CN109212073A - The extraction and measuring method of 4 kinds of benzotriazole ultra-violet stabilizer residual quantities in dyeing waste water - Google Patents
The extraction and measuring method of 4 kinds of benzotriazole ultra-violet stabilizer residual quantities in dyeing waste water Download PDFInfo
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- CN109212073A CN109212073A CN201811123566.8A CN201811123566A CN109212073A CN 109212073 A CN109212073 A CN 109212073A CN 201811123566 A CN201811123566 A CN 201811123566A CN 109212073 A CN109212073 A CN 109212073A
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
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Abstract
The invention discloses the extraction and measuring method of 4 kinds of benzotriazole ultra-violet stabilizer residual quantities in a kind of dyeing waste water, sample is adjusted ionic strength and pH, with C18Solid phase extraction column purification, purified sample liquid inject gas-chromatography-series connection quadrupole rod chromatography (GC-MS-MS) system, the 4 kinds of ultra-violet stabilizers wherein contained are detected under multiple-reaction monitoring pattern, qualitative confirmation, standard solution quantified by external standard method are carried out with retention time and ion comparative example.This method has that sample pre-treatments are easy quickly, good purification, and detection sensitivity is high, the characteristics of can qualitatively and quantitatively being confirmed simultaneously.
Description
Technical field
The invention belongs to technical field of environmental detection, are related to gas chromatography tandem mass spectrometry combination method, in particular to a kind of print
Contaminate the extraction and measuring method of 4 kinds of benzotriazole ultra-violet stabilizer residual quantities in waste water.
Background technique
Benzotriazole ultra-violet stabilizer (BUVSs) is that the maximum a kind of ultraviolet radiation absorption type light of consumption figure is steady in the world
Determine agent.Since it has strong absorption to the ultraviolet light of 280-400nm, it is widely used in textile, suncream, skin care
In the personal belongings such as liquid, it is furthermore also often added to plastics, construction material, car paint, furniture paint, packaging material for food
In, for preventing degradation caused by ultraviolet light irradiation or discoloration.By the textile that BUVSs is handled, human body not only can protect
Skin also can avoid ultraviolet catalyzed reaction and destroy macromolecular structure, improve fabric and fiber from the injury of excessive ultraviolet light
Sun-proof, weather-proof, ageing resistance.
Existing research shows that part BUVSs is the compound with persistence, bioconcentration and toxicity, may destroy life
The endocrine of object elutes, and has an adverse effect to the reproduction and development of organism, and may have carcinogenesis.In recent years REACH
It pays high attention in substance (SVHC) candidate list and newly incorporates ultra-violet stabilizer, but do not make clearly limitation regulation.In OEKO-
It is then distinctly claimed in TEX Standard 100 in IV grades of product level newly-increased 2- (3,5- di-t-butyl -2- hydroxy benzenes) benzos three
Azoles (UV320), 2- (3- sec-butyl -5- tert-butyl -2- hydroxy benzenes) benzotriazole (UV350), 2- (bis- tertiary pentyl -2- hydroxyl of 3,5-
Base benzene) benzotriazole (UV328), 2- (3,5- di-t-butyl -2- hydroxy benzenes) this 4 kinds of -5- chlorobenzotriazole (UV327) be " ultraviolet
Line stabilizer " test item.The test item makes index request to four kinds of substances, and provides that every kind of substance Limited Doses are 0.1%
(1000 mg/kg).
A large amount of production and use cause benzotriazole ultra-violet stabilizer living by industrial and life contaminated water discharge etc.
It moves and moves in rivers,lakes and seas.China is the production and consumption big country of textile printing and dyeing product, and dyeing is industrial wastewater row
Amplify family.It is reported that thering is 10% dyestuff and dyeing and finishing agent to be lost in dyeing process with waste water, environment is seriously polluted.Chinese Ministry of Environmental Protection
" environmental statistics annual report in 2015 " display, the waste water that dye industry discharge is knitted in China in 2015 is 18.4 hundred million tons, accounts for industrial wastewater row
The 10.1% of total amount is put, discharge amount occupies third position.GB 4287-2012 " textile dyeing and finishing industrial water pollution object discharge standard " and GB
Main indicator as defined in 8978-1996 " integrated wastewater discharge standard " is pH value, coloration, ammonia nitrogen, COD, biochemical aerobic
The conventional indexs such as amount do not provide specific discharge value to the harmful substances such as dyestuff and dyeing and finishing agent, also not formed corresponding detection side
Method.
Summary of the invention
The purpose of the invention is to overcome shortcoming and defect of the existing technology, and provide 4 kinds of purples in dyeing waste water
The gas-chromatography of outside line stabilizer-series connection quadrupole rod mass spectrometry detection method, this method combination C18Solid phase extraction column purification-
Gas chromatography tandem mass spectrometry is combined method, can be to 2- in dyeing waste water (3,5- di-t-butyl -2- hydroxy benzenes) benzotriazole
(UV320), 2- (3- sec-butyl -5- tert-butyl -2- hydroxy benzenes) benzotriazole (UV350), 2- (bis- tertiary pentyl -2- hydroxyl of 3,5-
Benzene) benzotriazole (UV328), 2- (3,5- di-t-butyl -2- hydroxy benzenes) -5- chlorobenzotriazole (UV327) be total to UV stable
Agent carries out qualitative and quantitative determination simultaneously, and accurate, quick, high sensitivity that this method has the advantages that, is 2- (3,5- bis- tertiary fourths
Base -2- hydroxy benzenes) benzotriazole (UV320), 2- (3- sec-butyl -5- tert-butyl -2- hydroxy benzenes) benzotriazole (UV350), 2-
(bis- tertiary pentyl -2- hydroxy benzenes of 3,5-) benzotriazole (UV328), 2- (3,5- di-t-butyl -2- hydroxy benzenes) -5- chlorobenzene and three
Remaining quick detection of the azoles (UV327) in dyeing waste water provides reliable analysis method.
The present invention provides in a kind of dyeing waste water the extraction and measurement side of 4 kinds of benzotriazole ultra-violet stabilizer residual quantities
Method includes the following steps, includes the following steps,
(1) preparation of sample to be tested: taking sample 25mL to be placed in centrifuge tube, is put into supercentrifuge in 10000 r/min speed
Degree is lower to be centrifuged 5 min, takes 10 mL supernatant liquors, 100 μ L of 0.5mol/L ammonium formate solution is added and adjusts ionic strength, adds
Ammonium hydroxide or formic acid adjust sample pH to 7.0-9.0, obtain liquid to be clean；
(2) purification of liquid to be clean: C is taken18Solid phase extraction column is added the liquid to be clean in 2.5mL step (1), and discards
Effluent adds 3mL water to elute pillar, discards effluent, and 5mL ethyl acetate solution is added and elutes object, collects eluent simultaneously
It is placed in 40 DEG C of water-baths with being dried with nitrogen, obtains sample to be tested after being redissolved with 0.5mL ethyl acetate；
(3) preparation of mixed standard solution: 2- (3,5- di-t-butyl -2- hydroxy benzenes) benzotriazole, 2- (3- sec-butyl-is prepared
5- tert-butyl -2- hydroxy benzenes) benzotriazole, 2- (bis- tertiary pentyl -2- hydroxy benzenes of 3,5-) benzotriazole, 2- (3,5- di-t-butyl -
2- hydroxy benzenes) four kinds of ultra-violet stabilizer mixed standard solutions of -5- chlorobenzotriazole, the mixed standard solution concentration gradient point
It Wei not 0.2 μ g/L, 2.0 μ g/L, 10 μ g/L, 50 μ g/L, 100 μ g/L；
(4) detection of sample to be tested: by the testing sample solution and 2- (3,5- di-t-butyl -2- hydroxy benzenes) in step (2)
Benzotriazole, 2- (3- sec-butyl -5- tert-butyl -2- hydroxy benzenes) benzotriazole, 2- (bis- tertiary pentyl -2- hydroxy benzenes of 3,5-) benzo
Triazole, 2- (3,5- di-t-butyl -2- hydroxy benzenes) 4 kinds of ultra-violet stabilizer hybrid working solution of -5- chlorobenzotriazole are in gas phase
Sample introduction is distinguished on chromatography-tandem mass spectrometer, is obtained with 2- in mixed standard solution (3,5- di-t-butyl -2- hydroxy benzenes) benzo three
Azoles, 2- (3- sec-butyl -5- tert-butyl -2- hydroxy benzenes) benzotriazole, 2- (bis- tertiary pentyl -2- hydroxy benzenes of 3,5-) benzotriazole,
2- (3,5- di-t-butyl -2- hydroxy benzenes) -5- chlorobenzotriazole concentration is abscissa, with 2- (3,5- in mixed standard solution
Di-t-butyl -2- hydroxy benzenes) benzotriazole, 2- (3- sec-butyl -5- tert-butyl -2- hydroxy benzenes) benzotriazole, 2- (bis- uncle of 3,5-
Amyl -2- hydroxy benzenes) benzotriazole, 2- (3,5- di-t-butyl -2- hydroxy benzenes) -5- chlorobenzotriazole quota ion pair peak
Area is the working curve of ordinate, and then recruitment composition line computation obtains 2- (3,5- di-t-butyl -2- in testing sample solution
Hydroxy benzenes) benzotriazole, 2- (3- sec-butyl -5- tert-butyl -2- hydroxy benzenes) benzotriazole, 2- (bis- tertiary pentyl -2- hydroxyl of 3,5-
Benzene) benzotriazole, the concentration of 2- (3,5- di-t-butyl -2- hydroxy benzenes) -5- chlorobenzotriazole.
It is C that the present invention, which is further arranged to the solid phase extraction column filler in the step (2),18, activation process is every
1000mg solid phase extraction column is eluted with 6mL methanol solution and 6mL level-one water in advance in advance.
It is as follows that the present invention is further arranged to the ion chromatography-tandem mass spectrometer condition:
Chromatographic column: HP-5ms, 30m × 0.25mm × 0.25 μm；
Temperature program: after keeping 1min at 60 DEG C, 200 DEG C are increased under the speed per minute for increasing 30 DEG C, then every
280 DEG C are increased under the speed of 15 DEG C of minute raising and keep 3min；
Carrier gas: high-purity helium, purity >=99.999%, flow 1.0mL/min；
Collision gas: high-purity argon gas, purity >=99.999%；
Sample volume mouth temperature: 250 DEG C；
Sample volume: 1 μ L；
Ion source: electron impact ionization source (EI), temperature: 280 DEG C；
Interface temperature: 280 DEG C；
Scan pattern: MRM mode, ion pair and collision energy are as follows:
2- (3,5- di-t-butyl -2- hydroxy benzenes) benzotriazole: 308.0m/z → 252.1m/z, collision voltage 8eV,
323.1m/z → 308.2m/z, collision voltage 10eV；2- (3- sec-butyl -5- tert-butyl -2- hydroxy benzenes) benzotriazole:
323.1m/z → 294.1m/z, collision voltage 10eV, 323.1m/z → 308.2m/z, collision voltage 10eV；2-(3,5-
Two tertiary pentyl -2- hydroxy benzenes) benzotriazole: 322.0m/z → 252.1m/z, collision voltage 8eV, 351.1m/z →
322.2m/z, collision voltage 10eV；2- (3,5- di-t-butyl -2- hydroxy benzenes) -5- chlorobenzotriazole: 342.1m/z →
286.1m/z, collision voltage 22eV, 357.1m/z → 342.1m/z, collision voltage 10eV.
The beneficial effect being arranged in this way is: using the above scheme, firstly, the present invention is molten by the way that ammonium formate is added into sample
Liquid adjust sample ions intensity, and use ammonium hydroxide or formic acid tune sample pH, raising next step Solid Phase Extraction adsorbed target object effect
Rate.Secondly, the present invention uses C18Solid phase extraction column carries out purified treatment to extracting solution, is caused with reducing sample substrate to instrument
Pollution.Again, the present invention is by gas-chromatography-string for the qualitative and quantitative detection of 4 kinds of ultra-violet stabilizers in dyeing waste water
Join spectrometer analysis, is measured using multiple-reaction monitoring pattern (MRM), obtain higher detection sensitivity.First prepare one group of ladder
4 kinds of ultra-violet stabilizer mixed standard solutions of concentration, then by mixed standard solution and it is purified after the sample solution to be tested in gas
Sample introduction is distinguished on phase chromatography-tandem mass spectrometer.The chromatographic peak retention time occurred in the sample solution to be tested is consistent with standard working solution,
Tolerance is less than ± 5 %, the relative abundance of mass spectrometry ion pair corresponding to the chromatographic peak with concentration is comparable mixes mark
The relative abundance of quasi- solution is consistent, and relative abundance deviation is no more than regulation, then can determine and contain 4 kinds of purples in the sample solution to be tested
Outside line stabilizer.
The present invention is described further with specific embodiment with reference to the accompanying drawings of the specification.
Detailed description of the invention
Fig. 1 is the MRM spectrum of 2- (3,5- di-t-butyl -2- hydroxy benzenes) benzotriazole of 1.0 μ g/L in the embodiment of the present invention
Figure；
Fig. 2 is the MRM of 2- (3- sec-butyl -5- tert-butyl -2- hydroxy benzenes) benzotriazole of 1.0 μ g/L in the embodiment of the present invention
Spectrogram；
Fig. 3 is the MRM spectrogram of 2- (bis- tertiary pentyl -2- hydroxy benzenes of 3,5-) benzotriazole of 1.0 μ g/L in the embodiment of the present invention；
Fig. 4 is the MRM of 2- (3,5- di-t-butyl -2- hydroxy benzenes) -5- chlorobenzotriazole of 1.0 μ g/L in the embodiment of the present invention
Spectrogram；
The TLC spectrogram that Fig. 5 is 4 kinds of 2.0 μ g/L of substance mark-on in dyeing waste water sample in the embodiment of the present invention；
Fig. 6 is that the TLC in the embodiment of the present invention in positive sample containing 2- (3,5- di-t-butyl -2- hydroxy benzenes) benzotriazole is composed
Figure；
Fig. 7 is the standard working curve of 2- (3,5- di-t-butyl -2- hydroxy benzenes) benzotriazole in the embodiment of the present invention；
Fig. 8 is the standard working curve of 2- (3- sec-butyl -5- tert-butyl -2- hydroxy benzenes) benzotriazole in the embodiment of the present invention；
Fig. 9 is the standard working curve of 2- (bis- tertiary pentyl -2- hydroxy benzenes of 3,5-) benzotriazole in the embodiment of the present invention；
Figure 10 is that the standard work of 2- (3,5- di-t-butyl -2- hydroxy benzenes) -5- chlorobenzotriazole in the embodiment of the present invention is bent
Line.
Specific embodiment
According to the experimental data of Fig. 1 to Figure 10 with reference to figure, wherein (1), (2), (3) and (4) respectively refers to be referred to as in Fig. 5
2- (the tertiary fourth of 3- sec-butyl -5- that 2- (3,5- di-t-butyl -2- hydroxy benzenes) benzotriazole that UV320 is, referred to as UV350 are
Base -2- hydroxy benzenes) benzotriazole, referred to as UV328 be 2- (bis- tertiary pentyl -2- hydroxy benzenes of 3,5-) benzotriazole, referred to as
UV327 is 2- (3,5- di-t-butyl -2- hydroxy benzenes) -5- chlorobenzotriazole these four ultra-violet stabilizers are in the graph
Position, wherein (1) refers to the position of UV-320 in the graph in Fig. 6, and present embodiment discloses 4 kinds of benzos three in a kind of dyeing waste water
The extraction and measuring method of azole ultra-violet stabilizer residual quantity, comprising the following steps:
(1) it the preparation of sample to be tested: takes sample about 25mL to be placed in 50 mL centrifuge tubes, is put into supercentrifuge in 10000
R/min is centrifuged 5 min, takes 10 mL of supernatant liquor, sequentially adds 100 μ L of 0.5mol/L ammonium formate solution and adjusts ionic strength, then
The pH to 7.0-9.0 that sample is adjusted with ammonium hydroxide or formic acid, obtains liquid to be clean；
(2) purification of liquid to be clean: C is taken18Solid phase extraction column is added the liquid to be clean in 2.5mL step (1), and discards
Effluent, add 3mL water elute pillar, discard effluent, add 5mL ethyl acetate solution elute object, collect eluent in
In 10mL graduated centrifuge tube, eluent is dried with nitrogen in 40 DEG C of water-baths, for gas-chromatography-after being redissolved with 0.5mL ethyl acetate
Tandem mass spectrum measurement；
(3) preparation of mixed standard solution: 2- (3,5- di-t-butyl -2- hydroxy benzenes) benzotriazole, 2- (3- sec-butyl-is prepared
5- tert-butyl -2- hydroxy benzenes) benzotriazole, 2- (bis- tertiary pentyl -2- hydroxy benzenes of 3,5-) benzotriazole, 2- (3,5- di-t-butyl -
2- hydroxy benzenes) 4 kinds of ultra-violet stabilizer mixed standard solutions of -5- chlorobenzotriazole, mixed standard solution concentration gradient difference
For 0.2 μ g/L, 1.0 μ g/L, 10 μ g/L, 50 μ g/L, 100 μ g/L；
(4) detection of testing sample solution: by the testing sample solution and 2- (3,5- di-t-butyl -2- hydroxyl in step (2)
Benzene) benzotriazole, 2- (3- sec-butyl -5- tert-butyl -2- hydroxy benzenes) benzotriazole, 2- (bis- tertiary pentyl -2- hydroxy benzenes of 3,5-)
Benzotriazole, 2- (3,5- di-t-butyl -2- hydroxy benzenes) 4 kinds of ultra-violet stabilizer hybrid working solution of -5- chlorobenzotriazole exist
Sample introduction is distinguished on gas chromatography tandem mass spectrometry instrument, is obtained with 2- in mixed standard solution (3,5- di-t-butyl -2- hydroxy benzenes) benzene
And triazole, 2- (3- sec-butyl -5- tert-butyl -2- hydroxy benzenes) benzotriazole, 2- (bis- tertiary pentyl -2- hydroxy benzenes of 3,5-) benzo three
Azoles, 2- (3,5- di-t-butyl -2- hydroxy benzenes) -5- chlorobenzotriazole concentration be abscissa, with 2- in mixed standard solution (3,
5- di-t-butyl -2- hydroxy benzenes) benzotriazole, 2- (3- sec-butyl -5- tert-butyl -2- hydroxy benzenes) benzotriazole, 2- (3,5- bis-
Tertiary pentyl -2- hydroxy benzenes) benzotriazole, 2- (3,5- di-t-butyl -2- hydroxy benzenes) -5- chlorobenzotriazole ion pair peak face
Product is the working curve of ordinate, and then recruitment composition line computation obtains 2- (3,5- di-t-butyl -2- hydroxyls in testing sample solution
Base benzene) benzotriazole, 2- (3- sec-butyl -5- tert-butyl -2- hydroxy benzenes) benzotriazole, 2- (bis- tertiary pentyl -2- hydroxyl of 3,5-
Benzene) benzotriazole, the concentration of 2- (3,5- di-t-butyl -2- hydroxy benzenes) -5- chlorobenzotriazole.
It is as shown in the table for the MRM condition of 4 kinds of ultra-violet stabilizers in the embodiment of the present invention:
*MS/MS quota ion pair
The MRM testing conditions of each compound of table 1
It is as shown in the table for the linear equation of 4 kinds of substances, related coefficient and quantitative limit in the embodiment of the present invention:
Linear equation, the related coefficient, quantitative limit of each compound of table 2
It is as shown in the table for the TIANZHU XINGNAO Capsul and precision of 4 kinds of substances in the embodiment of the present invention:
Each compound various concentration TIANZHU XINGNAO Capsul, precision (n=6) in 3 dyeing waste water of table
The present invention is not limited to above-mentioned specific embodiment, and persons skilled in the art according to the present disclosure, can
It is of the invention or all using design structure and thinking of the invention to be implemented using other a variety of specific embodiments, it does
Simple change or change, both fall within protection scope of the present invention.
Claims (3)
1. the extraction and measuring method of 4 kinds of benzotriazole ultra-violet stabilizer residual quantities, feature exist in a kind of dyeing waste water
In: include the following steps,
The preparation of step (1) sample to be tested: taking sample 25mL to be placed in centrifuge tube, is put into supercentrifuge in 10000 r/
It is centrifuged 5 min under min speed, takes 10 mL supernatant liquors, 100 μ L of 0.5mol/L ammonium formate solution is added and adjusts ionic strength, then
Ammonium hydroxide is added or formic acid adjusts sample pH to 7.0-9.0, obtains liquid to be clean；
The purification of step (2) liquid to be clean: C is taken18The liquid to be clean in 2.5mL step (1) is added in solid phase extraction column, and
Effluent is discarded, 3mL water is added to elute pillar, discards effluent, 5mL ethyl acetate solution is added and elutes object, collects elution
Liquid is placed in 40 DEG C of water-baths with being dried with nitrogen, and obtains sample to be tested after being redissolved with 0.5mL ethyl acetate；
Step (3) prepares mixed standard solution: preparing 2- (3,5- di-t-butyl -2- hydroxy benzenes) benzotriazole, 2- (3- Zhong Ding
Base -5- tert-butyl -2- hydroxy benzenes) benzotriazole, 2- (bis- tertiary pentyl -2- hydroxy benzenes of 3,5-) benzotriazole, 2- (the tertiary fourth of 3,5- bis-
Base -2- hydroxy benzenes) four kinds of ultra-violet stabilizer mixed standard solutions of -5- chlorobenzotriazole, the mixed standard solution concentration gradient
Respectively 0.2 μ g/L, 2.0 μ g/L, 10 μ g/L, 50 μ g/L, 100 μ g/L；
The detection of step (4) sample to be tested: by the testing sample solution and 2- (3,5- di-t-butyl -2- hydroxyl in step (2)
Benzene) benzotriazole, 2- (3- sec-butyl -5- tert-butyl -2- hydroxy benzenes) benzotriazole, 2- (bis- tertiary pentyl -2- hydroxy benzenes of 3,5-)
Benzotriazole, 2- (3,5- di-t-butyl -2- hydroxy benzenes) 4 kinds of ultra-violet stabilizer hybrid working solution of -5- chlorobenzotriazole exist
Sample introduction is distinguished on gas chromatography tandem mass spectrometry instrument, is obtained with 2- in mixed standard solution (3,5- di-t-butyl -2- hydroxy benzenes) benzene
And triazole, 2- (3- sec-butyl -5- tert-butyl -2- hydroxy benzenes) benzotriazole, 2- (bis- tertiary pentyl -2- hydroxy benzenes of 3,5-) benzo three
Azoles, 2- (3,5- di-t-butyl -2- hydroxy benzenes) -5- chlorobenzotriazole concentration be abscissa, with 2- in mixed standard solution (3,
5- di-t-butyl -2- hydroxy benzenes) benzotriazole, 2- (3- sec-butyl -5- tert-butyl -2- hydroxy benzenes) benzotriazole, 2- (3,5- bis-
Tertiary pentyl -2- hydroxy benzenes) benzotriazole, 2- (3,5- di-t-butyl -2- hydroxy benzenes) -5- chlorobenzotriazole quota ion pair
Peak area is the working curve of ordinate, and then recruitment composition line computation obtains 2- (3,5- di-t-butyls-in testing sample solution
2- hydroxy benzenes) benzotriazole, 2- (3- sec-butyl -5- tert-butyl -2- hydroxy benzenes) benzotriazole, 2- (bis- tertiary pentyl -2- hydroxyl of 3,5-
Base benzene) benzotriazole, the concentration of 2- (3,5- di-t-butyl -2- hydroxy benzenes) -5- chlorobenzotriazole.
2. the extraction and survey of 4 kinds of benzotriazole ultra-violet stabilizer residual quantities in dyeing waste water according to claim 1
Determine method, it is characterised in that: the solid phase extraction column filler in the step (2) is C18, activation process is solid for every 1000mg
Mutually extraction pillar is eluted with 6mL methanol solution and 6mL level-one water in advance in advance.
3. in dyeing waste water according to claim 1 or 2 the extraction of 4 kinds of benzotriazole ultra-violet stabilizer residual quantities and
Measuring method, it is characterised in that: the ion chromatography-tandem mass spectrometer condition is as follows:
Chromatographic column: HP-5ms, 30m × 0.25mm × 0.25 μm；
Temperature program: after keeping 1min at 60 DEG C, 200 DEG C are increased under the speed per minute for increasing 30 DEG C, then every
280 DEG C are increased under the speed of 15 DEG C of minute raising and keep 3min；
Carrier gas: high-purity helium, purity >=99.999%, flow 1.0mL/min；
Collision gas: high-purity argon gas, purity >=99.999%；
Sample volume mouth temperature: 250 DEG C；
Sample volume: 1 μ L；
Ion source: electron impact ionization source (EI), temperature: 280 DEG C；
Interface temperature: 280 DEG C；
Scan pattern: MRM mode, ion pair and collision energy are as follows:
2- (3,5- di-t-butyl -2- hydroxy benzenes) benzotriazole: 308.0m/z → 252.1m/z, collision voltage 8eV,
323.1m/z → 308.2m/z, collision voltage 10eV；2- (3- sec-butyl -5- tert-butyl -2- hydroxy benzenes) benzotriazole:
323.1m/z → 294.1m/z, collision voltage 10eV, 323.1m/z → 308.2m/z, collision voltage 10eV；2-(3,5-
Two tertiary pentyl -2- hydroxy benzenes) benzotriazole: 322.0m/z → 252.1m/z, collision voltage 8eV, 351.1m/z →
322.2m/z, collision voltage 10eV；2- (3,5- di-t-butyl -2- hydroxy benzenes) -5- chlorobenzotriazole: 342.1m/z →
286.1m/z, collision voltage 22eV, 357.1m/z → 342.1m/z, collision voltage 10eV.
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| CN109870520A (en) * | 2019-03-15 | 2019-06-11 | 广州纤维产品检测研究院 | A kind of method that ultra high efficiency closes phase chromatography measurement benzotriazole UV stabilizer |
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