CN109001366A - Ion chromatography-post-column derivation method measures the System and method for of trivalent chromium and content of 6-valence Cr ions simultaneously - Google Patents
Ion chromatography-post-column derivation method measures the System and method for of trivalent chromium and content of 6-valence Cr ions simultaneously Download PDFInfo
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Abstract
The invention discloses the System and method fors that a kind of ion chromatography-post-column derivation method measures trivalent chromium and content of 6-valence Cr ions simultaneously, should including sample flow path, leacheate flow path, post-column derivation liquid stream road, analysis flow path, sampling valve, injection annulus, UV-vis detector and computer processing system, the analysis flow path by cation-exchange chromatography column, triple valve, braiding reaction tube, optical flow cell be sequentially connected in series.The method of the present invention tests trivalent chromium and content of 6-valence Cr ions using IC-UV-Vis method simultaneously, this method has application in water quality detection, and existing research person is low with trivalent chromium and Cr VI, detection limit in Simultaneous Determination drinking water, the favorable reproducibility of method, high sensitivity.Since trivalent chromium and Cr VI need first to extract re-test in toy material, the leach extraction method in EN71-3 is continued to use in this research, after leaching liquor is handled, optimizes chromatographic condition, then the content of three prices and Cr VI in leaching liquor is tested, it is this method high sensitivity, reproducible.
Description
Technical field
The present invention relates to the technical fields of trivalent chromium and content of 6-valence Cr ions measurement, after a kind of ion chromatography-column
Derivatization method measures the System and method for of trivalent chromium and content of 6-valence Cr ions simultaneously.
Background technique
Due to the particularity of toy for children, the toy of especially less than three years old children, frequently with the body of children and face
Location contacts, if any the exceeded situation of content of beary metal, Long Term Contact, which gets off, to damage children.Cr VI is very
It is easy to be absorbed by the body, it can invade human body by digestion, respiratory tract, skin and mucous membrane, and intake be potentially carcinogenic, there is environment
Lasting risk.Each department toy product regulation has Cr VI stringent limitation requirement.Although trivalent chromium is to human body poison
Property is relatively low, but trivalent chromium and Cr VI can mutually convert under certain condition, so the content of trivalent chromium is in toy
Also it is taken seriously.
On July 20th, 2013, new edition " instruction of European Union's toy safety " EN71-3:2013 chemical part start formally to implement.
The instruction not only proposes strict demand to the machinery of toy, physical property, chemical property；Limitation to heavy metal element
Increase to 19 kinds by original 8 kinds, original total chromium is divided into trivalent chromium and Cr VI, and lowered each element the amount of migration
Limited Doses；Wherein the Limited Doses of trivalent chromium and Cr VI are even more lower than most of sexavalences well below the requirement of old edition this standard
The detection limit of chromium content detection method.The test method that new edition regulation is recommended at present is ICP-AES method and LC-ICP-MS method,
ICP-AES method can satisfy the test request of most elements in regulation, but but test cannot be distinguished not in ICP-AES method
With the trivalent chromium and Cr VI the amount of migration of valence state, and the Limited Doses of Cr VI are lower, and the detection limit of ICP-AES method can not also expire
Foot requires.LC-ICP-MS method can carry out separation test to trivalent chromium and Cr VI, and measuring accuracy also meets test request,
But equipment cost is costly, in vitro popularity rate is lower, and test method is unfavorable for popularizing.
Summary of the invention
The purpose of the present invention is to solve the deficiency of the above background technology, and provides that a kind of detection accuracy is high, at sample
It manages quick and easy ion chromatography-post-column derivation method while measuring the System and method for of trivalent chromium and content of 6-valence Cr ions.
To achieve the above object, ion chromatography provided by the present invention-post-column derivation method measures trivalent chromium and sexavalence simultaneously
The system of chromium content, including sample flow path, leacheate flow path, post-column derivation liquid stream road, analysis flow path, sampling valve, injection annulus, purple
Outer visible detection device and computer processing system, it is described analysis flow path by cation-exchange chromatography column, triple valve, braiding react
Pipe, optical flow cell are sequentially connected in series.
The present invention also provides the sides that a kind of ion chromatography-post-column derivation method measures trivalent chromium and content of 6-valence Cr ions simultaneously
Method includes the following steps:
1) sample is protected from light mechanical shaking extraction 0.5~1.5 hour under the conditions of 37 DEG C with simulate the gastric juice, extracting solution is filtered
Afterwards, column front derivation liquid is added, boiling water bath 3~6 minutes, trivalent chromium in extracting solution is made to react generation trivalent chromium network with column front derivation liquid
Object is closed, reaction solution to be measured is obtained；
2) analysis instrument is arranged in sample introduction state, leacheate is made to enter analysis flow path through leacheate flow path, sampling valve；Column
Derive liquid afterwards and enters analysis flow path through post-column derivation liquid stream road, triple valve, the leacheate in the braiding reaction tube in analysis flow path
It is mixed to form mixed liquor with post-column derivation liquid phase, the mixed liquor enters optical flow cell, through UV-vis detector by signal
Obtain baseline after being transferred to computer system processor, baseline mapping while, reaction solution to be measured through sample flow path, sampling valve into
Enter injection annulus and is full of injection annulus；
3) analysis instrument is converted into analysis state, under the promotion of leacheate, the reaction solution to be measured in injection annulus is sent
Enter the cation-exchange chromatography column analyzed in flow path, contained trivalent chromium complex and Cr VI are handed in cation in reaction solution to be measured
It changes chromatographic column to be separated, Cr VI and trivalent chromium complex are successively flowed out from chromatographic column under the action of leacheate, and are spread out after column
Raw liquid mixes in triple valve, and the reaction in braiding reaction tube of Cr VI and post-column derivation liquid generates sexavalence chromium complex, sexavalence
Chromium complex and trivalent chromium complex sequentially enter optical flow cell, measure absorbance value respectively through UV-vis detector and incite somebody to action
Signal is transferred to computer system processor and obtains the spectrogram of Cr VI and trivalent chromium；
4) sample is replaced using the trivalent chromium of known concentration and Cr VI standard specimen, repeated the above steps 1) to 3) respectively obtaining
Corresponding standard specimen spectrogram using the concentration of standard specimen as abscissa, draws working curve by ordinate of the peak height of standard specimen spectrogram；
5) by the sample spectrogram drawn compared with standard specimen spectrogram, pass through the regression equation calculation of the standard specimen working curve
Trivalent chromium and content of 6-valence Cr ions in sample out.
Further, the molar concentration of HCl is 0.05~0.08mol/L in the simulate the gastric juice.
Preferably, the molar concentration of HCl is 0.07mol/L in the simulate the gastric juice.
Further, the formula of the column front derivation liquid is as follows: 2,6- 15~25mmol/L of pyridinedicarboxylic acid, phosphoric acid hydrogen two
15~25mmol/L of sodium, 80~120mmol/L of potassium iodide, 450~550mmol/L of ammonium acetate, 25~30mmol/L of sodium hydroxide.
Preferably, the formula of the column front derivation liquid is as follows: 2,6- pyridinedicarboxylic acid 20mmol/L, disodium hydrogen phosphate
20mmol/L, potassium iodide 100mmol/L, ammonium acetate 500mmol/L, sodium hydroxide 30mmol/L.
Further, the formula of the leacheate is as follows: 2,6- 1.5~2.5mmol/L of pyridinedicarboxylic acid, disodium hydrogen phosphate
1.5~2.5mmol/L, 8~12mmol/L of potassium iodide, 45~55mmol/L of ammonium acetate, 2.5~3mmol/L of sodium hydroxide.
Preferably, the formula of the leacheate is as follows: 2,6- pyridinedicarboxylic acid 2mmol/L, disodium hydrogen phosphate 2mmol/L,
Potassium iodide 10mmol/L, ammonium acetate 50mmol/L, sodium hydroxide 3mmol/L.
Further, the formula of the post-column derivation liquid is as follows: 1,5- diphenylcarbazide 1.5-2.5mmol/L, methanol
8-12% (v/v), sulfuric acid 2-3% (v/v).
Further, the ion chromatography test condition is as follows: chromatographic column be IonPac CS5A analytical column (250mm ×
4mm) with IonPac CG5A guard column (50mm × 4mm)；Elution flow velocity is 1.0~2.0ml/min；Post-column derivation flow velocity
For 0.4~0.5ml/min, sample volume is 250~260uL.
Further, the Detection wavelength of trivalent chromium is 365nm；The Detection wavelength of Cr VI is 530nm.
Compared with prior art, the present invention has the advantage that
First, the method for the present invention tests trivalent chromium and content of 6-valence Cr ions simultaneously using IC-UV-Vis method, this method is in water quality
Having application in detection, for existing research person with trivalent chromium and Cr VI in Simultaneous Determination drinking water, detection limit is low,
The favorable reproducibility of method, high sensitivity.Since trivalent chromium and Cr VI need first to extract re-test, this research edge in toy material
With the leach extraction method in EN71-3, after leaching liquor is handled, optimizes chromatographic condition, then test three prices and sexavalence in leaching liquor
The content of chromium, this method high sensitivity is reproducible, can satisfy the test request of EN71-3.
Second, being extracted using simulate the gastric juice to trivalent chromium in toy material and Cr VI in this method, by extracting solution
With 2,6- pyridinedicarboxylic acid solution hybrid reaction, trivalent chromic ion therein and 2,6- pyridinedicarboxylic acid generates complex compound, then
By cation-exchange chromatography column, separated using Cr VI and trivalent chromium complex affinity different from chromatographic column；
Generation complexing is reacted in braiding reaction tube with Cr VI with the post-column derivation liquid of the diphenylcarbazide containing 1,5- after chromatographic column
Object；The trivalent chromium complex and sexavalence chromium complex of generation have absorption maximum at 365nm and 530nm wavelength respectively, and use is ultraviolet
Visible detection device is switched under 365nm and 530nm wavelength by wavelength and measures trivalent chromium and sexavalence according to the difference of absorbance
The content of chromium.
Detailed description of the invention
Fig. 1 is structural schematic diagram of the analysis instrument of the present invention in sample introduction state；
Fig. 2 is structural schematic diagram of the analysis instrument of the present invention in the state of analysis；
Fig. 3 is the calibration curve of Cr of the present invention (III)；
Fig. 4 is the calibration curve of Cr of the present invention (VI).
Specific embodiment
The present invention is described in further detail combined with specific embodiments below.
The system that ion chromatography of the present invention-post-column derivation method measures trivalent chromium and content of 6-valence Cr ions simultaneously, including sample flow
Road A, leacheate flow path B, post-column derivation liquid stream road C, analysis flow path, sampling valve 1, injection annulus 2, UV-vis detector 4 and meter
The analysis instrument of calculation machine processing system 3, the analysis flow path is by the cation-exchange chromatography column 5, the triple valve that are sequentially connected in series
6, reaction tube 7, the composition of optical flow cell 8 are woven, Fig. 1 is detailed in.
The method that ion chromatography of the present invention-post-column derivation method measures trivalent chromium and content of 6-valence Cr ions simultaneously, its step are as follows:
1) sample is protected from light mechanical shaking extraction 1 hour under the conditions of 37 DEG C with the simulate the gastric juice for being equivalent to 50 times of sample quality,
After extracting solution is filtered, the column front derivation liquid for containing 2,6- pyridinedicarboxylic acid is added, boiling water bath 5 minutes, makes trivalent in extracting solution
Chromium and 2, the reaction of 6- pyridinedicarboxylic acid generate trivalent chromium complex, obtain reaction solution to be measured；
2) analysis instrument is arranged at sample introduction state (Fig. 1), leacheate is made to enter analysis through eluent flow path B, sampling valve 1
Flow path；Post-column derivation liquid enters analysis flow path through post-column derivation liquid stream road C, triple valve 6, in the braiding reaction tube of analysis flow path
(7) leacheate and post-column derivation liquid phase are mixed to form mixed liquor in, and the mixed liquor enters optical flow cell 8, through UV, visible light
Detector 4 transmits a signal to after computer system 3 is handled and obtains baseline, and while baseline mapping, reaction solution to be measured is through sample
Product flow path A, sampling valve 1 enter injection annulus 2 and are full of injection annulus；
3) analysis instrument is converted into analysis state (such as Fig. 2), it is to be measured anti-in injection annulus 2 under the promotion of leacheate
Liquid is answered to be admitted to the cation-exchange chromatography column 5 in analysis flow path, contained trivalent chromium complex and Cr VI in reaction solution to be measured
It is separated in cation-exchange chromatography column 5, Cr VI and trivalent chromium complex are successively handed over from cation under the action of leacheate
The outflow of chromatographic column 5 is changed, is mixed in triple valve 6 with post-column derivation liquid, 1, the 5- hexichol phosphinylidyne in Cr VI and post-column derivation liquid
The reaction in braiding reaction tube 7 of two hydrazines generates sexavalence chromium complex, and sexavalence chromium complex and trivalent chromium complex sequentially enter light
Flow cell 8 is learned, measures absorbance value at 365nm and 530nm wavelength respectively through UV-vis detector 4, and signal is transmitted
The spectrogram of Cr VI and trivalent chromium is obtained to the processing of computer system 3；
4) sample is replaced using a series of standard specimen known to trivalent chromiums and hexavalent chromium concentration, repeated the above steps 1) to 3),
Corresponding standard specimen spectrogram is respectively obtained, using the concentration of standard specimen as abscissa, draws work by ordinate of the peak height of standard specimen spectrogram
Curve；
5) by the sample spectrogram drawn compared with standard specimen spectrogram, pass through the regression equation calculation of the standard specimen working curve
Trivalent chromium and content of 6-valence Cr ions in sample out.
The formula of each solution and the preparation method is as follows:
(1) preparation of standard serial solution
Take standard solution (10mg/L containing trivalent chromium, Cr VI 0.1mg/L) 0.025ml, 0.125ml, 0.25ml,
0.50ml, 1.25ml are respectively placed in 25ml colorimetric cylinder, are settled to scale with the sodium chloride solution of 0.07mol/L, obtain standard system
Column solution.The standard serial solution concentration is shown in Table 1.
1 concentration of standard solution ug/L of table
(2) preparation of simulate the gastric juice
5.8mL hydrochloric acid solution accurately is pipetted, is settled to 1000mL with second level water, concentration of hydrochloric acid is 0.07mol/ in the solution
L。
(3) column front derivation liquid is prepared
Accurately weigh 2,6- pyridinedicarboxylic acid 3.34g, disodium hydrogen phosphate dodecahydrate 7.16g, potassium iodide 16.6g, acetic acid
Ammonium 38.54g, sodium hydroxide 1.20g, are placed in 1000ml volumetric flask, dilute constant volume with ultrapure water, which is leacheate deposit
Liquid is also used as column front derivation liquid, is added in extracting solution and reacts generation trivalent chromium complex with trivalent chromium.
(4) leacheate is prepared
The leacheate stock solution 100ml of above-mentioned steps (3) preparation is accurately pipetted in 1000ml volumetric flask, is diluted with ultrapure water
To scale, solution pH value is adjusted to 6.8 with 2mol/L sodium hydroxide solution, which is that leacheate uses liquid, with 0.22um's
It is used after film filtering, each material concentration is shown in Table 2.
2 eluent concentration of table
(5) post-column derivation liquid is prepared
It accurately weighs 1,5- diphenylcarbazide 0.48g and is dissolved in 100ml methanol, 25ml is added in about 500ml ultrapure water
The concentrated sulfuric acid, above-mentioned solution is mixed, and is settled to 1000ml with ultrapure water, is used after being filtered with the film of 0.22um.
(6) calibration solution measurement
It pipettes in standard solution 20mL to 25mL colorimetric cylinder, 2.5mL leacheate stock solution is added, is settled to quarter with pure water
Degree, heating is boiled 2min, is measured after cooling, and using peak area as ordinate, concentration of standard solution is that abscissa draws standard work
Curve.
(7) sample extraction
Sample 0.5g (being accurate to 0.0001g) is weighed, 25mL simulate the gastric juice and sample mixed is uniform, in 37 DEG C of water-bath
Under the conditions of be protected from light oscillation 1 hour, after being then allowed to stand 1 hour, extracting solution crosses the filter membrane of 0.22um, avoid light place.
(8) sample column front derivation
20ml extracting solution accurately is pipetted in 25ml colorimetric cylinder, 2.5ml column front derivation liquid is added, with 1mol/L sodium hydroxide
Solution adjusts pH to 6.8 ± 0.1, is then settled to scale with ultrapure water, boiling water bath 5min is cooling, to be measured.
(9) blank test
In addition to sample is not added, carried out according to step (5)-(7), for eliminating the sound because of impurity and instrument in water, reagent
Answer error.
(10) ion chromatography condition
In order to determine Detection wavelength, using ultraviolet-uisible spectrophotometer respectively to after derivative trivalent chromium and Cr VI into
Traveling wave long scan, the results showed that, the trivalent chromium after deriving has maximum absorption band at 365nm, and Cr VI then has at 530nm
Absorption maximum, it is thus determined that the Detection wavelength of trivalent chromium and Cr VI is respectively 365nm and 530nm. in experiment
A) chromatographic column: IonPac CS5A analytical column (250mm × 4mm) and IonPac CG5A guard column (50mm × 4mm)；
B) leacheate: solution pyridinedicarboxylic acid containing 2,6- 2mmol/L, disodium hydrogen phosphate 2mmol/L, potassium iodide 10mmol/
L, ammonium acetate 50mmol/L, sodium hydroxide 2.8mmol/L, isocratic elution；；
C) flow velocity: 1.0ml/min is eluted；
D) post-column derivation reagent: solution diphenylcarbazide containing 1,5- 2mmol/L, methanol 10% (v/v), sulfuric acid 2.5%
(v/v)；
E) post-column derivation flow velocity: 0.4ml/min；
F) sample volume: 250uL；
G) Detection wavelength: 0-5.0min, 365nm；5.0-8.0min, 530nm；
(11) in sample the content of trivalent chromium and Cr VI calculating, according to following formula calculate sample in trivalent chromium and six
The content of valence chromium:
In formula:
wi--- the content of trivalent chromium or Cr VI, mg/kg in sample；
ci--- trivalent chromium or hexavalent chromium concentration, mg/L in extracting solution；
c0i--- the concentration of trivalent chromium or Cr VI, mg/L in blank sample extracting solution；
M --- sample mass, g；
V --- the final constant volume of sample, mL.
The analysis method of trivalent chromium and Cr VI in toy material of the present invention, the range of linearity of trivalent chromium are 10-
500 μ g/L, detection are limited to 8.7mg/L (N/S=3), and relative standard deviation (RSD) is 1.32% (n=7)；Cr VI it is linear
Range is 0.1-5.0 μ g/L, and detection is limited to 0.1mg/L (N/S=3), and relative standard deviation (RSD) is 2.17% (n=7).
(12) test result
Using measuring method of the invention, 10 toy fittings of unlike material, including plastics, paper, cloth, painting are chosen
The standard substance of various concentration level is added in layer in the sample, tests recovery of standard addition, calibration curve and rate of recovery test result
See Fig. 3, Fig. 4 and table 3, sample test recovery of standard addition meets toy material trivalent chromium and Cr VI within the scope of 90-110%
The testing requirements of content.
The test of 3 sample recovery rate of table
The above description is merely a specific embodiment, it is noted that anyone skilled in the art exists
Disclosed herein technical scope in, any changes or substitutions that can be easily thought of, should all cover protection scope of the present invention it
It is interior.
Claims (10)
1. the system that a kind of ion chromatography-post-column derivation method measures trivalent chromium and content of 6-valence Cr ions simultaneously, it is characterised in that: including
It is sample flow path (A), leacheate flow path (B), post-column derivation liquid stream road (C), analysis flow path, sampling valve (1), injection annulus (2), ultraviolet
Visible detection device (4) and computer processing system (3), it is described analysis flow path by cation-exchange chromatography column (5), triple valve
(6), reaction tube (7) are woven, optical flow cell (8) is sequentially connected in series.
2. it is a kind of measure trivalent chromium and content of 6-valence Cr ions simultaneously using ion chromatography described in claim 1-post-column derivation method be
The method that system is measured, which comprises the steps of:
1) sample is protected from light mechanical shaking extraction 0.5~1.5 hour under the conditions of 37 DEG C with simulate the gastric juice, after extracting solution is filtered, added
Enter column front derivation liquid, boiling water bath 3~6 minutes, trivalent chromium in extracting solution made to react generation trivalent chromium complex with column front derivation liquid,
Obtain reaction solution to be measured；
2) analysis instrument is arranged in sample introduction state, leacheate is made to enter analysis flow path through leacheate flow path (B), sampling valve (1)；
Post-column derivation liquid enters analysis flow path through post-column derivation liquid stream road (C), triple valve (6), in the braiding reaction tube (7) of analysis flow path
Middle leacheate and post-column derivation liquid phase are mixed to form mixed liquor, and the mixed liquor enters optical flow cell (8), examines through UV, visible light
It surveys after device (4) transmit a signal to computer system (3) processing and obtains baseline, while baseline mapping, reaction solution warp to be measured
Sample flow path (A), sampling valve (1) enter injection annulus (2) and are full of injection annulus；
3) analysis instrument is converted into analysis state, under the promotion of leacheate, the reaction solution to be measured in injection annulus (2) is admitted to
The cation-exchange chromatography column (5) in flow path is analyzed, contained trivalent chromium complex and Cr VI are in cation in reaction solution to be measured
Exchange chromatography column (5) is separated, and Cr VI and trivalent chromium complex are under the action of leacheate successively from cation-exchange chromatography
Column (5) outflow mixes in triple valve (6) with post-column derivation liquid, and Cr VI and post-column derivation liquid are anti-in braiding reaction tube (7)
Sexavalence chromium complex should be generated, sexavalence chromium complex and trivalent chromium complex sequentially enter optical flow cell (8), through UV, visible light
Detector (9), which measures absorbance value respectively and transmits a signal to computer system (3) processing, obtains Cr VI and trivalent chromium
Spectrogram；
4) sample is replaced using the trivalent chromium of known concentration and Cr VI standard specimen, repeated the above steps 1) corresponding to 3) respectively obtaining
Standard specimen spectrogram, using the concentration of standard specimen as abscissa, by ordinate of the peak height of standard specimen spectrogram draw working curve；
5) by the sample spectrogram drawn compared with standard specimen spectrogram, go out to try by the regression equation calculation of the standard specimen working curve
Trivalent chromium and content of 6-valence Cr ions in sample.
3. according to the method described in claim 2, it is characterized in that, in the simulate the gastric juice HCl molar concentration be 0.05~
0.08mol/L。
4. according to the method described in claim 2, it is characterized in that, the formula of the column front derivation liquid is as follows: 2,6- pyridines two
15~25mmol/L of formic acid, 15~25mmol/L of disodium hydrogen phosphate, 80~120mmol/L of potassium iodide, ammonium acetate 450~
550mmol/L, 25~30mmol/L of sodium hydroxide.
5. according to the method described in claim 4, it is characterized in that, the formula of the column front derivation liquid is as follows: 2,6- pyridines two
Formic acid 20mmol/L, disodium hydrogen phosphate 20mmol/L, potassium iodide 100mmol/L, ammonium acetate 500mmol/L, sodium hydroxide
30mmol/L。
6. according to the method described in claim 2, it is characterized in that, the formula of the leacheate is as follows: 2,6- pyridinedicarboxylic acids
1.5~2.5mmol/L, 1.5~2.5mmol/L of disodium hydrogen phosphate, 8~12mmol/L of potassium iodide, 45~55mmol/L of ammonium acetate,
2.5~3mmol/L of sodium hydroxide.
7. according to the method described in claim 6, it is characterized in that, the formula of the leacheate is as follows: 2,6- pyridinedicarboxylic acids
2mmol/L, disodium hydrogen phosphate 2mmol/L, potassium iodide 10mmol/L, ammonium acetate 50mmol/L, sodium hydroxide 3mmol/L.
8. according to the method described in claim 2, it is characterized in that, the formula of the post-column derivation liquid is as follows: 1,5- hexichol carbon
Two hydrazine 1.5-2.5mmol/L of acyl, methanol 8-12% (v/v), sulfuric acid 2-3% (v/v).
9. according to the method described in claim 2, it is characterized in that, the ion chromatography test condition is as follows: chromatographic column is
IonPac CS5A analytical column (250mm × 4mm) and IonPac CG5A guard column (50mm × 4mm)；Elute flow velocity be 1.0~
2.0ml/min；Post-column derivation flow velocity is 0.4~0.5ml/min, and sample volume is 250~260uL.
10. according to the method described in claim 2, it is characterized in that, the Detection wavelength of trivalent chromium is 365nm；The prison of Cr VI
Survey wavelength is 530nm.
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| CN109655548A (en) * | 2019-01-22 | 2019-04-19 | 南开大学 | A kind of high efficiency extraction and rapid assay methods of soil inorganic iodine form |
| CN111157650A (en) * | 2020-01-07 | 2020-05-15 | 中国电子技术标准化研究院 | Ion chromatography detection method for hexavalent chromium content in polymer material of electronic and electrical product |
| CN114247398A (en) * | 2021-12-17 | 2022-03-29 | 沈磊 | Lipid nanoparticle preparation system and equipment |
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