CN103760270A - Method for measuring acrylic acid in air in working spaces by using ion chromatography - Google Patents
Method for measuring acrylic acid in air in working spaces by using ion chromatography Download PDFInfo
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- CN103760270A CN103760270A CN201410037155.2A CN201410037155A CN103760270A CN 103760270 A CN103760270 A CN 103760270A CN 201410037155 A CN201410037155 A CN 201410037155A CN 103760270 A CN103760270 A CN 103760270A
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Abstract
The invention belongs to the technical field of chemical measurement methods and in particular relates to a method for measuring acrylic acid in air in working spaces by using ion chromatography. The rapid, sensitive, accurate, environment-friendly and low-cost method for measuring acrylic acid in air in working spaces by using ion chromatography is constructed by collecting the acrylic acid through a silicone tube and by taking environment-friendly pollution-free sodium carbonate/sodium bicarbonate as desorption solution and chromatographic mobile phase. A novel feasible way is provided for rapidly and accurately measuring acrylic acid in air in the working spaces, and the application of the ion chromatography in occupational health inspection is widened.
Description
Technical field
The invention belongs to the technical field of chemistry in detecting, be specially with acrylic acid in air of workplace by ion chromatography.
Background technology
In occupational health testing, the pollution condition of the objectionable impurities such as acrylic acid in accurate evaluation workplace air, healthy for protection laborer, avoid occupational hazards to occur, ensure enterprise safety operation, the stable actual meaning that has promotes social harmony.Acrylic acid (crylic acid) is a kind of important organic synthesis raw material and synthetic resin monomer, in industry, be mainly used to produce esters of acrylic acid, be widely used in the fields such as daily-use chemical industry, weaving, papermaking, building materials, packing, metallurgy, leather, plastic processing.Acrylic acid has pungency effect, and high concentration contact can cause skin burn, may damage lung hepatic and renal function.At present, in workplace, acrylic acid mensuration adopts vapor-phase chromatography conventionally, but has following shortcoming: 1. detection sensitivity is lower.Detecting of the Propylene By Gas Chromatography acid adopting in China's occupational health examination criteria is limited to 100 μ g/ml, and its mensuration detection limit of other carboxylic-acid substances (formic acid, acetic acid etc.) is all less than 10 μ g/ml.2. sample is after adsorbent gathers, and need, with the larger organic solvent of toxicity as acetone etc. carries out desorb, can work the mischief to human body and environment.3. gas chromatograph need be done carrier gas with gas, is equipped with air-channel system and temperature control program, and loaded down with trivial details during operating cost, operating cost cost is higher.Therefore, be necessary acrylic acid assay method in existing workplace air to carry out Improvement, set up and generally apply and specific accurate, reliable, the sensitive monitoring method of tool.
The chromatography of ions has advantages of that selectivity is good, quick, sensitive, easy, and the U.S. state-run occupational safety and health research institute (NIOSH) adopts 17 kinds of materials such as formic acid, chloroacetic acid in air of workplace by ion chromatography in analytical approach guide (NMAM).China starts late for the applied research in air of workplace by ion chromatography, in the < < workplace air of at present China health State Family Planning Commission issue in the mensuration > > standard of noxious material, only list hydrochloric acid, sulfuric acid, iodine, 4 kinds of ion chromatography methods of oxalic acid, the detection of most of materials also rests in vapor-phase chromatography, and vapor-phase chromatography exists, operating cost is higher, coexisting substances disturbs, and some method also needs to use the shortcomings such as toxic reagent.
Therefore, the application of the chromatography of ions is also nowhere near, and for overcoming these shortcomings, improves the application of chromatography of ions in occupational health detects, and steps up the research of noxious material chromatography of ions detection method in workplace air to be very important.
Summary of the invention
The object of the invention is to the defect for above-mentioned existence, and provide a kind of with acrylic acid in air of workplace by ion chromatography, with silicone tube, gather acrylic acid, a kind of environment friendly and pollution-free sodium carbonate/bicarbonate solution of take is stripping liquid and chromatogram flow phase, set up acrylic acid in a kind of quick, sensitive, accurate, environmental protection and chromatography of ions testing place air with low cost, this has widened the application of the chromatography of ions in occupational health detects, for the detection of carboxylic acids objectionable impurities in workplace provides new feasible way.
Technical scheme of the present invention is:
With acrylic acid in air of workplace by ion chromatography, adopt the airborne acrylic acid in silicone tube collecting work place to complete sampling, adopt 2.0 mmol/L NaHCO
3+ 1.5 mmol/L Na
2cO
3sample introduction after stripping liquid desorb, separated through anion analysis post, chromatogram flow phase is identical with stripping liquid, and electric conductivity detector detects, and will detect data and typical curve contrast, and then substitution computing formula calculates acrylic acid concentration in air.
As preferably, described anion analysis post is Metrosep A SUPP 4-250/4.0 type anion analysis post, and specification is 4.0 mm * 250.0 mm.
As preferably, described sampling concrete steps are: in sampling location, open silicone tube two ends, 150 mg ends are connected with air sampler, flow 0.3 L/min, gather 15 min, 2 sections of the front and back silica gel of adopting sample is poured into respectively in 15 ml tool plug test tubes, respectively add 10 ml 2.0 mmol/L NaHCO
3+ 1.5 mmol/L Na
2cO
3chromatogram eluate desorb, sealing jolting 1 min, standing 30 min, stripping liquid is after filtering for measuring.
As preferably, the configuration of described typical curve is as follows: get 10 ml volumetric flasks, add 5 ml stripping liquids, after accurately weighing, add several acrylic acid, accurately weigh again, with stripping liquid, be settled to scale, mix, by the difference of twice weighing, calculate its concentration, for standard reserving solution, with stripping liquid, be diluted to 200 μ g/ml acrylic acid standard solution before use, configuration 0.1 μ g/ml, 0.5 μ g/ml, 1.0 μ g/ml, 1.5 μ g/ml, 2.0 μ g/ml, 3.0 μ g/ml, 4.0 μ g/ml acrylic acid standard series, for measuring.
Of the present invention with acrylic acid in air of workplace by ion chromatography, its detailed step is as follows:
A. sample and in sampling location, open silicone tube two ends, 150 mg ends are connected with air sampler, flow 0.3 L/min, gathers 15 min, and 2 sections of the front and back silica gel of adopting sample is poured into respectively in 15 ml tool plug test tubes, respectively adds 10 ml 2.0 mmol/L NaHCO
3+ 1.5 mmol/L Na
2cO
3chromatogram eluate desorb, sealing jolting 1 min, standing 30 min, stripping liquid is after filtering for measuring;
B. chromatographic condition mobile phase: 2.0 mmol/L NaHCO
3+ 1.5 mmol/L Na
2cO
3, flow velocity: 1.0 ml/min, sampling volume: 20 μ l, regenerated liquid: 0.1 mol/L sulfuric acid solution;
C. 10 ml volumetric flasks are got in typical curve preparation, add 5 ml stripping liquids, after accurately weighing, add several acrylic acid, more accurately weigh, with stripping liquid, be settled to scale, mix, by the difference of twice weighing, calculating its concentration, is standard reserving solution, is diluted to 200 μ g/ml acrylic acid standard solution before use with stripping liquid, configure 0.1 μ g/ml, 0.5 μ g/ml, 1.0 μ g/ml, 1.5 μ g/ml, 2.0 μ g/ml, 3.0 μ g/ml, 4.0 μ g/ml acrylic acid standard series, for measuring;
D. in data calculating air, the computing formula of acrylic acid concentration is: C=10 (c
1+ c
2)/(V
0d), wherein C is acrylic acid concentration in air, mg/m
3; c
1,c
2for acrylic acid concentration in section silica gel stripping liquid before and after recording, μ g/ml; 10 is the cumulative volume of stripping liquid, ml; V
0for standard sample volume, L; D is desorption efficiency, %.
As preferably, the air sampler described in a step is GilAir-5 air sampler, is equipped with low discharge adjustment module, by U.S. GILIAN company, is produced.
As preferably, in a step, adopt 0.45 μ m water-based miillpore filter to filter.
Beneficial effect of the present invention is:
The present invention has set up acrylic acid ion chromatography method in workplace, and method adopts silicone tube collected specimens, adopts NaHCO
3-Na
2cO
3stripping liquid desorb, adopts 2.0 mmol/L NaHCO
3+ 1.5 mmol/L Na
2cO
3mobile phase, flow velocity 1.0 ml/min, measure, for method of the present invention, acrylic acid presents good linear relationship within the scope of 0.1 μ g/ml-4.0 μ g/ml, linearly dependent coefficient is 0.9999, with signal to noise ratio (S/N ratio) (
s/N) be 3 to determine that methods detect and be limited to 0.0033 μ g/ml, relative standard deviation 0.89%-1.15%, in silicone tube, acrylic acid desorption efficiency is 94.0%-102.1%, sample can be at 4 ℃ at least stable 7 d that preserve.Adopt the method to measure acrylic acid in certain building materials enterprise workplace air, obtained good result, the Common Anions existing in scene or silicone tube and other impurity are analyzed noiseless to acrylic acid.
Method of the present invention and existing vapor-phase chromatography, the method is highly sensitive, precision is good, with low cost, simple to operate, and selected stripping liquid is pollution-free, be applicable to batch samples and detect, the method can be used for the mensuration of acrylic acid short time concentration and time weighted average concentration in workplace air.This method, for accurate evaluation acrylic acid provides effective mensuration means to the harm of health, provides reference frame for further studying carboxylic-acid substance in ion chromatography workplace air.
As fully visible, method of the present invention is by selecting rational condition and device combination, by selecting the coordinative role of the configuration of suitable typical curve, suitable each steps such as parameter selection, realized in the application of ion chromatography method and acrylic acid mensuration, and the method is quick, sensitive, accurately, with low cost, being applicable to acrylic acid in workplace air detects, this result of study contributes to promote the application development of the chromatography of ions in occupational health testing, possesses outstanding substantive distinguishing features and progressive significantly.
Accompanying drawing explanation
Fig. 1 is Common Anions and acrylic acid separate colors spectrogram, 1-F
-, 2-crylic acid, 3-Cl
-, 4-Br
-, 5-NO
3 -, 6-PO
4 3-, 7-SO
4 2-.
Fig. 2 is the chromatogram of test example sample.
Embodiment
Below by specific embodiment, technical scheme of the present invention is described in detail.
instrument
883 type ion chromatographs, 863 type automatic samplers, electric conductivity detector, Metrosep A SUPP 4-250/4.0 type anion analysis post (4.0 mm * 250.0 mm) (Switzerland Wan Tong company), GilAir-5 air sampler (being equipped with low discharge adjustment module) (U.S. GILIAN company), silicone tube (solvent desorption type, in-built 300 mg/150 mg silica gel) (Yancheng purple light Electron equipment Co., Ltd), 0.45 μ m water-based miillpore filter (system in Beijing Jing Hui Kai industry Science and Technology Ltd.).
reagent
Acrylic acid (chromatographically pure, Chengdu Ai De Chemical Co., Ltd., lot number: 201205151).NaHCO
320130110), Na (top grade is pure, Tianjin Kermel Chemical Reagent Co., Ltd., lot number:
2cO
3(top grade is pure, Tianjin Kermel Chemical Reagent Co., Ltd., and lot number: 20130323), deionized water (resistivity >18.0 M Ω cm).
1. chromatography condition and interference test
The selection of mobile phase and concentration directly affect separation efficiency and the detection sensitivity of chromatographic peak, because the anion chromatographic behavior that acrylic acid is common to part is similar, particularly more approaching with the retention time of fluorine ion, chlorion, therefore need to select suitable chromatographic column and chromatographic condition to analyze, through Optimal Experimental, find to adopt 2.0 mmol/L NaHCO
3+ 1.5 mmol/L Na
2cO
3mobile phase, flow velocity 1.0 ml/min, acrylic acid can with F
-, Cl
-completely separated, acrylic acid retention time is 4.46 min.Common Anions and acrylic acid separate colors spectrogram are as shown in Figure 1.
2. linear relationship and method detection limit
According to above-mentioned experiment condition, standard series sample is analyzed, sample introduction 20 μ l, to record the corresponding corresponding acrylic acid concentration drawing standard curve of peak area average, gained typical curve linear equation is y=0.0564x+0.0004, related coefficient
r=0.9999, with 3 times of signal to noise ratio (S/N ratio)s (
s/N=3) calculate it and detect and be limited to 0.0033 μ g/ml, by sampling volume 4.5 L, concentration limit is 0.0073 mg/m
3.The vapor-phase chromatography adopting in the assay method > > (GBZ/T160.59-2004) of carboxylic acid compound in China occupational health standard < < workplace air at present detects and is limited to 100 μ g/ml, and concentration limit is 3.3 mg/m
3.Can relatively draw thus, the sensivity indexes such as its detection limit of this chromatography of ions and concentration limit are obviously better than vapor-phase chromatography.
3. Precision Experiment
Under selected chromatographic condition, to get concentration and be the acrylic acid sample of 1.0 μ g/ml, 2.0 μ g/ml, 3.0 μ g/ml and analyze, every kind of concentration replication 6 times, the results are shown in Table 1, acrylic acid
rSDfor 0.89%-1.15%, meet chemical substance assay method > > requirement in < < workplace air.
table 1 Precision Experiment result (
n=6)
4. analyzing efficiency experiment
Adopt NaHCO
3-Na
2cO
3solution is as stripping liquid, the acetone stripping liquid that in the GB of comparing < < workplace air, in the assay method > > (GBZ/T160.59-2004) of carboxylic acid compound, vapor-phase chromatography adopts, NaHCO
3-Na
2cO
3stripping liquid has the advantages such as environment friendly and pollution-free, with low cost.18 silicone tubes are got in employing, are divided into 3 groups, with micro syringe, respectively add 10 μ g, 20 μ g, 30 μ g acrylic acid, immediately sealed silicon sebific ducts.Placement is spent the night, and 2 sections of front and back silica gel is poured in 20 ml tool plug test tubes, adds 10 ml leacheate desorbs, jam-pack pipe close, and jolting 1 min, places after 1 h, and sample introduction 20 μ l analyze.Make one group of silicone tube blank simultaneously, during calculating, deduct blank value.Result is as shown in table 2, and acrylic acid desorption efficiency is 94.0%-102.1%, meets chemical substance assay method > > requirement in < < workplace air.
table 2 desorption efficiency measurement result
5. sample stability experiment
Get 12 silicone tubes, add respectively a certain amount of acrylic acid, sealed silicon sebific duct immediately, first 3 silicone tubes of random taking-up are analyzed mensuration immediately, and all the other are placed in 4 ℃ of preservations of refrigerator, then respectively at the 3rd d, 5 d, 7 d, analyze mensuration, the loss percentage of different time sample is deposited in calculating, experimental result shows, it is 95.2% that sample is deposited its average recovery rate after 7 d, shows that sample at least can preserve 7 d under 4 ℃ of environment.
By above-mentioned test, can be learnt, assay method of the present invention is easy fast, and accuracy is good, highly sensitive, with low cost, and agents useful for same environmental protection, pollution-free, is applicable to acrylic acid mensuration in workplace air.
test example
With acrylic acid in air of workplace by ion chromatography, its detailed step is as follows:
A. sample and in sampling location, open silicone tube two ends, 150 mg ends are connected with air sampler, flow 0.3 L/min, gathers 15 min, and 2 sections of the front and back silica gel of adopting sample is poured into respectively in 15 ml tool plug test tubes, respectively adds 10 ml 2.0 mmol/L NaHCO
3+ 1.5 mmol/L Na
2cO
3chromatogram eluate desorb, sealing jolting 1 min, standing 30 min, stripping liquid supplies to measure after 0.45 μ m water-based miillpore filter filters; Described air sampler is GilAir-5 air sampler, is equipped with low discharge adjustment module, by U.S. GILIAN company, is produced;
B. chromatographic condition mobile phase: 2.0 mmol/L NaHCO
3+ 1.5 mmol/L Na
2cO
3, flow velocity: 1.0 ml/min, sampling volume: 20 μ l, regenerated liquid: 0.1 mol/L sulfuric acid solution;
C. 10 ml volumetric flasks are got in typical curve preparation, add 5 ml stripping liquids, after accurately weighing, add several acrylic acid, more accurately weigh, with stripping liquid, be settled to scale, mix, by the difference of twice weighing, calculating its concentration, is standard reserving solution, is diluted to 200 μ g/ml acrylic acid standard solution before use with stripping liquid, configure 0.1 μ g/ml, 0.5 μ g/ml, 1.0 μ g/ml, 1.5 μ g/ml, 2.0 μ g/ml, 3.0 μ g/ml, 4.0 μ g/ml acrylic acid standard series, for measuring;
D. in data calculating air, the computing formula of acrylic acid concentration is: C=10 (c
1+ c
2)/(V
0d), wherein C is acrylic acid concentration in air, mg/m
3; c
1,c
2for acrylic acid concentration in section silica gel stripping liquid before and after recording, μ g/ml; 10 is the cumulative volume of stripping liquid, ml; V
0for standard sample volume, L; D is desorption efficiency, %.
The newly-built concrete admixture project of certain building materials enterprise, produce polycarboxylate water-reducer, raw material comprises acrylic acid, by the method for setting up to acrylic acid sampling in its different workplace air, gather altogether 26 duplicate samples, analyze according to the method described above mensuration, result shows only to have 5 samples to detect and contains acrylic acid, content has 2 parts at the sample of 0.2-1.0 μ g/ml, and content has 3 parts at the sample of 1.5-2.5 μ g/ml.Above result all meets country about the short time Exposed limit value of acrylic acid content regulation in workplace air.From on-the-spot sample chromatogram figure (Fig. 2), in scene or silicone tube, there are other materials simultaneously, but analyze noiseless to acrylic acid; Acrylic acid and impurity degree of separation are better, noiseless peak.Result shows that this detection method can be applicable to the detection of acrylic acid content in workplace air.
Claims (7)
1. with acrylic acid in air of workplace by ion chromatography, adopt the airborne acrylic acid in silicone tube collecting work place to complete sampling, adopt 2.0 mmol/L NaHCO
3+ 1.5 mmol/L Na
2cO
3sample introduction after stripping liquid desorb, separated through anion analysis post, chromatogram flow phase is identical with stripping liquid, and electric conductivity detector detects, and will detect data and typical curve contrast, and then substitution computing formula calculates acrylic acid concentration in air.
2. acrylic acid in use air of workplace by ion chromatography according to claim 1, is characterized in that, anion analysis post is Metrosep A SUPP 4-250/4.0 type anion analysis post, and specification is 4.0 mm * 250.0 mm.
3. according to claim 1 with acrylic acid in air of workplace by ion chromatography, it is characterized in that, described sampling concrete steps are: in sampling location, open silicone tube two ends, 150 mg ends are connected with air sampler, flow 0.3 L/min, gather 15 min, 2 sections of the front and back silica gel of adopting sample is poured into respectively in 15 ml tool plug test tubes, respectively add 10 ml 2.0 mmol/L NaHCO
3+ 1.5 mmol/L Na
2cO
3chromatogram eluate desorb, sealing jolting 1 min, standing 30 min, stripping liquid is after filtering for measuring.
4. according to claim 1 with acrylic acid in air of workplace by ion chromatography, it is characterized in that, the configuration of described typical curve is as follows: get 10 ml volumetric flasks, add 5 ml stripping liquids, after accurately weighing, add several acrylic acid, accurately weigh again, with stripping liquid, be settled to scale, mix, by the difference of twice weighing, calculate its concentration, for standard reserving solution, with stripping liquid, be diluted to 200 μ g/ml acrylic acid standard solution before use, configure 0.1 μ g/ml, 0.5 μ g/ml, 1.0 μ g/ml, 1.5 μ g/ml, 2.0 μ g/ml, 3.0 μ g/ml, 4.0 μ g/ml acrylic acid standard series, for measuring.
5. according to claim 1 with acrylic acid in air of workplace by ion chromatography, its detailed step is as follows:
A. sample and in sampling location, open silicone tube two ends, 150 mg ends are connected with air sampler, flow 0.3 L/min, gathers 15 min, and 2 sections of the front and back silica gel of adopting sample is poured into respectively in 15 ml tool plug test tubes, respectively adds 10 ml 2.0 mmol/L NaHCO
3+ 1.5 mmol/L Na
2cO
3chromatogram eluate desorb, sealing jolting 1 min, standing 30 min, stripping liquid is after filtering for measuring;
B. chromatographic condition mobile phase: 2.0 mmol/L NaHCO
3+ 1.5 mmol/L Na
2cO
3, flow velocity: 1.0 ml/min, sampling volume: 20 μ l, regenerated liquid: 0.1 mol/L sulfuric acid solution;
C. 10 ml volumetric flasks are got in typical curve preparation, add 5 ml stripping liquids, after accurately weighing, add several acrylic acid, more accurately weigh, with stripping liquid, be settled to scale, mix, by the difference of twice weighing, calculating its concentration, is standard reserving solution, is diluted to 200 μ g/ml acrylic acid standard solution before use with stripping liquid, configure 0.1 μ g/ml, 0.5 μ g/ml, 1.0 μ g/ml, 1.5 μ g/ml, 2.0 μ g/ml, 3.0 μ g/ml, 4.0 μ g/ml acrylic acid standard series, for measuring;
D. in data calculating air, the computing formula of acrylic acid concentration is: C=10 (c
1+ c
2)/(V
0d), wherein C is acrylic acid concentration in air, mg/m
3; c
1,c
2for acrylic acid concentration in section silica gel stripping liquid before and after recording, μ g/ml; 10 is the cumulative volume of stripping liquid, ml; V
0for standard sample volume, L; D is desorption efficiency, %.
6. according to claim 5 with acrylic acid in air of workplace by ion chromatography, it is characterized in that, air sampler described in a step is GilAir-5 air sampler, is equipped with low discharge adjustment module, by U.S. GILIAN company, is produced.
7. acrylic acid in use air of workplace by ion chromatography according to claim 5, is characterized in that, adopts 0.45 μ m water-based miillpore filter to filter in a step.
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CN110441464A (en) * | 2019-08-09 | 2019-11-12 | 南通化学环境监测站有限公司 | Monoxone method for measurement of concentration in a kind of workplace carboxylic acids |
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