CN102192893B - Infrared photometric method for fast detecting oils in water - Google Patents
Infrared photometric method for fast detecting oils in water Download PDFInfo
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- CN102192893B CN102192893B CN 201110138832 CN201110138832A CN102192893B CN 102192893 B CN102192893 B CN 102192893B CN 201110138832 CN201110138832 CN 201110138832 CN 201110138832 A CN201110138832 A CN 201110138832A CN 102192893 B CN102192893 B CN 102192893B
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Abstract
The invention discloses an infrared photometric method for fast detecting oils in water, belonging to the field of water quality detection. The method comprises the following steps of: (1) extracting the oils in the water by using carbon tetrachloride and drying by using anhydrous sodium sulfate; (2) detecting infrared absorption of an extract liquor at 2930 cm<-1>, 2960 cm<-1> and 3030 cm<-1> by using a Fourier infrared spectral measuring instrument so as to determine the mass-volume concentration of the total oils; (3) determining the mol concentration of animal and plant oils through detecting the infrared absorption of the extract liquor at 1750-1735 cm<-1>, and figuring out the mass-volume concentration of the animal and plant oils in combination with the molecular weights of the animal and plant oils or a coefficient determined by an early detected sample; and (4) subtracting the mass-volume concentration of the total oils from the mass-volume concentrations of the animal and plant oils to obtain the mass-volume concentration of the petroleum. By using the method disclosed by the invention, the step processes of two scanning and one magnesium silicate adsorption adopted by using a general method are amplified into one scanning; and errors possibly brought by the use of a reagent and a multi-analysis step are reduced while the fast detection is realized.
Description
Technical field
The present invention relates to infrared spectrum detection method, the infrared range method of oils in a kind of fast measuring water of saying so more specifically.
Background technology
What abroad be widely used is that basic oil measuring method mainly contains EPA (1978) Method 418.1, ASTM (2003) Method D 3921-96 and APHA (2000) Method 5520C with the infrared absorption; They with domestic current GB GB/T 16488-1996 and the revised edition (having released exposure draft) that is near completion this year thereof though the extractant of principle and employing is slightly different; But after the testing process that adopts all is the extract pre-service; Scanning (always) extract is measured the quality-volumetric concentration (mg/L) of total oils for the first time; Remove the vegetable and animals oils in (always) extract through magnesium silicate absorption; Quality-the volumetric concentration of the extract mensuration petroleum-type after the vegetable and animals oils is removed in scanning for the second time; The difference of the quality-volumetric concentration of total oils and the quality-volumetric concentration of petroleum-type is quality-volumetric concentration (" the mensuration infrared spectrophotometry of water quality petroleum-type and animals and plants oils " (exposure draft) explanation of compilation of vegetable and animals oils; Environmental monitoring central station in Changchun is submitted in August, 2010, downloads network address: www.es.org.cn/download/2008-4.pdf).The mensuration process comprises 2 scanning step, 1 magnesium silicate adsorption step: length consuming time, can't realize the fast measuring to petroleum-type/vegetable and animals oils.
Summary of the invention
1. invent the technical matters that will solve
The infrared spectrophotometry that the purpose of this invention is to provide oils in a kind of fast measuring water, the mensuration that can be used for oils in the water be the instant mensuration in the contamination accident emergency monitoring particularly.
2. technical scheme
Principle of the present invention: the method for utilizing GB (comprising that original GB GB/T 16488-1996 reaches the revise method of having accomplished exposure draft) to adopt, measure 2930cm
-1, 2960cm
-1And 3030cm
-1The absorbance A at bands of a spectrum place
2930, A
2960, A
3030, use formula
Calculate the quality-volumetric concentration (mg/L) of total oils; Measure vegetable and animals oils ester group key (C=O) simultaneously at 1750cm
-1～1735cm
-1The absorbance A 1750～1735 at place is confirmed the vegetable and animals oils volumetric molar concentration, in conjunction with by vegetable and animals oils molecular weight or early stage surveying the coefficient that sample is confirmed, calculates vegetable and animals oils quality-volumetric concentration (mg/L).Quality-the volumetric concentration of total oils and the difference of vegetable and animals oils quality-volumetric concentration are petroleum-type quality-volumetric concentration.Single pass can be measured the quality-volumetric concentration of total oils, vegetable and animals oils and petroleum-type simultaneously, realizes the target of fast measuring.
Technical scheme of the present invention is following:
The infrared spectrophotometry of oils the steps include: in a kind of fast measuring water
(1), uses anhydrous sodium sulfate drying through the oils in the carbon tetrachloride extraction water;
(2) measure extract at 2930cm with Fourier's infrared spectrum measurement appearance
-1, 2960 cm
-1, 3030 cm
-1Infrared absorption confirm the quality-volumetric concentration (mg/L) of total oils;
(3) simultaneously through measuring extract at 1750-1735 cm
-1Infrared absorption confirm the volumetric molar concentration (mol/L) of vegetable and animals oils, in conjunction with by vegetable and animals oils molecular weight or early stage surveying the coefficient that sample is confirmed, calculate vegetable and animals oils quality-volumetric concentration (mg/L);
(4) quality-volumetric concentration and the vegetable and animals oils quality-volumetric concentration of total oils are subtracted each other the quality-volumetric concentration that draws petroleum-type.
Different according to the mode that the vegetable and animals oils volumetric molar concentration is converted into quality-volumetric concentration, can be subdivided into 2 kinds of schemes:
First kind of scheme: confirm that by the vegetable and animals oils molecular weight vegetable and animals oils volumetric molar concentration is converted into the scheme of the coefficient of quality-volumetric concentration.
Its detailed principle is: GB, EPA (1978) 418.1, ASTM D 3921-96, APHA 5520C etc. are the quality-volumetric concentration that is c h bond of relevant monitoring method mensuration both at home and abroad; Vegetable and animals oils is that the c h bond quality-volumetric concentration of triglyceride is not comprise three O-C=O keys in its molecule, just quality-the volumetric concentration of three O-C=O keys of vegetable and animals oils (triglyceride) molecule deduction.The mensuration that is applied to vegetable and animals oils concentration converts, and can be expressed as: identical A1750～1735 absorbances, promptly identical vegetable and animals oils volumetric molar concentration; The molecular weight of deducting behind three O-C=O keys is big more; Quality-the volumetric concentration of c h bond is big more, and proportional relation (also can equivalent be: identical c h bond quality-volumetric concentration, the molecular weight behind three O-C=O keys of vegetable and animals oils deduction is big more; A1750～1735 absorbances/vegetable and animals oils volumetric molar concentration is more little, and is inverse relation).
May further comprise the steps:
A1750～1735-olive oil quality-the volumetric concentration of (1) drawing olive oil (also can select other vegetable and animals oils for use) carbon tetrachloride solution is marked bent;
(2) nonpolar organic matters such as oils in the use carbon tetrachloride extraction water behind the use anhydrous sodium sulfate drying, carry out IR spectrum scanning to extract, are determined at 2930cm by national standard method
-1, 2960 cm
-1, 3030 cm
-1Quality-the volumetric concentration of total oils is calculated in the absorption at place
ρ 1 (mg/L);
(3) while sweep measuring 1750～1735 cm
-1The absorbance (A1750～1735) at place, contrast A1750～1735-olive oil quality-volumetric concentration mark is bent, confirms corresponding olive oil quality-volumetric concentration
ρ 2 (mg/L), design factor α=
(Mr ＇
1Be the molecular weight behind three O-C=O keys of olive oil molecule deduction; Mr ＇
2Be the molecular weight behind three O-C=O keys of animals and plants molecule deduction in the testing sample),
ρ 3 =α ρ 2 Be the quality-volumetric concentration of vegetable and animals oils in the sample;
(4) difference of total oils quality-volumetric concentration and vegetable and animals oils quality-volumetric concentration is petroleum-type quality-volumetric concentration.
Second kind of scheme: by surveying the scheme that sample is confirmed coefficient early stage
Its detailed principle is: similar with second piece of non-dispersion infrared photometry in the GB/T16488-1996 method; Introducing the vegetable and animals oils standard oil generally practices; Suppose that the vegetable and animals oils component ratio is identical in same project, the incident petroleum-type/vegetable and animals oils sample: first sample is measured 1750cm when detecting with national standard method
-1～1735cm
-1The absorbance A 1750～1735 at place is obtained ratio cc=ρ/A1750～1735 of the same A1750 of vegetable and animals oils concentration ρ～1735 in the sample.Subsequent sample detects then only need measure A1750～1735 draws simultaneously
A 2930 , A 2960 , A 3030 , α A1750～1735 are vegetable and animals oils concentration, with the method in the GB by
A 2930 , A 2960 And A 3030 Calculate total oil concentration, the difference of total oil concentration and vegetable and animals oils concentration is petroleum-type concentration.
May further comprise the steps:
(1) mensuration of first sample of same project, incident
1. measure total oils, petroleum-type and vegetable and animals oils with national standard method;
2. in the scanning first time of measuring total oils, sweep measuring 1750～1735 cm simultaneously
-1The absorbance (A1750～1735) at place;
The ratio of the vegetable and animals oils quality of 3. measuring according to the national standard method-same A1750 of volumetric concentration ρ～1735 is confirmed factor beta=ρ/A1750～1735;
(2) mensuration of the subsequent sample of same project, incident
1. use the nonpolar organic matters such as oils in the carbon tetrachloride extraction water, behind the use anhydrous sodium sulfate drying, extract is carried out IR spectrum scanning, be determined at 2930cm by national standard method
-1, 2960 cm
-1, 3030 cm
-1Quality-the volumetric concentration (mg/L) of total oils is calculated in the absorption at place;
2. sweep measuring 1750～1735 cm simultaneously
-1The absorbance (A1750～1735) at place, β A1750～1735 are the quality-volumetric concentration of vegetable and animals oils;
The difference of 3. total oils quality-volumetric concentration and vegetable and animals oils quality-volumetric concentration is petroleum-type quality-volumetric concentration.
2 kinds of transform modes can realize that all single pass measures total oils, vegetable and animals oils and petroleum-type concentration simultaneously.
3. beneficial effect
The inventive method has following beneficial effect: 2 scannings that universal method is adopted, the step process of 1 magnesium silicate absorption are simplified to 1 scanning, when having realized fast measuring, reduced reagent use and many analytical procedures the error that possibly bring.Can tackle desired instant, the fast measuring of emergency monitoring such as oil pollution incident.Single pass of the present invention can be measured total oil, vegetable and animals oils, petroleum-type concentration simultaneously; Realized the target of fast measuring: comprised 2 scanning step than what domestic and foreign current monitoring methods such as national standard method, EPA (1978) 418.1, ASTM D 3921-96, APHA 5520C adopted, the mensuration process convenient of 1 magnesium silicate adsorption step, quick.
Description of drawings
Fig. 1 is the infrared absorption peak figure of variable concentrations (0.2,2,5,10,20,50ppm) coconut oil;
Fig. 2 is 50ppm coconut oil and the infrared comparison diagram of 100ppm pristane;
Fig. 3 is the stack spectrogram of five vegetable oil spectrograms;
Fig. 4 is the enlarged drawing (2600cm of the stack of five vegetable oil spectrograms
-1~ 3100 cm
-1).
Embodiment
Further specify the present invention below in conjunction with accompanying drawing and embodiment.The embodiment of the invention adopts following cuvette to measure:
A kind of wide infrared band cuvette is made up of cuvette lid, cuvette quartz cell body and cuvette ZnSe window, the optical crystal that its light transmission part window materials are zinc selenide (as the crystalline material of optical medium material).ZnSe window materials transmission range 0.5～20 μ m, the ZnSe window materials are in refractive index inhomogeneity＜6 * 10 at 632.8nm place
-6 Cuvette pond body adopts the quartzy material of low hydroxyl.The absorption coefficient of ZnSe window materials at 10.6 μ m places is 0.0005/cm ± 0.0001.
The preparation method of wide infrared band cuvette, it may further comprise the steps:
(1) selects the crystalline material ZnSe optical crystal of making the optical medium material for use; The ZnSe crystal is carried out optical polish, plated film not; Process thick 2～3 (± 0.1) mm; Wide by 5～35 (± 0.1) mm, the rectangle window of high by 10～40 (± 0.1) mm or thick 2～4 (± 0.1) mm, the circular window of diameter 5～40 (± 0.1) mm;
(2) cuvette U type or circular pond body adopt the quartzy material of low hydroxyl; Size: wide (corresponding cuvette height or diameter) 20～40 (± 0.1) mm; Long (corresponding cuvette light path) has 10mm, three kinds of specifications of 40mm, 70～100 (± 0.1) mm, the product of three kinds of specifications such as Fig. 1～and shown in Figure 3;
(3) utilize tackifier that pond body and ZnSe window are linked together, process cuvette.
Embodiment 1 (A1750～1735-olive oil quality-the volumetric concentration mark is bent to be drawn)
With the olive oil is that benchmark is done typical curve, measures the peak area value (instrument integration) of each concentration, result such as table 1:
Table 1 A1750～1735-olive oil quality-volumetric concentration
Embodiment 2 (the infrared absorption peak figure of variable concentrations coconut oil)
Use the coconut oil solution of high-purity phenixin configuration variable concentrations (0.2,2,5,10,20,50ppm) (0.2,2,5,10,20,50ppm), use anhydrous sodium sulfate drying after, be determined at 2930cm
-1, 2960 cm
-1, 3030 cm-
1With 1750～1735 cm
-1Absorbance (the A at place
1), infrared spectrogram is as shown in Figure 1.The oils peak height/peak area of surveying and the proportional relation of concentration.
Embodiment 3 (mensuration of dissimilar oils)
Use high-purity phenixin configuration vegetable and animals oils (being example) and petroleum-type (being example), behind the use anhydrous sodium sulfate drying, be determined at 2930cm with pristane with coconut oil
-1, 2960 cm
-1, 3030 cm-
1With 1750～1735 cm
-1Absorbance (the A at place
1), infrared spectrogram is as shown in Figure 2.Vegetable and animals oils is at 1750～1735 cm
-1There is obvious absorption at the place, and petroleum-type does not have absorption herein basically.
Embodiment 4 (with the olive oil is reference, and first kind of scheme confirms that by the vegetable and animals oils molecular weight vegetable and animals oils volumetric molar concentration is converted into the plan-validation of the coefficient of quality-volumetric concentration)
A. receive each 10 in beaker, 50mL volumetric flask; Stick vegetable and animals oils (olive oil, soybean oil, palm oil, coconut oil, rapeseed oil) title; Pour a small amount of vegetable and animals oils into and go into beaker; Each pipettes 5 μ L vegetable and animals oils with micro syringe goes into to post in the volumetric flask of respective labels, and constant volume respectively disposes solution concentration with oil content analyzer mensuration.An amount of dilution, configuration 50mg/L solution, and with oil content analyzer mensuration, affirmation concentration.Table 2 has been listed the mean molecular weight of common vegetable and animals oils and has been deducted three molecular weight behind the O-C=O key.
Common vegetable and animals oils mean molecular weight of table 2 and deduction O-C=O key molecular weight thereof
| Fat type | English name | Molecular weight (Mr) | Molecular weight (Mr ＇) behind the deduction O-C=O key |
| Rapeseed oil | Colza | 932 | 800 |
| Olive oil | Olive Oil | 897 | 765 |
| Soybean (soya bean) oil | Chinese Bean | 873 | 741 |
| Palm oil | Palm | 853 | 721 |
| Coconut oil | Coconut | 655 | 523 |
B. measure olive oil, soybean oil, palm oil, coconut oil, rapeseed oil 50mg/L solution at 1750-1735cm
-1The characteristic absorption peak area at place, and checking " identical c h bond quality-volumetric concentration, the molecular weight behind three O-C=O keys of vegetable and animals oils deduction is big more, A1750～1735 absorbances/vegetable and animals oils volumetric molar concentration is more little, and is inverse relation ".Table 3 has been listed the checking result.
Table 3 formula (2) checking measured result
Relative deviation scope-3.0%～7.4%, measured result and theoretical prediction basically identical.
Embodiment 5 (actual sample is measured and second kind of plan-validation)
(1) determination step of actual sample
Get the same measuring point of same enterprise and check and accept monitoring 4 of water samples (4 times, 1 day), sample is all gathered 500ml by the requirement of GB revision exposure draft.
A. the mensuration of the 1st sample
A. the sample that collects all is transferred in the 1000ml separating funnel, behind 20ml phenixin (the same GB of purity requirement, as follows) washing sample bottle, all is transferred in the separating funnel, the 2min that fully vibrates, and often open the piston exhaust.Behind the standing demix, extract is transferred in the 50ml volumetric flask through the glass sand core funnel of placing about 10mm thickness anhydrous sodium sulfate (the same GB of purity requirement).With 20ml phenixin re-extract once, get an amount of phenixin cleaning glass sand core funnel, cleansing solution is transferred in the volumetric flask in the lump, with the phenixin constant volume and shake up.
The upper water phase transfer to the 500ml graduated cylinder, is confirmed the volume Vw of water sample.
B. extract is poured in the 4cm cuvette, made reference solution, in 2930 cm with phenixin
-1, 2960 cm
-1, 3030 cm
-1Its absorbance is measured at the place
A 1.2930 , A 1.2960 , A 1.3030 , calculate total oily concentration (computing method are revised exposure draft with GB); Measure 1750-1735cm simultaneously
-1Absorption A1750～1735 at place.
C. then about 20ml extract is transferred in the tool plug ground conical flask; Add about 5g magnesium silicate, place on the gyrate shaker, with the speed continuous oscillation 20min of 180-200rpm; After staticly settling, supernatant is filtered in the tool plug ground conical flask through the glass sand core funnel and is used to measure petroleum-type.
D. in 2930 cm
-1, 2960 cm
-1, 3030 cm
-1Its absorbance is measured at the place
A 2.2930 , A 2.2960 , A 2.3030 ,And calculate the concentration (computing method are revised exposure draft with GB) of petroleum-type.。
The difference of e. total oil concentration and petroleum-type concentration is animals and plants oils concentration.
F. the ratio of the design factor vegetable and animals oils quality-same A1750 of volumetric concentration ρ～1735, β=ρ/A1750～1735.
B. subsequent sample (mensuration of the 2nd, 3,4 sample)
A, b step be the mensuration of the 1st sample together
c.?βA1750～1735。Be vegetable and animals oils concentration, total oils is petroleum-type concentration with the difference of vegetable and animals oils.
(2) actual sample monitoring result
Table 4 rapid test method is measured the result
| Sample number into spectrum | The A-peak area | Total oils concentration (mg/L) | Petroleum-type concentration (mg/L) | Vegetable and animals oils concentration (mg/L) | ρ/A1750～1735 |
| 1 | 1.072315 | 15.89 | 3.67 | 12.22 | 11.3959 |
| 2 | 1.145457 | 16.77 | 3.72 | 13.05 | ? |
| 3 | 1.187434 | 17.81 | 4.28 | 13.53 | ? |
| 4 | 1.534325 | 21.93 | 4.44 | 17.49 | ? |
Annotate: relative deviation is relatively drawn by each measured value in ρ/A1750～1735 and mensuration average.
(3) by surveying the plan-validation that sample is confirmed coefficient early stage
For proof scheme, when the 2nd, 3,4 sample being measured, measure result such as table 5 with the method for GB revision exposure draft simultaneously with this rapid test method.
Table 5 National Standard Method (revision exposure draft) is measured the result
| Sample number into spectrum | Total oils concentration (mg/L) | Petroleum-type concentration (mg/L) | Vegetable and animals oils concentration (mg/L) |
| 1 | 15.89 | 3.67 | 12.22 |
| 2 | 16.77 | 3.73 | 13.04 |
| 3 | 17.81 | 3.87 | 13.94 |
| 4 | 21.93 | 3.84 | 18.09 |
The result who 2 kinds of methods is measured vegetable and animals oils compares, like table 6
2 kinds of method vegetable and animals oils of table 6 concentration determination result contrast
| Sample number into spectrum | Express method is measured vegetable and animals oils concentration (mg/L) | National Standard Method is measured vegetable and animals oils concentration 2 (mg/L) | Relative deviation (%) |
| 2 | 13.05 | 13.04 | -0.08 |
| 3 | 13.53 | 13.94 | 3.03 |
| 4 | 17.49 | 18.09 | 3.43 |
Claims (2)
1. the infrared spectrophotometry of oils in the fast measuring water the steps include:
(1), uses anhydrous sodium sulfate drying through the oils in the carbon tetrachloride extraction water;
(2) measure extract at 2930cm with Fourier's infrared spectrum measurement appearance
-1, 2960 cm
-1, 3030 cm
-1Infrared absorption confirm the quality-volumetric concentration of total oils;
(3) simultaneously through measuring extract at 1750-1735 cm
-1Infrared absorption confirm the volumetric molar concentration of vegetable and animals oils, in conjunction with the coefficient of confirming by the vegetable and animals oils molecular weight, calculate vegetable and animals oils quality-volumetric concentration, the determination step of vegetable and animals oils quality-volumetric concentration wherein is:
A1750～1735-quality-the volumetric concentration of (A) drawing the olive oil carbon tetrachloride solution is marked bent;
(B) oils in the use carbon tetrachloride extraction water, this oils is nonpolar organic matter, behind the use anhydrous sodium sulfate drying, extract is carried out IR spectrum scanning, is determined at 2930cm by national standard method
-1, 2960 cm
-1, 3030 cm
-1Quality-the volumetric concentration of total oils is calculated in the absorption at place
ρ 1
(C) while sweep measuring 1750～1735 cm
-1The absorbance A 1750～1735 at place, contrast A1750～1735-olive oil quality-volumetric concentration mark is bent, confirms corresponding olive oil quality-volumetric concentration
ρ 2 , design factor α=
, wherein
Mr 1 ＇Be the molecular weight behind three O-C=O keys of olive oil molecule deduction;
Mr ＇ 2 Be the molecular weight behind three O-C=O keys of vegetable and animals oils molecule deduction in the testing sample,
ρ 3 =α ρ 2 Be the quality-volumetric concentration of vegetable and animals oils in the sample;
(4) quality-volumetric concentration and the vegetable and animals oils quality-volumetric concentration of total oils are subtracted each other the quality-volumetric concentration that draws petroleum-type.
2. according to the infrared spectrophotometry of oils in the fast measuring water described in the claim 1, it is characterized in that single pass measures total oil, vegetable and animals oils, petroleum-type concentration simultaneously.
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| CN102749285A (en) * | 2012-06-29 | 2012-10-24 | 苏州国环环境检测有限公司 | Method for determining oil substances in water sample by infrared spectrophotometry |
| CN102798605A (en) * | 2012-06-29 | 2012-11-28 | 苏州国环环境检测有限公司 | Method for determining oil substances in water sample according to infrared spectrophotometry |
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| CN105181922B (en) * | 2015-09-18 | 2017-04-19 | 上海昂林科学仪器有限公司 | Device for measuring animal and plant oil |
| CN107490559A (en) * | 2016-06-13 | 2017-12-19 | 中国石油化工股份有限公司 | A kind of method for determining oily area's solid waste petrochina class content |
| CN106404707A (en) * | 2016-08-30 | 2017-02-15 | 惠州市东森检测技术有限公司 | Rapid determination method of petroleum and animal and vegetable oils in water |
| CN106483089B (en) * | 2016-09-19 | 2019-07-30 | 河海大学 | A kind of multiduty hydrometric cableway current surveying device of multi-mode set and method |
| CN110487733A (en) * | 2019-08-09 | 2019-11-22 | 南通化学环境监测站有限公司 | A kind of measurement surface water, underground water, in seawater petroleum-type measuring method |
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