CN103604899A - Method for detecting n-propyl bromide in leather and textiles - Google Patents
Method for detecting n-propyl bromide in leather and textiles Download PDFInfo
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Abstract
The invention discloses a method for detecting n-propyl bromide in leather and textiles. The method is characterized in that the gas chromatography-mass spectrometry combination is used for detection. The detection method is simple, convenient and fast and has high sensitivity. A sample to be detected is in the linear relationship in the range of 0.1-50mg/L, the correlation coefficient is 0.9995, the method detection limit is 0.1mg/L, the standard recovery rate is 96%-112%, and the relative standard deviation (RSD) (n is equal to 7) is less than 2%. The method can be used for detecting the n-propyl bromide in the leather and textiles very well.
Description
Technical field
The present invention relates to field of chemical detection, particularly relate to the detection method of n-propyl bromide in a kind of leather, textile.
Background technology
54 the new SVHC candidate substances of official confirmation that give out information in Qi official website of in Dec, 2012 17， EU chemicals management board (ECHA), SVHC candidate substances will be increased to 138.
54 new SVHC materials that n-propyl bromide (1-Bromopropane) is confirmed as the 8th crowd of REACH, have another name called propyl bromide (Propylbromide), are colourless liquid, by hydrogen bromide and propyl alcohol, through catalyzing and synthesizing, are obtained.N-propyl bromide main application has at present: as the solvent of fat, paraffin, resin etc.; Manufacture the intermediate of medicine, pesticide, essence, flavoring etc.; The clean-out system of precision electronic device; Solvent in detergent and spray adhesive etc.
Studies show that, n-propyl bromide all has toxicity to nervous system, reproductive system and liver etc., wherein obvious with neurotoxicity.Poisoner's main manifestations is the neurotoxicity symptoms such as numbness of lower limbs, difficulty in walking, seismesthesia decline, pathologic reflex, cacesthesia.N-propyl bromide is also irritant to skin and eye.Now determined that n-propyl bromide has carcinogenic, mutagenicity.
For the detection of n-propyl bromide, being limited at present the detection of air and water, is mainly Headspace-Gas Chromatography Analysis, but not yet has at present in the world also less than unified standard and method for the detection of textile and leather and fur products n-propyl bromide.
Summary of the invention
Based on this, be necessary for the problems referred to above, the detection method of n-propyl bromide in a kind of leather, textile is provided.The inventive method adopts methyl alcohol to carry out ultrasonic extraction to the n-propyl bromide in textile and leather and fur products, with gas chromatograph-mass spectrometer, detects, and has set up a kind of pre-treatment effectively and rapidly and analysis and testing technology, for formulating corresponding standard, provides reliable foundation.
For realizing above-mentioned technical purpose, concrete technical scheme is as follows:
A detection method for n-propyl bromide in leather, textile, adopts gas chromatography-mass spectrography to detect, and comprises following steps:
A, sample pre-treatments:
Accurately take pretreated sample 0.5～2.0g(and be accurate to 0.0001g), be placed in 20～60mL glass reaction bottle, add organic solvent, ultrasonic extraction 55-65min, be cooled to after room temperature, the PTFE filtering with microporous membrane of 0.45 μ m for extract, getting filtrate is testing sample;
B, testing sample is carried out to gas chromatography-mass spectrography detection, GC conditions is: chromatographic column: Rxi-624sil MS; Column temperature condition: 40～60 ℃ of initial temperature, keep 1～3min, then the speed with 15～25 ℃/min rises to 180～250 ℃, keeps 1～2min; Injector temperature: 250～280 ℃; Input mode: split sampling, split ratio: 5:1; Sample size: 1 μ L; Carrier gas: high-pure helium, purity >99.999%, flow: 1～2ml/min;
Mass spectrum condition is as follows: ionization mode: electron impact ionization, electron energy 70eV; Ion source temperature: 230 ℃; Chromatography-mass spectroscopy interface temperature: 260 ℃; Solvent delay: 2～4min; Drainage pattern: full ion scan is qualitative, selects ion scan quantitative.
In some embodiment, in described steps A, ultrasonic extraction time is 60min therein; Described organic solvent is methyl alcohol.
In some embodiment, in described steps A, sample pretreatment is for being cut into described sample 5mm * 5mm size therein.
In some embodiment, accurately take pretreated sample 1.0g in described steps A therein, be placed in 60mL glass reaction bottle, described organic solvent is methyl alcohol, and addition is 10mL.
In some embodiment, the GC conditions in described step B is: chromatographic column: Rxi-624silMS therein; Column temperature condition: 50 ℃ of initial temperature, keep 2min, then the speed with 20 ℃/min rises to 200 ℃, keeps 1min; Injector temperature: 250 ℃; Input mode: split sampling, split ratio: 5:1; Sample size: 1 μ L; Carrier gas: high-pure helium, purity >99.999%, flow: 2ml/min;
Mass spectrum condition is as follows: ionization mode: electron impact ionization, electron energy 70eV; Ion source temperature: 230 ℃; Chromatography-mass spectroscopy interface temperature: 260 ℃; Solvent delay: 3min; Drainage pattern: full ion scan is qualitative, selects ion scan quantitative.
In some embodiment, the specifications parameter of the chromatographic column in described step B is 60m * 0.32mm * 1.8 μ m therein.
In some embodiment, in described leather, textile, detecting of the detection method of n-propyl bromide is limited to 0.1mg/L therein.
Therein in some embodiment, the relative standard deviation < 2% of the detection method of n-propyl bromide in described leather, textile.
In some embodiment, in described leather, textile, the recovery of standard addition of the detection method of n-propyl bromide is 96%～112% therein.
The present invention with respect to advantage and the beneficial effect of prior art is:
Detection method of the present invention is usingd methyl alcohol as extracting solvent, n-propyl bromide in ultrasonic extraction textile and leather and fur products, by chromatographic column type is selected, and extraction conditions is optimized and has carried out the experiments such as linearity, the recovery, precision, set up gas chromatography mass spectrometry detection method of the present invention.The present inventor is by a large amount of experiments and research, the sample pre-treatments mode of more optimizing (as adopted methyl alcohol, ultrasonic extraction time is 55-65min) and testing conditions (as adopted Rxi-624sil MS(60m * 0.32mm * 1.8 μ m) chromatographic column have been determined).
Detection method of the present invention is simple and efficient, highly sensitive, linear within the scope of 0.1～50mg/L, related coefficient is 0.9995, method detects and is limited to 0.1mg/L, recovery of standard addition is 96%～112%, relative standard deviation RSD (n=7) is less than 2%, can be good at being applied to the detection of n-propyl bromide in textile and leather.
Accompanying drawing explanation
Fig. 1 is the chromatogram of n-propyl bromide in embodiment, and wherein horizontal ordinate is retention time, and ordinate is signal intensity;
Fig. 2 is the standard working curve figure of n-propyl bromide in embodiment;
Fig. 3 is the chromatogram that comparative example 1 adopts the n-propyl bromide of HP-5 chromatographic column, and wherein horizontal ordinate is retention time, and ordinate is signal intensity;
Fig. 4 is the chromatogram that comparative example 2 adopts the n-propyl bromide of DB-WAX chromatographic column, and wherein horizontal ordinate is retention time, and ordinate is signal intensity;
Fig. 5 is the optimization extraction time experimental result picture of n-propyl bromide in embodiment 7.
Embodiment
All instrument, the reagent of following embodiment comprises:
1, instrument
GCMS-Q2010Ultra type gas chromatography-GC-MS (Japanese Shimadzu company);
2300HT type ultrasonic generator (Town in Shanghai spectrum scientific instrument company limited);
XW-80A eddy mixer (above Industrial Co., Ltd. of Nereid section);
Rxi-624sil MS(60m * 0.32mm * 1.8 μ m) chromatographic column (U.S. Restek company);
0.45 μ m polytetrafluoroethylene (PTFE) filtering head.
2, reagent
Standard items: n-propyl bromide (purity 99.0%, German Dr.Ehrenstorfer company), methyl alcohol (chromatographically pure, Town in Shanghai spectrum scientific instrument company limited), all purchased from Town in Shanghai spectrum scientific instrument company limited.
A detection method for n-propyl bromide in leather, textile, adopts GC-MS(gas chromatography-mass spectrography) to detect, and comprises following steps:
A, standard solution preparation
The preparation of n-propyl bromide standard reserving solution: take a certain amount of n-propyl bromide standard items, in 50mL volumetric flask, be made into the storing solution of 1000mg/L with Chromatographic Pure Methanol constant volume.
The preparation of n-propyl bromide standard operation solution: accurately pipette appropriate standard reserving solution, use Chromatographic Pure Methanol stepwise dilution, be made into the standard operation liquid of 0.1mg/L, 0.5mg/L, 1mg/L, 2mg/L, 5mg/L, 10mg/L, 20mg/L, 50mg/L.
B, sample pre-treatments
Sampling: get representational sample, be cut into about 5mm * 5mm size, accurately take 1.0g(and be accurate to 0.0001g), be placed in 60mL glass reaction bottle; Add extractant: in glass reaction bottle, add methyl alcohol 10mL, jump a queue airtight; Ultrasonic extraction: above-mentioned reaction bulb is placed in to ultrasonic generator, ultrasonic extraction 60min; Filter: be cooled to after room temperature, the PTFE filtering with microporous membrane of 0.45 μ m for extract, getting filtrate is testing sample.
C, gas chromatography-GC-MS for testing sample (GC-MS) is analyzed, retention time is qualitative, and typical curve external standard method is quantitative.
GC conditions:
Chromatographic column: Rxi-624sil MS(60m * 0.32mm * 1.8 μ m);
Column temperature condition: 50 ℃ of initial temperature, keep 2min, then the speed with 20 ℃/min rises to 200 ℃, keeps 1min;
Injector temperature: 250 ℃;
Input mode: split sampling, split ratio: 5:1;
Sample size: 1 μ L;
Carrier gas: high-pure helium (purity >99.999%), flow: 2ml/min;
Mass spectrum condition:
Ionization mode: electronics bombardment (EI) ionization, electron energy 70eV;
Ion source temperature: 230 ℃;
Chromatography-mass spectroscopy interface temperature: 260 ℃;
Solvent delay: 3min;
Drainage pattern: full ion scan (SCAN) is qualitative, selects ion scan (SIM) quantitative.
In embodiment 2 embodiment, the retention time of object (n-propyl bromide), feature fragmention are in Table 1.
The retention time of table 1 object, feature fragmention and abundance ratio
| Material title | Retention time/min | Feature fragmention/amu | Abundance ratio |
| N-propyl bromide | 6.564 | 43，122，124 | 100/8.5/8.2 |
From table 1 and Fig. 1, under the testing conditions of embodiment 1, object (n-propyl bromide) can access good separation.
Embodiment 3 linear relationships
Under the testing conditions of optimizing in the present invention, n-propyl bromide standard solution is detected in 0.1～50mg/L concentration range.Standard working curve is shown in Fig. 2, and as shown in Figure 2, its concentration and response have good linear relationship, linear equation: Y=4741.42X+1050.904, coefficient R
2=0.9995.
Under the testing conditions of optimizing in the present invention, the standard specimen of variable concentrations is carried out to analyzing and testing, the concentration limit (S/N>3) that records n-propyl bromide is 0.1mg/L.EU REACH Legislation is 0.1% (being 1000mg/L) to the organic Limited Doses of this high attention rate of n-propyl bromide, and the inventive method detection limit is far below Limited Doses.
Under the testing conditions that the present invention optimizes, with the standard specimen continuous detecting of 5.0mg/L 7 times, result (in Table 2) shows, its relative standard deviation RSD=1.887%, and hence one can see that, and under detection method condition of the present invention, precision can meet the requirement of analyzing and testing.
The Precision Experiment of table 2 n-propyl bromide
Embodiment 6 recovery
Under the testing conditions of optimization of the present invention to not containing the object that adds three mark-on levels in the sample of object, by the method for embodiment 1, carry out sample pre-treatments, detect the recovery of standard addition of object, each mark-on level do 3 times parallel, the results are shown in Table 3, obtain the recovery of n-propyl bromide between 96～112%, the accuracy of visible the inventive method can meet the requirement of analyzing and testing.
Table 3 n-propyl bromide recovery testu
From embodiment 1-6, the range of linearity of detection method of the present invention is wide, the recovery is high, precision is good, and detection limit is far below the Limited Doses of REACH rules.Detection method economical and efficient of the present invention and be easy to promote the use of between laboratory, can be advantageously applied to the detection of n-propyl bromide in textile and leather and fur products.
Comparative example 1
Comparative example 1 is the detection method of n-propyl bromide in a kind of leather, textile, adopt gas chromatography-mass spectrography to detect, comparative example 1 except the chromatographic column adopting be HP-5 (30m * 0.32mm0.25 * μ m), all the other detecting steps and parameter are identical with embodiment 1, and the chromatogram of resulting n-propyl bromide is asked for an interview Fig. 3.
Comparative example 2
Comparative example 2 is the detection method of n-propyl bromide in a kind of leather, textile, adopt gas chromatography-mass spectrography to detect, comparative example 2 except the chromatographic column adopting be DB-WAX(30m * 0.25mm * 0.25 μ m), all the other detecting steps and parameter are identical with embodiment 1, and the chromatogram of resulting n-propyl bromide is asked for an interview Fig. 4.
The separating effect that shows Rxi-624sil MS according to the result of Fig. 1, Fig. 3, Fig. 4 is best, have that retention time is short, highly sensitive, peak shape symmetrical without hangover, quantitatively accurately, high repeatability and other advantages, therefore preferred Rxi-624sil MS chromatographic column.
Embodiment 7 n-propyl bromide extraction time experiments
Under the testing conditions of optimization of the present invention, to 3 samples that contain object, by the method for embodiment 1, carry out sample pre-treatments, detect object content, each sample do 2 times parallel, sample number into spectrum respectively: 1-1,1-2,2-1,2-2,3-1,3-2, the results are shown in Figure 5.
From the result of Fig. 5, show: along with the increase of extraction time, the extraction efficiency of the n-propyl bromide in sample first improves thereupon, after tend towards stability; Extraction efficiency during 60min is the highest, and extraction efficiency during 60-90min tends towards stability.Therefore selecting preferred extraction time is 60 ± 5min, and optimum extraction time is 60min.
From embodiment 1-7, the sample pre-treatments of detection method of the present invention only needs 60min, the more existing pre-treatment time that is not less than 5h, has greatly improved extraction and detection efficiency.
The above embodiment has only expressed several embodiment of the present invention, and it describes comparatively concrete and detailed, but can not therefore be interpreted as the restriction to the scope of the claims of the present invention.It should be pointed out that for the person of ordinary skill of the art, without departing from the inventive concept of the premise, can also make some distortion and improvement, these all belong to protection scope of the present invention.Therefore, the protection domain of patent of the present invention should be as the criterion with claims.
Claims (9)
1. a detection method for n-propyl bromide in leather, textile, is characterized in that, adopts gas chromatography-mass spectrography to detect, and comprises following steps:
A, sample pre-treatments:
Accurately take pretreated sample 0.5～2.0g, be placed in 20～60mL glass reaction bottle, add organic solvent, ultrasonic extraction 55-65min, is cooled to after room temperature, the PTFE filtering with microporous membrane of 0.45 μ m for extract, and getting filtrate is testing sample;
B, testing sample is carried out to gas chromatography-mass spectrography detection, GC conditions is: chromatographic column: Rxi-624sil MS; Column temperature condition: 40～60 ℃ of initial temperature, keep 1～3min, then the speed with 15～25 ℃/min rises to 180～250 ℃, keeps 1～2min; Injector temperature: 250～280 ℃; Input mode: split sampling, split ratio: 5:1; Sample size: 1 μ L; Carrier gas: high-pure helium, purity >99.999%, flow: 1～2ml/min;
Mass spectrum condition is as follows: ionization mode: electron impact ionization, electron energy 70eV; Ion source temperature: 230 ℃; Chromatography-mass spectroscopy interface temperature: 260 ℃; Solvent delay: 2～4min; Drainage pattern: full ion scan is qualitative, selects ion scan quantitative.
2. the detection method of n-propyl bromide in leather as claimed in claim 1, textile, is characterized in that, in described steps A, ultrasonic extraction time is 60min; Described organic solvent is methyl alcohol.
3. the detection method of n-propyl bromide in leather as claimed in claim 1, textile, is characterized in that, in described steps A, sample pretreatment is for being cut into described sample 5mm * 5mm size.
4. the detection method of n-propyl bromide in leather as claimed in claim 1, textile, is characterized in that, accurately takes pretreated sample 1.0g in described steps A, is placed in 60mL glass reaction bottle, and described organic solvent is methyl alcohol, and addition is 10mL.
5. the detection method of n-propyl bromide in leather as claimed in claim 1, textile, is characterized in that, the GC conditions in described step B is: chromatographic column: Rxi-624sil MS; Column temperature condition: 50 ℃ of initial temperature, keep 2min, then the speed with 20 ℃/min rises to 200 ℃, keeps 1min; Injector temperature: 250 ℃; Input mode: split sampling, split ratio: 5:1; Sample size: 1 μ L; Carrier gas: high-pure helium, purity >99.999%, flow: 2ml/min;
Mass spectrum condition is as follows: ionization mode: electron impact ionization, electron energy 70eV; Ion source temperature: 230 ℃; Chromatography-mass spectroscopy interface temperature: 260 ℃; Solvent delay: 3min; Drainage pattern: full ion scan is qualitative, selects ion scan quantitative.
6. the detection method of n-propyl bromide in leather as claimed in claim 1, textile, is characterized in that, the specifications parameter of the chromatographic column in described step B is 60m * 0.32mm * 1.8 μ m.
7. the detection method of n-propyl bromide in the leather as described in claim 1-6 any one, textile, is characterized in that, in described leather, textile, detecting of the detection method of n-propyl bromide is limited to 0.1mg/L.
8. the detection method of n-propyl bromide in the leather as described in claim 1-6 any one, textile, is characterized in that the relative standard deviation < 2% of the detection method of n-propyl bromide in described leather, textile.
9. the detection method of n-propyl bromide in the leather as described in claim 1-6 any one, textile, is characterized in that, in described leather, textile, the recovery of standard addition of the detection method of n-propyl bromide is 96%～112%.
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| CN106596775A (en) * | 2016-12-19 | 2017-04-26 | 广电计量检测（成都）有限公司 | Detection method of tetradecahydro-1,4A-dimethyl-7-(1-methylethyl)-1-phenanthrene methanol in plastic |
| CN107290457A (en) * | 2017-07-28 | 2017-10-24 | 缪荣明 | 1 N-Propyl Bromide headspace gas chromatography assay method in urine |
| CN107632081A (en) * | 2017-09-06 | 2018-01-26 | 浙江中鼎检测技术有限公司 | A kind of method of octamethylcy-clotetrasiloxane content in gas chromatography mass spectrometry detection textile |
| CN111077292A (en) * | 2019-12-23 | 2020-04-28 | 上海微谱化工技术服务有限公司 | Pretreatment method for analysis of artificial leather material for vehicle |
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| CN106596775A (en) * | 2016-12-19 | 2017-04-26 | 广电计量检测（成都）有限公司 | Detection method of tetradecahydro-1,4A-dimethyl-7-(1-methylethyl)-1-phenanthrene methanol in plastic |
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