CN104569176A - Method for detecting concentration of acetaldehyde in aliphatic aldehydes of workplaces - Google Patents
Method for detecting concentration of acetaldehyde in aliphatic aldehydes of workplaces Download PDFInfo
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- CN104569176A CN104569176A CN201410736549.7A CN201410736549A CN104569176A CN 104569176 A CN104569176 A CN 104569176A CN 201410736549 A CN201410736549 A CN 201410736549A CN 104569176 A CN104569176 A CN 104569176A
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Abstract
The invention discloses a method for detecting concentration of acetaldehyde in aliphatic aldehydes of workplaces. The method comprises the steps of collecting a sample, treating the sample, preparing and detecting a standard solution, and manufacturing and detecting a standard curve. The method is characterized in that in the detecting steps, the gas phase condition of a gas chromatograph is set in the following way: an HP-INWWAX capillary chromatographic column is adopted, the column temperature is 100 DEG C, the temperature of a vaporizing chamber is 230 DEG C, the temperature of a detecting chamber is 230 DEG C, and the carrier gas flow is 5ml/min. By selecting the HP-INWWAX capillary, other compounds in aliphatic aldehyde compounds can be detected simultaneously after a proper detecting condition is set, so that the problem that easily broken column and time waste caused by frequently changing the column can be solved, cost and time can be reduced, and more importantly the data accuracy can be guaranteed. Regarding preparation of a standard solution, the usage of the standard solution is reduced by adopting the improved method, so that an excellent promoting effect for guaranteeing the precision and accuracy for sample detection can be achieved.
Description
Technical field
The present invention relates to acetaldehyde concentration assay method in the aliphatics aldehydes of a kind of workplace, belong to compound chemistry detection field.
Background technology
During workplace air noxious material is measured, the detection method of aliphatic aldehyde compounds is generally adopt vapor-phase chromatography, national standard requires that the mensuration of acetaldehyde in aliphatics aldehydes adjusts part to be 2m × 4mm glass column, FFAP:chromosorb WAW DMCS=15:100 chromatographic column, column temperature: 90 degree; Temperature of vaporization chamber: 150 degree; Sensing chamber's temperature: 150 degree; Carrier gas (nitrogen) flow: 30ml/min.Same, also can adopt vapor-phase chromatography in the mensuration of other class Air toxic substances, its core technology is the chromatographic column and suitable column temperature, temperature of vaporization chamber, sensing chamber's temperature and carrier gas flux that choice for use is suitable.If grope less than suitable condition, peak can not be gone out or go out peak not exclusively thus impact detects the accuracy of data.
For numerous projects utilizing vapor-phase chromatography to detect, require to use different chromatographic columns according to standard-required disparity items, change chromatographic column frequently for this reason and cause appearance to increase the risk of pillar infringement.One root chromatogram column price very expensive (about more than 5000 yuan one of kapillary) and continually replacing pillar easily cause the damage of pillar, and time-consuming.
Therefore how choice for use one capillary post, be suitable for all kinds of aliphatic aldehyde compounds to measure, the condition that the various project of same compound measures, and guarantee that every detection data accurately and meet the requirements, accomplishing that saving saves time and data multiple advantage accurately, is the researchist's urgent need to solve the problem in current detection industry.
Summary of the invention
The object of the invention is to for deficiency of the prior art, acetaldehyde concentration assay method in the aliphatics aldehydes of a kind of workplace is provided, there is cost and reduce, save time, the advantage that accuracy is high.
For solving the problems of the technologies described above, the technical solution used in the present invention is: acetaldehyde concentration assay method in the aliphatics aldehydes of a kind of workplace, comprise sample collection, sample preparation, the preparation of standard solution and mensuration, the making of typical curve and mensuration, its innovative point is: in described determination step, the gas phase condition of gas chromatograph is set to adopt HP-INWWAX capillary chromatographic column, column temperature is 100 degree, temperature of vaporization chamber is 200 degree, and sensing chamber's temperature is 230 degree, and carrier gas flux is 5ml/min.
Further, described standard solution is formulated as and accurately takes 0.66941g acetaldehyde in 10ml volumetric flask, add stripping liquid water constant volume and be made into the dense mark liquid of 26.60mg/ml acetaldehyde, draw the dense mark liquid of 0,5,10,20 μ l respectively in 1ml desorption bottle, be made into 0,133.0,266.0,532.0 μ g/ml standard series successively.
Further, described sample collection comprises short time sampling and blank sample sampling; The described short time is sampled as at sampled point, opens silicone tube two ends, with 100mL/min flow collection 15min air sample; Described blank sample is sampled as and silicone tube is brought to sampled point, and except not connecting samplers sample air sample, all the other operate same sample.
Further, described sample handling procedure is that the front and back section silica gel adopting sample is put into solvent desorption bottle respectively, respectively adds 2.0ml and 1.0ml stripping liquid water, after closing, jolting 1min, desorb 30min, shakes up, stripping liquid, for measuring, if concentration exceedes measurement range, can measure after dilute with water.
Further, described Specification Curve of Increasing step is conditioning instrumentation operating conditions, and sample introduction 2.0 μ l, measures each standard series, each concentration replication 3 times, with peak height or peak area average to corresponding acetaldehyde concentration drawing standard curve.
Further, described determination step comprises sample determination and reference substance mensuration; Described reference substance is determined as and measures blank stripping liquid, obtains peak height or peak area value; Described sample determination is the similarity condition working sample stripping liquid by bioassay standard series, after the sample peak height recorded or peak area value deduct blank peak height or peak area value, is obtained the concentration of two acetaldehyde in sample by typical curve.
Beneficial effect of the present invention is as follows:
(1) acetaldehyde concentration assay method in the aliphatics aldehydes of this workplace of the present invention, adopt HP-INWWAX capillary chromatographic column, column temperature is 100 degree, temperature of vaporization chamber is 200 degree, sensing chamber's temperature is 230 degree, and carrier gas flux is 5ml/min, detects acetaldehyde compound result detection data in aliphatics aldehydes accurate, meet national requirements, time-saving and efficiency.
(2) this HP-INWWAX kapillary is selected, after setting suitable condition determination, the detection of other compounds in aliphatic aldehyde compounds can also be carried out simultaneously, solve and change pillar continually and easily cause the damage of pillar and time-consuming problem, the accuracy the more important thing is and ensure that data of not only having saved but also saved time.
(3) for the preparation of standard solution, adopt the method after improvement of the present invention, the use amount of standard solution is reduced, for ensureing that the preci-sion and accuracy of sample determination serves good facilitation.
Embodiment
Below in conjunction with specific embodiment, technical scheme of the present invention is elaborated.
Embodiment 1
Adopt the detection method of gas chromatography determination acetaldehyde:
1, instrument
Silicone tube, solvent desorption type, 400mg/200mg silica gel.
Air sampler, flow 0-500ml/min.
Solvent desorption bottle, 5ml.
Micro syringe, 10 μ l.
Gas chromatograph: Shimadzu GC-2014C.
2, instrument testing conditions:
HP-INWWAX capillary chromatographic column.
Column temperature is 100 degree.
Temperature of vaporization chamber is 200 degree.
Sensing chamber's temperature is 230 degree,
Carrier gas flux is 5ml/min.
3, reagent
Distilled water
Sulfuric acid, density is 1.84mg/ml.
4, sample collection:
Short time samples: at sampled point, open silicone tube two ends, with 100mL/min flow collection 15min air sample;
Blank sample is sampled: silicone tube is brought to sampled point, and except not connecting samplers sample air sample, all the other operate same sample.
After sampling, close solid absorbent tubes two ends immediately, put transport and preservation in cleaning container.
5, mensuration is analyzed:
5.1 sample preparation: the front and back section silica gel adopting sample is put into solvent desorption bottle respectively, respectively adds 2.0ml and 1.0ml stripping liquid water, after closing, jolting 1min, desorb 30min, shakes up, and stripping liquid is for measuring.
The preparation of 5.2 standard solution and mensuration: preparation: accurately take 0.66941g acetaldehyde (colour code in 10ml volumetric flask, Tianjin recovery fine chemistry industry research institute, lot number 20100701,40%), add stripping liquid water constant volume and be made into the dense mark liquid of 26.60mg/ml acetaldehyde, draw the dense mark liquid of 0,5,10,20 μ l respectively in 1ml desorption bottle, be made into 0,133.0,266.0,532.0 μ g/ml standard series successively, measure under prescribed conditions.
The making of 5.3 typical curves: conditioning instrumentation operating conditions, sample introduction 2.0 μ l, measures each standard series, each concentration replication 3 times, with peak height or peak area average to corresponding diphenyl ether concentration drawing standard curve.
5.4 measure: one, the similarity condition of bioassay standard series measures blank stripping liquid, obtains peak height or peak area value; Two, the similarity condition working sample stripping liquid of bioassay standard series, after the sample peak height recorded or peak area value deduct blank peak height or peak area value, is obtained the concentration of acetaldehyde in sample by typical curve.
6, sample concentration computing method:
By formula 1, sampling volume is converted into standard sample volume:
Formula 1:
In formula: Vo-standard sample volume, L;
V-sampling volume, L;
The temperature of t-sampled point, DEG C;
The atmospheric pressure of P-sampled point, kPa.
The concentration of acetaldehyde is calculated by formula 2:
Formula 2:
In formula: the concentration of acetaldehyde in C-air, mg/m
3;
C
1,c
2-record the concentration (deducting sample blank) of acetaldehyde in the section active carbon desorption liquid of front and back, μ g/mL;
Vo-standard sample volume, L;
The volume of v-stripping liquid, mL;
D-desorption efficiency, %.
Embodiment 2
The precision test experiments of the inventive method:
Drawing four parts of sample 20 μ l to four 1ml resolves in bottles, label 1,2,3 and 4 respectively, by embodiment 1 sample determination method carry out the mensuration of sample concentration, result is as follows:
As calculated, the mean concentration of acetaldehyde is 556.46 μ g/ml, and coupon results shows the requirement that the Precision Experiment of diphenyl ether meets standard and specifies.
Embodiment 3
Recovery of standard addition is tested:
Draw the cyclohexane sample that 10 μ l concentration are the dense mark of 26.60mg/ml and 20 μ l respectively, resolve in bottle to 1ml, respective recovery of standard addition is as shown in the table:
As calculated: the recovery of standard addition of sample 1 is 96.72%;
The recovery of standard addition of sample 2 is 97.27%;
The recovery of standard addition of sample 3 is 96.45%;
The recovery of standard addition of sample 4 is 97.00%.
Comparative example 1
GB standard method is adopted to measure the concentration of the acetaldehyde sample of embodiment 1.Experiment proves, the time that GB detects is 2 ~ 3h, and sample detection concentration is 556.51 μ g/ml, basic identical with embodiment detectable concentration, and the detection time of embodiment shorter be 1.5 ~ 2.2h.
Claims (6)
1. acetaldehyde concentration assay method in a workplace aliphatics aldehydes, comprise sample collection, sample preparation, the preparation of standard solution and mensuration, the making of typical curve and mensuration, it is characterized in that: in described determination step, the gas phase condition of gas chromatograph is set to adopt HP-INWWAX capillary chromatographic column, column temperature is 100 degree, temperature of vaporization chamber is 200 degree, sensing chamber's temperature is 230 degree, and carrier gas flux is 5ml/min.
2. acetaldehyde concentration assay method in the aliphatics aldehydes of workplace according to claim 1, it is characterized in that: described standard solution is formulated as and accurately takes 0.66941g acetaldehyde in 10ml volumetric flask, add stripping liquid water constant volume and be made into the dense mark liquid of 26.60mg/ml acetaldehyde, draw the dense mark liquid of 0,5,10,20 μ l respectively in 1ml desorption bottle, be made into 0,133.0,266.0,532.0 μ g/ml standard series successively.
3. acetaldehyde concentration assay method in the aliphatics aldehydes of workplace according to claim 1, is characterized in that: described sample collection comprises short time sampling and blank sample sampling; The described short time is sampled as at sampled point, opens silicone tube two ends, with 100mL/min flow collection 15min air sample; Described blank sample is sampled as and silicone tube is brought to sampled point, and except not connecting samplers sample air sample, all the other operate same sample.
4. acetaldehyde concentration assay method in the aliphatics aldehydes of workplace according to claim 1, it is characterized in that: described sample handling procedure is that the front and back section silica gel adopting sample is put into solvent desorption bottle respectively, respectively add 2.0ml and 1.0ml stripping liquid water, after closing, jolting 1min, desorb 30min, shake up, stripping liquid, for measuring, if concentration exceedes measurement range, can measure after dilute with water.
5. acetaldehyde concentration assay method in the aliphatics aldehydes of workplace according to claim 1, it is characterized in that: described Specification Curve of Increasing step is conditioning instrumentation operating conditions, sample introduction 2.0 μ l, measure each standard series, each concentration replication 3 times, with peak height or peak area average to corresponding acetaldehyde concentration drawing standard curve.
6. acetaldehyde concentration assay method in the aliphatics aldehydes of workplace according to claim 1, is characterized in that: described determination step comprises sample determination and reference substance measures; Described reference substance is determined as and measures blank stripping liquid, obtains peak height or peak area value; Described sample determination is the similarity condition working sample stripping liquid by bioassay standard series, after the sample peak height recorded or peak area value deduct blank peak height or peak area value, is obtained the concentration of two acetaldehyde in sample by typical curve.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| RU2595869C1 (en) * | 2015-05-22 | 2016-08-27 | Федеральное государственное бюджетное образовательное учреждение высшего образования "Кабардино-Балкарский государственный университет им. Х.М. Бербекова" (КБГУ) | Method and device for determining weight ratio of acetaldehyde |
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| KR20130106465A (en) * | 2012-03-19 | 2013-09-30 | 대한민국(관리부서 : 산림청 국립산림과학원장) | Attractant for glyphodes perpectalis comprising aldehyde-based pheromone, glyphodes perpectalis for attracting resin composition comprising thereof |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| KR20130106465A (en) * | 2012-03-19 | 2013-09-30 | 대한민국(관리부서 : 산림청 국립산림과학원장) | Attractant for glyphodes perpectalis comprising aldehyde-based pheromone, glyphodes perpectalis for attracting resin composition comprising thereof |
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| MIKLÓS GORGÉNYI ET AL.: "Enthalpies of Solution and Excess Enthalpies of Oxo Compounds by Capillary Gas Chromatography", 《JOURNAL OF CHROMATOGRAPHIC SCIENCE》 * |
| 中华人民共和国卫生部: "《中华人民共和国国家职业卫生标准 GBZ/T 160.54-2007》", 13 June 2007 * |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| RU2595869C1 (en) * | 2015-05-22 | 2016-08-27 | Федеральное государственное бюджетное образовательное учреждение высшего образования "Кабардино-Балкарский государственный университет им. Х.М. Бербекова" (КБГУ) | Method and device for determining weight ratio of acetaldehyde |
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Application publication date: 20150429 |