CN104897814A - Method for detecting aldehyde ketone concentration in atmosphere through combination of DNPH-silica-gel adsorption small columns and HPLC-UV - Google Patents
Method for detecting aldehyde ketone concentration in atmosphere through combination of DNPH-silica-gel adsorption small columns and HPLC-UV Download PDFInfo
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- CN104897814A CN104897814A CN201510315054.1A CN201510315054A CN104897814A CN 104897814 A CN104897814 A CN 104897814A CN 201510315054 A CN201510315054 A CN 201510315054A CN 104897814 A CN104897814 A CN 104897814A
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Abstract
The invention relates to a method for detecting aldehyde ketone concentration in the atmosphere through combination of DNPH-silica-gel adsorption small columns and a HPLC-UV. The method comprises the following steps: (1) a sampling efficiency experiment: connecting two DNPH-silica-gel adsorption small columns in series, connecting the combined small columns with a sampling pump, and collecting an aldehyde ketone gas sample of which the concentration is known; (2) an atmosphere collection experiment: connecting a flowmeter, a potassium iodide copper pipe, the DNPH-silica-gel adsorption small columns and the sampling pump in sequence, so as to collect an aldehyde ketone gas sample in the ambient air; (3) sample treatment and analysis: slowly flushing the collected samples with acetonitrile, quantifying with a volumetric flask, and then carrying out detection through the HPLC-UV. The method has the advantages that the sampling efficiency can be 99 percent or above, the replicate analysis standard deviation of experiment data is less than 5 percent, the detection limit is as low as 0.05 to 0.15 microgram/m<3>, the detection accuracy is 3.01 to 9.65 percent, and the method is high in practicability.
Description
Technical field
The present invention relates to the analyzing detecting method of air aldehyde ketone concentration, specifically a kind of DNPH-silica gel adsorption pillar that adopts detects the method for air aldehyde ketone concentration in conjunction with HPLC-UV.
Background technology
When quantitative detecting analysis air aldehyde ketone concentration, DNPH (DNPH) uses a kind of derivating agent very widely, and itself is not volatile, can react rapidly generate stable product phenylhydrazone with aldehyde ketone.At present, in the laboratory of Domestic Environment study on monitoring mechanism, the spending used in order to reduction of expenditure and cost, often adopt half commercialization homemade DNPH-silica gel adsorption pipe collection analysis air aldehyde ketone concentration, it exists, and adsorption tube manufacturing process be loaded down with trivial details, the blank content of adsorption tube is high, sampling efficiency is unstable, the shortcoming of adsorption tube shelf lives short (be generally 1 to 4 week).Recently, Waters company is commercially proposed a commercialization DNPH-silica gel adsorption pillar (Sep-Pak Silica Gel Cartridge, Millipore Co.), but, use this DNPH-silica gel adsorption pillar how on earth to detect the effect of air aldehyde ketone concentration in conjunction with HPLC-UV in environment measuring, also there is no concrete data report and explanation up till now for this reason.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of sampling efficiency is high, detectability is low, precision is high, practical employing DNPH-silica gel adsorption pillar detects air aldehyde ketone concentration method in conjunction with HPLC-UV.
The present invention solves the problems of the technologies described above taked technical scheme: a kind of DNPH-silica gel adsorption pillar that adopts detects the method for air aldehyde ketone concentration in conjunction with HPLC-UV, comprises following concrete steps:
(1) sampling efficiency experiment: 2 DNPH-silica gel adsorption pillars are connected successively, then after being connected with sampling pump, gather the aldehyde ketone gaseous sample of concentration known;
(2) air collection experiment: flowmeter, potassium iodide copper pipe, DNPH-silica gel adsorption pillar are connected successively with sampling pump, gather aldehyde ketone gaseous sample in surrounding air, gather flow identical with the aldehyde ketone gaseous sample of the collection concentration known described in step (1) with acquisition time; Potassium iodide copper pipe is for removing the ozone in air;
(3) sample preparation and analysis: the sample acetonitrile of collection is rinsed lentamente, quantitative with volumetric flask, then detect with HPLC-UV.
DNPH-silica gel adsorption pillar described in step (1) is the commercialization DNPH-silica gel adsorption pillar of Waters company.
The collection flow 2L/min of aldehyde ketone gaseous sample, acquisition time 120min in the aldehyde ketone gaseous sample of the collection concentration known described in step (1) and the collection surrounding air described in step (2).
During HPLC-UV described in step (3) detects, analytical column is C
18reversed-phase column, adopt acetonitrile and water as eluent gradient wash-out, gradient is 60 ~ 70% acetonitrile 20min, 70 ~ 100% acetonitrile 3min, 100% acetonitrile 6min, 100 ~ 60% acetonitrile 5min, 60% acetonitrile 5min.Flow rate of mobile phase 1mL/min, determined wavelength 360nm, sample size 10 μ L.
The present invention adopts commercialization DNPH-silica gel adsorption pillar in conjunction with HPLC-UV technology, and achieve the accurate detection of air aldehyde ketone concentration, sampling efficiency reaches more than 99%, and the standard deviation of experimental data replicate analysis is lower than 5%; Detectability is low to moderate 0.05 ~ 0.15 μ g/m
3, precision is 3.01 ~ 9.65%, method practical.
Embodiment
To further describe technical scheme of the present invention by embodiment below, but the present invention is not limited to illustrated embodiment.
The present embodiment Selection utilization DNPH-silica gel adsorption pillar gathers aldehyde ketone pollutant in air, in conjunction with HPLC-UV technology, achieves the accurate detection of air aldehyde ketone concentration.
Main Analysis instrument:
The commercialization DNPH-silica gel adsorption pillar (Sep-Pak Silica Gel Cartridge, Millipore Co.) of Waters company
Hewlett Packard company HP1100 type high performance liquid chromatograph.
The concrete steps of the present embodiment are as follows:
1, standard specimen is prepared: by the aldehyde ketone-DNPH standard items dilution in acetonitrile bought, obtain the DNPH-aldehyde ketone standard model of concentration known.
2, DNPH-silica gel adsorption pillar blank tube preserves experiment: the blank DNPH-silica gel adsorption pillar newly bought is preserved 1 month, 2 months, 4 months, 8 months, 12 months respectively in laboratory, detects residual aldehyde ketone content in blank pillar.
3, sampling efficiency experiment: with high-purity N
2(99.99%) to find time reaction bag with sampling pump after rinsing Teflon reaction bag, after aldehyde ketone gaseous sample after volatilization is injected reaction bag, to be connected with sampling pump with self-control DNPH-silica gel adsorption pillar again and to carry out sampling efficiency experiment, collection flow 2L/min, acquisition time 120min; The little sealing bag sealing of Teflon put into by sampling pipe after sampling, is placed in refrigerator and preserves.
4, potassium iodide (KI) copper pipe is made: the ozone in air and DNPH react, and affect testing result, so add a potassium iodide copper pipe filtering ozone before sampling pipe.Get one about 1 meter, internal diameter is about the copper pipe of 0.5cm, be simply processed into 3,4 circles by hand.Copper band inwall first cleans several times with water, then cleans with watery hydrochloric acid, then rinses with water.Then about soaking inwall half an hour with saturated KI solution, more slowly dry up with high pure nitrogen.
5, atmospheric sample collection: during sampling, air enters flowmeter, potassium iodide copper pipe, DNPH-silica gel adsorption pillar, valve (being used for regulating sampling flow), sampling pump successively, sampling time is 120min, sampling flow 2L/min, sampling position is center, city, Qinzhou City.The little sealing bag sealing of Teflon put into by sampling pipe after sampling, is placed in refrigerator and preserves.
6, sample preparation and instrumental analysis: the sample acetonitrile of collection rinses lentamente, quantitative with the volumetric flask of 2mL, then detect with HPLC-UV.HPLC system model is HP1100, and analytical column is Agilent SB-C
18reversed-phase column (250mm × 4.6mm, 5 μm).Use mobile phase to be acetonitrile and water, gradient is 60 ~ 70% acetonitrile 20min, 70 ~ 100% acetonitrile 3min, 100% acetonitrile 6min, 100 ~ 60% acetonitrile 5min, 60% acetonitrile 5min.Flow rate of mobile phase 1mL/min, determined wavelength 360nm, sample size 10 μ L.
7, method recruitment evaluation: sampling flow of the present invention is 2mL/min, sampling efficiency two self-control DNPH silica gel adsorption pillar tandem sampling is assessed; Experiment Cmin does 10 times continuously, draws detectability, detectability be calculated as 3.14 × SD, SD is standard deviation; The standard deviation of experimental data replicate analysis all does often kind of sample repeatedly to analyze, and calculation deviation scope and method precision, method assessment result is in table 1.
The sample effect assessment result of table 1. the inventive method, comprises the standard deviation of sampling efficiency, method detectability, method precision, experimental data replicate analysis
Experimental result shows, blank DNPH-silica gel adsorption pillar is within the time reaching 12 months, and in DNPH-silica gel adsorption pillar, the content of aldehyde ketone is without detecting.In addition, as shown in Table 1, sampling efficiency reaches more than 99%, and detectability is low to moderate 0.05 ~ 0.15 μ g/m
3, method precision is 3.01 ~ 9.65%, and the standard deviation of experimental data replicate analysis is lower than 5%.And atmospheric sample gathers gained aldehyde ketone concentration (if concentration of formaldehyde is 6.70 ± 6.36 μ g/m
3) good stability of data.Visible, commodity in use DNPH-silica gel adsorption pillar, in conjunction with HPLC-UV technology, sampling efficiency is high, and method is respond well, method practical.
Claims (4)
1. adopt DNPH-silica gel adsorption pillar to detect a method for air aldehyde ketone concentration in conjunction with HPLC-UV, it is characterized in that, comprise following concrete steps:
(1) sampling efficiency experiment: 2 DNPH-silica gel adsorption pillars are connected successively, then after being connected with sampling pump, gather the aldehyde ketone gaseous sample of concentration known;
(2) air collection experiment: flowmeter, potassium iodide copper pipe, DNPH-silica gel adsorption pillar are connected successively with sampling pump, gathers aldehyde ketone gaseous sample in surrounding air; Potassium iodide copper pipe is for removing the ozone in air;
(3) sample preparation and analysis: the sample acetonitrile of collection is rinsed, quantitative with volumetric flask, then detect with HPLC-UV.
2. employing DNPH-silica gel adsorption pillar according to claim 1 detects the method for air aldehyde ketone concentration in conjunction with HPLC-UV, it is characterized in that, the DNPH-silica gel adsorption pillar described in step (1) is the commercialization DNPH-silica gel adsorption pillar of Waters company.
3. employing DNPH-silica gel adsorption pillar according to claim 1 detects the method for air aldehyde ketone concentration in conjunction with HPLC-UV, the collection flow 2L/min of aldehyde ketone gaseous sample, acquisition time 120min in the aldehyde ketone gaseous sample of the collection concentration known described in step (1) and the collection surrounding air described in step (2).
4. employing DNPH-silica gel adsorption pillar according to claim 1 detects the method for air aldehyde ketone concentration in conjunction with HPLC-UV, and during the HPLC-UV described in step (3) detects, analytical column is C
18reversed-phase column, adopt acetonitrile and water as eluent gradient wash-out, gradient is 60 ~ 70% acetonitrile 20min, 70 ~ 100% acetonitrile 3min, 100% acetonitrile 6min, 100 ~ 60% acetonitrile 5min, 60% acetonitrile 5min.Flow rate of mobile phase 1mL/min, determined wavelength 360nm, sample size 10 μ L.
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| CN105572256A (en) * | 2015-12-28 | 2016-05-11 | 田琳琳 | Method for detecting concentration of formaldehyde in air |
| CN105651563A (en) * | 2015-02-04 | 2016-06-08 | 广西大学 | Method for collecting atmospheric aldehyde ketone pollutants by use of self-made DNPH silica gel adsorption tube |
| US10495552B2 (en) | 2014-06-27 | 2019-12-03 | Pulse Health Llc | Breath analysis system |
| CN114894933A (en) * | 2022-05-09 | 2022-08-12 | 台州市产品质量安全检测研究院 | Method for measuring volatile aldehyde ketone substances of automotive interior parts by environment test cabin method |
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| CN105572256A (en) * | 2015-12-28 | 2016-05-11 | 田琳琳 | Method for detecting concentration of formaldehyde in air |
| CN114894933A (en) * | 2022-05-09 | 2022-08-12 | 台州市产品质量安全检测研究院 | Method for measuring volatile aldehyde ketone substances of automotive interior parts by environment test cabin method |
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Application publication date: 20150909 |