CN104569181A - Method for detecting concentration of naphthalene in polycyclic aromatic hydrocarbon compounds - Google Patents
Method for detecting concentration of naphthalene in polycyclic aromatic hydrocarbon compounds Download PDFInfo
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- CN104569181A CN104569181A CN201410739938.5A CN201410739938A CN104569181A CN 104569181 A CN104569181 A CN 104569181A CN 201410739938 A CN201410739938 A CN 201410739938A CN 104569181 A CN104569181 A CN 104569181A
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Abstract
The invention discloses a method for detecting concentration of naphthalene in polycyclic aromatic hydrocarbon compounds. The method comprises the steps of collecting a sample, treating the sample, preparing and detecting a standard solution, and manufacturing and detecting a standard curve. The method is characterized in that in the detecting steps, the gas phase condition of a gas chromatograph is set in the following way: an HP-INWWAX capillary chromatographic column is adopted, the column temperature is 120 DEG C, the temperature of a vaporizing chamber is 200 DEG C, the temperature of a detecting chamber is 230 DEG C, and the carrier gas flow is 10ml/min. By selecting the HP-INWWAX capillary, other compounds in polycyclic aromatic hydrocarbon compounds can be detected simultaneously after a proper detecting condition is set, so that the problem that easily broken column and time waste caused by frequently changing column can be solved, cost and time can be reduced, and more importantly the data accuracy can be guaranteed. Regarding preparation of a standard solution, the usage of the standard solution is reduced by adopting the improved method, so that an excellent promoting effect for guaranteeing the precision and accuracy for sample detection can be achieved.
Description
Technical field
The present invention relates to naphthalene method for measurement of concentration in a kind of polynuclear aromatics compounds, belong to compound chemistry detection field.
Background technology
During workplace air noxious material is measured, the detection method of polynuclear aromatics compounds is generally adopt vapor-phase chromatography, national standard requires that the mensuration of naphthalene in many benzene polycyclic aromatic hydrocarbons adjusts part to be 2m × 4mm, carbowax-20M: Apiezon L: chromosorbWAW DMCS=5:10:100 chromatographic column, column temperature: 150 degree; Temperature of vaporization chamber: 180 degree; Sensing chamber's temperature: 200 degree; Carrier gas (nitrogen) flow: 35ml/min.Same, also can adopt vapor-phase chromatography in the mensuration of other class Air toxic substances, its core technology is the chromatographic column and suitable column temperature, temperature of vaporization chamber, sensing chamber's temperature and carrier gas flux that choice for use is suitable.If grope less than suitable condition, peak can not be gone out or go out peak not exclusively thus impact detects the accuracy of data.
For numerous projects utilizing vapor-phase chromatography to detect, require to use different chromatographic columns according to standard-required disparity items, change chromatographic column frequently for this reason and cause appearance to increase the risk of pillar infringement.One root chromatogram column price very expensive (about more than 5000 yuan one of kapillary) and continually replacing pillar easily cause the damage of pillar, and time-consuming.
Therefore how choice for use one capillary post, be suitable for all kinds of polycyclic aromatic hydrocarbons compound determination, the condition that the various project of same compound measures, and guarantee that every detection data accurately and meet the requirements, accomplishing that saving saves time and data multiple advantage accurately, is the researchist's urgent need to solve the problem in current detection industry.
Summary of the invention
The object of the invention is to for deficiency of the prior art, naphthalene method for measurement of concentration in a kind of polynuclear aromatics compounds is provided, there is cost and reduce, save time, the advantage that accuracy is high.
For solving the problems of the technologies described above, the technical solution used in the present invention is: naphthalene method for measurement of concentration in a kind of polynuclear aromatics compounds, comprise sample collection, sample preparation, the preparation of standard solution and mensuration, the making of typical curve and mensuration, its innovative point is: in described determination step, the gas phase condition of gas chromatograph is set to adopt HP-INWWAX capillary chromatographic column, column temperature is 120 degree, temperature of vaporization chamber is 200 degree, and sensing chamber's temperature is 230 degree, and carrier gas flux is 10ml/min.
Further, described standard solution is formulated as and accurately takes 0.10580g naphthalene in 10ml volumetric flask, add stripping liquid carbon disulphide and be made into the dense mark liquid of 10.58mg/ml naphthalene, draw the dense mark liquid of 0,5,10,20,40 μ l respectively in 1ml stripping liquid, obtain 0,52.9,105.8,211.6,423.2 μ g/ml standard solution series.
Further, described sample collection comprises short time sampling, long-time sampling, personal sampling and blank sample sampling; The described short time is sampled as at sampled point, opens activated carbon tube two ends, with 200mL/min flow collection 15min air sample; Describedly to be sampled as a long time at sampled point, to open activated carbon tube two ends, with 50mL/min flow collection 2 ~ 8h air sample; Described personal sampling is at sampled point, opens activated carbon tube two ends, is worn on the top, shirtfront of sample objects, as far as possible close to breathing zone, with 50mL/min flow collection 2 ~ 8h air sample; Described blank sample is sampled as and activated carbon tube is brought to sampled point, and except not connecting samplers sample air sample, all the other operate same sample.
Further, described sample handling procedure is section before and after the activated carbon tube adopting sample poured into respectively in solvent desorption bottle, adds 1.0ml stripping liquid carbon disulphide, after jog, and desorb 30min, stripping liquid is for measuring; If the concentration of determinand exceedes measurement range in sample liquid, measure after available stripping liquid dilution, during calculating, be multiplied by extension rate.
Further, described Specification Curve of Increasing step is conditioning instrumentation operating conditions, and sample introduction 2.0 μ l, measures each standard series, each concentration replication 3 times, with peak height or peak area average to corresponding naphthalene concentration drawing standard curve.
Further, described determination step comprises sample determination and reference substance mensuration; Described reference substance is determined as and measures blank stripping liquid, obtains peak height or peak area value; Described sample determination is the similarity condition working sample stripping liquid by bioassay standard series, after the sample peak height recorded or peak area value deduct blank peak height or peak area value, is obtained the concentration of naphthalene in sample by typical curve.
Beneficial effect of the present invention is as follows:
(1) this workplace of the present invention, naphthalene method for measurement of concentration in polynuclear aromatics compounds, adopt HP-INWWAX capillary chromatographic column, column temperature is 120 degree, and temperature of vaporization chamber is 200 degree, and sensing chamber's temperature is 230 degree, carrier gas flux is 10ml/min, detect naphthalene compound result in polycyclic aromatic hydrocarbons and detect data accurately, meet national requirements, time-saving and efficiency.
(2) this HP-INWWAX kapillary is selected, after setting suitable condition determination, the detection of other compounds in polynuclear aromatics compounds can also be carried out simultaneously, solve and change pillar continually and easily cause the damage of pillar and time-consuming problem, the accuracy the more important thing is and ensure that data of not only having saved but also saved time.
(3) for the preparation of standard solution, adopt the method after improvement of the present invention, the use amount of standard solution is reduced, for ensureing that the preci-sion and accuracy of sample determination serves good facilitation.
Embodiment
Below in conjunction with specific embodiment, technical scheme of the present invention is elaborated.
Embodiment 1
Adopt the detection method of gas chromatography determination naphthalene:
1, instrument
Activated carbon tube, solvent desorption type, in-built 100mg/50mg activated charcoal.
Air sampler, flow 0 ~ 500ml/min.
Solvent desorption bottle, 5ml.
Micro syringe, 10 μ l.
Gas chromatograph: Shimadzu GC-2014C(TJ-S-054)
2, instrument testing conditions:
HP-INWWAX capillary chromatographic column;
Column temperature is 120 degree;
Temperature of vaporization chamber is 200 degree;
Sensing chamber's temperature is 230 degree;
Carrier gas flux is 10ml/min.
3, reagent
Stripping liquid, carbon disulphide
4, sample collection:
Short time samples: at sampled point, open activated carbon tube two ends, with 200mL/min flow collection 15min air sample;
Long-time sampling: at sampled point, opens activated carbon tube two ends, with 50mL/min flow collection 2 ~ 8h air sample;
Personal sampling: at sampled point, opens activated carbon tube two ends, is worn on the top, shirtfront of sample objects, as far as possible close to breathing zone, with 50mL/min flow collection 2 ~ 8h air sample;
Contrast blank sample is sampled as and activated carbon tube is brought to sampled point, and except not connecting samplers sample air sample, all the other operate same sample.
After sampling, close solid absorbent tubes two ends immediately, put transport and preservation in cleaning container.
5, mensuration is analyzed:
5.1 sample preparation: section before and after the activated carbon tube adopting sample poured into respectively in solvent desorption bottle, add 1.0ml stripping liquid carbon disulphide, after jog, desorb 30min, stripping liquid is for measuring.
The preparation of 5.2 standard solution and mensuration: preparation: accurately take 0.10580g naphthalene in 10ml volumetric flask, add stripping liquid carbon disulphide and be made into the dense mark liquid of 10.58mg/ml naphthalene, draw the dense mark liquid of 0,5,10,20,40 μ l respectively in 1ml stripping liquid, obtain 0,52.9,105.8,211.6,423.2 μ g/ml standard solution series, measure under prescribed conditions.
The making of 5.3 typical curves: conditioning instrumentation operating conditions, sample introduction 2.0 μ l, measures each standard series, each concentration replication 3 times, with peak height or peak area average to corresponding concentration drawing standard curve.
5.4 measure: one, the similarity condition of bioassay standard series measures blank stripping liquid, obtains peak height or peak area value; Two, the similarity condition working sample stripping liquid of bioassay standard series, after the sample peak height recorded or peak area value deduct blank peak height or peak area value, is obtained the concentration of naphthalene in sample by typical curve.
6, sample concentration computing method:
By formula 1, sampling volume is converted into standard sample volume:
Formula 1:
In formula: Vo-standard sample volume, L;
V-sampling volume, L;
The temperature of t-sampled point, DEG C;
The atmospheric pressure of P-sampled point, kPa.
The concentration of naphthalene is calculated by formula 2:
Formula 2:
In formula: the concentration of naphthalene in C-air, mg/m
3;
C
1,c
2-record the concentration of naphthalene in the section active carbon desorption liquid of front and back,
;
Vo-standard sample volume, L;
The volume of v-stripping liquid, mL;
D-desorption efficiency, %.
Embodiment 2
The precision test experiments of the inventive method:
Drawing four parts of sample 20 μ l to four 1ml resolves in bottles, label 1,2,3 and 4 respectively, by embodiment 1 sample determination method carry out the mensuration of sample concentration, result is as follows:
| Sample label | A (absorbance) | C (concentration μ g/ml) |
| Naphthalene 1 | 245.416 | 212.62 |
| Naphthalene 2 | 244.248 | 211.61 |
| Naphthalene 3 | 244.242 | 211.60 |
| Naphthalene 4 | 245.178 | 212.41 |
As calculated, naphthalene mean concentration is 121.06 μ g/ml, and coupon results shows the requirement that the Precision Experiment of naphthalene meets standard and specifies.
Embodiment 3
Recovery of standard addition is tested:
Draw the naphthalene sample that 20 μ l concentration are the dense mark of 10.58mg/ml and 20 μ l respectively, resolve in bottle to 1ml, respective recovery of standard addition is as shown in the table:
| Sample label | A | C |
| Naphthalene 1 | 246.382 | 213.46 |
| Naphthalene 2 | 247.967 | 214.83 |
| Naphthalene 3 | 248.587 | 215.36 |
| Naphthalene 4 | 247.979 | 214.84 |
As calculated: the recovery of standard addition of sample 1 is 98.88%;
The recovery of standard addition of sample 2 is 99.52%;
The recovery of standard addition of sample 3 is 99.77%;
The recovery of standard addition of sample 4 is 99.53%.
Comparative example 1
GB standard method is adopted to measure the concentration of the naphthalene sample of embodiment 1.Experiment proves, the National Standard Method working sample time is 2 ~ 3h, and concentration determination is 121.036 μ g/ml, substantially close with the mensuration concentration of embodiment, and the minute of embodiment is 1.5 ~ 2.2h.
Claims (6)
1. naphthalene method for measurement of concentration in a polynuclear aromatics compounds, comprise sample collection, sample preparation, the preparation of standard solution and mensuration, the making of typical curve and mensuration, it is characterized in that: in described determination step, the gas phase condition of gas chromatograph is set to adopt HP-INWWAX capillary chromatographic column, column temperature is 120 degree, temperature of vaporization chamber is 200 degree, sensing chamber's temperature is 230 degree, and carrier gas flux is 10ml/min.
2. naphthalene method for measurement of concentration in polynuclear aromatics compounds according to claim 1, it is characterized in that: described standard solution is formulated as and accurately takes 0.10580g naphthalene in 10ml volumetric flask, add stripping liquid carbon disulphide and be made into the dense mark liquid of 10.58mg/ml naphthalene, draw the dense mark liquid of 0,5,10,20,40 μ l respectively in 1ml stripping liquid, obtain 0,52.9,105.8,211.6,423.2 μ g/ml standard solution series.
3. naphthalene method for measurement of concentration in polynuclear aromatics compounds according to claim 1, is characterized in that: described sample collection comprises short time sampling, long-time sampling, personal sampling and blank sample sampling; The described short time is sampled as at sampled point, opens activated carbon tube two ends, with 200mL/min flow collection 15min air sample; Describedly to be sampled as a long time at sampled point, to open activated carbon tube two ends, with 50mL/min flow collection 2 ~ 8h air sample; Described personal sampling is at sampled point, opens activated carbon tube two ends, is worn on the top, shirtfront of sample objects, as far as possible close to breathing zone, with 50mL/min flow collection 2 ~ 8h air sample; Described blank sample is sampled as and activated carbon tube is brought to sampled point, and except not connecting samplers sample air sample, all the other operate same sample.
4. naphthalene method for measurement of concentration in polynuclear aromatics compounds according to claim 1, it is characterized in that: described sample handling procedure is pour in solvent desorption bottle respectively by section before and after the activated carbon tube adopting sample, add 1.0ml stripping liquid carbon disulphide, after jog, desorb 30min, stripping liquid is for measuring; If the concentration of determinand exceedes measurement range in sample liquid, measure after available stripping liquid dilution, during calculating, be multiplied by extension rate.
5. naphthalene method for measurement of concentration in polynuclear aromatics compounds according to claim 1, it is characterized in that: described Specification Curve of Increasing step is conditioning instrumentation operating conditions, sample introduction 2.0 μ l, measure each standard series, each concentration replication 3 times, with peak height or peak area average to corresponding naphthalene concentration drawing standard curve.
6. naphthalene method for measurement of concentration in polynuclear aromatics compounds according to claim 1, is characterized in that: described determination step comprises sample determination and reference substance measures; Described reference substance is determined as and measures blank stripping liquid, obtains peak height or peak area value; Described sample determination is the similarity condition working sample stripping liquid by bioassay standard series, after the sample peak height recorded or peak area value deduct blank peak height or peak area value, is obtained the concentration of naphthalene in sample by typical curve.
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| CN201410739938.5A CN104569181A (en) | 2014-12-08 | 2014-12-08 | Method for detecting concentration of naphthalene in polycyclic aromatic hydrocarbon compounds |
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| CN201410739938.5A CN104569181A (en) | 2014-12-08 | 2014-12-08 | Method for detecting concentration of naphthalene in polycyclic aromatic hydrocarbon compounds |
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| CN201410739938.5A Pending CN104569181A (en) | 2014-12-08 | 2014-12-08 | Method for detecting concentration of naphthalene in polycyclic aromatic hydrocarbon compounds |
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- 2014-12-08 CN CN201410739938.5A patent/CN104569181A/en active Pending
Non-Patent Citations (3)
| Title |
|---|
| 中国人民共和国卫生部: "《GBZ/T 160.44－2004 工作场所空气中多环芳香烃化合物的测定方法》", 21 May 2004 * |
| 金岚: "毛细管气相色谱法同时测定空气中三苯、萘", 《中国卫生检验杂志》 * |
| 陈月萌等: "毛细管气相色谱法测定工作场所空气中3种多环芳烃", 《理化检验-化学分册》 * |
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Application publication date: 20150429 |