CN102175671A - Schiff's reagent suitable for fast measuring formaldehyde in indoor air of family - Google Patents
Schiff's reagent suitable for fast measuring formaldehyde in indoor air of family Download PDFInfo
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Abstract
The invention relates to a Schiff's reagent suitable for fast measuring formaldehyde in indoor air of a family, and belongs to the technical field of formaldehyde measurement. The Schiff's reagent comprises fuchsine, sodium sulphite and organic acid, wherein the organic acid is a mixture of one or more of formic acid, acetic acid, propionic acid, oxalic acid, malonic acid, succinic acid, malic acid, tartaric acid and citric acid; and the concentration of the organic acid is 1%-90%. The Schiff's reagent related by the invention has the characteristics of low corrosivity and short colour developing reaction time, so that the Schiff's reagent is more suitable for fast measuring the formaldehyde in the indoor air of the family.
Description
Technical field
The present invention relates to a kind of Schiff's reagent that is suitable for fast measuring formaldehyde in the family room air, belong to the formaldehyde determination technical field.
Background technology
Formaldehyde is one of main room atmosphere pollution in the modern day life, and formaldehyde is in second on China's toxic chemical list.Airborne formaldehyde will produce harm to the respiratory tract of humans and animals when surpassing certain content; The formaldehyde of high concentration all has damaging effect to nervous system, immune system and liver.Be defined as suspicious teratogenesis, carcinogen by The World Health Organization (WHO).
Along with the development of modern petroleum industry, various chemical materials are applied in the modern life articles for use, as clothing, and furniture, building materials, wrappage etc.Because a large amount of chemical materials is used in interior decoration, make that organic content increases greatly in the room air, cause room air pollution serious day by day.Therefore symptoms such as dizziness, allergy, respiratory tract infection appear in many people.Formaldehyde is exactly one of comparatively serious major pollutants of wherein influence.Therefore, in time understand the content of formaldehyde of living environment, to guaranteeing resident's physical and mental health, it is significant to improve the resident living quality.China is respectively at 1995,2000, puts into effect serial concerned countries standard in 2001 and 2002.GB/T16127-1995 " hygienic standard of formaldehyde in the indoor air ", GB/T15516-1995 " the mensuration diacetone spectrophotometric method of air quality formaldehyde ", GB/T 16129-1995 2 " formaldehyde health test method spectrophotometric method in the atmosphere of residential district ", GB 18582-2001 " limits of harmful substances in the indoor decorating material interior wall coating ", GB18583-2001 " limits of harmful substances in the indoor decorating adhesive ", GB/T 18204.26-2000 " method for determining formaldehyde in the public place air ", GB50325-2001 " civil building engineering indoor environmental pollution control standard ", and GB/T18883-2002 " IAQ (indoor air quality) national standard ".As seen, the attention degree that is subjected to of formaldehyde in indoor air pollution monitoring.
Divide by principle, the method for formaldehyde determination can be divided into spectroscopic methodology, chromatography and electrochemical process three major types.Chromatography comprises liquid phase chromatography and vapor-phase chromatography, all belongs to the large-scale instrument analytical approach, and principal feature is a sensitivity accuracy height.The galvanochemistry ratio juris is to utilize the variation of the oxidation-reduction potential of formaldehyde itself, directly measures the content of formaldehyde.Have highly sensitive, the characteristics that selectivity is good.It is a kind of method that is suitable for content of formaldehyde fast monitored in the gas.Portable formaldehyde analyser in the market adopts this monitoring principle mostly, as: 4160 serial air formaldehyde determination instrument of American I nterscan company Development and Production, the Z-300 series formaldehyde determination instrument that U.S. ESC Inc. produces etc. adopt the principle of electrochemical monitoring exactly.But, studies show that the application of this instrument and the restriction (referring to " Chinese Journal of Preventive Medicine; 2003; 37 (3): 195-196 ") that popularization is subjected to big self performance, the shortcoming of the formaldehyde determination instrument maximum of this principle is that the influence of carbon dioxide in air is not easy to eliminate, the performance of electrochemical detector is received the influence that the instrument absorbing medium runs off easily in addition, and needs long-time preheating before using.The principle that methylene oxide detecting instrument employing electrochemical monitoring in the homemade gas is also arranged in the market, as: the CPR-B formaldehyde gas detector that Jinan ancient cooking vessel promise gas detection company limited produces, the GD80-CH2O that the Cole of Shenzhen promise electronics technology company limited produces, the serial methylene oxide detecting instrument that the ease skies, Shenzhen Electronics Co., Ltd. produces etc.
The principle of spectrographic determination formaldehyde is to utilize formaldehyde and some chemical reagent to react colorific variation, and the depth of color is linear relevant with the content of formaldehyde, thereby calculates the content of formaldehyde.Only need the variation of the light absorption value of record reaction solution in the actual measurement process, just can calculate the content of formaldehyde.Have fast, easy, sensitive characteristics is suitable for developing easy on-the-spot formaldehyde determination instrument.The method of spectrographic determination formaldehyde comprises following several: iodine/starch method, acetylacetone method, AHMT method, phenol reagent process, magenta-sulfurous method.In said method, iodine/starch method is a method more accurately, the demarcation of content of formaldehyde in being usually used in standard formalin.Formaldehyde and iodine generation quantitative reaction are faded iodamylum.But operate more loaded down with trivial detailsly, be not suitable for the fast monitored of formaldehyde.Acetylacetone method, the AHMT method, phenol reagent process all was selected in the national standard method that content of formaldehyde is measured in the different times air.Similar with the iodamylum method, acetylacetone method need pass through processes such as adding thermal response, is not suitable for the express-analysis of formaldehyde, and AHMT method reagent price is expensive, uses less at present.Phenol reagent process is the method for existing national air quality standard, has sensitivity, stable characteristics (referring to " Shanghai metrology and measurement, 2003,30 (5): 17-19 ").The developer has developed the formaldehyde determination instrument in order to cater to request of national standard according to this principle design.The main composition of this instrument is a formaldehyde collection tube, a reaction tube, and a spectrophotometer is formed.Formaldehyde collection, chromogenic reaction and light absorption value are measured and are carried out respectively.The formaldehyde determination instrument of this method exploitation can carry out field monitoring, and sensitivity as a result, accurately and reliably.But, need to divide and manually add reagent several times, collect, react and measure and manually carry out, affected too loaded down with trivial details.Because exploitation is made according to national standard, thus relatively be suitable for functional department, or corresponding professional institution uses.Another shortcoming of this instrument is that proceed step by step (referring to " life science instrument 2008; 6 (4): 11-13 ") is collected and measured to formaldehyde, can only realize collecting the airborne sample of certain volume according to schedule, measure then, be unfavorable for adjusting the volume of collecting sample flexibly according to the needs of different spaces.The JC-3 methylene oxide detecting instrument of Xuzhou brocade journey environmental protection equipment company limited production in the market, products such as the refreshing board methylene oxide detecting instrument in sky that Beijing Health-care Science ﹠ Technology Co., Ltd. produces adopt this principle.It is the air quality standard assay method that magenta-sulfurous method is measured formaldehyde not selected because adopt mercury reagent (referring to " beverage industry; 2002; 5 (5): 47-48 ") in the early stage method, but measure free formaldehyde in China's standards of pharmacopoeia and adopt this method (referring to " " 2005 editions 3 ones of Chinese pharmacopoeia, appendix VI L ").Improved magenta-sulphurous acid formaldehyde determination method does not use mercury reagent (referring to " physical and chemical inspection-chemical fascicle, 2005,41:17-20; Modern instrument, 2008, (4): 9-12; Agricultural University Of Shenyang's journal, 2007,38 (2): 202-206; Analytica Chimica acta2008, (23): 109-116 ").As far back as 1996 formaldehyde fast detecting instrument (referring to " modern instrument, 2008, (4): 9-12 ") in the air that adopts this principle development is just arranged, but employing is passive type (diffusion type) reaction, and spectrophotometer and two kinds of metering systems of range estimation are arranged.The sensitivity of measurement result, accuracy, and reappearance all cannot ensure.Zhang Xiumin etc. prepare the reagent that magenta-sulfurous method is measured formaldehyde, reaction conditions, and the relation of response time and concentration of formaldehyde, color ranges etc. have been carried out systematic research, prove that this method is suitable for the fast monitored of formaldehyde in the air.Because collection and the chromogenic reaction of formaldehyde can be carried out simultaneously, therefore, this method can absorb formaldehyde, colour developing and spectrophotometer colorimetric are integrated in the color comparison tube and carry out, so be more suitable for producing portable field formaldehyde repid test instrument.
Consider that from the cost aspect price of formaldehyde determination instrument in the market is 500 yuan to several ten thousand yuan and does not wait (referring to " modern instrument, 2008, (4): 9-12; Http:// price.c-bm.com/2009/4/25-17-0-132058.html; Http:// www.cntrades.com/info/detail-458252.html; Http:// www.metalnews.cn/price/show-281118-1.html; Http:// china.53trade.com/ProductDetail/59712.htm ").In general adopt the spectrophotometric method need be at the integrated spectrophotometer of instrument internal, the instrument price comparison be expensive and relatively heavier, but the result accurately and reliably, is more suitable for using with professional institution.It is very little to use chemical sensor to accomplish product, but the result is relatively more unstable.In fact, the effect of the formaldehyde determination instrument of Shi Yonging is just done oneself's understanding to gaseous contamination degree in the room in daily life, does not need accurate especially measurement result, therefore, adopts the mode of color range range estimation to meet the demands.
Employed formaldehyde determination instrument is seen patent " formaldehyde determination instrument " among the present invention, and its patent No. is 201020647709.8.
Summary of the invention
The objective of the invention is in order to propose a kind of Schiff's reagent that is suitable for fast measuring formaldehyde in the family room air.
The objective of the invention is to be achieved through the following technical solutions.
A kind of Schiff's reagent that is suitable for fast measuring formaldehyde in the family room air of the present invention comprises magenta, sodium sulphite and organic acid;
Wherein organic acid is one or more the potpourri in formic acid, acetate, propionic acid, ethane diacid, malonic acid, succinic acid, malic acid, tartrate, the citric acid; Organic acid concentration is 1%～90%.
The mensuration scheme of content of formaldehyde is as follows in the air:
1) Schiff's reagent is joined on the reaction medium of formaldehyde determination instrument chromoscope;
2) start aspiration pump, and start timer, the connecting pipe at air process reaction medium (filter paper) place under the twitch of pump;
3) time of bleeding of air is suitably adjusted according to the depth of the color of chromogenic reaction generation;
4) color of reaction medium (filter paper) and the color of colorimetric card are compared the content of formaldehyde in the air that estimation is measured;
5) according to the speed of evacuation with the volume of the air that Time Calculation measures of bleeding;
6) calculate the concentration of formaldehyde in the air of being measured divided by the volume of air measured with the amount of the formaldehyde of estimation.
Beneficial effect
Schiff's reagent corrosivity of the present invention is low, and the chromogenic reaction time is short, is more suitable in the family fast measuring of formaldehyde in the air.
Embodiment
Embodiment 1
A kind of Schiff's reagent that is suitable for fast measuring formaldehyde in the family room air comprises 0.2% fuchsin solution, 10% sodium sulfite solution and 50% formic acid solution, and the volume ratio of three kinds of solution is 1: 2: 2.
Traditional and comparison Schiff's reagent developing time of the present invention
Formaldehyde is 150 micrograms, when 75 micrograms and 30 micrograms, is respectively 15 seconds with first apparent time of the Schiff's reagent of hydrochloric acid preparation, and 15 seconds and 20 seconds, just the apparent time was 6 seconds with the Schiff's reagent of formic acid preparation.Illustrate that the Schiff's reagent colour developing of formic acid preparation is faster than the Schiff's reagent of hydrochloric acid preparation.The Schiff's reagent color balance time with the formic acid preparation is 10 minutes, and the Schiff's reagent color balance time of preparing with hydrochloric acid needs 60 minutes, illustrates that the former is more suitable in express-analysis.
The sensitivity of Schiff's reagent of the present invention
0.15 during microgram formaldehyde, range estimation can be differentiated the change color of reaction.The detection that this reagent PARA FORMALDEHYDE PRILLS(91,95) is described is limited the quantity of and is lower than 0.15 microgram.If bleed 30 liters, the formaldehyde absorption efficiency according to 50% is calculated, and contains 1.0 microgram formaldehyde in every cubic metres of air and promptly can be observed change in color.According to existing national standard, in the indoor air formaldehyde limit the quantity of be every cubic metre of 80 microgram (0.08 milligram every cubic metre, GB/T16127-1995; 0.08 every cubic metre of milligram GB/T18883-2002), so the sensitivity of this method surpasses 80 times that GB is limited the quantity of, satisfies the fast detecting needs of formaldehyde in the gas of room fully.
Formaldehyde determination result's accuracy
Found that of the light absorption value comparison of the formaldehyde reaction liquid that Schiff's reagent absorbs in the formaldehyde determination instrument and the reactant liquor of solution reaction, Schiff's reagent can adsorb the formaldehyde of 70%-80% in the fixed gas, single measurement maximum error 41%, when formaldehyde is 1.5 micrograms, 0.75 average error is respectively 24% when microgram and 0.3 microgram, 27% and 17%, illustrate that measurement result can represent formaldehyde actual content in the air to a certain extent.The relative standard deviation that duplicate measurements is 3 times is lower than 20%, illustrates that this instrument has stability preferably, can satisfy test request.
The stability of Schiff's reagent
Placed 0 hour from Schiff's reagent of the present invention, after 6 hours and 24 hours, with the color of 0.75 microgram formaldehyde reaction solution as can be seen, Schiff's reagent of the present invention was stable in six hours at least, can satisfy test request.
The making of color range colorimetric card
Get pinkish red aqueous solution, sodium sulfite aqueous solution and aqueous formic acid by 1: 2: 2, fully mix in order, be mixed with Schiff's reagent.Respectively get above-mentioned Schiff's reagent 60 microlitres, add 22.5 micrograms respectively, 15 micrograms, 7.5 micrograms, 1.5 micrograms, 0.75 microgram, 0.3 microgram and 0.15 microgram formaldehyde inject chromoscope with reaction mixture, and it is adsorbed on the colour developing test paper, the record connecting pipe is made the color range colorimetric card of visual colorimetry together with the color of filter paper rapidly.
The mensuration scheme of content of formaldehyde is as follows in the air:
1) will be on the reaction medium of Schiff's reagent that 1: 2: 2 0.2% fuchsin solution, 10% sodium sulfite solution and 50% formic acid solution the prepare chromoscope that joins the formaldehyde determination instrument by volume ratio;
2) start aspiration pump, and start timer, the connecting pipe at air process reaction medium place under the twitch of pump;
3) write down the bleed time and the speed of evacuation;
4) color of reaction medium and the color of colorimetric card are compared the content of formaldehyde in the air that estimation is measured;
5) according to the speed of evacuation with the volume of the air that Time Calculation measures of bleeding;
6) calculate the concentration of formaldehyde in the air of being measured divided by the volume of air measured with the amount of the formaldehyde of estimation.
Respectively to certain office, and the air of newly purchasing certain brand file cabinet inside measures, and the sampling time was respectively 20 minutes and 10 minutes, and Ventilation Rate is 1 liter/minute.
The result calculates:
20 liters of about 0.75 micrograms of formaldehyde in indoor air content, so the content of the formaldehyde that records in the room air is about:
0.75 every cubic metre of * (1000 ÷ 20)=37.5 microgram
Because the absorptivity of formaldehyde is approximately 70%, so the actual content of formaldehyde is about in the air:
37.5 every cubic metre of ÷ 0.7=53.5 microgram
The content of formaldehyde is about every cubic metre of 107.0 microgram in the identical method calculation document cabinet
Content of formaldehyde is for being no more than every cubic metre of 100 microgram in the indoor air of stipulating in China's construction work examination air quality standard, find out that from the result who detects the content of formaldehyde of air the office that is measured requires content a little less than national standard, the content of formaldehyde of air is a little more than national standard in the file cabinet.
Embodiment 2
Chromogenic reaction with fuchsin acetate reagent
According to pinkish red aqueous solution, sodium sulfite aqueous solution and 1: 2: 2 ratio of 50% acetic acid aqueous solution volume ratio, earlier pinkish red aqueous solution and sodium sulfite aqueous solution are mixed, treat that fuchsin solution fades after, add 50% acetic acid solution, be configured to fuchsin acetate reagent.Get above-mentioned Schiff's reagent 40 microlitres, add formalin 10 microlitres, mixing.The mixed solution displaing amaranth.
Embodiment 3
Ethane diacid, malonic acid, succinic acid, malic acid, tartrate, the chromogenic reaction of the Schiff's reagent of propionic acid preparation
According to pinkish red aqueous solution, sodium sulfite aqueous solution and 1: 2: 2 ratio of 30% aqueous acid volume ratio, earlier pinkish red aqueous solution and sodium sulfite aqueous solution are mixed, treat that fuchsin solution fades after, add above-mentioned acid solution respectively, be configured to Schiff's reagent.Get above-mentioned Schiff's reagent 40 microlitres, add formalin 10 microlitres, mixing.The mixed solution displaing amaranth.
Embodiment 4
The chromogenic reaction of the Schiff's reagent of the formic acid preparation of variable concentrations
According to pinkish red aqueous solution, sodium sulfite aqueous solution and 1: 2: 2 ratio of 2.5% aqueous formic acid volume ratio, earlier pinkish red aqueous solution and sodium sulfite aqueous solution are mixed, treat that fuchsin solution fades after, add above-mentioned formic acid solution, be configured to Schiff's reagent.
Other gets pinkish red aqueous solution, sodium sulfite aqueous solution and 50% aqueous formic acid according to 1: 2: 2 ratio of volume ratio, earlier pinkish red aqueous solution and sodium sulfite aqueous solution is mixed, treat that fuchsin solution fades after, add above-mentioned formic acid solution, be configured to Schiff's reagent.
Other gets pinkish red aqueous solution, each 5 microlitre of sodium sulfite aqueous solution, fully mixes, and the back of fading adds pure formic acid 90 microlitres, and fully mixing is standby.
Get above-mentioned Schiff's reagent 40 microlitres, add formalin 10 microlitres, mixing.The mixed solution displaing amaranth.
Claims (3)
1. a Schiff's reagent that is suitable for fast measuring formaldehyde in the family room air is characterized in that: comprise magenta, sodium sulphite and organic acid.
2. a kind of Schiff's reagent that is suitable for fast measuring formaldehyde in the family room air according to claim 1 is characterized in that: organic acid is one or more the potpourri in formic acid, acetate, propionic acid, ethane diacid, malonic acid, succinic acid, malic acid, tartrate, the citric acid.
3. a kind of Schiff's reagent that is suitable for fast measuring formaldehyde in the family room air according to claim 1 is characterized in that: organic acid concentration is 1%～90%.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103217419A (en) * | 2013-04-08 | 2013-07-24 | 陕西理工学院 | Quick detecting method for formaldehyde content in aquatic product |
| CN105388153A (en) * | 2015-11-30 | 2016-03-09 | 湖北微控生物科技有限公司 | Rapid qualitative analysis method of formaldehyde in glutaraldehyde |
| CN106841193A (en) * | 2017-01-27 | 2017-06-13 | 广州能源检测研究院 | A kind of method that the preparation method and application of test solution test solution tests concentration of formaldehyde |
| CN107340289A (en) * | 2017-06-28 | 2017-11-10 | 防城港市质量技术监督局 | A kind of formaldehyde determination kit |
| CN115025059A (en) * | 2022-05-19 | 2022-09-09 | 浙江华光胶囊股份有限公司 | Gelatin hollow capsule with self-color development function and application thereof in pharmaceutical field |
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| GB1498192A (en) * | 1975-09-11 | 1978-01-18 | Kodak Ltd | Material for determining sulphur dioxide |
| CN101000310A (en) * | 2007-01-15 | 2007-07-18 | 浙江大学 | Method for investigating formol |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| GB1498192A (en) * | 1975-09-11 | 1978-01-18 | Kodak Ltd | Material for determining sulphur dioxide |
| CN101000310A (en) * | 2007-01-15 | 2007-07-18 | 浙江大学 | Method for investigating formol |
Non-Patent Citations (1)
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| 《中国卫生检验杂志》 20100430 胡亚奇，等 品红亚硫酸法测定居室空气中的甲醛 765－766 1－3 第20卷, 第4期 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103217419A (en) * | 2013-04-08 | 2013-07-24 | 陕西理工学院 | Quick detecting method for formaldehyde content in aquatic product |
| CN105388153A (en) * | 2015-11-30 | 2016-03-09 | 湖北微控生物科技有限公司 | Rapid qualitative analysis method of formaldehyde in glutaraldehyde |
| CN106841193A (en) * | 2017-01-27 | 2017-06-13 | 广州能源检测研究院 | A kind of method that the preparation method and application of test solution test solution tests concentration of formaldehyde |
| CN107340289A (en) * | 2017-06-28 | 2017-11-10 | 防城港市质量技术监督局 | A kind of formaldehyde determination kit |
| CN115025059A (en) * | 2022-05-19 | 2022-09-09 | 浙江华光胶囊股份有限公司 | Gelatin hollow capsule with self-color development function and application thereof in pharmaceutical field |
| CN115025059B (en) * | 2022-05-19 | 2023-07-14 | 浙江华光胶囊股份有限公司 | Gelatin hollow capsule with self-color development function and application thereof in pharmaceutical field |
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Application publication date: 20110907 |