CN102854269B - Method for measuring concentration of elemental substance sulfur in air - Google Patents
Method for measuring concentration of elemental substance sulfur in air Download PDFInfo
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- CN102854269B CN102854269B CN201210384375.3A CN201210384375A CN102854269B CN 102854269 B CN102854269 B CN 102854269B CN 201210384375 A CN201210384375 A CN 201210384375A CN 102854269 B CN102854269 B CN 102854269B
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- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 title claims abstract description 129
- 238000000034 method Methods 0.000 title abstract description 14
- 239000011593 sulfur Substances 0.000 title abstract description 7
- 229910052717 sulfur Inorganic materials 0.000 title abstract description 7
- 239000000126 substance Substances 0.000 title abstract 6
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 claims abstract description 34
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims abstract description 31
- 150000002500 ions Chemical class 0.000 claims abstract description 18
- 235000010265 sodium sulphite Nutrition 0.000 claims abstract description 17
- DWAQJAXMDSEUJJ-UHFFFAOYSA-M Sodium bisulfite Chemical compound [Na+].OS([O-])=O DWAQJAXMDSEUJJ-UHFFFAOYSA-M 0.000 claims abstract description 14
- 235000010267 sodium hydrogen sulphite Nutrition 0.000 claims abstract description 12
- 238000004458 analytical method Methods 0.000 claims abstract description 8
- 239000011259 mixed solution Substances 0.000 claims abstract description 7
- 239000007788 liquid Substances 0.000 claims description 70
- 238000010521 absorption reaction Methods 0.000 claims description 62
- 238000005070 sampling Methods 0.000 claims description 49
- 238000003556 assay Methods 0.000 claims description 18
- 239000012086 standard solution Substances 0.000 claims description 18
- 235000011187 glycerol Nutrition 0.000 claims description 14
- 238000005406 washing Methods 0.000 claims description 6
- 238000010828 elution Methods 0.000 claims description 5
- 239000004289 sodium hydrogen sulphite Substances 0.000 claims description 5
- 238000005349 anion exchange Methods 0.000 claims description 4
- 238000012360 testing method Methods 0.000 abstract description 10
- 239000000243 solution Substances 0.000 abstract description 7
- 238000001514 detection method Methods 0.000 abstract description 6
- 239000003153 chemical reaction reagent Substances 0.000 abstract description 2
- 230000035945 sensitivity Effects 0.000 abstract description 2
- 229940079827 sodium hydrogen sulfite Drugs 0.000 abstract 1
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 9
- 238000004519 manufacturing process Methods 0.000 description 6
- 238000011084 recovery Methods 0.000 description 4
- 239000011734 sodium Substances 0.000 description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 239000005864 Sulphur Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 206010006458 Bronchitis chronic Diseases 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 239000002250 absorbent Substances 0.000 description 1
- 230000002745 absorbent Effects 0.000 description 1
- 206010006451 bronchitis Diseases 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 208000007451 chronic bronchitis Diseases 0.000 description 1
- 230000001684 chronic effect Effects 0.000 description 1
- 231100000762 chronic effect Toxicity 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- OMZSGWSJDCOLKM-UHFFFAOYSA-N copper(II) sulfide Chemical compound [S-2].[Cu+2] OMZSGWSJDCOLKM-UHFFFAOYSA-N 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000003337 fertilizer Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000002085 irritant Substances 0.000 description 1
- 231100000021 irritant Toxicity 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000012046 mixed solvent Substances 0.000 description 1
- 210000003695 paranasal sinus Anatomy 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 208000023504 respiratory system disease Diseases 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical compound [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000005486 sulfidation Methods 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- -1 volume is 5-50mL Substances 0.000 description 1
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Abstract
The invention discloses a high-sensitivity, accurate and rapid method for measuring the concentration of elemental substance sulfur in indoor and outdoor air environments. The method comprises the following steps of: acquiring air through an air sampler; absorbing the elemental substance sulfur in the air by using the mixed solution of sodium sulfite (or sodium hydrogensulfite) and glycerol so as to quantitatively convert the elemental substance sulfur into S2O3<2->; and measuring the concentration of S2O3<2-> in the absorbed solution by using an ion chromatograph with an electrical conductivity detector, and further converting the concentration of S2O3<2-> into the concentration of the elemental substance sulfur in the air. The method is high in sensitivity, accurate in result, high in repeatability, simple in experimental steps and high in analysis speed, the detection limit of the elemental sulfur in the air can reach 1 mu g/m<3>, the detection can be finished through two steps only, the testing time is only 15 minutes, and the reagent is pollution-free and safe. The method has significance of measuring the concentration of the elemental substance sulfur in the indoor and outdoor air environments.
Description
Technical field
The present invention relates in a kind of air detection field the assay method of elemental sulfur concentration in various indoor-outdoor air environment.
Background technology
Elemental sulfur at occurring in nature ubiquity, is yellow crystals (being commonly called as sulphur) that different from its reducibility gas product, elemental sulfur does not have smell.Elemental sulfur is widely used in industry, is mainly used in the sulfidation of rubber, and it can be used for manufacturing multiple sulfocompound (as sodium sulphide, copper sulfide, sulfuric acid etc.) as starting material, also can be used for preparing pesticide, germifuge and fertilizer.
Elemental sulfur toxicity is lower, less to Health Impact, but known according to Long Term Contact sulphur dirt miner's professional research report, elemental sulfur comprises vision, respiratory disorders to healthy impact, chronic bronchitis and nasal sinus problem, the workman who is coated with stain sulfur-bearing dirt material also often has eyes and skin irritant problem to occur.Elemental sulfur has sublimable feature, be sublimate into airborne elemental sulfur and can produce Chronic Effect to health on the one hand, can produce corrosion to the metallic article such as copper, silver on the other hand, greatly shorten life of product, as cause circuit board damage, electron device malfunctioning etc.
Owing to it is conventionally believed that elemental sulfur is to exist with solid-state form, ignored in air and also had elemental sulfur (gaseous state), so the assay method of elemental sulfur concentration in air all not studies have reported that to there is no relevant examination criteria and limit index all the time yet.Therefore the assay method of, setting up elemental sulfur concentration in a kind of air for the harmfulness of research elemental sulfur, that elemental sulfur concentration in air is carried out to reasonable classification is significant.
Summary of the invention
The object of this invention is to provide a kind of highly sensitive, assay method of elemental sulfur concentration in indoor-outdoor air environment accurately and rapidly.
The assay method of elemental sulfur concentration in a kind of air provided by the present invention, comprises the following steps:
1) collection of elemental sulfur sample in air: gather air sample with air sampler, absorption liquid is the mixed solution of glycerine and sodium sulphite (or sodium bisulfite), and elemental sulfur in air sample is converted into S
2o
3 2-, liquid sample is absorbed;
2) measure: with ion chromatograph (band electric conductivity detector), measure the peak area value of absorption liquid sample, measure the peak area value of the blank of corresponding absorption liquid simultaneously, the peak area value that deducts blank with the sample peak area value recording obtains a difference A;
3) making of typical curve: measure the elemental sulfur standard solution of concentration known with ion chromatograph (band electric conductivity detector), the peak area (μ Smin) of take is ordinate, and the elemental sulfur concentration (μ g/L) of take is horizontal ordinate, obtains standard working curve;
4) concentration of the corresponding elemental sulfur of difference A the determining of elemental sulfur concentration in absorption liquid sample: according to the standard working curve determining step 2 of step 3)), elemental sulfur concentration c in the liquid sample that is absorbed (μ g/L);
5) calculating of elemental sulfur concentration in air: according to absorption liquid volume V(mL), formula (1) calculates the sampling volume V under the status of criterion
0(L) elemental sulfur concentration c (μ g/L) calculates concentration (the μ g/m of elemental sulfur in air and in absorption liquid sample
3).
Wherein: the flow velocity of sampling in described step 1) is 0.5-2L/min, and the sampling time is 5-30min, in absorption liquid, sodium sulphite or concentration of sodium bisulphite are 5-15mM, and the content of glycerine is 0.1~5wt%, and absorption liquid volume is 5-50mL; Preferred sampling flow velocity 1L/min, sampling time 20min, sodium sulphite or concentration of sodium bisulphite 10mM in absorption liquid, glycerine content 0.5wt%, absorption liquid volume 10mL.
Step 2) and the ion chromatograph condition determination with electric conductivity detector described in step 3) be: anion-exchange column adopts As18 type separating column (250mm * 4mm) or AG18 type guard column (50mm * 4mm); mobile phase adopts 20-40mmol/L KOH drip washing such as degree of grade or gradient elution; flow rate of mobile phase is 0.8-2.0mL/min; sample size 5-1000 μ l; be 15min analysis time, 30 ℃ of column temperatures.
The concentration of the elemental sulfur standard solution of concentration known described in step 3) is respectively 2 μ g/L, 10 μ g/L, 25 μ g/L, 50 μ g/L, 100 μ g/L.
In step 5), according to the running parameter of air sampler, by formula (1), calculate the sampling volume V under its status of criterion
0(L), by formula (2), calculate the concentration of elemental sulfur in air;
In formula:
V
0for the sampling volume under the status of criterion, unit is L;
V is the sampling flow velocity of air sampler, and unit is L/min;
T is the sampling time, and unit is min;
T
0for the absolute temperature of the status of criterion, 273K;
The air themperature that T is when sampling, unit is ℃;
P
0for the atmospheric pressure of the status of criterion, 101.3kPa;
Atmospheric pressure when P is sampling, unit is kPa;
In formula:
C
sfor the concentration of elemental sulfur in air sample, unit is μ g/m
3;
C is the concentration of elemental sulfur in absorption liquid, according to the typical curve of drawing, calculates, and unit is μ g/L;
V is absorption liquid volume, and unit is mL;
V
0for the sampling volume under the status of criterion, unit is L.
Concrete, the inventive method comprises the following steps:
1) collection of elemental sulfur sample in air: gather air sample with air sampler, the sodium sulphite (Na that absorption liquid is 10mM for the concentration containing 0.5wt% glycerine
2sO
3) solution, volume is 5-50mL, liquid sample is absorbed; Air sampler sampling flow velocity is 0.5-2L/min, and the sampling time is 5-30min;
2) measure: with the ion chromatograph with electric conductivity detector, measure the peak area value of absorption liquid sample, measure the peak area value of the blank of corresponding absorption liquid simultaneously, the peak area value that deducts blank with the sample peak area value recording obtains a difference A; Condition determination is: anion-exchange column adopts As18 type separating column (250mm * 4mm) or AG18 type guard column (50mm * 4mm), mobile phase adopts 20-40mmol/L KOH drip washing such as degree of grade or gradient elution, flow rate of mobile phase is 0.8-2.0mL/min, sample size 5-1000 μ l, be 15min analysis time, 30 ℃ of column temperatures;
3) making of typical curve: with the ion chromatograph of electric conductivity detector in step 2) measure respectively the peak area value that concentration is the elemental sulfur standard solution of 2 μ g/L, 10 μ g/L, 25 μ g/L, 50 μ g/L, 100 μ g/L under described condition determination, the peak area (μ Smin) of take is ordinate, the elemental sulfur concentration (μ g/L) of take is horizontal ordinate, obtains standard working curve;
4) concentration of the corresponding elemental sulfur of difference A the determining of elemental sulfur concentration in absorption liquid sample: according to the standard working curve determining step 2 of step 3)), elemental sulfur concentration c in the liquid sample that is absorbed (μ g/L);
5) calculating of elemental sulfur concentration in air: according to absorption liquid volume V(mL), formula (1) calculates the sampling volume V under the status of criterion
0(L) elemental sulfur concentration c (μ g/L) and in absorption liquid sample, calculates concentration (the μ g/m of elemental sulfur in air by formula (2)
3).
The invention provides a kind of highly sensitive, assay method of elemental sulfur concentration in indoor-outdoor air environment accurately and rapidly.The method is to gather air with air sampler, and the mixed solution of certain density sodium sulphite for airborne elemental sulfur (or sodium bisulfite) and glycerine absorbs, and by elemental sulfur Quantitative yield, is S
2o
3 2-, with ion chromatograph (band electric conductivity detector), measure the S in absorption liquid
2o
3 2-concentration, is further scaled elemental sulfur, thereby obtains the concentration of elemental sulfur in air.The present invention has the following advantages:
1, highly sensitive: at sampling volume 20L, under the condition of sampling volume 25 μ L, the detection limit of measuring elemental sulfur in air by method of the present invention can reach 1 μ g/m
3;
2, result is accurate, reproducible;
3, experimental procedure is simple: only need 2 steps can complete detection;
4, analysis speed is fast: the test duration only needs 15min;
5, reagent is pollution-free, safety.
In sum, the present invention, by playing a significant role in the mensuration of elemental sulfur concentration in indoor-outdoor air environment, has a extensive future.
Below in conjunction with specific embodiment, the present invention is described in further details.
Accompanying drawing explanation
Fig. 1 surveys the typical curve of elemental sulfur in air in the present invention.
Embodiment
The object of this invention is to provide a kind of highly sensitive, assay method of elemental sulfur concentration in indoor-outdoor air environment accurately and rapidly.
The assay method of elemental sulfur concentration provided by the present invention, can comprise the following steps:
1) collection of elemental sulfur sample in air: with 5-50mL sodium sulphite (Na
2sO
3) or sodium bisulfite (NaHSO
3) and the mixed solution of glycerine (in mixed solution, the concentration of sodium sulphite or sodium bisulfite is 5~15mM, the content of glycerine is 0.1~5wt%) as absorption liquid, with air sampler, gather air, gas production flow velocity is 0.5-2L/min, and the gas production time is 5-30min.During air sampler gas production, gas can pass through absorption liquid, is directly absorbed by liquid absorption, and elemental sulfur is wherein converted into S by sodium sulphite or solution of sodium bisulfite absorption
2o
3 2-, Equation formula is: S+SO
3 2-=S
2o
3 2-;
2) mensuration of elemental sulfur concentration in absorption liquid:
With ion chromatograph (band electric conductivity detector), measure the elemental sulfur standard solution of concentration known, the elemental sulfur peak area A (μ Smin) recording of take is ordinate, the concentration c (μ g/L) of elemental sulfur of take is horizontal ordinate, obtains standard working curve (as Fig. 1);
With ion chromatograph (electric conductivity detector), measure the peak area value of blank (absorption liquid contrast) and absorption liquid sample, with the sample peak area value recording, deduct after the peak area value (this peak area value corresponding be elemental sulfur) of blank, then according to the be absorbed concentration (μ g/L) of elemental sulfur in liquid of typical curve;
3) calculating of elemental sulfur concentration in air:
According to formula (1), calculate the sampling volume under the status of criterion, according to formula (2), calculate the concentration of elemental sulfur in air:
In formula:
V
0for the sampling volume under the status of criterion, unit is L;
V is the sampling flow velocity of air sampler, and unit is L/min;
T is the sampling time, and unit is min;
T
0for the absolute temperature of the status of criterion, 273K;
The air themperature that T is when sampling, unit is ℃;
P
0for the atmospheric pressure of the status of criterion, 101.3kPa;
Atmospheric pressure when P is sampling, unit is kPa;
In formula:
C
sfor the concentration of elemental sulfur in air sample, unit is μ g/m
3;
C is the concentration of elemental sulfur in absorption liquid, according to the typical curve of drawing, calculates, and unit is μ g/L;
V is absorption liquid volume, and unit is mL;
V
0for the sampling volume under the status of criterion, unit is L.
In concrete operations, sampling flow velocity v is preferably 1L/min, and the sampling time, t was preferably 20min, sodium sulphite (Na in absorption liquid
2sO
3) or sodium bisulfite (NaHSO
3) concentration be preferably 10mM, the concentration of glycerine is preferably 0.5wt%, absorption liquid volume is preferably 10mL.
In the bent making of standard operation, the concentration of the elemental sulfur standard solution of horizontal ordinate concentration known can be respectively 2 μ g/L, 10 μ g/L, 25 μ g/L, 50 μ g/L, 100 μ g/L; What peak area value that ordinate records was corresponding is the data of elemental sulfur.
With ion chromatograph (band electric conductivity detector), measure S in absorption liquid
2o
3 2-the chromatographic determination condition of concentration is: chromatographic column adopting As 18 type separating columns (250mm * 4mm) and AG18 type guard column (50mm * 4mm); mobile phase adopts 20-40mmol/L KOH drip washing such as degree of grade or gradient elution; flow rate of mobile phase is 0.8-2.0mL/min; sample size 5-1000 μ L, 30 ℃ of column temperatures.
Embodiment implements take technical solution of the present invention under prerequisite, provided detailed embodiment and concrete operating process, but protection scope of the present invention is not limited to following embodiment.
In following embodiment, method therefor is conventional method if no special instructions.
Embodiment: the mensuration of elemental sulfur concentration in the air ambient of indoor and outdoor
By method of the present invention, elemental sulfur concentration in the air ambient of indoor and outdoor is detected, specifically comprises the following steps:
One, the collection of elemental sulfur sample in air
Sodium sulphite (the Na that the 10mL of take is 10mM containing the concentration of 0.5wt% glycerine
2sO
3) solution is as absorption liquid, with air sampler, gathers air, gas production flow velocity is 1L/min, the gas production time is 20min, records sampling volume (20L).
During collected specimens, should establish blank simultaneously, blank carries out as follows: an absorption bottle that 10mL sodium sulphite absorption liquid is housed is brought to sampled point, except not connecting air sampler, gather air sample, all the other operate same sample collection, as the blank of sample.
Two, the mensuration of elemental sulfur concentration in absorption liquid
1, the preparation of elemental sulfur standard solution
100mg/L elemental sulfur standard solution: accurately take the pure sublimed sulfur 0.1000g of top grade in 300mL glass beaker, add wherein (by volume 95% methyl alcohol+5% phenixin) mixed solvent 200mL, after dissolving completely, sublimed sulfur is transferred in 1000mL volumetric flask, with methyl alcohol, be diluted to graticule, shake up, be stored in vial.
1mg/L elemental sulfur standard solution: accurately pipette 100mg/L elemental sulfur standard solution 1mL, to 100mL volumetric flask, be diluted to scale with methyl alcohol, shake up, be stored in vial.
Elemental sulfur standard solution series: pipette respectively elemental sulfur standard solution 20 μ l, 100 μ l, 250 μ l, 0.5mL, the 1mL of above-mentioned 1mg/L in 10mL volumetric flask, by absorbent solution, be diluted to scale, shake up, obtain standard solution series 2 μ g/L, 10 μ g/L, 25 μ g/L, 50 μ g/L, the 100 μ g/L of elemental sulfur.
2, the mensuration of elemental sulfur concentration in the drafting of standard working curve and absorption liquid
With the ion chromatograph with electric conductivity detector, measure the elemental sulfur standard solution that concentration is respectively 2 μ g/L, 10 μ g/L, 25 μ g/L, 50 μ g/L, 100 μ g/L, chromatographic determination condition is: chromatographic column adopting As18 type separating column (250mm * 4mm) and AG18 type guard column (50mm * 4mm), mobile phase adopts drip washing such as 35mmol/LKOH degree of grade, flow rate of mobile phase is 1mL/min, sample size 25 μ L, be 15min, 30 ℃ of column temperatures analysis time (referring to that absorption liquid injects the analysis time of instrument); Then, with peak area A (μ Smin, what this peak area value was corresponding is elemental sulfur), be ordinate, the concentration c (μ g/L) of take is horizontal ordinate, obtains standard working curve, sees Fig. 1.
Then, with the peak area value (this peak area value corresponding be elemental sulfur) of measuring blank and absorption liquid sample under this ion chromatograph (band electric conductivity detector) similarity condition, the peak area value of blank is 0, the peak area value of absorption liquid sample is 0.0141, the peak area value that deducts blank with the sample peak area value recording is 0.0141, then is 28.5(μ g/L according to the typical curve inquiry concentration (c) of elemental sulfur in liquid that is absorbed).
Three, the calculating of elemental sulfur concentration in air
According to formula (1) and formula (2), calculate the concentration of elemental sulfur in air:
V is the sampling flow velocity of air sampler, is 1.0L/min;
T is the sampling time, is 20min;
T
0for the absolute temperature of the status of criterion, 273K;
Air themperature when T is sampling is 25 ℃;
P
0for the atmospheric pressure of the status of criterion, 101.3kPa;
Atmospheric pressure when P is sampling is 101.3kPa;
According to formula (1), calculate the sampling volume V under the status of criterion
0, be 18.3L;
By absorption liquid volume V(10mL), the concentration c of elemental sulfur in the absorption liquid obtaining according to typical curve (28.5 μ g/L) and formula (1) calculate the sampling volume V under the status of criterion
0(18.3L) substitution formula (2), obtains the concentration C of elemental sulfur in air sample
s(15.6 μ g/m
3).
Test one, precision test
Select elemental sulfur concentration to be respectively 2 μ g/L(numberings 1), 10 μ g/L(numberings 2) two standard solution, by the step 2 in embodiment, distinguish METHOD FOR CONTINUOUS DETERMINATION 6 times, calculate its relative standard deviation (n=6).
Measurement result is as shown in table 1, shows that the assay method of elemental sulfur concentration of the present invention has higher precision.
Table 1 Precision test result unit: μ g/L
Test two, recovery test
In elemental sulfur concentration (with c
1represent) be in the absorption liquid sample of 5 μ g/L, to add respectively the elemental sulfur standard solution of high concentration, add scalar (with c
irepresent) be 2 μ g/L(numberings 1) and 10 μ g/L(numbering 2), by elemental sulfur concentration in solution after the method mensuration mark-on in embodiment (with c
2represent), calculate recovery rate η.
η=(c
2-c
1)÷c
i×100%
Mensuration and result of calculation are as shown in table 2, show that the assay method of elemental sulfur concentration in air sample of the present invention has the higher recovery.
Table 2 recovery test result
Test three, sensitivity test
At air sample sampling volume 20L, under the condition of ion chromatograph sampling volume 25 μ l, by the method in embodiment 1, measure the air sample that contains variable concentrations elemental sulfur, in result air sample, the detection limit of elemental sulfur can reach 1 μ g/m
3.
Claims (7)
1. an assay method for elemental sulfur concentration in air, comprises the following steps:
1) collection of elemental sulfur sample in air: gather air sample with air sampler, absorption liquid is the mixed solution of glycerine and sodium sulphite or sodium bisulfite, and elemental sulfur in air sample is converted into S
2o
3 2-, liquid sample is absorbed;
2) measure: with the ion chromatograph with electric conductivity detector, measure the peak area value of absorption liquid sample, measure the peak area value of the blank of corresponding absorption liquid simultaneously, the peak area value that deducts blank with the sample peak area value recording obtains a difference A;
3) making of typical curve: measure the elemental sulfur standard solution of concentration known with the ion chromatograph with electric conductivity detector, take peak area as ordinate, take elemental sulfur concentration as horizontal ordinate, obtain standard working curve; Peak area unit is μ Smin, and elemental sulfur concentration unit is μ g/L;
4) concentration of the corresponding elemental sulfur of difference A the determining of elemental sulfur concentration in absorption liquid sample: according to the standard working curve determining step 2 of step 3)), elemental sulfur concentration c in the liquid sample that is absorbed, unit is μ g/L;
5) calculating of elemental sulfur concentration in air: according to absorption liquid volume V, unit is that mL, formula (1) calculate the sampling volume V under the status of criterion
0calculate the concentration of elemental sulfur in air with elemental sulfur concentration c in absorption liquid sample, unit is μ g/m
3;
In formula:
V
0for the sampling volume under the status of criterion, unit is L;
V is the sampling flow velocity of air sampler, and unit is L/min;
T is the sampling time, and unit is min;
T
0for the absolute temperature of the status of criterion, 273K;
The air themperature that T is when sampling, unit is ℃;
P
0for the atmospheric pressure of the status of criterion, 101.3kPa;
Atmospheric pressure when P is sampling, unit is kPa.
2. assay method according to claim 1, it is characterized in that: the flow velocity of sampling in described step 1) is 0.5-2L/min, and the sampling time is 5-30min, in absorption liquid, sodium sulphite or concentration of sodium bisulphite are 5-15mM, the content of glycerine is 0.1~5wt%, and absorption liquid volume is 5-50mL.
3. assay method according to claim 2, is characterized in that: sampling flow velocity 1L/min, sampling time 20min, sodium sulphite or concentration of sodium bisulphite 10mM in absorption liquid, glycerine content 0.5wt%, absorption liquid volume 10mL.
4. assay method according to claim 1; it is characterized in that: step 2) and step 3) described in ion chromatograph condition determination be: anion-exchange column adopts the As18 type separating column of 250mm * 4mm and the AG18 type guard column of 50mm * 4mm; mobile phase adopts 20-40mmol/L KOH drip washing such as degree of grade or gradient elution; flow rate of mobile phase is 0.8-2.0mL/min; sample size 5-1000 μ l; be 15min analysis time, 30 ℃ of column temperatures.
5. assay method according to claim 1, is characterized in that: the concentration of the elemental sulfur standard solution of concentration known described in step 3) is respectively 2 μ g/L, 10 μ g/L, 25 μ g/L, 50 μ g/L, 100 μ g/L.
6. according to the assay method described in claim 1 or 2 or 3 or 4 or 5, it is characterized in that: the concentration of calculating elemental sulfur in air in step 5) by formula (2);
In formula:
C
sfor the concentration of elemental sulfur in air sample, unit is μ g/m
3;
C is the concentration of elemental sulfur in absorption liquid, according to the typical curve of drawing, calculates, and unit is μ g/L;
V is absorption liquid volume, and unit is mL;
V
0for the sampling volume under the status of criterion, unit is L.
7. assay method according to claim 6, is characterized in that: comprise the following steps:
1) collection of elemental sulfur sample in air: gather air sample with air sampler, absorption liquid is the mixed solution of glycerine and sodium sulphite or sodium bisulfite, in absorption liquid, sodium sulphite or concentration of sodium bisulphite are 5-15mM, the content of glycerine is 0.1~5wt%, absorption liquid volume is 5-50mL, and liquid sample is absorbed; Air sampler sampling flow velocity is 0.5-2L/min, and the sampling time is 5-30min;
2) measure: with the ion chromatograph with electric conductivity detector, measure the peak area value of absorption liquid sample, measure the peak area value of the blank of corresponding absorption liquid simultaneously, the peak area value that deducts blank with the sample peak area value recording obtains a difference A; Condition determination is: anion-exchange column adopts the As18 type separating column of 250mm * 4mm and the AG18 type guard column of 50mm * 4mm, mobile phase adopts 20-40mmol/L KOH drip washing such as degree of grade or gradient elution, flow rate of mobile phase is 0.8-2.0mL/min, sample size 5-1000 μ l, be 15min analysis time, 30 ℃ of column temperatures;
3) making of typical curve: with the ion chromatograph of electric conductivity detector in step 2) measure respectively the peak area value that concentration is the elemental sulfur standard solution of 2 μ g/L, 10 μ g/L, 25 μ g/L, 50 μ g/L, 100 μ g/L under described condition determination, take peak area as ordinate, take elemental sulfur concentration as horizontal ordinate, obtain standard working curve;
4) concentration of the corresponding elemental sulfur of difference A the determining of elemental sulfur concentration in absorption liquid sample: according to the standard working curve determining step 2 of step 3)), elemental sulfur concentration c in the liquid sample that is absorbed;
5) calculating of elemental sulfur concentration in air: calculate the sampling volume V under the status of criterion according to absorption liquid volume V, formula (1)
0with elemental sulfur concentration c in absorption liquid sample, by formula (2), calculate the concentration of elemental sulfur in air.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
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CN201210384375.3A CN102854269B (en) | 2012-10-11 | 2012-10-11 | Method for measuring concentration of elemental substance sulfur in air |
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