CN105067590A - Method for measuring content of lead and bismuth elements in depollution solution - Google Patents
Method for measuring content of lead and bismuth elements in depollution solution Download PDFInfo
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- CN105067590A CN105067590A CN201510419894.2A CN201510419894A CN105067590A CN 105067590 A CN105067590 A CN 105067590A CN 201510419894 A CN201510419894 A CN 201510419894A CN 105067590 A CN105067590 A CN 105067590A
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Abstract
The method for measuring the content of lead and bismuth elements in a depollution solution comprises steps as follows: (1) preparing a to-be-measured element standard solution; (2) preparing a sample solution I from the depollution solution before cleaning of parts for use; (3) preparing a sample solution II from the equivalent depollution solution after cleaning of the parts for use; (4) setting test conditions of inductive coupled plasma atomic emission spectrometry, measuring element content of deionized water, the to-be-measured element standard solution, the sample solution I and the sample solution II through an inductive coupled plasma atomic emission spectrometer; (5) recording measuring results, subtracting the lead element content of the sample solution I from the lead element content of the sample solution II, subtracting the bismuth element content of the sample solution I from the bismuth element content of the sample solution II, if the two results are up to the standard, judging the content to be qualified, and otherwise, judging the content to be unqualified. The analysis process is convenient to operate, the reagent consumption is low, and the working efficiency can be improved substantially.
Description
Technical field
The invention belongs to chemical analysis technology field, be specifically related to a kind of method measuring lead and bismuth element content in depollution solution.
Background technology
Acid cleaning process is generally applied in military enterprise, adding man-hour requirement at blade of aviation engine uses sn-bi alloy to position, the sn-bi alloy of location should be removed after process finishing, residue in the low melting point elements such as the lead of blade surface, bismuth very large to the harm of material, can grain boundary corrosion be produced to material thus cause the generation of crackle and finally cause leaf destruction, therefore, need to use depollution solution clean blade thus remove the low melting point element such as lead, bismuth residuing in blade surface.
Prior art requirement, after a collection of part depollution solution cleaning, must detect the lead in depollution solution after the lead in depollution solution before cleaning components, bismuth element content and cleaning components, bismuth element content simultaneously, depollution solution after cleaning components is compared with the depollution solution before cleaning components, and the difference of Qi Zhongqian, bismuth element content should be less than 1PPM.Therefore need that a kind of cost is low, easy and simple to handle, reagent consumption less, method that environmental pollution is little carrys out content that is plumbous in express-analysis depollution solution, bismuth element.Existing method uses flame atomic absorption method, the method complex steps, need first to carry out evaporate to dryness, the sample handling procedure such as dissolved salt, plumbous during analysis, bismuth element needs to use different analysis conditions to measure respectively, being in great demand to spare part, need when measuring lead element content to use lead element hollow cathode lamp, measure bismuth element and replace with bismuth element hollow cathode lamp and T-shaped quartz ampoule atomizer again, therefore, even the technician of skilled operation uses the lead in flame atomic absorption spectrometry depollution solution, bismuth element content, also need within 2 hours, just can complete test.The consumption of flame atomic absorption method reagent is many, need use lead, bismuth standard solution and the reagent such as hydrochloric acid, boron potassium cyanide, and the pollution produced environment is larger.
Summary of the invention
The object of the invention is to for above-mentioned the problems of the prior art, provide a kind of cost low, easy and simple to handle, finding speed is fast, and reagent consumption is few, the method for lead and bismuth element content in the mensuration depollution solution that environmental pollution is little.
To achieve these goals, the technical solution used in the present invention comprises the following steps:
(1) preparation of elemental standards solution to be measured: first divide the concentration of getting equivalent be the plumbous standard solution of 1mg/mL and bismuth standard solution in same volumetric flask, then dilute with deionized water, shake up and obtain elemental standards solution for standby to be measured;
(2) sample solution one is prepared: first divide the some mL of depollution solution before getting cleaning components in volumetric flask, then dilute with deionized water, obtain sample solution one after shaking up for subsequent use;
(3) prepare sample solution two: first divide get with step (2) equivalent cleaning components after depollution solution in another volumetric flask, be then diluted to and sample solution one equivalent with deionized water, obtain sample solution two after shaking up for subsequent use;
(4) set the test condition of ICP-AES, measure deionized water by inductively coupled plasma atomic emission spectrometer, elemental standards solution to be measured, the constituent content of sample solution one and sample solution two;
(5) measurement result of inductively coupled plasma atomic emission spectrometer is recorded, the lead element content of sample solution one is deducted with the lead element content of sample solution two, the bismuth element content of sample solution one is deducted with the bismuth element content of sample solution two, two results all reach technological requirement and are then judged to be qualified, otherwise are judged to be defective.
Described plumbous standard solution and bismuth standard solution divide gets 0.2 ~ 10mL, and described plumbous standard solution and bismuth standard solution are diluted to 100mL with deionized water in same volumetric flask.
Described wash part before depollution solution and depollution solution after cleaning components divide and get 5 ~ 10mL, described sample solution one and sample solution two are diluted to 25 ~ 50mL with deionized water,
The test condition of described ICP-AES comprises the operation wavelength of plumbous bismuth element, atomization gas flow, high frequency power, plasma gas flow rate, assisted gas flow, observed altitude, observed ray, integral way, automatic integration time, sample introduction pump speed, the volume after point sample solution volume got and sample solution dilute.
The test condition of described ICP-AES is:
Set the operation wavelength of plumbous bismuth element, lead is 220.353nm, 217.000nm, 261.418nm, 283.306nm, 224.688nm or 405.781nm, and bismuth is 223.061nm, 190.171nm, 306.766nm, 222.821nm or 206.170nm; Atomization gas flow is 0 ~ 2L/min; High frequency power is 750 ~ 1350W; Plasma gas flow rate is 0 ~ 20L/min; Assisted gas flow is 0 ~ 2L/min; Observed altitude is 0 ~ 30mm; Observed ray is level or vertical; Integral way is integrating peak areas or peak height integration; The automatic integration time is 2 ~ 500 seconds; Sample introduction pump speed is 0 ~ 10mL/min; The sample solution volume got is divided to be 1 ~ 20mL; Volume after sample solution dilution is 5 ~ 100mL.
Working curve is made by elemental standards solution to be measured in described step (1).
Compared with prior art, the present invention has following beneficial effect: the present invention uses ICP-AES to test, and analytic process is easy and simple to handle, does not need extra spare part, and sample handling processes is simple, only need divides and get constant volume and namely can complete mensuration.Adopt the reagent consumption of ICP-AES few, only use lead, bismuth standard solution two kinds of reagent, little to the pollution of environment.Use ICP-AES to measure content that is plumbous in depollution solution, bismuth element, complete total Test and only need 15 minutes, is foreshortened to 1/8th of flame atomic absorption method the production cycle, improve production efficiency dramatically.In sum, the present invention has very high using value and market economy is worth, and can increase substantially work efficiency, reduces experimentation cost and reduce the pollution to environment.
Further, the use of the present invention to each test condition of ICP-AES is tested, and comprises the operation wavelength of plumbous bismuth element, atomization gas flow, high frequency power, plasma gas flow rate, assisted gas flow, observed altitude, observed ray, integral way, the automatic integration time, sample introduction pump speed, the volume after point sample solution volume got and sample solution dilute, can obtain plumbous in depollution solution and bismuth element content measurement result accurately.
Embodiment
Below in conjunction with specific embodiment, the present invention is described in further detail.
Embodiment one
(1) preparation of plumbous bismuth mixed standard solution: first divide and get in 1mg/mL plumbous standard solution 0.5mL to 100mL volumetric flask, then divide and get 1mg/mL bismuth standard solution 0.5mL in same 100mL volumetric flask, be diluted to scale with deionized water, shake up rear for subsequent use.It is the elemental standards solution to be measured that 5mg/ rises that this step obtains plumbous bi content, and elemental standards solution to be measured is for making working curve.
(2) divide in depollution solution 5mL to the 25mL volumetric flask before getting cleaning components, be diluted to scale with deionized water, shake up rear for subsequent use.This step obtains sample solution one.
(3) divide the depollution solution 5mL after getting cleaning components in another 25mL volumetric flask, be diluted to scale with deionized water, shake up rear for subsequent use.This step obtains sample solution two.
(4) in the working software of inductively coupled plasma atomic emission spectrometer, following condition determination is set:
The operation wavelength of plumbous bismuth element: plumbous 220.353nm
Bismuth 223.061nm
Atomization gas flow: 0.8L/min
High frequency power: 1200W
Carrier gas flux: 15L/min
Assisted gas flow: 0.2L/min
Observed altitude: 15.0mm
Observed ray: level is observed
Integral way: integrating peak areas
The automatic integration time: minimum 5 seconds, maximum 10 seconds
Sample introduction pump speed: 1.00mL/min
Divide the volume of extracting sample solution: 5mL
Volume after sample solution dilution: 25mL
(5) measure: use the blank deionized water of inductively coupled plasma atomic emission spectrometer sequentially determining, elemental standards solution to be measured, sample solution one, sample solution two.
(6) record the test result of sample solution one and sample solution two, test completes.
(7) according to test result, the lead element content of sample solution one is deducted with the lead element content of sample solution two, deduct the bismuth element content of sample solution one with the bismuth element content of sample solution two, two results all reach technological requirement and are then judged to be qualified, otherwise are judged to be defective.
Embodiment two
(1) preparation of plumbous bismuth mixed standard solution: first divide and get in 1mg/mL plumbous standard solution 1mL to 100mL volumetric flask, then divide and get 1mg/mL bismuth standard solution 1mL in same 100mL volumetric flask, be diluted to scale with deionized water, shake up rear for subsequent use.It is the elemental standards solution to be measured that 10mg/ rises that this step obtains plumbous bi content, and elemental standards solution to be measured is for making working curve.
(2) divide in depollution solution 10mL to the 50mL volumetric flask before getting cleaning components, be diluted to scale with deionized water, shake up rear for subsequent use.This step obtains sample solution one.
(3) divide the depollution solution 10mL after getting cleaning components in another 50mL volumetric flask, be diluted to scale with deionized water, shake up rear for subsequent use.This step obtains sample solution two.
(4) in the working software of inductively coupled plasma atomic emission spectrometer, following condition determination is set:
The operation wavelength of plumbous bismuth element: plumbous 217.000nm
Bismuth 190.171nm
Atomization gas flow: 0.9L/min
High frequency power: 1300W
Carrier gas flux: 16L/min
Assisted gas flow: 0.3L/min
Observed altitude: 14.0mm
Observed ray: Vertical Observation
Integral way: integrating peak areas
The automatic integration time: minimum 2 seconds, maximum 10 seconds
Sample introduction pump speed: 1.20mL/min
Divide the volume of extracting sample solution: 10mL
Volume after sample solution dilution: 50mL
(5) measure: use inductively coupled plasma atomic emission spectrometer sequentially determining blank (deionized water), elemental standards solution to be measured, sample solution one, sample solution two.
(6) record the test result of sample solution one and sample solution two, test completes.
(7) according to test result, the lead element content of sample solution one is deducted with the lead element content of sample solution two, deduct the bismuth element content of sample solution one with the bismuth element content of sample solution two, two results all reach technological requirement and are then judged to be qualified, otherwise are judged to be defective.
Embodiment three
(1) preparation of plumbous bismuth mixed standard solution: first divide and get in 1mg/mL plumbous standard solution 0.2mL to 100mL volumetric flask, then divide and get 1mg/mL bismuth standard solution 0.2mL in same 100mL volumetric flask, be diluted to scale with deionized water, shake up rear for subsequent use.It is the elemental standards solution to be measured that 2mg/ rises that this step obtains plumbous bi content, and elemental standards solution to be measured is for making working curve.
(2) divide in depollution solution 5mL to the 50mL volumetric flask before getting cleaning components, be diluted to scale with deionized water, shake up rear for subsequent use.This step obtains sample solution one.
(3) divide the depollution solution 5mL after getting cleaning components in another 50mL volumetric flask, be diluted to scale with deionized water, shake up rear for subsequent use.This step obtains sample solution two.
(4) in the working software of inductively coupled plasma atomic emission spectrometer, following condition determination is set:
The operation wavelength of plumbous bismuth element: plumbous 261.418nm
Bismuth 306.766nm
Atomization gas flow: 1.0L/min
High frequency power: 1250W
Carrier gas flux: 14L/min
Assisted gas flow: 0.1L/min
Observed altitude: 16.0mm
Observed ray: level is observed
Integral way: integrating peak areas
The automatic integration time: minimum 5 seconds, maximum 20 seconds
Sample introduction pump speed: 1.4mL/min
Divide the volume of extracting sample solution: 5mL
Volume after sample solution dilution: 50mL
(5) measure: sequentially determining blank (deionized water) in the manual analyzing window of inductively coupled plasma atomic emission spectrometer working software, elemental standards solution to be measured, sample solution one, sample solution two.
(6) record the test result of sample solution one and sample solution two, test completes.
(7) according to test result, the lead element content of sample solution one is deducted with the lead element content of sample solution two, deduct the bismuth element content of sample solution one with the bismuth element content of sample solution two, two results all reach technological requirement and are then judged to be qualified, otherwise are judged to be defective.
Claims (6)
1. measure a method that is plumbous in depollution solution and bismuth element content, it is characterized in that, comprise the following steps:
(1) preparation of elemental standards solution to be measured: first divide the concentration of getting equivalent be the plumbous standard solution of 1mg/mL and bismuth standard solution in same volumetric flask, then dilute with deionized water, shake up and obtain elemental standards solution for standby to be measured;
(2) sample solution one is prepared: first divide the some mL of depollution solution before getting cleaning components in volumetric flask, then dilute with deionized water, obtain sample solution one after shaking up for subsequent use;
(3) prepare sample solution two: first divide get with step (2) equivalent cleaning components after depollution solution in another volumetric flask, be then diluted to and sample solution one equivalent with deionized water, obtain sample solution two after shaking up for subsequent use;
(4) set the test condition of ICP-AES, measure deionized water by inductively coupled plasma atomic emission spectrometer, elemental standards solution to be measured, the constituent content of sample solution one and sample solution two;
(5) measurement result of inductively coupled plasma atomic emission spectrometer is recorded, the lead element content of sample solution one is deducted with the lead element content of sample solution two, the bismuth element content of sample solution one is deducted with the bismuth element content of sample solution two, two results all reach technological requirement and are then judged to be qualified, otherwise are judged to be defective.
2. the method for plumbous in mensuration depollution solution according to claim 1 and bismuth element content, it is characterized in that: described plumbous standard solution and bismuth standard solution divide gets 0.2 ~ 10mL, and described plumbous standard solution and bismuth standard solution are diluted to 100mL with deionized water in same volumetric flask.
3. the method for plumbous in mensuration depollution solution according to claim 1 and 2 and bismuth element content, it is characterized in that: the depollution solution before described cleaning components and the depollution solution after cleaning components divide gets 5 ~ 10mL, and described sample solution one and sample solution two are diluted to 25 ~ 50mL with deionized water.
4. the method for plumbous in mensuration depollution solution according to claim 1 and bismuth element content, it is characterized in that: the test condition of described ICP-AES comprises the operation wavelength of plumbous bismuth element, atomization gas flow, high frequency power, plasma gas flow rate, assisted gas flow, observed altitude, observed ray, integral way, the automatic integration time, sample introduction pump speed, the volume after point sample solution volume got and sample solution dilute.
5. the method for lead and bismuth element content in the mensuration depollution solution according to claim 1 or 4, it is characterized in that, the test condition of described ICP-AES is:
Set the operation wavelength of plumbous bismuth element, lead is 220.353nm, 217.000nm, 261.418nm, 283.306nm, 224.688nm or 405.781nm, and bismuth is 223.061nm, 190.171nm, 306.766nm, 222.821nm or 206.170nm; Atomization gas flow is 0 ~ 2L/min; High frequency power is 750 ~ 1350W; Plasma gas flow rate is 0 ~ 20L/min; Assisted gas flow is 0 ~ 2L/min; Observed altitude is 0 ~ 30mm; Observed ray is level or vertical; Integral way is integrating peak areas or peak height integration; The automatic integration time is 2 ~ 500 seconds; Sample introduction pump speed is 0 ~ 10mL/min; The sample solution volume got is divided to be 1 ~ 20mL; Volume after sample solution dilution is 5 ~ 100mL.
6. the method for plumbous in mensuration depollution solution according to claim 1 and bismuth element content, is characterized in that: make working curve by elemental standards solution to be measured in described step (1).
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