CN107202769A - A kind of method of room air sample pretreatment during detection formaldehyde - Google Patents
A kind of method of room air sample pretreatment during detection formaldehyde Download PDFInfo
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- CN107202769A CN107202769A CN201710562123.8A CN201710562123A CN107202769A CN 107202769 A CN107202769 A CN 107202769A CN 201710562123 A CN201710562123 A CN 201710562123A CN 107202769 A CN107202769 A CN 107202769A
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- solution
- room air
- sample pretreatment
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- air sample
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- 238000000034 method Methods 0.000 title claims abstract description 22
- 238000001514 detection method Methods 0.000 title claims abstract description 21
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 title claims description 87
- WTDHULULXKLSOZ-UHFFFAOYSA-N Hydroxylamine hydrochloride Chemical compound Cl.ON WTDHULULXKLSOZ-UHFFFAOYSA-N 0.000 claims abstract description 29
- 239000000523 sample Substances 0.000 claims abstract description 26
- 238000010521 absorption reaction Methods 0.000 claims abstract description 23
- 239000012488 sample solution Substances 0.000 claims abstract description 23
- 239000000243 solution Substances 0.000 claims abstract description 20
- 238000007789 sealing Methods 0.000 claims abstract description 18
- 239000007864 aqueous solution Substances 0.000 claims abstract description 17
- 238000004519 manufacturing process Methods 0.000 claims abstract description 17
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 claims abstract description 5
- SQDFHQJTAWCFIB-UHFFFAOYSA-N n-methylidenehydroxylamine Chemical compound ON=C SQDFHQJTAWCFIB-UHFFFAOYSA-N 0.000 claims description 10
- 238000002835 absorbance Methods 0.000 claims description 7
- 150000001875 compounds Chemical class 0.000 claims description 2
- 238000000870 ultraviolet spectroscopy Methods 0.000 claims description 2
- 238000012360 testing method Methods 0.000 abstract description 6
- 238000010790 dilution Methods 0.000 abstract description 3
- 239000012895 dilution Substances 0.000 abstract description 3
- 238000010828 elution Methods 0.000 abstract description 3
- 238000011084 recovery Methods 0.000 abstract description 3
- 238000011017 operating method Methods 0.000 abstract description 2
- -1 colorimetric method Chemical compound 0.000 description 6
- 238000005070 sampling Methods 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 3
- 238000010812 external standard method Methods 0.000 description 3
- 238000004737 colorimetric analysis Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 125000002485 formyl group Chemical class [H]C(*)=O 0.000 description 2
- 230000035945 sensitivity Effects 0.000 description 2
- 238000002798 spectrophotometry method Methods 0.000 description 2
- 208000031404 Chromosome Aberrations Diseases 0.000 description 1
- 208000014085 Chronic respiratory disease Diseases 0.000 description 1
- 206010067477 Cytogenetic abnormality Diseases 0.000 description 1
- 229930040373 Paraformaldehyde Natural products 0.000 description 1
- 206010047700 Vomiting Diseases 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000004064 dysfunction Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 230000001900 immune effect Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229920002866 paraformaldehyde Polymers 0.000 description 1
- 238000005375 photometry Methods 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 238000007781 pre-processing Methods 0.000 description 1
- 210000002345 respiratory system Anatomy 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 208000024891 symptom Diseases 0.000 description 1
- 238000000825 ultraviolet detection Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/33—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using ultraviolet light
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
Landscapes
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
- Investigating Or Analysing Materials By The Use Of Chemical Reactions (AREA)
Abstract
The invention discloses a kind of method of room air sample pretreatment during detection formaldehyde, comprise the following steps：Sealing absorption bottle, drier by air sampler, equipped with derivative solution are sequentially connected, then gas production, are stood, are then taken derivative solution as sample solution, wherein, derivative solution is the hydroxylamine hydrochloride aqueous solution.The present invention is easy to operate, sample is not required to through elution, repeatedly concentration, the step such as dilution, one step is completed, operating procedure is reduced, so that the error that sample pretreatment is brought is greatly reduced, the sample solution obtained after present invention pretreatment, its testing result is reproducible, RSD is 1.86%, and the rate of recovery is 98 103%, and RSD is 1.86%.
Description
Technical field
The present invention relates to Sample Pretreatment Technique Used field, more particularly to room air sample pretreatment during a kind of detection formaldehyde
Method.
Background technology
With economic fast development and the continuous improvement of national life level, when indoor decorating becomes a kind of
Still, however, people are while comfortable family life is enjoyed, it is faced with more and more prominent indoor air environment pollution and asks
Topic.At present, formaldehyde has turned into indoor pollution most one of universal, pollutant of most serious.Formaldehyde has a major impact to health,
There is strong impulse effect to eye, respiratory tract, skin, can cause to shed tears, the symptom such as Nausea and vomiting, uncomfortable in chest, general weakness, it is long
Phase contact low dosage formaldehyde can cause chronic respiratory disease, decrease of memory, chromosome abnormality, immunologic dysfunction etc..First
Aldehyde pollution problem has caused the extensive concern of society.
At present, many methods are applied to the measure of indoor formaldehyde, such as colorimetric method, electronic detector, ultraviolet spectrometry
Photometry etc., but colorimetric method error is larger, sensitivity is not high, it is impossible to determines specific content of formaldehyde；Although electronic detector
The occurrence of content of formaldehyde can be shown, but the degree of accuracy is relatively low, sensitivity is not high.
Although the ultraviolet spectrophotometry degree of accuracy is higher, be due to formaldehyde in 200-400nm wave-length coverages without absorption,
It is transformed into the material for having absorption in 200-400nm wave-length coverages so needing PARA FORMALDEHYDE PRILLS(91,95) to carry out pretreatment, could carry out
Detection；Current preprocess method operation is more so that the degree of accuracy of testing result is relatively low, so that ultraviolet spectrophotometry is obtained
Detection loses meaning.
The content of the invention
The technical problem existed based on background technology, room air specimen preprocessing when the present invention proposes a kind of detection formaldehyde
The method of reason, the present invention is easy to operate, and sample is not required to through elution, repeatedly concentration, the step such as dilution, and a step is completed, and reduces operation
Step, so that the error that sample pretreatment is brought is greatly reduced, the sample solution obtained after present invention pretreatment, it is detected
As a result reproducible, RSD is 1.86%, and the rate of recovery is 98-103%, and RSD is 1.86%.
The method of room air sample pretreatment, comprises the following steps during a kind of detection formaldehyde proposed by the present invention：By sky
Gas sampling, sealing absorption bottle, drier equipped with derivative solution are sequentially connected, then gas production, are stood, are then taken derivative solution
As sample solution, wherein, derivative solution is the hydroxylamine hydrochloride aqueous solution.
Preferably, sealing absorption bottle, the drier by air sampler, equipped with 10-20ml derivative solutions are sequentially connected, and are connect
Gas production 48-60h, 4-6min is stood, then takes derivative solution as sample solution.
Preferably, gas production Airflow to for：From drier to sealing absorption bottle again to air sampler.
Preferably, the concentration of the hydroxylamine hydrochloride aqueous solution is 8-12mmol/L.
Preferably, the concentration of the hydroxylamine hydrochloride aqueous solution can be 8.5,9,9.5,10,10.5,11 or 11.5mmol/L.
Preferably, compound concentration be 0.001,0.002,0.004,0.005,0.008,0.01mol/L formaldoxime it is water-soluble
Liquid detects the absorbance of the contrast solution of various concentrations with UV detector successively as contrast solution, draws standard bent
Line.
The absorbance of sample solution is detected, the content of the formaldoxime in sample solution is calculated according to standard curve external standard method,
The content of formaldehyde in air is calculated again.
Preferably, the Detection wavelength of UV detector is 203-207nm.
Preferably, the Detection wavelength of UV detector can for 203.1,203.2,203.3,203.4,203.5,
203.6、203.7、203.8、203.9、204、204.1、204.2、204.3、204.4、204.5、204.6、204.7、204.8、
204.9、205、205.1、205.2、205.3、205.4、205.5、205.6、205.7、205.8、205.9、206、206.1、
206.2nd, 206.3,206.4,206.5,206.6,206.7,206.8 or 206.9nm.
The present invention Cleaning Principle be：Formaldehyde prepares formaldoxime with hydroxylamine hydrochloride reaction, and formaldoxime is in wavelength 203-
Have absorption maximum in the range of 207nm, and water, formaldehyde, hydroxylamine hydrochloride wavelength for 200-400nm ultraviolet detection region without suction
Receive, do not interfere with the detection of formaldoxime absorption value；Formaldehyde in air with excessive hydrochloric acid azanol reaction by obtaining formaldoxime simultaneously
The absorbance of sample solution is detected, the content for obtaining formaldoxime is calculated by standard curve external standard method, then calculate first in air
The content of aldehyde.
The present invention is by the way that air sampler, sealing absorption bottle, drier to be sequentially connected, and be directly added into absorption bottle
Excessive derivative solution so that the formaldehyde in air directly obtains formaldoxime as sample solution with hydroxylamine hydrochloride reaction, and directly
Access sample solution to be detected, whole process is easy to operate, sample is not required to through elution, repeatedly concentration, the step, a step such as dilution
Complete, reduce operating procedure, so as to greatly reduce the error that sample pretreatment is brought, increase the degree of accuracy of testing result；Through
The sample solution obtained after present invention pretreatment, its testing result is reproducible, and RSD is 1.86%, and the rate of recovery is 98-103%,
RSD is 1.86%.
Embodiment
Below, technical scheme is described in detail by specific embodiment.
Embodiment 1
The method of room air sample pretreatment, comprises the following steps during a kind of detection formaldehyde：By air sampler, it is equipped with
10ml concentration is sequentially connected for sealing absorption bottle, the drier of the 12mmol/L hydroxylamine hydrochloride aqueous solution, then gas production 48h, stands
6min, then the aqueous solution is as sample solution, wherein, gas production Airflow to for：From drier to sealing absorption bottle again to sky
Gas sampling.
Embodiment 2
The method of room air sample pretreatment, comprises the following steps during a kind of detection formaldehyde：By air sampler, it is equipped with
20ml concentration is sequentially connected for sealing absorption bottle, the drier of the 8mmol/L hydroxylamine hydrochloride aqueous solution, then gas production 60h, stands
4min, then the aqueous solution is as sample solution, wherein, gas production Airflow to for：From drier to sealing absorption bottle again to sky
Gas sampling.
Embodiment 3
The method of room air sample pretreatment, comprises the following steps during a kind of detection formaldehyde：By air sampler, it is equipped with
12ml concentration is sequentially connected for sealing absorption bottle, the drier of the 11mmol/L hydroxylamine hydrochloride aqueous solution, then gas production 50h, stands
5.5min, then the aqueous solution is as sample solution, wherein, gas production Airflow to for：From drier to sealing absorption bottle again to
Air sampler.
Embodiment 4
The method of room air sample pretreatment, comprises the following steps during a kind of detection formaldehyde：By air sampler, it is equipped with
18ml concentration is sequentially connected for sealing absorption bottle, the drier of the 9mmol/L hydroxylamine hydrochloride aqueous solution, then gas production 58h, stands
4.5min, then the aqueous solution is as sample solution, wherein, gas production Airflow to for：From drier to sealing absorption bottle again to
Air sampler.
Embodiment 5
The method of room air sample pretreatment, comprises the following steps during a kind of detection formaldehyde：By air sampler, it is equipped with
10ml concentration is sequentially connected for sealing absorption bottle, the drier of the 10mmol/L hydroxylamine hydrochloride aqueous solution, then gas production 48h, stands
5min, then the aqueous solution is as sample solution, wherein, gas production Airflow to for：From drier to sealing absorption bottle again to sky
Gas sampling.
Test example 1
It is identical in 6 formaldehyde in air contents, in volume identical confined space, sample solution is prepared according to embodiment 5,
And be that sample solution absorbance is detected at 205nm in wavelength, formaldehyde oxime content is calculated by standard curve external standard method, and calculating is obtained
The content of formaldehyde in air.
In above formula, WFormaldehydeFor content of formaldehyde, mg/L；ASampleFor the absorbance of sample solution；
AControlFor the absorbance of contrast solution；CControlFor the concentration of contrast solution, mol/L；
VSampleFor the volume of sample solution, L；30 be the relative molecular mass of formaldehyde；1000 be reduced unit；
VAirFor the volume of air, L.
6 groups of results are counted, it is as a result as follows：
The sample solution obtained as can be seen from the above table after present invention pretreatment, its testing result is reproducible, reclaims
Rate is high, and the degree of accuracy is good.
The foregoing is only a preferred embodiment of the present invention, but protection scope of the present invention be not limited thereto,
Any one skilled in the art the invention discloses technical scope in, technique according to the invention scheme and its
Inventive concept is subject to equivalent substitution or change, should all be included within the scope of the present invention.
Claims (6)
1. a kind of method of room air sample pretreatment during detection formaldehyde, it is characterised in that comprise the following steps：Air is adopted
Sample device, sealing absorption bottle, drier equipped with derivative solution are sequentially connected, then gas production, are stood, are then taken derivative solution conduct
Sample solution, wherein, derivative solution is the hydroxylamine hydrochloride aqueous solution.
2. the method for room air sample pretreatment when detecting formaldehyde according to claim 1, it is characterised in that adopt air
Sample device, sealing absorption bottle, drier equipped with 10-20ml derivative solutions are sequentially connected, then gas production 48-60h, stand 4-
6min, then takes derivative solution as sample solution.
3. the method for room air sample pretreatment during detection formaldehyde according to claim 1 or claim 2, it is characterised in that gas production
Airflow to for：From drier to sealing absorption bottle again to air sampler.
4. the method for room air sample pretreatment during detection formaldehyde according to any one of claim 1-3, it is characterised in that
The concentration of the hydroxylamine hydrochloride aqueous solution is 8-12mmol/L.
5. the method for room air sample pretreatment during detection formaldehyde according to any one of claim 1-4, it is characterised in that
Compound concentration be 0.001,0.002,0.004,0.005,0.008, the 0.01mol/L formaldoxime aqueous solution as contrast solution,
Detect the absorbance of the contrast solution of various concentrations successively with UV detector, draw standard curve.
6. the method for room air sample pretreatment when detecting formaldehyde according to claim 5, it is characterised in that ultraviolet spectrometry
The Detection wavelength of photometer is 203-207nm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710562123.8A CN107202769A (en) | 2017-07-11 | 2017-07-11 | A kind of method of room air sample pretreatment during detection formaldehyde |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710562123.8A CN107202769A (en) | 2017-07-11 | 2017-07-11 | A kind of method of room air sample pretreatment during detection formaldehyde |
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| Publication Number | Publication Date |
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| CN107202769A true CN107202769A (en) | 2017-09-26 |
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|---|---|---|---|
| CN201710562123.8A Pending CN107202769A (en) | 2017-07-11 | 2017-07-11 | A kind of method of room air sample pretreatment during detection formaldehyde |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE10063182A1 (en) * | 2000-12-19 | 2002-06-20 | Sven Niewiadomski | Device for removing methanal from air e.g. for air purifiers, comprises using an absorbent based on sheep's wool |
| CN101551338A (en) * | 2009-02-25 | 2009-10-07 | 北京中科中环环境应用技术研究中心 | Method for determining formaldehyde in air |
| CN201965044U (en) * | 2010-12-27 | 2011-09-07 | 中芯国际集成电路制造(上海)有限公司 | Air sample collector |
| CN103592237A (en) * | 2013-09-27 | 2014-02-19 | 苏州国环环境检测有限公司 | Method for detecting formaldehyde in indoor air by using acetylacetone spectrophotometric method |
| US9895671B2 (en) * | 2014-10-14 | 2018-02-20 | China Petroleum & Chemical Corporation | Fluidized bed reactor, reaction regeneration apparatus, process for preparing olefins, and process for preparing aromatic hydrocarbons |
-
2017
- 2017-07-11 CN CN201710562123.8A patent/CN107202769A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE10063182A1 (en) * | 2000-12-19 | 2002-06-20 | Sven Niewiadomski | Device for removing methanal from air e.g. for air purifiers, comprises using an absorbent based on sheep's wool |
| CN101551338A (en) * | 2009-02-25 | 2009-10-07 | 北京中科中环环境应用技术研究中心 | Method for determining formaldehyde in air |
| CN101551338B (en) * | 2009-02-25 | 2011-06-08 | 北京中科中环环境应用技术研究中心 | Method for determining formaldehyde in air |
| CN201965044U (en) * | 2010-12-27 | 2011-09-07 | 中芯国际集成电路制造(上海)有限公司 | Air sample collector |
| CN103592237A (en) * | 2013-09-27 | 2014-02-19 | 苏州国环环境检测有限公司 | Method for detecting formaldehyde in indoor air by using acetylacetone spectrophotometric method |
| US9895671B2 (en) * | 2014-10-14 | 2018-02-20 | China Petroleum & Chemical Corporation | Fluidized bed reactor, reaction regeneration apparatus, process for preparing olefins, and process for preparing aromatic hydrocarbons |
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Application publication date: 20170926 |
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