CN103760270B - With acrylic acid in air of workplace by ion chromatography - Google Patents
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- CN103760270B CN103760270B CN201410037155.2A CN201410037155A CN103760270B CN 103760270 B CN103760270 B CN 103760270B CN 201410037155 A CN201410037155 A CN 201410037155A CN 103760270 B CN103760270 B CN 103760270B
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- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 title claims abstract description 76
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 title claims abstract description 76
- 238000004255 ion exchange chromatography Methods 0.000 title claims abstract description 17
- 239000007788 liquid Substances 0.000 claims abstract description 36
- 229920001296 polysiloxane Polymers 0.000 claims abstract description 17
- 238000012360 testing method Methods 0.000 claims abstract description 13
- 238000001514 detection method Methods 0.000 claims description 12
- 238000005070 sampling Methods 0.000 claims description 12
- 150000001450 anions Chemical class 0.000 claims description 11
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 9
- 238000004458 analytical method Methods 0.000 claims description 9
- 239000000741 silica gel Substances 0.000 claims description 9
- 229910002027 silica gel Inorganic materials 0.000 claims description 9
- 239000000243 solution Substances 0.000 claims description 9
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 8
- 238000003795 desorption Methods 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 4
- 239000012086 standard solution Substances 0.000 claims description 4
- 238000005303 weighing Methods 0.000 claims description 4
- 230000001186 cumulative effect Effects 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 3
- 238000002360 preparation method Methods 0.000 claims description 3
- 238000004587 chromatography analysis Methods 0.000 abstract description 11
- 150000002500 ions Chemical class 0.000 abstract description 11
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 abstract description 4
- 230000007613 environmental effect Effects 0.000 abstract description 3
- BVKZGUZCCUSVTD-UHFFFAOYSA-M Bicarbonate Chemical compound OC([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-M 0.000 abstract description 2
- UIIMBOGNXHQVGW-UHFFFAOYSA-M sodium bicarbonate Substances [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 abstract description 2
- 229910000030 sodium bicarbonate Inorganic materials 0.000 abstract description 2
- 235000017557 sodium bicarbonate Nutrition 0.000 abstract description 2
- 229910000029 sodium carbonate Inorganic materials 0.000 abstract description 2
- 238000000034 method Methods 0.000 description 15
- 239000012071 phase Substances 0.000 description 7
- 238000003822 preparative gas chromatography Methods 0.000 description 7
- 238000003556 assay Methods 0.000 description 6
- 239000000126 substance Substances 0.000 description 6
- 238000002474 experimental method Methods 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 4
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 4
- 239000011734 sodium Substances 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 3
- 239000004566 building material Substances 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- -1 carboxylic acid compound Chemical class 0.000 description 2
- 150000001732 carboxylic acid derivatives Chemical class 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 239000003086 colorant Substances 0.000 description 2
- 230000006378 damage Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- 235000019253 formic acid Nutrition 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 230000014759 maintenance of location Effects 0.000 description 2
- 230000001473 noxious effect Effects 0.000 description 2
- 230000001737 promoting effect Effects 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 230000035945 sensitivity Effects 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 241000370738 Chlorion Species 0.000 description 1
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 150000001735 carboxylic acids Chemical class 0.000 description 1
- 239000012159 carrier gas Substances 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- FOCAUTSVDIKZOP-UHFFFAOYSA-N chloroacetic acid Chemical compound OC(=O)CCl FOCAUTSVDIKZOP-UHFFFAOYSA-N 0.000 description 1
- 229940106681 chloroacetic acid Drugs 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- PNDPGZBMCMUPRI-UHFFFAOYSA-N iodine Chemical compound II PNDPGZBMCMUPRI-UHFFFAOYSA-N 0.000 description 1
- 230000007794 irritation Effects 0.000 description 1
- 230000003907 kidney function Effects 0.000 description 1
- 239000010985 leather Substances 0.000 description 1
- 230000003908 liver function Effects 0.000 description 1
- 210000004072 lung Anatomy 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 231100000616 occupational exposure limit Toxicity 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 235000006408 oxalic acid Nutrition 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920005646 polycarboxylate Polymers 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 1
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 230000010076 replication Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 231100000075 skin burn Toxicity 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 229920003002 synthetic resin Polymers 0.000 description 1
- 239000000057 synthetic resin Substances 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 238000009941 weaving Methods 0.000 description 1
Landscapes
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
The invention belongs to the technical field of chemistry in detecting, be specially with acrylic acid in air of workplace by ion chromatography.Acrylic acid is gathered with silicone tube, with a kind of environment friendly and pollution-free sodium carbonate/bicarbonate solution for stripping liquid and chromatogram flow phase, establish a kind of quick, sensitive, accurate, environmental protection and acrylic acid in chromatography of ions testing place air with low cost, this provides new feasible way for measuring acrylic acid in workplace air fast and accurately, and has widened the application of the chromatography of ions in occupational health detects.
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, promoting social harmony stablely has actual meaning.Acrylic acid (crylicacid) is a kind of important organic synthesis raw material and synthetic resin monomer, be mainly used in the industry produce esters of acrylic acid, be widely used in the fields such as daily-use chemical industry, weaving, papermaking, building materials, packaging, metallurgy, leather, plastic processing.Acrylic acid has irritation 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 usually, but there is following shortcoming: 1. detection sensitivity is lower.Detecting of the Propylene By Gas Chromatography acid adopted 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 carry out desorb, can work the mischief to human body and environment with organic solvent such as the acetone etc. that toxicity is larger.3. gas chromatograph need do carrier gas with gas, and be equipped with air-channel system and temperature control program, loaded down with trivial details during operating cost, operating cost cost is higher.Therefore, be necessary to carry out Improvement to assay method acrylic acid in existing workplace air, set up and generally apply and specific accurate, reliable, the sensitive monitoring method of tool.
The chromatography of ions has good, quick, sensitive, the easy advantage of selectivity, and US National 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 mensuration of noxious material " in the workplace air " standard that health State Family Planning Commission of current China issues, only list hydrochloric acid, sulfuric acid, iodine, oxalic acid 4 kinds of ion chromatography methods, the detection of most of material also rests in vapor-phase chromatography, and vapor-phase chromatography exists, and operating cost is higher, coexisting substances interference, 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, improving the application of chromatography of ions in occupational health detects, stepping up to be very important to the research of noxious material chromatography of ions detection method in workplace air.
Summary of the invention
The object of the invention is to the defect for above-mentioned existence, and acrylic acid in one air of workplace by ion chromatography is provided, acrylic acid is gathered with silicone tube, with a kind of environment friendly and pollution-free sodium carbonate/bicarbonate solution for stripping liquid and chromatogram flow phase, establish a kind of quick, sensitive, accurate, environmental protection and acrylic acid in chromatography of ions testing place air with low cost, this has widened the application of the chromatography of ions in occupational health detects, in workplace, the detection of carboxylic acids objectionable impurities provides new feasible way.
Technical scheme of the present invention is:
With acrylic acid in air of workplace by ion chromatography, adopt the acrylic acid in the air of silicone tube collecting work place to complete sampling, adopt 2.0mmol/LNaHCO
3+ 1.5mmol/LNa
2cO
3sample introduction after stripping liquid desorb, be separated through anion analysis post, chromatogram flow phase is identical with stripping liquid, and electric conductivity detector detection, will detect data and typical curve contrasts, and then substitutes into computing formula and calculates acrylic acid concentration in air.
As preferably, described anion analysis post is MetrosepASUPP4-250/4.0 type anion analysis post, and specification is 4.0mm × 250.0mm.
As preferably, described sampling concrete steps are: open silicone tube two ends in sampling location, are connected by 150mg end with air sampler, flow 0.3L/min, gather 15min, 2 sections, the front and back silica gel adopting sample is poured in 15ml tool plug test tube respectively, respectively adds 10ml2.0mmol/LNaHCO
3+ 1.5mmol/LNa
2cO
3chromatogram eluate desorb, closes jolting 1min, leaves standstill 30min, and stripping liquid is after filtering for measuring.
As preferably, the configuration of described typical curve is as follows: get 10ml volumetric flask, add 5ml stripping liquid, several acrylic acid are added after precise, precise again, scale is settled to stripping liquid, mixing, its concentration is calculated by the difference of twice weighing, for standard reserving solution, be diluted to 200 μ g/ml acrylic acid standard solution with stripping liquid 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 mensuration.
Acrylic acid in air of workplace by ion chromatography of the present invention, its detailed step is as follows:
A. sample and open silicone tube two ends in sampling location, be connected by 150mg end with air sampler, flow 0.3L/min, gathers 15min, is poured into respectively in 15ml tool plug test tube by 2 sections, the front and back silica gel adopting sample, respectively add 10ml2.0mmol/LNaHCO
3+ 1.5mmol/LNa
2cO
3chromatogram eluate desorb, closes jolting 1min, leaves standstill 30min, and stripping liquid is after filtering for measuring;
B. chromatographic condition mobile phase: 2.0mmol/LNaHCO
3+ 1.5mmol/LNa
2cO
3, flow velocity: 1.0ml/min, sampling volume: 20 μ l, regenerated liquid: 0.1mol/L sulfuric acid solution;
C. 10ml volumetric flask is got in typical curve preparation, add 5ml stripping liquid, several acrylic acid are added after precise, then precise, be settled to scale with stripping liquid, mixing, calculating its concentration by the difference of twice weighing, 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 mensuration;
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 recording acrylic acid concentration in the section silica gel stripping liquid of front and back, 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, is produced by GILIAN company of the U.S..
As preferably, 0.45 μm of water-based miillpore filter in a step, is adopted to filter.
Beneficial effect of the present invention is:
The present invention establishes acrylic acid ion chromatography method in workplace, and method adopts silicone tube collected specimens, adopts NaHCO
3-Na
2cO
3stripping liquid desorb, adopts 2.0mmol/LNaHCO
3+ 1.5mmol/LNa
2cO
3mobile phase, flow velocity 1.0ml/min, measures, and 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, and linearly dependent coefficient is 0.9999, with signal to noise ratio (S/N ratio) (
s/N) be that 3 defining method detect and are 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%, and sample at least stablely at 4 DEG C can preserve 7d.Adopt the method to measure acrylic acid in certain building materials enterprise workplace air, achieve good result, Common Anions and other impurity of the interior existence of on-the-spot or silicone tube 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 is that the harm of accurate evaluation acrylic acid to health provides effective mensuration means, provides reference frame for studying carboxylic-acid substance in ion chromatography workplace air further.
As fully visible, method of the present invention is by selecting rational condition and equipment combination, by selecting the coordinative role of each steps such as suitable typical curve configuration, suitable Selecting parameter, achieve the application of ion chromatography method with in acrylic acid mensuration, and the method is quick, sensitive, accurately, with low cost, be applicable to acrylic acid in workplace air detect, this result of study contributes to promoting the application development of the chromatography of ions in occupational health testing, possesses outstanding substantive distinguishing features and progress significantly.
Accompanying drawing explanation
Fig. 1 is Common Anions and acrylic acid separate colors spectrogram, 1-F
-, 2-crylicacid, 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, MetrosepASUPP4-250/4.0 type anion analysis post (4.0mm × 250.0mm) (Wan Tong company of Switzerland), GilAir-5 air sampler (being equipped with low discharge adjustment module) (GILIAN company of the U.S.), silicone tube (solvent desorption type, in-built 300mg/150mg silica gel) (Yancheng purple light Electron equipment Co., Ltd), 0.45 μm of 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., lot number: 20130323), deionized water (resistivity >18.0M 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, the anion chromatographic behavior common due to acrylic acid and part is similar, particularly with the retention time of fluorine ion, chlorion relatively, therefore need to select suitable chromatographic column and chromatographic condition to analyze, through Optimal Experimental, find to adopt 2.0mmol/LNaHCO
3+ 1.5mmol/LNa
2cO
3mobile phase, flow velocity 1.0ml/min, acrylic acid can with F
-, Cl
-be separated completely, acrylic acid retention time is 4.46min.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, analyze standard series sample, 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 to detect and be limited to 0.0033 μ g/ml, by sampling volume 4.5L, concentration limit is 0.0073mg/m
3.The vapor-phase chromatography adopted in current China occupational health standard the assay method of carboxylic acid compound " in the workplace air " (GBZ/T160.59-2004) detects and is limited to 100 μ g/ml, and concentration limit is 3.3mg/m
3.Can compare thus and draw, its sensivity index such as detection limit and concentration limit of this chromatography of ions is obviously better than vapor-phase chromatography.
3. Precision Experiment
Under selected chromatographic condition, get that concentration is 1.0 μ g/ml, the acrylic acid samples of 2.0 μ g/ml, 3.0 μ g/ml is analyzed, often kind of concentration replication 6 times, the results are shown in Table 1, acrylic acid
rSDfor 0.89%-1.15%, meet " in workplace air chemical substance assay method " requirement.
table 1 Precision Experiment result (
n=6)
4. analyzing efficiency experiment
Adopt NaHCO
3-Na
2cO
3solution as stripping liquid, the acetone stripping liquid that in GB of comparing the assay method of carboxylic acid compound " in the workplace air " (GBZ/T160.59-2004), 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, respectively add 10 μ g, 20 μ g, 30 μ g acrylic acid, immediately sealed silicon sebific ducts with micro syringe.Placement is spent the night, and is poured in 20ml tool plug test tube by 2 sections, front and back silica gel, adds the desorb of 10ml leacheate, jam-pack pipe close, jolting 1min, and after placing 1h, sample introduction 20 μ l analyzes.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 " in workplace air chemical substance assay method " requirement.
table 2 desorption efficiency measurement result
5. sample stability experiment
Get 12 silicone tubes, add a certain amount of acrylic acid respectively, sealed silicon sebific duct immediately, first random taking-up 3 silicone tubes analyze mensuration immediately, and all the other are placed in the preservation of 4 DEG C, refrigerator, then carry out analysis respectively at 3d, 5d, 7d and measure, calculate the loss percentage depositing different time sample, experimental result shows, its average recovery rate after 7d deposited by sample is 95.2%, shows that sample at least can preserve 7d under 4 DEG C of environment.
Can be learnt by above-mentioned test, assay method of the present invention is fast easy, 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 open silicone tube two ends in sampling location, be connected by 150mg end with air sampler, flow 0.3L/min, gathers 15min, is poured into respectively in 15ml tool plug test tube by 2 sections, the front and back silica gel adopting sample, respectively add 10ml2.0mmol/LNaHCO
3+ 1.5mmol/LNa
2cO
3chromatogram eluate desorb, closes jolting 1min, leaves standstill 30min, and stripping liquid supplies to measure after 0.45 μm of water-based miillpore filter filters; Described air sampler is GilAir-5 air sampler, is equipped with low discharge adjustment module, is produced by GILIAN company of the U.S.;
B. chromatographic condition mobile phase: 2.0mmol/LNaHCO
3+ 1.5mmol/LNa
2cO
3, flow velocity: 1.0ml/min, sampling volume: 20 μ l, regenerated liquid: 0.1mol/L sulfuric acid solution;
C. 10ml volumetric flask is got in typical curve preparation, add 5ml stripping liquid, several acrylic acid are added after precise, then precise, be settled to scale with stripping liquid, mixing, calculating its concentration by the difference of twice weighing, 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 mensuration;
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 recording acrylic acid concentration in the section silica gel stripping liquid of front and back, 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 foundation to acrylic acid sampling in its different workplace air, gather 26 increment product altogether, carry out analysis according to the method described above and measure, result shows only have 5 samples to detect containing 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 the short time occupational exposure limit that country specifies about acrylic acid content in workplace air.From field sample chromatogram (Fig. 2), in scene or silicone tube, there are other materials simultaneously, but analyze noiseless to acrylic acid; Acrylic acid and magazins' layout degree are better, noiseless peak.Result shows that this detection method can be applicable to the detection of acrylic acid content in workplace air.
Claims (3)
1., with acrylic acid in air of workplace by ion chromatography, adopt the acrylic acid in the air of silicone tube collecting work place to complete sampling, adopt 2.0mmol/LNaHCO
3+ 1.5mmol/LNa
2cO
3sample introduction after stripping liquid desorb, be separated through anion analysis post, chromatogram flow phase is identical with stripping liquid, and electric conductivity detector detection, will detect data and typical curve contrasts, and then substitutes into computing formula and calculates acrylic acid concentration in air; Its detailed step is as follows:
A. sample and open silicone tube two ends in sampling location, be connected by 150mg end with air sampler, flow 0.3L/min, gathers 15min, is poured into respectively in 15ml tool plug test tube by 2 sections, the front and back silica gel adopting sample, respectively add 10ml2.0mmol/LNaHCO
3+ 1.5mmol/LNa
2cO
3chromatogram eluate desorb, closes jolting 1min, leaves standstill 30min, and stripping liquid is after filtering for measuring;
B. chromatographic condition mobile phase: 2.0mmol/LNaHCO
3+ 1.5mmol/LNa
2cO
3, flow velocity: 1.0ml/min, sampling volume: 20 μ l, regenerated liquid: 0.1mol/L sulfuric acid solution;
C. 10ml volumetric flask is got in typical curve preparation, add 5ml stripping liquid, several acrylic acid are added after precise, then precise, be settled to scale with stripping liquid, mixing, calculating its concentration by the difference of twice weighing, 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 mensuration;
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 recording acrylic acid concentration in the section silica gel stripping liquid of front and back, μ g/ml; 10 is the cumulative volume of stripping liquid, ml; V
0for standard sample volume, L; D is desorption efficiency, %;
Described anion analysis post is MetrosepASUPP4-250/4.0 type anion analysis post, and specification is 4.0mm × 250.0mm.
2. acrylic acid in air of workplace by ion chromatography according to claim 1, it is characterized in that, air sampler described in a step is GilAir-5 air sampler, is equipped with low discharge adjustment module, is produced by GILIAN company of the U.S..
3. acrylic acid in air of workplace by ion chromatography according to claim 1, is characterized in that, adopts 0.45 μm of water-based miillpore filter to filter in a step.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410037155.2A CN103760270B (en) | 2014-01-26 | 2014-01-26 | With acrylic acid in air of workplace by ion chromatography |
Applications Claiming Priority (1)
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| GB0605427D0 (en) * | 2006-03-17 | 2006-04-26 | Univ Cranfield | Materials For Binding Drugs Of Abuse |
| JP4860419B2 (en) * | 2006-10-11 | 2012-01-25 | 昭和電工株式会社 | Simultaneous analysis of anions using ion chromatography |
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