighing
0.1mg, the 1st part of sample is placed in 300mL beaker, adds nitric acid, the quality hundred of nitric acid by the amount of 40mL/g～50mL/g sample
Divide specific concentration to be 51%, beaker is placed in heating 10min～15min on electric furnace, use Filter paper filtering while hot, filtrate is filtered to capacity
Bottle, adds water after the solution in volumetric flask is cooled to room temperature and is settled to certain volume, obtain the 1st part of test liquid.Repeat above-mentioned side
Method, obtains 3 parts of test liquids of No. 1 reference material；
2) in reference material strontium mensure：
By embodiment 1 step 2b) testing conditions, by 3 parts of test liquid sample introductions one by one of the reference material of numbering 1, sample introduction
Sample liquid thickness be 15mm, the fluorescence intensity of display on register instrument, the calibration song being determined according to embodiment 1 with this fluorescence intensity
Line reads corresponding Sr mass percent concentration value；
Then calculate the mass percent concentration of strontium in the reference material of numbering 1 as follows：
Wherein, ω represents the mass percent concentration of strontium in sample, and unit is %；ω0Represent and read according to calibration curve
Sr 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；V represents the volume of actual constant volume after sample dissolving, and unit is for mL it is ensured that in solution after constant volume
The concentration of Sr is in calibration curve scope；500 represent the volume supposing sample size constant volume, and unit is mL；1.4338 representing Sr
Mass percentage concentration conversion coefficient.
Take wherein three result of calculation values mean value be numbering 1 strontium carbonate reference material content of strontium, and calculate it
The rate of recovery, the results are shown in Table 3.
By above-mentioned steps 1) and step 2) method, respectively prepare numbering 2 and 3 strontium carbonate reference material test liquid,
Calculate their content of strontium and the rate of recovery, the results are shown in Table 3.
Then directly carry out above-mentioned 2nd) step as the strontium standard liquid in table 3, each strontium titer equally do 3 parts parallel
Sample, takes the content of strontium as strontium standard liquid for the mean value of three result of calculation values, and result as indicated at 3, and calculates its rate of recovery,
The results are shown in Table 3.
Table 3：
As shown in Table 3, the method for the invention is in different main content strontium carbonate reference materials and series Sr standard liquid
The strontium element of different content measures has the good degree of accuracy.
Embodiment 3
Precision test using the testing result to strontium 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 strontium 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 1.2g～1.4g sample, be accurate to when weighing
0.1mg, the 1st part of sample is placed in 300mL beaker, adds nitric acid, the quality hundred of nitric acid by the amount of 40mL/g～50mL/g sample
Divide specific concentration to be 51%, be placed on heating 10min on electric furnace, be filtered hot to volumetric flask with filter paper, repeatedly rinse repeatedly with water,
It is cooled to after room temperature after filtrate, then is settled to certain volume with water, obtain the 1st part of test liquid.Repeat said method, obtain No. 4
4 parts of test liquids of reference material.
2) in reference material content of strontium 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 register instrument, with this fluorescence intensity
Corresponding Sr mass percent concentration value is read according to the calibration curve that embodiment 1 determines；
Then calculate the mass percent concentration of strontium in the reference material of numbering 1 as follows, result is as shown in table 4.
Wherein, ω represents the mass percent concentration of strontium in sample, and unit is %；ω0Represent and read according to calibration curve
Sr 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；V represents the volume of actual constant volume after sample dissolving, and unit is for mL it is ensured that in solution after constant volume
The concentration of Sr is in calibration curve scope；500 represent the volume supposing sample size constant volume, and unit is mL；1.4338 representing Sr
Mass percentage concentration conversion coefficient.
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 content of strontium, the results are shown in Table 4.
Table 4：
As shown in Table 4, the mensure to content of strontium in the fireworks and firecrackers strontium carbonate of different main contents for the method for the invention
There is good precision, maximum allowable difference is 0.4%.
Embodiment 4
The mensure of content of strontium in the actually used strontium carbonate in fireworks and firecrackers field：
1st, it is used for the fireworks and firecrackers strontium carbonate of detection：
1#：Sample is derived from Guangxi Pubei County fireworks station-service in the strontium carbonate producing 36 combination fireworks display effect medicines.
2#：Sample is derived from Guangxi Lingshan County fireworks station-service in the strontium carbonate producing display shell class product.
2nd, using the method for the invention, above-mentioned fireworks and firecrackers is detected with strontium 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 strontium carbonate sample 1.2g～3 parts of 1.4g sample respectively, when weighing, be accurate to 0.1mg, the 1st
Part sample is placed in 300mL beaker, adds nitric acid by the amount of 40mL/g～50mL/g sample, the mass percent concentration of nitric acid is
51%, it is placed on heating 10min on electric furnace, is filtered hot to volumetric flask with filter paper, is repeatedly rinsed repeatedly with water, treat that filtrate cools down
To room temperature, then it is settled to certain volume with water, obtain the 1st part of test liquid.Repeat said method, obtain 3 parts of examinations of No. 1 sample
Sample liquid.
2) in reference material content of strontium mensure：
By embodiment 1 step 2b) testing conditions, 3 parts of test liquids of 1# fireworks and firecrackers strontium carbonate sample are entered one by one
Sample, the sample path length loading specimen cup is 15mm, and the fluorescence intensity of display on register instrument, with this fluorescence intensity according to embodiment
The calibration curve of 1 determination reads corresponding Sr mass percent concentration value；
Then the mass percent concentration of 1# fireworks and firecrackers strontium in strontium carbonate sample, result such as table are calculated as follows
Shown in 5.
Wherein, ω represents the mass percent concentration of strontium in sample, and unit is %；ω0Represent and read according to calibration curve
Sr 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；V represents the volume of actual constant volume after sample dissolving, and unit is for mL it is ensured that in solution after constant volume
The concentration of Sr is in calibration curve scope；500 represent the volume supposing sample size constant volume, and unit is mL；1.4338 representing Sr
Mass percentage concentration conversion coefficient.
By above-mentioned steps 1) and step 2) method, prepare the test liquid of 2# strontium carbonate sample respectively, and calculate its strontium and contain
Amount, the results are shown in Table 5.
Table 5：
As shown in Table 5, accurately, deviation is little for the method for the invention measurement.
Claims (8)
1. a kind of method measuring content of strontium in fireworks and firecrackers strontium carbonate is it is characterised in that comprise the following steps：
1) draw calibration curve：
1.1) many parts of strontium working solutions are prepared, the wherein mass concentration of Sr controls in 0.18g/L～1.62g/L scope；
1.2) with energy dispersion type Xray fluorescence spectrometer as detecting instrument, with 2g for the sample size of calibration curve reference, adopt
The intensity correction method of X fluorescence spectrum quantitative analysis sets up analysis method；By step 1.1) many parts of strontium nitrate working solutions preparing
The mass concentration of middle Sr is converted into the mass percent concentration of Sr, then sample introduction one by one, and the fluorescence recording the Sr of each sample introduction is strong
Degree, the mass percent concentration of the Sr with each strontium nitrate working solution as abscissa, with the mass percent concentration pair with above-mentioned Sr
The fluorescence intensity answered is ordinate, makes calibration curve；Wherein, will be dense for the quality of Sr in strontium nitrate working solution by following formula
Degree is converted into the mass percent concentration of Sr：
Wherein, Sr% represents the mass percent concentration of Sr in strontium nitrate working solution, and unit is %；C represents strontium nitrate working solution
The mass concentration of middle Sr, unit is g/L；0.5 represents the volume supposing sample size constant volume, and unit is L；2 represent calibration curve ginseng
The sample size examined, unit is g；The conversion coefficient of the mass percentage concentration of 1.4338 expression Sr；
2) the quick content of strontium measuring in fireworks and firecrackers strontium carbonate：
2.1) prepare test liquid：With fireworks and firecrackers strontium carbonate as sample, when preparing test liquid, weigh a certain amount of sample, claim
It is accurate to 0.1mg when taking, is placed in beaker, add a certain amount of nitric acid, beaker is placed in heating 10min～15min on electric furnace, takes advantage of
Heat Filter paper filtering, filtrate is filtered to volumetric flask, adds water and be settled to certain volume after the solution in volumetric flask is cooled to room temperature；
2.2) press step 1.2) testing conditions, test liquid is loaded specimen cup it is ensured that sample liquid thickness >=15mm, on register instrument
The fluorescence intensity of the Sr of display, reads corresponding Sr percent mass with this fluorescence intensity according to the calibration curve of above-mentioned determination
Specific concentration value；
2.3) calculate the content of strontium in sample：
Calculate the mass percent concentration of simple substance strontium in sample as follows：
Wherein, ω represents the mass percent concentration of simple substance strontium in sample, and unit is %；ω0Represent according to calibration curve reading
Sr mass percent concentration value, unit is %；The sample size of 2 expression calibration curve references, unit is g；M represents that sample is actual and claims
The quality of amount, unit is g；V represents the volume of actual constant volume after sample dissolving, and unit is for mL it is ensured that Sr in solution after constant volume
Concentration in calibration curve scope；500 represent the volume supposing sample size constant volume, and unit is mL；1.4338 representing Sr's
The conversion coefficient of mass percentage concentration.
2. the method measuring content of strontium in fireworks and firecrackers strontium carbonate according to claim 1 is it is characterised in that described step
In rapid 1.1), the method preparing strontium working solution is：Weigh a certain amount of strontium nitrate reference material or other references containing strontium element
Material, adds appropriate water to be dissolved, is settled to after certain volume with nitric acid and water and obtains strontium solution, then pipette difference respectively
The strontium solution of volume, in the volumetric flask of multiple same specifications, obtains strontium working solution with after water constant volume；The wherein mass concentration of Sr
Control in 0.18g/L～1.62g/L scope；Add nitric acid volume be 10mL～20mL, mass percent concentration be 10%～
30%.
3. the method measuring content of strontium in fireworks and firecrackers strontium carbonate according to claim 1 is it is characterised in that described step
In rapid 1.2), testing conditions are：Using the X-ray light pipe collimater for 8.8mm～14mm for the aperture, energy can be filtered and be less than
The filter of the X-ray of 16.106KeV, setting voltage be 25kV～35kV, analysis time be 30s～100s, energy range be 0～
40keV, during counting rate is, gaseous environment is air, and electric current is automatic, and matrix effect is not consider.
4. the method measuring content of strontium in fireworks and firecrackers strontium carbonate according to claim 3 is it is characterised in that described step
In rapid 1.2), testing conditions are：Using the X-ray light pipe collimater of aperture 8.8mm, using fiber filter, arranging voltage is
30kV, analysis time is 35s, and energy range is 0～40keV.
5. according to claim 1 measure fireworks and firecrackers strontium carbonate in content of strontium method it is characterised in that：Described step
In rapid 2.1), the amount of weighing of sample is 1.2g～1.4g.
6. according to claim 1 measure fireworks and firecrackers strontium carbonate in content of strontium method it is characterised in that：Described step
In rapid 2.1), the amount that nitric acid presses 40mL～50mL/g sample adds, and the mass percent concentration of nitric acid is 40%～60%.
7. according to claim 6 measure fireworks and firecrackers strontium carbonate in content of strontium method it is characterised in that：Described step
In rapid 2.1), the mass percent concentration of nitric acid is 51%.
8. according to claim 1 measure fireworks and firecrackers strontium carbonate in content of strontium method it is characterised in that：Described step
In rapid 2.2), sample liquid thickness is 15mm～30mm.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110715947A (en) * | 2019-12-12 | 2020-01-21 | 湖南航天磁电有限责任公司 | Method for measuring barium calcium in industrial strontium carbonate by adopting gel X-ray fluorescence spectrometry |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH10123071A (en) * | 1996-08-27 | 1998-05-15 | Rigaku Ind Co | Method and equipment for x ray analysis |
| CN101799437A (en) * | 2009-02-06 | 2010-08-11 | 中国石油天然气股份有限公司 | Method for measuring content of phosphorus and iron in catalyst by using X-ray fluorescence method |
| CN103364426A (en) * | 2013-07-30 | 2013-10-23 | 广西出入境检验检疫局烟花爆竹检测中心 | Method for determining content of zinc in zinc concentrate through energy-dispersive X-ray fluorescence spectrometry |
| CN105021641A (en) * | 2015-07-10 | 2015-11-04 | 广西鱼峰水泥股份有限公司 | Method for rapidly measuring content of SO2 in cement clinker |
| WO2016002357A1 (en) * | 2014-07-01 | 2016-01-07 | 株式会社リガク | X-ray fluorescence analysis device and method |
| CN105241907A (en) * | 2015-11-10 | 2016-01-13 | 湖南华菱湘潭钢铁有限公司 | Method for analyzing pig iron components through X-ray fluorescence spectrometry |
-
2016
- 2016-08-31 CN CN201610776218.5A patent/CN106404815A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH10123071A (en) * | 1996-08-27 | 1998-05-15 | Rigaku Ind Co | Method and equipment for x ray analysis |
| CN101799437A (en) * | 2009-02-06 | 2010-08-11 | 中国石油天然气股份有限公司 | Method for measuring content of phosphorus and iron in catalyst by using X-ray fluorescence method |
| CN103364426A (en) * | 2013-07-30 | 2013-10-23 | 广西出入境检验检疫局烟花爆竹检测中心 | Method for determining content of zinc in zinc concentrate through energy-dispersive X-ray fluorescence spectrometry |
| WO2016002357A1 (en) * | 2014-07-01 | 2016-01-07 | 株式会社リガク | X-ray fluorescence analysis device and method |
| CN105021641A (en) * | 2015-07-10 | 2015-11-04 | 广西鱼峰水泥股份有限公司 | Method for rapidly measuring content of SO2 in cement clinker |
| CN105241907A (en) * | 2015-11-10 | 2016-01-13 | 湖南华菱湘潭钢铁有限公司 | Method for analyzing pig iron components through X-ray fluorescence spectrometry |
Non-Patent Citations (2)
| Title |
|---|
| S. P. LUNDBLAD ET AL.: "《Analysing Archaeological Basalt Using Non-Destructive Energu-Dispersive X-Ray Fluorescence（EDXRF）：Effects of Post-Depositional Chemical Weathering and Sample Size on Analytical Precision》", 《ARCHAEOMETRY》 * |
| 吕玉光: "《仪器分析》", 31 January 2016 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110715947A (en) * | 2019-12-12 | 2020-01-21 | 湖南航天磁电有限责任公司 | Method for measuring barium calcium in industrial strontium carbonate by adopting gel X-ray fluorescence spectrometry |
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