CN106124547A - A kind of measure the method for potassium content in industrial potassium nitrate - Google Patents
A kind of measure the method for potassium content in industrial potassium nitrate Download PDFInfo
- Publication number
- CN106124547A CN106124547A CN201610776265.XA CN201610776265A CN106124547A CN 106124547 A CN106124547 A CN 106124547A CN 201610776265 A CN201610776265 A CN 201610776265A CN 106124547 A CN106124547 A CN 106124547A
- Authority
- CN
- China
- Prior art keywords
- potassium
- sample
- mass percent
- percent concentration
- calibration curve
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
- G01N23/223—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material by irradiating the sample with X-rays or gamma-rays and by measuring X-ray fluorescence
Abstract
The invention discloses and a kind of measure the method for potassium content in industrial potassium nitrate, comprise the following steps: 1) draw calibration curve: prepare many parts of potassium chloride working solutions, the mass concentration of K in potassium chloride working solution is converted into the mass percent concentration of K, with energy dispersion type Xray fluorescence spectrometer as detecting instrument, the mass percent concentration of K in each potassium chloride working solution is as abscissa, with the fluorescence intensity corresponding with the mass percent concentration of above-mentioned K as vertical coordinate, make calibration curve；2) potassium content in industrial potassium nitrate is measured: preparation test liquid, by step 1.2) testing conditions, the fluorescence intensity of the K element of display on grapher, read corresponding K mass percent concentration value with this fluorescence intensity according to the above-mentioned calibration curve determined, calculate the mass percent concentration of potassium in sample further according to formula.The assay method profit of the present invention is simple to operate, the detection cycle is short, and testing result accuracy is good, and precision is high.
Description
Technical field
The invention belongs to analysis and testing technology field, be specifically related to a kind of measure the method for potassium content in industrial potassium nitrate.
Technical background
In prior art, the detection method of the main constituent potassium nitrate content in industrial potassium nitrate is based on traditional chemical analysis
Method, at present conventional method standard be " mensuration of fireworks and firecrackers potassium nitrate key index " (GB/T 22783-2008) and
" industrial potassium nitrate " (GB 1918-2011).The Method And Principle of these two standards is: in neutral medium, potassium ion and four benzene
Boron sodium reacts, and generates potassium tetraphenylborate precipitation.Exist if any ammonium ion, formalin can be added and eliminate the interference of ammonium ion.According to
The quality of the potassium tetraphenylborate generated, determines potassium nitrate content.
Method described in this standard has the disadvantage that (1) detection cycle is longer, and general those of skill in the art need 2 works
Make day just to complete one-time detection.It addition, be easy in concrete process of the test because testing crew skilled operation degree draws not
Enter to cause the uncertainty of measuring result error.(2) operating procedure is relatively complicated, and sample to experience dissolving successively, filter, uses first
(potassium nitrate made of ammonium salt in this way also needs with phenolphthalein as indicator solution and NaOH for base orange indicator solution and ethanol solution regulation pH value
Solution regulation pH value), the precipitation dropping of sodium tetraphenylborate ethanol solution (add have time requirement), precipitation enrichment, precipitation transfer, dry
The complex steps such as dry, weighing, content (3) method finally obtaining potassium ion requires height to operator, relates to repeatedly regulating examination
The multinomial steps being readily incorporated artificial uncertainty such as liquid pH value, precipitation enrichment, precipitation transfer, drying constant weight.
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 use nondestructive determination, powder pressing method and fusion method direct
Measure (such as: " the mensuration X-ray fluorescence spectroscopy of bullion content " (GB/T 18043-2008) uses nondestructive determination,
" aluminium 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 spectroscopy quickly measures in Potassium Chloride Product
Potassium, sodium, calcium, the content of magnesium " (analytical tool the 6th phase in 2013) use pressed disc method, " regulated substance in electronic and electrical equipment
The rapid screening X-ray fluorescence spectroscopy of lead, hydrargyrum, chromium, cadmium and bromine " (GB/Z 21277-2007) use pressed disc method or molten
Melt method).The most also energy dispersion type X-ray fluorescence spectra based on collective effect targeting control technology (solwution method) is had no
The open source literature report of potassium content in method detection industrial potassium nitrate.
Summary of the invention
It is an object of the invention to provide and a kind of measure the method for potassium content in industrial potassium nitrate, simple to operate, detection week
Phase is short, and testing result accuracy is good, and precision is high.
For achieving the above object, the present invention measures the method for potassium content in industrial potassium nitrate, comprises the following steps:
1) calibration curve is drawn:
1.1) preparing many parts of potassium chloride working solutions, wherein the mass concentration of K is 0.16g/L～0.99g/L, and the quality of Cl is dense
Degree is 0.18g/L～1.10g/L；
1.2) with energy dispersion type Xray fluorescence spectrometer as detecting instrument, the sample being calibration curve reference with 1.5g
Amount, uses the intensity correction method of X fluorescence spectrum quantitative analysis to set up analysis method；By step 1.1) many parts of potassium chloride preparing
In working solution, the mass concentration of K is converted into the mass percent concentration of K, the most one by one sample introduction, records the fluorescence of the K of each sample introduction
Intensity, the mass percent concentration of K in each potassium chloride working solution is as abscissa, with the mass percent concentration pair with above-mentioned K
The fluorescence intensity answered is vertical coordinate, makes calibration curve；Wherein, by following formula by dense for the quality of K in potassium chloride working solution
Degree is converted into the mass percent concentration of K:
Wherein, K% represents the mass percent concentration of K in potassium chloride working solution, and unit is %；C represents that potassium chloride works
The mass concentration of K in liquid, unit is g/L；0.5 represents the volume supposing sample size constant volume, and unit is L；1.5 represent calibration curve
The sample size of reference, unit is g；
2) potassium content in industrial potassium nitrate is quickly measured:
2.1) preparation test liquid: with industrial potassium nitrate as sample, during preparation test liquid, weighs a certain amount of sample, weighs
Time be accurate to 0.1mg, be placed in beaker, add 100mL～150mL water, beaker is placed on electric furnace heating 10min～15min,
While hot with filter paper filtering, filtrate is filtered to volumetric flask, adds a certain amount of nitric acid, adds after the solution in volumetric flask is cooled to room temperature
Water is settled to certain volume；
2.2) by step 1.2) testing conditions, test liquid is loaded specimen cup, it is ensured that sample liquid thickness >=15mm, monitor
The fluorescence intensity of display on device, reads corresponding K percent mass with this fluorescence intensity according to the above-mentioned calibration curve determined
Specific concentration value；
2.3) content of potassium in calculating sample:
The mass percent concentration of potassium in calculating sample as follows:
Wherein, ω represents the mass percent concentration of potassium in sample, and unit is %；ω0Represent and read according to calibration curve
K mass percent concentration value, unit is %；1.5 sample sizes representing calibration curve reference, unit is g；M represents that sample is real
The quality that border weighs, unit is g；V is the volume of actual constant volume after representing sample dissolution, and unit is mL, it is ensured that the solution after constant volume
The concentration of middle K is in calibration curve scope；500 represent the volume supposing sample size constant volume, and unit is mL.
Further, described step 1.1) in, the method for preparation potassium chloride working solution is: weigh a certain amount of potassium chloride ginseng
Examine the reference material of material or other potassium elements, add appropriate water and nitric acid dissolves, obtain after being settled to certain volume
Klorvess Liquid, then pipette the Klorvess Liquid of different volumes respectively in the volumetric flask of multiple same specifications, obtain after constant volume
Potassium chloride working solution, wherein the mass concentration of K is 0.16g/L～0.99g/L, and the mass concentration of Cl is 0.18g/L～1.10g/
L.This concentration range, is entered through applicant on the basis of the matrix effect considering energy dispersion type Xray fluorescence spectrometer
Having gone what substantial amounts of test determined, changing this numerical value will affect the accuracy of test result.
Preferably, described step 1.1) in, the volume adding nitric acid is 10mL～20mL, and mass percent concentration is 10%
～30%.
Further, described step 1.2) in, testing conditions is: the X-ray light pipe using aperture to be 8.8mm～14mm is accurate
Straight device, it is possible to filtering the filter of the energy X-ray less than 3.607KeV, arranging voltage is 8kV～16kV, and analysis time is 30s
～80s, energy range is 0～40keV, and during counting rate is, gaseous environment is air, and electric current is that matrix effect is not for examine automatically
Consider.
Preferably, described step 1.2) in, testing conditions is: use the X-ray light pipe collimator of aperture 8.8mm, uses
Fiber filter, arranging voltage is 12kV, and analysis time is 35s, and energy range is 0～20keV.
Preferably, described step 2.1) in, the amount of weighing of sample is 0.6g～0.8g.This range of weighing is through applicant
On the basis of the matrix effect considering energy dispersion type Xray fluorescence spectrometer, carry out what substantial amounts of test determined, changed
This numerical value dynamic will affect the accuracy of test result.
Preferably, described step 2.1) in, the volume adding nitric acid is 10mL～20mL, and mass percent concentration is 10%
～30%.
Preferably, described step 2.1) in, the mass percent concentration of nitric acid is 20%.
Preferably, described step 2.2) in, sample liquid thickness is 15mm～30mm.
The substantive distinguishing features of the present invention and progress be:
The ultimate principle of the inventive method: for the feature of industrial potassium nitrate chemical composition, set up special mathematical model,
Global optimization can directly affect each factor of measurement result, including: dissolve the solvent species of test portion, chemical composition and body
Product, test portion dissolution conditions, test solution constant volume, for setting up the matrix effect mathmetic correction type of analysis method, be used for
Make matrix composition, concentration range and the standard solution point value of the test portion supposition sample size of calibration curve, series standard solution
Interval and quantity, the actual sample weighting amount of test portion and the matrix effect interaction type of energy dispersion type X fluorescence spectrum instrument, electricity
In the work in every parameters such as pressure, electric current, the selection of filter, analysis time, counting rate, gaseous environment, energy range and specimen cup
The thickness etc. of test solution.First, consideration based on solvent compositing characteristic, select water to dissolve test portion as solvent, can be by the K in test portion
Element is kept completely separate with water-insoluble impurity element components in test portion, and other interference elements being not introduced in addition to H and O element；
Secondly, global optimization test portion dissolution conditions, test solution constant volume, for setting up the matrix effect mathmetic correction class of analysis method
Type, the test portion of making calibration curve suppose matrix composition, concentration range and the standard solution point value of sample size, series standard solution
Interval and quantity, the actual sample weighting amount of test portion and the matrix effect interaction type of energy dispersion type X fluorescence spectrum instrument, electricity
In the work in every parameters such as pressure, electric current, the selection of filter, analysis time, counting rate, gaseous environment, energy range and specimen cup
In the work in every parameters such as the thickness of test solution and specimen cup, the thickness etc. of test solution directly affects each factor of measurement result, sets up
It is specifically designed for the calibration trace that in industrial potassium nitrate, K element measures, in this test condition, due to Cl, Fe and S in sample test solution
Extremely low etc. impurity element concentration, the element such as H, O and N belongs to the light element that Xray fluorescence spectrometer is insensitive, and K element
Matrix effect is negligible in calibration trace standard point interval concentration range, it is achieved thereby that targeting controls each element in test solution
Between matrix effect；Finally, can determine whether to adjust sample size according to the diversity of industrial potassium nitrate sample, bent based on this correction
Line carries out the quantitative analysis of K element.The method profit is simple to operate, the detection cycle is short, and testing result accuracy is good, precision
High.
Compared with prior art, the having the beneficial effect that of the method for the invention
1, utilize solwution method eliminate or substantially eliminate matrix effect, thus can directly use energy dispersion type XRF
Spectrographic method Accurate Determining goes out the potassium content in industrial potassium nitrate；Solwution method is used to eliminate or substantially eliminate matrix effect and advantage thereof
Being in particular in: (1) liquor sample eliminates the intrinsic inhomogeneities of solid sample and physical-chemical effect, obtain divides
Analysis result more can represent whole analysis sample；(2) composition of Macrodilution based on solvent, sample and standard specimen is close to the group of solvent
Becoming, and solvent is mainly made up of light element, absorption-enhancement effect becomes the least, and matrix effect substantially can not consider；And
And, owing to X-ray penetration depth is relatively deep, fluorescent radiation absorbs less, so higher absolute sensitivity can be obtained；(3) standard specimen
If solution made by the sample being difficult to obtain, calibration curve can use standard reagent to synthesize, and estimates the blank of the factors such as background
Sample is readily made；(4) constant volume is to certain volume after water-soluble for sample, and in test liquid, H, O, N in addition to K and Cl element are first
The matrix effect that K element is produced by element is the least, is negligible.
2, the method for the invention is simple to operate, and the detection cycle is short, and after establishing calibration curve, whole mensuration process is only
Including sample weighing, dissolving, shift 4 easy steps such as constant volume, examination with computer, total time-consuming less than 2h, labor intensity is relatively low
And it is less demanding to operator.
3, using the method for the invention to detect, accuracy is good, and precision is high.
Accompanying drawing explanation
Fig. 1 is the calibration curve of the mass percent concentration fluorescence intensity of the K that inventive embodiments 1 obtains, the most horizontal seat
Being designated as the mass percent concentration of K in each potassium chloride working solution, unit is %；Vertical coordinate is dense with the mass percent of above-mentioned K
The fluorescence intensity that degree is corresponding, unit is cps/mA.
Detailed description of the invention
Further illustrate technical scheme below by specific embodiment, but the invention is not limited in that these are real
Execute example.
Embodiment 1
Making calibration curve:
1) prepare many parts of potassium chloride working solutions (require in the potassium chloride working solution of gained the mass concentration of K be 0.16g/L～
The mass concentration of 0.99g/L, Cl is 0.18g/L～1.10g/L):
Concrete compound method is with reference to as follows:
Accurately weigh 3.5g potassium chloride reference material (being accurate to 0.1mg), be placed in 300mL beaker, add 100mL～
150mL water, is placed in beaker on electric furnace heating 10min～15min, is transferred to 500mL volumetric flask after solution is cooled to room temperature,
Add 10mL nitric acid, be settled to scale with water.Wherein, the mass percent concentration of nitric acid is 10%～30%.
Prepare 6 parts of potassium chloride working solutions: pipette respectively the potassium chloride working solution 5mL after above-mentioned constant volume, 10mL, 15mL,
20mL, 25mL and 30mL, in one group of 100mL volumetric flask, are diluted with water to scale, mixing, respectively numbered work 1, work 2, work 3,
Work 4, work 5 and work 6, in them, the concentration of K and Cl is shown in Table 1 respectively.
2) calibration curve is drawn:
2a) with energy dispersion type Xray fluorescence spectrometer (power & light company of the U.S. (Thermo Electron
Corporation) producing, model is QUANT ' X EDXRY Analyzer) it is detecting instrument, with 1.5g for calibration curve reference
Sample size, by step 1) mass concentration of K is become the quality hundred of K by following formula scales in many parts of potassium chloride working solutions preparing
Proportion by subtraction concentration, the results are shown in Table 1；
Wherein, K% represents the mass percent concentration of K in potassium chloride working solution, and unit is %；C represents that potassium chloride works
The mass concentration of K in liquid, unit is g/L；0.5 represents the volume supposing sample size constant volume, and unit is L；1.5 represent calibration curve
The sample size of reference, unit is g.
Table 1:
2b) at 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；The intensity correction method using X fluorescence spectrum quantitative analysis sets up analysis side
Method, and use fiber filter, arranging voltage is 12kV, and analysis time is 35s, and energy range is 0～20keV, during counting rate is,
Gaseous environment is air, and electric current is that matrix effect is not for consider automatically.The each method of energy dispersion type Xray fluorescence spectrometer
Parameter is as shown in table 2.
Table 2:
2c) start sample introduction one by one with the K mass percent concentration after conversion in table 1 for initial data and adopt spectrum, each sample introduction
Sample liquid thickness be 15mm, record the fluorescence intensity of each sample introduction, with the mass percent concentration of K in each potassium chloride working solution be
Abscissa, with the fluorescence intensity corresponding with the mass percent concentration of above-mentioned K as vertical coordinate, makes calibration curve, such as Fig. 1 institute
Show.
Embodiment 2
The controlled trial that potassium nitrate reference material or standard solution are measured by employing the method for the invention:
Test with reference material listed in table 3 and potassium standard solution, wherein reference material and potassium standard solution
Potassium nominal content is as shown in table 3.When using the method for the invention to measure, reference material prepares test liquid as follows
After carry out potassium content mensuration again.
1) preparation test liquid:
Prepare test liquid with the reference material of numbering 1 for sample, weigh 3 parts of 0.6g～0.8g sample, be accurate to when weighing
0.1mg, the 1st part of sample is placed in 300mL beaker, adds 100mL water, is placed on electric furnace heating 10min, by filter paper mistake while hot
Filter, to volumetric flask, is rinsed repeatedly repeatedly with water, after filtrate is cooled to room temperature, adds 10mL nitric acid, the mass percent of nitric acid
Concentration is 20%, then is settled to certain volume with water, obtains the 1st part of test liquid.Repeat said method, obtain No. 1 reference material
3 parts of test liquids.
2) mensuration of potassium in reference material:
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 grapher, the calibration determined according to embodiment 1 with this fluorescence intensity is bent
Line reads corresponding K mass percent concentration value；
The mass percent concentration of potassium in the reference material of calculating numbering 1 the most as follows:
Wherein, ω represents the mass percent concentration of potassium in sample, and unit is %；ω0Represent and read according to calibration curve
K mass percent concentration value, unit is %；1.5 sample sizes representing calibration curve reference, unit is g；M represents that sample is real
The quality that border weighs, unit is g；V is the volume of actual constant volume after representing sample dissolution, and unit is mL, it is ensured that the solution after constant volume
The concentration of middle K is in calibration curve scope；500 represent the volume supposing sample size constant volume, and unit is mL.
Take the potassium content of the reference material that meansigma methods is numbering 1 of wherein three result of calculation values, and calculate its response rate,
The results are shown in Table 3.
By above-mentioned steps 1) and step 2) method, the test liquid of reference material of preparation numbering 2 and 3, calculates it respectively
Potassium content and the response rate, the results are shown in Table 3.
The most directly carry out the above-mentioned 2nd as the potassium standard solution in table 3) step, each potassium titer do equally 3 parts parallel
Sample, takes the meansigma methods potassium content as potassium standard solution of three result of calculation values, and calculates its response rate, the results are shown in Table 3.
Table 3:
As shown in Table 3, the method for the invention is molten to different main content industrial potassium nitrate reference materials and series potassium standard
In liquid, the potassium element of different content measures and has good accuracy.
Embodiment 3
The employing the method for the invention precision test to the testing result of potassium nitrate reference material:
Separately taking three different industrial potassium nitrate reference materials in the present embodiment is that sample is tested, numbering respectively 4,
5 and 6.
1) preparation test liquid:
Prepare test liquid with the reference material of numbering 4 for sample, weigh 4 parts of 0.6g～0.8g sample, be accurate to when weighing
0.1mg, the 1st part of sample is placed in 300mL beaker, adds 100mL water, is placed on electric furnace heating 10min, by filter paper mistake while hot
Filter, to volumetric flask, is rinsed repeatedly repeatedly with water, after filtrate is cooled to room temperature, adds 10mL nitric acid, the mass percent of nitric acid
Concentration is 20%, then is settled to certain volume with water, obtains the 1st part of test liquid.Repeat said method, obtain No. 4 reference materials
4 parts of test liquids.
2) mensuration of potassium content in reference material:
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 each sample introduction makes sample liquid thickness be 15mm, and the fluorescence intensity of display on grapher, with this fluorescence intensity
Corresponding K mass percent concentration value is read according to the calibration curve that embodiment 1 determines.
Calculating the mass percent concentration of potassium in the reference material of numbering 4 the most as follows, result is as shown in table 4.
Wherein, ω represents the mass percent concentration of potassium in sample, and unit is %；ω0Represent and read according to calibration curve
K mass percent concentration value, unit is %；1.5 sample sizes representing calibration curve reference, unit is g；M represents that sample is real
The quality that border weighs, unit is g；V is the volume of actual constant volume after representing sample dissolution, and unit is mL, it is ensured that the solution after constant volume
The concentration of middle K is in calibration curve scope；500 represent the volume supposing sample size constant volume, and unit is mL.
By above-mentioned steps 1) and step 2) method, the test liquid of reference material of preparation numbering 5 and 6 respectively, and calculating
Their potassium content, the results are shown in Table 4.
Table 4:
As shown in Table 4, the mensuration of potassium content in different main content industrial potassium nitrates is had well by the method for the invention
Precision, maximum allowable difference is 0.4%.
Embodiment 4
The mensuration of potassium content in the potassium nitrate that fireworks and firecrackers field is actually used:
1, for the industrial potassium nitrate of detection:
1#: sample combines the potassium nitrate of fireworks display effect medicines from Pubei County, Guangxi fireworks station-service in production 36.
2#: sample from Lingshan County, Guangxi fireworks station-service in produce display shell series products potassium nitrate.
2, use the method for the invention that above-mentioned industrial potassium nitrate sample is detected:
Because using the calibration curve that embodiment 1 determines, therefore, the step for of saving drafting calibration curve, directly carry out
Preparation test liquid carries out the step of upper machine mensuration, specific as follows:
2.1) preparation test liquid:
Weigh 1# industrial potassium nitrate sample 0.6g～3 parts of 0.8g sample respectively, when weighing, be accurate to 0.1mg, the 1st part of sample
It is placed in 300mL beaker, adds 100mL water, be placed on electric furnace heating 10min, be filtered hot to volumetric flask with filter paper, use water
Repeatedly rinsing repeatedly, after filtrate is cooled to room temperature, add 10mL nitric acid, the mass percent concentration of nitric acid is 20%, then uses
Water is settled to certain volume, obtains the 1st part of test liquid.Repeat said method, obtain 3 parts of test liquids of No. 1 reference material.
2) mensuration of potassium content in reference material:
By embodiment 1 step 2b) testing conditions, by 3 parts of test liquid sample introductions one by one of 1# industrial potassium nitrate sample, load
The sample path length of specimen cup is 15mm, and on grapher, the fluorescence intensity of display, determines according to embodiment 1 with this fluorescence intensity
Calibration curve reads corresponding K mass percent concentration value；
Calculating the mass percent concentration of potassium in 1# industrial potassium nitrate sample the most as follows, result is as shown in table 5.
Wherein, ω represents the mass percent concentration of potassium in sample, and unit is %；ω0Represent and read according to calibration curve
K mass percent concentration value, unit is %；1.5 sample sizes representing calibration curve reference, unit is g；M represents that sample is real
The quality that border weighs, unit is g；V is the volume of actual constant volume after representing sample dissolution, and unit is mL, it is ensured that the solution after constant volume
The concentration of middle K is in calibration curve scope；500 represent the volume supposing sample size constant volume, and unit is mL.
By above-mentioned steps 1) and step 2) method, prepare the test liquid of 2# potassium nitrate sample respectively, and calculate its potassium and contain
Amount, the results are shown in Table 5.
Table 5:
As shown in Table 5, the method for the invention is measured accurately, and deviation is little.
Claims (8)
1. one kind measures the method for potassium content in industrial potassium nitrate, it is characterised in that comprise the following steps:
1) calibration curve is drawn:
1.1) preparing many parts of potassium chloride working solutions, wherein the mass concentration of K is 0.16g/L～0.99g/L, and the mass concentration of Cl is
0.18g/L～1.10g/L；
1.2) with energy dispersion type Xray fluorescence spectrometer as detecting instrument, with 1.5g for the sample size of calibration curve reference, adopt
Analysis method is set up by the intensity correction method of X fluorescence spectrum quantitative analysis；By step 1.1) many parts of potassium chloride work of preparing
In liquid, the mass concentration of K is converted into the mass percent concentration of K, the most one by one sample introduction, records the fluorescence intensity of each sample introduction, with
In each potassium chloride working solution, the mass percent concentration of K is abscissa, with the fluorescence corresponding with the mass percent concentration of above-mentioned K
Intensity is vertical coordinate, makes calibration curve；Wherein, by following formula, the mass concentration of K in potassium chloride working solution is converted into K
Mass percent concentration:
Wherein, K% represents the mass percent concentration of K in potassium chloride working solution, and unit is %；C represents K in potassium chloride working solution
Mass concentration, unit is g/L；0.5 represents the volume supposing sample size constant volume, and unit is L；1.5 represent calibration curve reference
Sample size, unit is g；
2) potassium content in industrial potassium nitrate is quickly measured:
2.1) preparation test liquid: with industrial potassium nitrate as sample, during preparation test liquid, weighs a certain amount of sample, essence when weighing
Really to 0.1mg, it is placed in beaker, adds 100mL～150mL water, beaker is placed on electric furnace heating 10min～15min, while hot
With filter paper filtering, filtrate is filtered to volumetric flask, is added a certain amount of nitric acid, adds water fixed after the solution in volumetric flask is cooled to room temperature
Hold to certain volume；
2.2) by step 1.2) testing conditions, test liquid is loaded specimen cup, it is ensured that sample liquid thickness >=15mm, on grapher
The fluorescence intensity of display, reads corresponding K mass percent with this fluorescence intensity according to the above-mentioned calibration curve determined dense
Angle value；
2.3) content of potassium in calculating sample:
The mass percent concentration of potassium in calculating sample as follows:
Wherein, ω represents the mass percent concentration of potassium in sample, and unit is %；ω0Represent the K matter read according to calibration curve
Amount percent concentration value, unit is %；1.5 sample sizes representing calibration curve reference, unit is g；M represents that sample is actual and weighs
Quality, unit is g；V is the volume of actual constant volume after representing sample dissolution, and unit is mL, it is ensured that in the solution after constant volume, K's is dense
Degree is in calibration curve scope；500 represent the volume supposing sample size constant volume, and unit is mL.
The method of potassium content in mensuration industrial potassium nitrate the most according to claim 1, it is characterised in that: described step 1.1)
In, the method for preparation potassium chloride working solution is: weigh the reference material of a certain amount of potassium chloride reference material or other potassium elements,
Add appropriate water and nitric acid dissolves, obtain Klorvess Liquid after being settled to certain volume, then pipette different volumes respectively
Klorvess Liquid in the volumetric flask of multiple same specifications, obtain potassium chloride working solution after constant volume, wherein the mass concentration of K is
The mass concentration of 0.16g/L～0.99g/L, Cl is 0.18g/L～1.10g/L；Wherein, add nitric acid volume be 10mL～
20mL, mass percent concentration is 10%～30%.
The method of potassium content in mensuration industrial potassium nitrate the most according to claim 1, it is characterised in that described step 1.2)
In, testing conditions is: the X-ray light pipe collimator using aperture to be 8.8mm～14mm, it is possible to filter energy less than 3.607KeV
The filter of X-ray, arranging voltage is 8kV～16kV, and analysis time is 30s～80s, and energy range is 0～40keV, counting
During rate is, gaseous environment is air, and electric current is that matrix effect is not for consider automatically.
The method of potassium content in mensuration industrial potassium nitrate the most according to claim 3, it is characterised in that described step 1.2)
In, testing conditions is: use the X-ray light pipe collimator of aperture 8.8mm, uses fiber filter, and arranging voltage is 12kV, analyzes
Time is 35s, and energy range is 0～20keV.
The method of potassium content in mensuration industrial potassium nitrate the most according to claim 1, it is characterised in that: described step 2.1)
In, the amount of weighing of sample is 0.6g～0.8g.
The method of potassium content in mensuration industrial potassium nitrate the most according to claim 1, it is characterised in that: described step 2.1)
In, the volume adding nitric acid is 10mL～20mL, and mass percent concentration is 10%～30%.
The method of potassium content in mensuration industrial potassium nitrate the most according to claim 6, it is characterised in that: described step 2.1)
In, the mass percent concentration of nitric acid is 20%.
The method of potassium content in mensuration industrial potassium nitrate the most according to claim 1, it is characterised in that: described step 2.2)
In, sample liquid thickness is 15mm～30mm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610776265.XA CN106124547A (en) | 2016-08-31 | 2016-08-31 | A kind of measure the method for potassium content in industrial potassium nitrate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610776265.XA CN106124547A (en) | 2016-08-31 | 2016-08-31 | A kind of measure the method for potassium content in industrial potassium nitrate |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106124547A true CN106124547A (en) | 2016-11-16 |
Family
ID=57273317
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610776265.XA Pending CN106124547A (en) | 2016-08-31 | 2016-08-31 | A kind of measure the method for potassium content in industrial potassium nitrate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106124547A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111830026A (en) * | 2020-07-21 | 2020-10-27 | 固安桑普生化技术有限公司 | Rapid detection method and kit for potassium ions |
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 CN201610776265.XA patent/CN106124547A/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 |
|---|
| DETERMINATION OF POTASSIUM AND CALCIUM IN MILK POWDER BY ENERGY-: "《Determination of Potassium and Calcium in Milk Powder by Energy-Dispersive X-Ray Fluorescence Spectrometry》", 《X-RAY SPECTROMETRY》 * |
| 吕玉光: "《仪器分析》", 31 January 2016, 中国医药科技出版社 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111830026A (en) * | 2020-07-21 | 2020-10-27 | 固安桑普生化技术有限公司 | Rapid detection method and kit for potassium ions |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103364426B (en) | Method for determining content of zinc in zinc concentrate through energy-dispersive X-ray fluorescence spectrometry | |
| CN102033101B (en) | Method for measuring metal impurities in high-purity MgO film material by using inductively coupled plasma mass spectrometer | |
| CN106404814A (en) | Method for measuring potassium content of black powder | |
| CN106370684A (en) | Method for measuring titanium content in titanium powder for fireworks and crackers | |
| CN106093098A (en) | A kind of measure the method for copper content in fireworks and firecrackers firework medicament | |
| CN110274925A (en) | Method based on the gold in energy-dispersion X-ray fluorescence spectrometry measurement ore | |
| CN105651799A (en) | X fluorescence detection method of impurity content in quartz sand | |
| CN108414675B (en) | Method for rapidly determining low-concentration boric acid in aqueous solution by using pH meter | |
| CN102323254A (en) | A kind of method of testing of free uranium content | |
| CN106248709A (en) | A kind of measure the method for potassium content in fireworks and firecrackers firework medicament | |
| CN106168587A (en) | A kind of measure the method for iron content in fireworks and firecrackers firework medicament | |
| CN105301031A (en) | Method for determining hydrogen-containing silicone oil residual quantity in trisiloxane surfactant by one-dimensional hydrogen nuclear magnetic resonance method | |
| CN106404817A (en) | Method for measuring content of titanium in pyrotechnic composition for fireworks and crackers | |
| CN106370685A (en) | Method for determining content of potassium in industrial potassium chloride | |
| CN106124546A (en) | A kind of measure the method for potassium content in industry potassium chlorate | |
| CN103115881B (en) | Evaluate and reduce the method for the uncertainty numerical value of potassium in iron ore | |
| CN106248867A (en) | The method of polynary resultant in polynary positive pole material precursor is measured based on EDTA back titration automatic titering process | |
| CN106324005A (en) | Method for determining content of Ba in pyrotechnic composition for fireworks and firecrackers | |
| CN106093097A (en) | A kind of measure the method for content of strontium in fireworks and firecrackers firework medicament | |
| CN106124547A (en) | A kind of measure the method for potassium content in industrial potassium nitrate | |
| CN106168586A (en) | A kind of measure the method for iron content in fireworks and firecrackers iron powder | |
| CN106226340A (en) | A kind of measure the method for copper content in fireworks and firecrackers copper sulfate | |
| CN106168588A (en) | A kind of measure the method for potassium content in potassium perchlorate used for fireworks and crackers | |
| CN106093096A (en) | A kind of measure the method for barium content in fireworks and firecrackers barium nitrate | |
| CN106370686A (en) | Method for determining copper content in basic copper carbonate for fireworks and firecrackers |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20161116 |