CN106526062B - The ion chromatographic method of trace chloro ion in a kind of measure triethyl aluminum - Google Patents
The ion chromatographic method of trace chloro ion in a kind of measure triethyl aluminum Download PDFInfo
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Abstract
The ion chromatographic method of trace chloro ion in a kind of measure triethyl aluminum, including 1 testing sample pre-treatment：TEAL samples are dissolved with isopropanol, scale is settled to secondary deionized water, carries out ultrasound, centrifugal treating, take supernatant to be analyzed after crossing 0.22 μm of syringe filter and H type pre-treatment posts into ion chromatography system；2 configuration work curve solutions；The analysis of 3 standard addition method solution：To repeated solution continuous sample introduction 6 times, Cl is obtained‑The chromatogram of Standard entertion liquor analysis, by the triethyl aluminum sample solution row ion chromatography after pre-treatment, Cl peak area is obtained, according to working curve and Cl peak area, obtains the content of Cl in triethyl aluminum.The present invention is simple to operate, reproducible, and high sensitivity, can effectively determine chloride ion content in TEAL, solves the problems, such as that heavy metal aluminium is to chromatographic column and suppressor pollution damage in continuous mode.
Description
Technical field
The present invention relates to measure trace chloro ion ion chromatographic method, more particularly to measure triethyl aluminum in trace amounts of chlorine from
The ion chromatographic method of son, belongs to chemical analysis technology field.
Background technology
Triethyl aluminum TEAL can be used as catalyst, initiator and rocket fuel, also act as the raw material of MOVCD techniques,
It is used to make precipitation aluminium film in diode, transistor, integrated circuit production.Require that the content of chlorion exists in such applications
In certain limit, use demand could be met.Therefore need to establish a kind of method to the trace in TEAL products and production process
Amount chlorion is measured, to ensure the performance of product.
Report on trace chloro ion in TEAL has no relevant report.Therefore it is simple, easy to establish a kind of pre-treating method
Repeat, and method high sensitivity, while solve heavy metal aluminium in continuous mode and chromatographic column and suppressor pollution damage are asked
Topic, trace chloro ion in measure TEAL is had very important significance.
The content of the invention
It is an object of the invention to provide a kind of pre-treating method of trace chloro ion in ion chromatography TEAL, this method
It is simple to operate, it is reproducible, and high sensitivity.
The ion chromatographic method of trace chloro ion in a kind of measure triethyl aluminum, it is characterised in that comprise the following steps：
(1) testing sample pre-treatment：
1.1 under nitrogen protection, and it is 0.2g accurately to weigh TEAL sample qualities, is placed in 100ml volumetric flasks；
1.2, which accurately pipette 10mL isopropanols, is slowly dropped on sample, and sample is dissolved, and is added, is shaken in shaking
10min is shaken, scale is settled to secondary deionized water, and ultrasonic 10min is carried out to accelerate the extraction of chlorion to solution, is obtained
To TEAL sample solution, and stand 60min；
1.3 are transferred to sample solution in centrifuge tube, centrifuge 10min with 10000r/min rotating speeds, obtain need testing solution；
1.4 take need testing solution supernatant cross 0.22 μm of syringe filter and H type pre-treatment posts after enter chromatography of ions
System is analyzed, and the preceding 3mL sample solutions of wherein sample will discard；
(2) configuration work curve solution, carry out ion chromatography, obtain the peak area of Cl- under various concentrations, with chlorine from
The concentration of son is abscissa, using its peak area as ordinate drawing curve；Chromatographic condition in the chromatography is：
The quasi- stock solution 1000mg/L of chlorion；Leacheate is sodium carbonate and sodium acid carbonate mixed solution, flow velocity：
1.0mL/min；Electric conductivity detector temperature：40℃；Column temperature：30℃；
Suppress electric current：30mA；Sample size：20μL；Wherein,
The preparation of 2.1 standard working solutions
Accurately pipette 50 μ L Cl-Standard Stock solutions 50mL is settled to scale into volumetric flask, with secondary deionized water,
It is 1.0mg/L to obtain Cl- concentration；
The preparation of 2.2 blank solutions
The accurate isopropanol for pipetting 10mL, 100mL is diluted to secondary deionized water；
The preparation of 2.3 standard working curve solution
The accurate standard liquid for pipetting the μ g/mL Cl- of 0,10,20,50,100 and 200 μ L 1.0 is to 6 2mL sample bottles
In, and 1000,990,980,950,900 and 800 μ L blank solution is separately added into, mix, the Cl- concentration point of obtained solution
Wei not 0,10,20,50,100 and 200 μ g/L；
The preparation of 2.4 repeated solution
It is accurate to pipette 10.0 μ L standard working solutions, 990 μ L blank solutions are added, mixes, produces the μ g/L's of mark-on 10
Cl- solution；
(3) analysis of standard liquid
It is 3.1 repeated
To repeated solution continuous sample introduction 6 times, the chromatogram of Cl- standards solution analysis is obtained, and obtain chlorion chromatogram
The retention time at peak and the relative standard deviation of peak area are respectively 0.24% and 0.65%；
3.2 linear relationship
To working curve solution, sample introduction analysis is carried out according to the Loading sequence from low concentration to high concentration, is obtained different dense
The lower Cl- of degree peak area, with the concentration (mg/L) of chlorion for abscissa, using its peak area as ordinate drawing curve；
Triethyl aluminum sample solution after pre-treatment is carried out ion chromatography by 3.3, obtains Cl- peak area；
3.4, according to working curve and Cl- peak area, obtain the content of Cl- in triethyl aluminum.
The ion chromatographic method of trace chloro ion in a kind of measure triethyl aluminum, it is characterised in that comprise the following steps：
(1) testing sample pre-treatment：
1.1 under nitrogen protection, and it is 0.2g accurately to weigh TEAL sample qualities, is placed in 100ml volumetric flasks；
1.2, which accurately pipette 10mL isopropanols, is slowly dropped on sample, and sample is dissolved, and is added, is shaken in shaking
10min is shaken, scale is settled to secondary deionized water, and ultrasonic 10min is carried out to accelerate the extraction of chlorion to the solution, is obtained
To TEAL sample solution, and stand 60min；
1.3 are transferred to sample solution in centrifuge tube, centrifuge 10min with 10000r/min rotating speeds, obtain need testing solution；
1.4 take need testing solution supernatant cross 0.22 μm of syringe filter and H type pre-treatment posts after enter chromatography of ions
System is analyzed, and the preceding 3mL sample solutions of wherein sample will discard；
(2) configuration standard curve solution；
The accurate standard working solution for pipetting the μ g/mL chlorions of 100 μ L 1.0, adds 900 μ L secondary deionized waters, mixes
Even, it is 100 μ g/L to obtain its concentration；
(3) standard addition method curve solution and the triethyl aluminum sample solution after pre-treatment are entered under identical chromatographic conditions
Row ion chromatography, Cl- peak area is respectively obtained, is compared, is produced；
(4) it is repeated
To repeated solution continuous sample introduction 6 times, Cl is obtained-The chromatogram of Standard entertion liquor analysis, and obtain chlorion
The retention time of chromatographic peak and the relative standard deviation of peak area are respectively 0.24% and 0.65%；
(5) linear relationship
To the linear solvent of the standard addition method of preparation, sample introduction point is carried out according to the Loading sequence from low concentration to high concentration
Analysis, obtains the peak area of Cl- under various concentrations, with the concentration (mg/L) of chlorion for abscissa, using its peak area as ordinate
Drawing curve.
H type pre-treatment posts must be activated using preceding using 15mL secondary deionized waters, and activation method is：Noted using 5mL
Emitter is rinsed with 2.0mL/min speed, and the volume of flushing is 15mL, and the secondary deionized water to finally developing
Be measured, if measure contain Cl-, need to continue to rinse, until in the secondary deionized water developed Cl- not by
Detection.
The type of the sample pre-treatments post is H posts, and its capacity is 2.5cc.
Because the substantial amounts of aluminium contained in TEAL samples can cause damage to chromatographic column and suppressor, therefore enter ion color
, it is necessary to which sample solution is crossed into H type pre-treatment posts before spectra system.Eliminate the principle of heavy metal aluminium：Due to filling out in H type pre-treatment posts
Expect for sulfonic acid ion exchange resin (i.e. there is substantial amounts of H+ on surface), the trivalent aluminium ion in H+ and sample solution is put
Change reaction, the trivalent aluminium ion in sample solution is incorporated on H type pre-treatment posts, so as to reach in removal sample solution
The purpose of heavy metal aluminium.
Leacheate used is sodium carbonate and sodium acid carbonate mixed solution in the ion chromatography；Described leacheate
Concentration is 1.8mmol/L sodium carbonate and the mixed solution of 1.6mmol/L sodium acid carbonates.
To ensure the determination of chloride ion degree of accuracy, it is necessary to assure chlorion chromatographic peak is not disturbed by other peaks, i.e., with it is adjacent
Separating degree between chromatographic peak reaches more than 1.5；In the experiment, the interference of chlorion is mainly derived from the hydrogen-oxygen in sample solution
Radical ion, therefore retention time hydroxy can be changed by adjusting the concentration of bicarbonate radical in leacheate.In selected chromatographic column
On the premise of, the present invention is respectively to 1.7/1.0,1.9/1.7,1.8/1.8,1.7/1.6,1.8/1.6 and 1.8/2.5 (carbonic acid
Sodium/sodium acid carbonate) chromatographic condition tested, obtain under six kinds of chromatographic conditions point between chlorion and adjacent chromatographic peak
From degree and analysis deadline.As a result show, 1.7/1.6,1.8/1.6 (sodium carbonate/bicarbonate) meets measure separating degree
It is required that and from the point of view of whole process analysis time, select 1.8/1.6 chromatographic condition, its analysis efficiency will improve it is a lot, therefore
The eluent concentration of final choice is 1.8mmol/L sodium carbonate and the mixed solution of 1.6mmol/L sodium acid carbonates.
Chromatographic condition in the chromatography is：The quasi- stock solution 1000mg/L of chlorion；Flow velocity： 1.0mL/min；
Electric conductivity detector temperature：40℃；Column temperature：30℃；Suppress electric current：30mA；Sample size： 20μL.
Technical solution of the present invention has the advantages that compared with prior art：
The pre-treating method of trace chloro ion is simple to operate in ion chromatography TEAL of the present invention, reproducible, and spirit
Sensitivity is high, can effectively determine chloride ion content in TEAL, while solves in continuous mode heavy metal aluminium to chromatographic column and suppression
The problem of device pollution damage.
Brief description of the drawings
The μ g/L Chloride Solution chromatograms of Fig. 1 Standard entertions 10
Chromatographic peak (μ g/L):1..Cl-(10.0)
Fig. 2 standard addition method working curves
Chlorine ion concentration corresponding to Fig. 3 different volumes isopropanols
The concentration of chlorion corresponding to Fig. 4 different excusing from death times
Fig. 5 chlorion standard liquid chromatograms.
Chromatographic peak:(μg/L):1..Cl-(100.0)
Fig. 6 sample solution chromatograms
Chromatographic peak：1.Cl-
Embodiment
1.1 instruments and reagent
AnL-IC2600 types ion chromatograph (Qingdao Ai Li analysis experiments Science and Technology Ltd.)；Anion suppressor；Conductance
Detector；H type pre-treatments post (Qingdao Ai Li analysis experiments science and technology)；
TEAL samples (client's offer)；Sodium carbonate (standard reagent)；Sodium acid carbonate (top pure grade)；Isopropanol (chromatographically pure).
1.2 chromatographic condition
The quasi- stock solution 1000mg/L of chlorion；Flow velocity：1.0mL/min；Electric conductivity detector temperature：40℃；Column temperature：30
℃；Suppress electric current：30mA；Sample size：20μL.
The configuration of 1.3 solution
(1) preparation of leacheate
Accurate weighing 0.1918g sodium carbonate standard reagent and 0.1344g sodium acid carbonates, are placed in 1000mL volumetric flasks, use
Secondary deionized water dissolves and is settled to scale, obtains the mixing of 1.8mmol/L sodium carbonate and 1.6mmol/L sodium acid carbonates
Solution, in this, as leacheate.
(2) preparation of standard working solution
Accurately pipette in 50 μ L Cl- Standard Stock solutions 50mL volumetric flasks, be settled to scale with secondary deionized water, obtain
It is 1.0mg/L to Cl- concentration.
(3) preparation of blank solution
The accurate sulfuric acid solution for pipetting 1.0mL5%, 10mL is diluted to 0.125mol/L sodium hydroxide solution.
(4) preparation of standard addition method working curve solution
The accurate standard liquid for pipetting the μ g/mL Cl- of 0,10,20,50,100 and 200 μ L 1.0 is to 6 2mL sample bottles
In, and 1000,990,980,950,900 and 800 μ L blank solution is separately added into, mix, obtain the Cl-'s of standard addition method
Concentration is respectively 0,10,20,50,100 and 200 μ g/L.
(5) preparation of calibration curve solution
The accurate standard working solution for pipetting the μ g/mL chlorions of 100 μ L 1.0, adds 900 μ L secondary deionized waters, mixes
Even, it is 100 μ g/L to obtain its concentration.
(6) preparation of repeated solution
It is accurate to pipette 10.0 μ L standard working solutions, 990 μ L blank solutions are added, mixes, produces the μ g/L's of mark-on 10
Cl- solution.
First, the determination of leacheate sodium carbonate/bicarbonate ratio
To ensure the determination of chloride ion degree of accuracy, it is necessary to assure chlorion chromatographic peak is not disturbed by other peaks, i.e., with it is adjacent
Separating degree between chromatographic peak reaches more than 1.5；In the experiment, the interference of chlorion is mainly derived from the system in sample solution
Peak, therefore retention time hydroxy can be changed by adjusting the concentration of bicarbonate radical in leacheate.Before selected chromatographic column
Put, this method is respectively to 1.7/1.0,1.9/1.7,1.8/1.8,1.7/1.6,1.8/1.6 and 1.8/2.5 (sodium carbonate/carbon
Sour hydrogen sodium) chromatographic condition tested, obtain separating degree under six kinds of chromatographic conditions between chlorion and system peak and point
The deadline is analysed, is shown in Table 1.1.7/1.0,1.8/1.8,1.7/1.6 and 1.8/1.6 (sodium carbonate/carbonic acid as can be seen from Table 1
Hydrogen sodium) meet the requirement of measure separating degree, and from the point of view of whole process analysis time, 1.8/1.6 chromatographic condition is selected, its point
Analysing efficiency will improve a lot, therefore the eluent concentration of final choice is 1.8mmol/L sodium carbonate and 1.6mmol/L carbonic acid
The mixed solution of hydrogen sodium.
Table 1
2nd, the determination of sample pre-treatments parameter
(1) determination of the selection of solvent
Exploded because triethyl aluminum TAEL meets water, so the selection of solvent eliminates water.Triethyl aluminum is soluble in
The organic solvents such as benzene, gasoline and isopropanol, it is contemplated that triethyl aluminum dissolving after chlorion extraction and anion chromatographic column it is resistance to
By sex chromosome mosaicism, solvent of the isopropanol for selecting to dissolve each other with water as dissolving TAEL.
(2) determination of isopropanol volume
Into TAEL samples, addition 6,7,8,9,10,11 and 12mL isopropanols dissolve to it respectively, and respectively with two
Secondary deionized water constant volume is to 100mL.The chlorion in 7 parts of sample solutions is measured respectively, obtains corresponding chlorion
Concentration.Curve is drawn to chlorine ion concentration by isopropanol volume, sees Fig. 3, can be with isopropanol liquid from the curve of drafting
Long-pending increase, its recovery rate are also that raising trend is presented, and recovery rate tends towards stability when 10mL, therefore isopropanol in the invention
Addition volume be 10.0mL.(3) determination of ultrasonic extraction time
The purpose of ultrasonic extraction is that the chlorion in sample is extracted in the step.The present invention is to the same as a sample sample
Product solution, the sample solution of the ultrasonic extraction by 5,6,7,8,9,10 and 11min is determined respectively.By extraction time to chlorion
Concentration draw curve, Fig. 4 is seen, it can be seen that with the increase of ultrasonic extraction time, its recovery rate from the curve of drafting
It is that raising trend is presented, recovery rate tends towards stability after 9min, therefore the time of ultrasonic extraction is 10min in the invention.
3rd, trace chloro ion determines in TEAL
The processing of 1 sample solution
(1) under nitrogen protection, the quality for accurately weighing TEAL samples is 0.2g, is placed in 100mL volumetric flasks；
(2) 10mL isopropanols accurately are pipetted to be slowly dropped on sample, sample is dissolved, added, shake in shaking
10min is shaken, scale is settled to secondary deionized water, obtains TEAL sample solution, and stand 60min；
(3) 10mLTEAL sample solution is transferred in centrifuge tube, 10min is centrifuged with 10000r/min rotating speeds, obtained
Need testing solution；
(4) take the supernatant of the need testing solution in (3) cross after 0.22 μm of syringe filter and H type pre-treatment posts enter from
Sub- chromatographic system is analyzed, and the preceding 3mL sample solutions of wherein sample will discard.
Wherein because the substantial amounts of aluminium contained in TEAL samples can cause damage to chromatographic column and suppressor, thus enter from
, it is necessary to sample solution be crossed into H type pre-treatment posts, i.e., before sub- chromatographic system：H type pre-treatment posts are gone for bis- times using preceding palpus using 15mL
Ionized water is activated, and activation method is：5mL syringes are used to be rinsed with 2.0mL/min speed, the volume of flushing
For 15mL, and the secondary deionized water to finally developing is measured, if measure contains Cl-, needs to continue to rush
Wash, until Cl- is not detected in the secondary deionized water developed.
Eliminate the principle of heavy metal aluminium：Because the filler in H type pre-treatment posts is sulfonic acid ion exchange resin (i.e. table
There is substantial amounts of H+ in face), the trivalent aluminium ion in H+ and sample solution enters line replacement reaction, the trivalent aluminium ion quilt in sample solution
It is attached on H type pre-treatment posts, so as to reach the purpose for removing heavy metal aluminium in sample solution.
The analysis of 2 standard addition method solution
(1) it is repeated
To repeated solution continuous sample introduction 6 times, Cl is obtained-The chromatogram (see Fig. 1) of Standard entertion liquor analysis, and obtain
The retention time of chlorion chromatographic peak and the relative standard deviation of peak area are respectively 0.24% and 0.65%.
(2) linear relationship
To the linear solvent of the standard addition method of preparation, sample introduction point is carried out according to the Loading sequence from low concentration to high concentration
Analysis, obtains the peak area of Cl- under various concentrations, with the concentration (mg/L) of chlorion for abscissa, using its peak area as ordinate
Drawing curve, is shown in Fig. 2.
The analysis of 3 calibration curve solutions
To 100 μ g/L of preparation Cl-Standard liquid sample introduction is analyzed, and obtains Cl-Chromatogram, see Fig. 5.
The measure and recovery of standard addition of chloride ion content in 4TAEL samples
Under selected chromatographic condition, the TAEL sample solutions handled well are detected, obtain actual sample detection
Chromatogram, see accompanying drawing 6, while respectively according to standard addition method and single-point external standard method to the Cl in actual sample-Quantified, and
Obtain Cl in the sample solution using two kinds of computational methods-Concentration, be shown in Table 2, as can be seen from the table, according to standard addition method and
The relative standard deviation of the concentration of chlorion is calculated between 2.47~5.99% in calibration curve method, it was demonstrated that both sides
Result uniformity is preferable in chloride ion conductor in for TEAL for method.Recovery of standard addition experiment is carried out to actual sample, is shown in Table
3, the sample recovery rate that mark-on 10.0,20.0 and 100 can be obtained from table is 84.2~106.6%, demonstrates the experiment side
The reliability of method.
Cl in the sample solution of table 2-The measurement result of concentration
Table 3 carries out recovery of standard addition test specimen determination of recovery rates result to sample
Claims (4)
1. a kind of ion chromatographic method for determining trace chloro ion in triethyl aluminum, it is characterised in that comprise the following steps：
(1) testing sample pre-treatment：
1.1 under nitrogen protection, and it is 0.2g accurately to weigh TEAL sample qualities, is placed in 100ml volumetric flasks；
1.2, which accurately pipette 10mL isopropanols, is slowly dropped on sample, and sample is dissolved, and is added, is shaken in shaking
10min, scale is settled to secondary deionized water, and ultrasonic 10min is carried out to accelerate the extraction of chlorion to solution, obtained
TEAL sample solution, and stand 60min；
1.3 are transferred to sample solution in centrifuge tube, centrifuge 10min with 10000r/min rotating speeds, obtain need testing solution；
1.4 take need testing solution supernatant cross 0.22 μm of syringe filter and H type pre-treatment posts after enter ion chromatography system
Analyzed, the preceding 3mL sample solutions of wherein sample will discard；
(2) configuration work curve solution, ion chromatography is carried out, the peak area of Cl- under various concentrations is obtained, with chlorion
Concentration is abscissa, using its peak area as ordinate drawing curve；Chromatographic condition in the chromatography is：Chlorion
Quasi- stock solution 1000mg/L；Leacheate is sodium carbonate and sodium acid carbonate mixed solution, flow velocity：1.0mL/min；Electric conductivity detector
Temperature：40℃；Column temperature：30℃；Suppress electric current：30mA；Sample size：20μL；Wherein,
The preparation of 2.1 standard working solutions
50 μ L Cl- Standard Stock solutions 50mL accurately are pipetted into volumetric flask, are settled to scale with secondary deionized water, are obtained
Cl- concentration is 1.0mg/L；
The preparation of 2.2 blank solutions
The accurate isopropanol for pipetting 10mL, 100mL is diluted to secondary deionized water；
The preparation of 2.3 standard working curve solution
The accurate standard liquid for pipetting the μ g/mL Cl- of 0,10,20,50,100 and 200 μ L 1.0 divides into 6 2mL sample bottles
Not Jia Ru 1000,990,980,950,900 and 800 μ L blank solution, mix, the Cl- concentration of obtained solution is respectively 0,
10th, 20,50,100 and 200 μ g/L；
The preparation of 2.4 repeated solution
It is accurate to pipette 10.0 μ L standard working solutions, 990 μ L blank solutions are added, are mixed, the Cl- for producing the μ g/L of mark-on 10 is molten
Liquid；
(3) analysis of standard liquid
It is 3.1 repeated
To repeated solution continuous sample introduction 6 times, the chromatogram of Cl- standards solution analysis is obtained, and obtain chlorion chromatographic peak
Retention time and the relative standard deviation of peak area are respectively 0.24% and 0.65%；
3.2 linear relationship
To standard working curve solution, sample introduction analysis is carried out according to the Loading sequence from low concentration to high concentration, is obtained different dense
The lower Cl- of degree peak area, using the concentration of chlorion as abscissa, using its peak area as ordinate drawing curve；
Triethyl aluminum sample solution after pre-treatment is carried out ion chromatography by 3.3, obtains Cl- peak area；
3.4, according to working curve and Cl- peak area, obtain the content of Cl- in triethyl aluminum.
2. the method as described in claim 1, it is characterised in that H type pre-treatments post must use 15mL secondary deionized waters before using
Activated, activation method is：5mL syringes are used to be rinsed with 2.0mL/min speed, the volume of flushing is 15mL,
And the secondary deionized water to finally developing is measured, if measure contains Cl-, need to continue to rinse, until
Cl- is not detected in the secondary deionized water developed.
3. the method as described in claim 1, it is characterised in that the type of the sample pre-treatments post is H posts, and its capacity is
2.5cc。
4. the method as described in claim 1, it is characterised in that the leacheate described in the ion chromatography is
1.8mmol/L sodium carbonate and the mixed solution of 1.6mmol/L sodium acid carbonates.
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| CN113063873B (en) * | 2021-03-29 | 2023-05-12 | 中国船舶重工集团公司第七二五研究所 | Method for measuring chlorine content in zirconium sponge |
| CN115166075B (en) * | 2022-06-24 | 2024-02-27 | 南大光电半导体材料有限公司 | Method for detecting chloride ion content in MO source |
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