CN103389291A - Resonance Rayleigh scattering spectrum method for formaldehyde determination - Google Patents
Resonance Rayleigh scattering spectrum method for formaldehyde determination Download PDFInfo
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- CN103389291A CN103389291A CN2013103047486A CN201310304748A CN103389291A CN 103389291 A CN103389291 A CN 103389291A CN 2013103047486 A CN2013103047486 A CN 2013103047486A CN 201310304748 A CN201310304748 A CN 201310304748A CN 103389291 A CN103389291 A CN 103389291A
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Abstract
The invention discloses a resonance Rayleigh scattering spectrum method for formaldehyde determination. The resonance Rayleigh scattering spectrum method comprises the following steps of 1, preparing a formaldehyde standard solution system, 2, preparing a blank control solution system, 3, respectively determining resonance Rayleigh scattering peak intensity values I standard and I blank of the formaldehyde standard solution system and the blank control solution system and calculating delta I according to a formula of delta I=I blank-I standard, 4, drawing a working curve of a formaldehyde concentration relationship by the delta I, 5, determining a sample and calculating delta I sample according to a formula of delta I sample=Ib-I sample, and 6, calculating a formaldehyde concentration of the sample by the working curve obtained by the step 4 according to the determined delta I sample. The resonance Rayleigh scattering spectrum method adopts simple equipment, can be operated fast, and has high sensitivity and good selectivity.
Description
Technical field
The present invention relates to the analytical chemistry field, specifically measure the Resonance Rayleigh Scattering Spectral Method of formaldehyde.
Background technology
Formaldehyde is a kind of colourless, and the gas of intense stimulus type smell is arranged.Formaldehyde is gaseous state at normal temperatures, usually with the aqueous solution form, occurs, 35～40% formalin is called formalin.formaldehyde is a kind of important Organic Ingredients, be mainly used in plastics industry (as phenolics processed, urea-formaldehyde plastics-electricity is beautiful), synthon (as synthetic vinylon-polyvinyl formal), leather industry, medicine, dyestuff, paint industry department etc., it has spread effect to human central nervous system and retina, nerve to the people, lung, liver all can produce infringement, and has a potential carcinogenesis, point out in the report that american chemical in 1980 industry toxicological study is announced, formaldehyde has carcinogenicity, by the World Health Organization (WHO), be defined as carcinogenic and teratogen, allergen and strong mutagen, formaldehyde is all forbidden adding in regulation food in countries in the world.But due to ordering about of interests, many illegal retailers add formaldehyde and are used for anticorrosion and keep product form in food.Therefore the content in food must strictly be controlled and check.Therefore set up content sensitive, analytical approach mensuration formaldehyde fast and accurately and just seem extremely important.Present method for detection of formaldehyde has multiple, comprises fluorescence method, electrochemical process, photometry, vapor-phase chromatography, high performance liquid chromatography, oscilloscopic polarography and colourimetry.Wherein after 33 kinds the method sample pre-treatments is loaded down with trivial details and instrument is expensive.Off-color acid method, phenol reagent process and acetylacetone method or to be difficult to eliminate interference or severe reaction conditions or sensitivity high and all need coordinate instrument to use in colourimetry.Also have some analytical approachs such as phenol reagent process for detection of formaldehyde, acetylacetone method, off-color acid method and magenta-sulfurous method etc.These methods mostly will heat in the water-bath of higher temperature, chromogenic reaction just can be carried out fully, and it is very inconvenient to operate.Resonance Rayleigh Scattering Spectral Method has easy, quick, sensitive characteristics and has been used for trace inorganics and organic analysis.Cationic surfactant (CS) be first stability and at visible-range without the Resonance Rayleigh Scattering Spectra analytical reagent that absorbs, measure the method report of formaldehyde but yet there are no so far the resonance Rayleigh that utilizes ionic surface active agent the to make probe scattering spectrometry that shakes.
Summary of the invention
The objective of the invention is in order to provide a kind of Simple fast to measure the Resonance Rayleigh Scattering Spectral Method of formaldehyde.
A kind of Resonance Rayleigh Scattering Spectral Method of measuring formaldehyde, comprise the steps:
(1) prepare formaldehyde standard solution system: get the scale test tube, pipette successively 10～60 μ L 0.0034 mol/L formaldehyde standard solution, 100～250 μ L 1.6 * 10
-3The mol/L iodine solution, 100～400 μ L 1.0 mol/L NaOH solution, shake up, and after reaction 15 min, adds 600～800 μ L 1.0 mol/L HCl solution to make solution be acid, then add 200～400 μ L 1.0 * 10
-4Mol/L chloro-hexadecane yl pyridines, shake up, and with redistilled water, is settled to 5.0 mL, mixes;
(2) prepare the blank solution system: do not add the formaldehyde titer with the method for step (1) and prepare the blank solution system;
(3) get respectively by formaldehyde standard solution system and the blank solution system of step (1), (2) preparation appropriate, be placed in cuvette, on fluorospectrophotometer, synchronous scanning excitation wavelength and emission wavelength, the Resonance Rayleigh Scattering Spectra of acquisition system, the Resonance Rayleigh Scattering peak intensity value of mensuration system maximum wavelength 530 nm place formaldehyde standard solution systems
I, and the Resonance Rayleigh Scattering peak intensity value of measuring the blank solution system
I b, calculate Δ
I=
I b-
I
(4) with Δ
IThe concentration relationship of the PARA FORMALDEHYDE PRILLS(91,95) curve of working;
(5) measured object sample determination: take food the category sample, dry product is pulverized (or wet product rubbing), under phosphoric acid medium and defoamer existence, through steam distillation, absorb effluent with redistilled water and obtain to contain the measured object of formaldehyde, then pipette a certain amount of replacement formaldehyde standard solution, by step (1)～(3) operation.Calculate the Δ of measured object
I Sample=
I b-
I Sample
(6) Δ that records per sample
I Sample, look into the working curve of step (4), calculate the concentration of formaldehyde in measured object.
Realize that principle of the present invention is: in alkaline medium, formaldehyde is by the iodine oxidation, and remaining iodine generates (CPC-I with chloro-hexadecane yl pyridines (CPC) reaction in acid solution
3)
nParticulate, this particulate are that 530 nm places have a Resonance Rayleigh Scattering peak at wavelength.Formaldehyde is more by the iodine oxidation, and remaining iodine is fewer, (the CPC-I of generation
3)
nParticulate reduces, so the linear reduction of Resonance Rayleigh Scattering peak intensity, thus available Resonance Rayleigh Scattering Spectral Method for Determination content of formaldehyde.
Advantage of the present invention is: compare with existing method, this assay method is easy and simple to handle, and is highly sensitive, selectivity good.
Description of drawings
Fig. 1 is the partial resonance Rayleigh scattering light spectrogram that the embodiment of the present invention is measured formaldehyde.
In figure: a:64
μ mol/L I
2-0.06 mol/L NaOH-0.14 mol/L HCl-6
μ mol/L CPC; B:a+27.2 μ mol/L CH
2O; C:a+40.8 μ mol/L CH
2O。
Embodiment
Embodiment:
Application Resonance Rayleigh Scattering Spectral Method for Determination formaldehyde, comprise the steps:
(1) prepare formaldehyde standard solution system: get the scale test tube, pipette successively 10 μ L, 20 μ L, 30 μ L, 40 μ L, 60 μ L 0.0034 mol/L formaldehyde standard solution, 200 μ L 1.6 * 10
-3The mol/L iodine solution, 300 μ L 1.0 mol/L NaOH solution, shake up, and after reaction 15 min, adds 700 μ L 1.0 mol/L HCl solution, makes solution be acid, then add 300 μ L 1.0 * 10
-4Mol/L chloro-hexadecane yl pyridines, shake up, and with redistilled water, is settled to 5.0 mL, mixes;
(2) prepare the blank solution system: do not add the formaldehyde titer with the method for step (1) and prepare the blank solution system;
(3) get respectively by formaldehyde standard solution system and the blank solution system of step (1), (2) preparation appropriate, be placed in cuvette, on Cary Eclipse type fluorospectrophotometer, set instrument parameter, detector voltage is made as 400 volts, excitation wavelength slit and emission wavelength slit all are set as 5nm, synchronous scanning excitation wavelength and emission wavelength, the Resonance Rayleigh Scattering Spectra of acquisition system, the Resonance Rayleigh Scattering peak intensity value of mensuration system maximum wavelength 530 nm place formaldehyde standard solution systems
I, and the Resonance Rayleigh Scattering peak intensity value of measuring the blank solution system
I b, calculate Δ
I=
I b-
I
(4) with Δ
IThe concentration relationship of the PARA FORMALDEHYDE PRILLS(91,95) curve of working;
(5) measured object sample determination: in the actual sample test, we have selected representational foodstuff dry product and wet product, dry product class sample rubs with meat grinder with comminutor pulverizing, wet product class sample, then accurately take sample 5.0～10.0 g through pulverizing or rubbing, be placed in 500 mL cucurbits, add 20 mL redistilled waters, whiteruss 2.5 mL and 10% phosphoric acid solution 10 mL, pass into immediately steam distillation, the condenser pipe end opening first inserts the container that fills 10 mL distilled water and be placed in ice bath, accurately collects distillate 100 mL.Get 3.0 mL distillates and replace the formaldehyde standard solution, by step (1)～(3) operation.Calculate the Δ of measured object
I Sample=
I b-
I Sample
(6) Δ that records per sample
I Sample, look into the working curve of step (4), calculate the content of formaldehyde in measured object and see the following form.
It is 6.8-40.8 μ mol/L that the embodiment of the present invention is measured the content of formaldehyde scope, and regression equation is
Δ I=3.25
C+ 0.71,0, detect and be limited to 6.2 nmol/L.
The checking of detection method of the present invention:
The sample solution of getting above-mentioned steps (5) preparation is appropriate, press list of references: Liu Jiakun, Chen Lanhua. Catalytic kinetic spectrofluorimetric determination of trace formaldehyde in food products ［ J ］. assay laboratory, 2006,25 (9): 78-80 measures the content of formaldehyde, and the content of formaldehyde that sequence number 1-12 sample records is respectively 215.7 mg/kg, 290.8 mg/kg, 17.2 mg/kg, 32.1 mg/kg, 4.3 mg/kg, 3.8mg/kg, 366.1 mg/kg, 161.1 mg/kg, 236.4 mg/kg, 413.9 mg/kg, 517.8mg/kg, 679.3 mg/kg.Measurement result is consistent with method of the present invention.
Claims (1)
1. a Resonance Rayleigh Scattering Spectral Method of measuring formaldehyde, comprise the steps:
(1) prepare formaldehyde standard solution system: get the scale test tube, pipette successively 10～60 μ L 0.0034 mol/L formaldehyde standard solution, 100～250 μ L 1.6 * 10
-3The mol/L iodine solution, 100～400 μ L 1.0 mol/L NaOH solution, shake up, and after reaction 15 min, adds 600～800 μ L 1.0 mol/L HCl solution to make solution be acid, then add 200～400 μ L 1.0 * 10
-4Mol/L chloro-hexadecane yl pyridines, shake up, and with redistilled water, is settled to 5.0 mL, mixes;
(2) prepare the blank solution system: do not add the formaldehyde titer with the method for step (1) and prepare the blank solution system;
(3) get respectively by formaldehyde standard solution system and the blank solution system of step (1), (2) preparation appropriate, be placed in cuvette, on fluorospectrophotometer, synchronous scanning excitation wavelength and emission wavelength, the Resonance Rayleigh Scattering Spectra of acquisition system, the Resonance Rayleigh Scattering peak intensity value of mensuration system maximum wavelength 530 nm place formaldehyde standard solution systems
I, and the Resonance Rayleigh Scattering peak intensity value of measuring the blank solution system
I b, calculate Δ
I=
I b-
I
(4) with Δ
IThe concentration relationship of the PARA FORMALDEHYDE PRILLS(91,95) curve of working;
(5) measured object sample determination: take food the category sample, dry product is pulverized or wet product is rubbed, under phosphoric acid medium and defoamer existence, through steam distillation, absorb effluent with redistilled water and obtain to contain the measured object of formaldehyde, then pipette a certain amount of replacement formaldehyde standard solution,, by step (1)～(3) operation, calculate the Δ of measured object
I Sample=
I b-
I Sample
(6) Δ that records per sample
I Sample, look into the working curve of step (4), calculate the concentration of formaldehyde in measured object.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103604756A (en) * | 2013-11-29 | 2014-02-26 | 广西师范大学 | Resonance Rayleigh scattering (RRS) method for measuring azide ion |
| CN103645168A (en) * | 2013-12-10 | 2014-03-19 | 天津工业大学 | Preparation method of high-sensitivity formaldehyde gas sensor |
| CN104181136A (en) * | 2014-08-25 | 2014-12-03 | 广西师范大学 | Resonance Rayleigh scattering energy transfer spectroscopy for simply and rapidly measuring formaldehyde |
| CN104359879A (en) * | 2014-11-05 | 2015-02-18 | 广西师范大学 | Resonance Rayleigh scattering spectra method measuring tea polyphenol |
| CN104359865A (en) * | 2014-11-05 | 2015-02-18 | 广西师范大学 | Resonance Rayleigh scattering spectra method measuring ammonia |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103604756A (en) * | 2013-11-29 | 2014-02-26 | 广西师范大学 | Resonance Rayleigh scattering (RRS) method for measuring azide ion |
| CN103604756B (en) * | 2013-11-29 | 2016-02-03 | 广西师范大学 | A kind of Resonance Rayleigh Scattering Technique measuring azides ion |
| CN103645168A (en) * | 2013-12-10 | 2014-03-19 | 天津工业大学 | Preparation method of high-sensitivity formaldehyde gas sensor |
| CN104181136A (en) * | 2014-08-25 | 2014-12-03 | 广西师范大学 | Resonance Rayleigh scattering energy transfer spectroscopy for simply and rapidly measuring formaldehyde |
| CN104181136B (en) * | 2014-08-25 | 2017-03-29 | 广西师范大学 | A kind of Resonance Rayleigh Scattering energy transfer spectrographic method for determining formaldehyde |
| CN104359879A (en) * | 2014-11-05 | 2015-02-18 | 广西师范大学 | Resonance Rayleigh scattering spectra method measuring tea polyphenol |
| CN104359865A (en) * | 2014-11-05 | 2015-02-18 | 广西师范大学 | Resonance Rayleigh scattering spectra method measuring ammonia |
| CN104359865B (en) * | 2014-11-05 | 2017-03-22 | 广西师范大学 | Resonance Rayleigh scattering spectra method measuring ammonia |
| CN104359879B (en) * | 2014-11-05 | 2017-03-29 | 广西师范大学 | A kind of Resonance Rayleigh Scattering Spectral Method for determining tea polyphenols |
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Application publication date: 20131113 |