CN112945939A - Method for detecting content of phosphorus element in grease by utilizing ICP organic sample injection - Google Patents
Method for detecting content of phosphorus element in grease by utilizing ICP organic sample injection Download PDFInfo
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- 229910052698 phosphorus Inorganic materials 0.000 title claims abstract description 98
- 239000011574 phosphorus Substances 0.000 title claims abstract description 98
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 title claims abstract description 94
- 239000004519 grease Substances 0.000 title claims abstract description 77
- 238000000034 method Methods 0.000 title claims abstract description 64
- 238000002347 injection Methods 0.000 title claims abstract description 17
- 239000007924 injection Substances 0.000 title claims abstract description 17
- 238000009616 inductively coupled plasma Methods 0.000 claims abstract description 55
- 239000012086 standard solution Substances 0.000 claims abstract description 43
- 230000003595 spectral effect Effects 0.000 claims abstract description 33
- 238000005259 measurement Methods 0.000 claims abstract description 29
- 238000007865 diluting Methods 0.000 claims abstract description 19
- 238000010790 dilution Methods 0.000 claims abstract description 5
- 239000012895 dilution Substances 0.000 claims abstract description 5
- 150000003017 phosphorus Chemical class 0.000 claims abstract description 4
- 239000003921 oil Substances 0.000 claims description 50
- 235000019198 oils Nutrition 0.000 claims description 50
- 239000003350 kerosene Substances 0.000 claims description 23
- 241001048891 Jatropha curcas Species 0.000 claims description 22
- 239000003085 diluting agent Substances 0.000 claims description 14
- 239000002540 palm oil Substances 0.000 claims description 12
- 239000003549 soybean oil Substances 0.000 claims description 11
- 239000002699 waste material Substances 0.000 claims description 11
- 235000019482 Palm oil Nutrition 0.000 claims description 10
- 239000010779 crude oil Substances 0.000 claims description 10
- 235000012424 soybean oil Nutrition 0.000 claims description 9
- NHTMVDHEPJAVLT-UHFFFAOYSA-N Isooctane Chemical compound CC(C)CC(C)(C)C NHTMVDHEPJAVLT-UHFFFAOYSA-N 0.000 claims description 4
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 4
- JVSWJIKNEAIKJW-UHFFFAOYSA-N dimethyl-hexane Natural products CCCCCC(C)C JVSWJIKNEAIKJW-UHFFFAOYSA-N 0.000 claims description 4
- 239000008096 xylene Substances 0.000 claims description 4
- 238000012417 linear regression Methods 0.000 claims description 3
- 238000005070 sampling Methods 0.000 claims 7
- 150000003904 phospholipids Chemical class 0.000 abstract description 18
- 239000000523 sample Substances 0.000 description 95
- 238000004458 analytical method Methods 0.000 description 15
- 238000001514 detection method Methods 0.000 description 13
- 238000012360 testing method Methods 0.000 description 12
- 238000005303 weighing Methods 0.000 description 8
- 238000011084 recovery Methods 0.000 description 7
- 239000007789 gas Substances 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 6
- 238000010561 standard procedure Methods 0.000 description 6
- 239000002383 tung oil Substances 0.000 description 6
- 238000004380 ashing Methods 0.000 description 4
- 239000003960 organic solvent Substances 0.000 description 4
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 3
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 3
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 3
- 229910019142 PO4 Inorganic materials 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 3
- 238000004737 colorimetric analysis Methods 0.000 description 3
- 235000013305 food Nutrition 0.000 description 3
- 238000004128 high performance liquid chromatography Methods 0.000 description 3
- 229910052750 molybdenum Inorganic materials 0.000 description 3
- 239000011733 molybdenum Substances 0.000 description 3
- 239000010452 phosphate Substances 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- 239000002199 base oil Substances 0.000 description 2
- 230000002349 favourable effect Effects 0.000 description 2
- 238000005984 hydrogenation reaction Methods 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 238000000120 microwave digestion Methods 0.000 description 2
- 235000014593 oils and fats Nutrition 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 241000319057 Kalopanax septemlobus Species 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 150000001414 amino alcohols Chemical class 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000012490 blank solution Substances 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- OEYIOHPDSNJKLS-UHFFFAOYSA-N choline Chemical compound C[N+](C)(C)CCO OEYIOHPDSNJKLS-UHFFFAOYSA-N 0.000 description 1
- 229960001231 choline Drugs 0.000 description 1
- 239000000571 coke Substances 0.000 description 1
- 238000010411 cooking Methods 0.000 description 1
- 235000014113 dietary fatty acids Nutrition 0.000 description 1
- 230000029087 digestion Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000003995 emulsifying agent Substances 0.000 description 1
- 230000001804 emulsifying effect Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000005281 excited state Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 229930195729 fatty acid Natural products 0.000 description 1
- 239000000194 fatty acid Substances 0.000 description 1
- 150000004665 fatty acids Chemical class 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 150000002632 lipids Chemical class 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- MEFBJEMVZONFCJ-UHFFFAOYSA-N molybdate Chemical compound [O-][Mo]([O-])(=O)=O MEFBJEMVZONFCJ-UHFFFAOYSA-N 0.000 description 1
- 235000015097 nutrients Nutrition 0.000 description 1
- 238000001637 plasma atomic emission spectroscopy Methods 0.000 description 1
- 239000002574 poison Substances 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000011002 quantification Methods 0.000 description 1
- 239000012488 sample solution Substances 0.000 description 1
- 238000002798 spectrophotometry method Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
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- 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
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/71—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited
- G01N21/73—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited using plasma burners or torches
-
- 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
- G01N1/38—Diluting, dispersing or mixing samples
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- 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)
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- Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Abstract
The invention relates to a method for detecting the content of phosphorus element in grease by ICP organic sample injection, which comprises the following steps: step 1, setting working conditions of an inductively coupled plasma spectrometer; step 2, preparing a series of phosphorus standard solutions with concentration; step 3, sequentially introducing the phosphorus standard solution obtained in the step 2 into an inductively coupled plasma spectrometer for measurement to obtain a corresponding relation between a spectral line signal value and the concentration of the phosphorus standard solution; step 4, diluting the oil sample to be detected, and then determining to obtain a spectral line signal value of the oil sample to be detected; step 5, obtaining the phosphorus concentration C of the grease sample to be detected according to the corresponding relation obtained in the step 3 and the spectral line signal value of the grease sample to be detected, and calculating by using a formula I to obtain the phosphorus content M in the grease sample to be detected;
Description
Technical Field
The invention belongs to the field of oil analysis and detection, and particularly relates to a method for detecting the content of phosphorus in oil by using an ICP (inductively coupled plasma) organic sample injection technology.
Background
The phospholipid in the oil is a complex organic mixture composed of glycerol, fatty acid, phosphoric acid, amino alcohol and choline or cholamine. Oil seeds contain more phospholipids, and the phospholipids are easily transferred into oil in the oil pressing process, so that the oil which is not refined contains a large amount of phospholipids. Phospholipids are fat-soluble substances and have adverse effects on purification, storage and application of lipids: the water-soluble hydrophilic grease has hydrophilicity, and can increase the moisture of the grease and promote the hydrolysis and rancidity of the grease; the product has emulsifying property, and can generate a large amount of foam during cooking and heating; the fried food is easy to oxidize and becomes black and bitter when being heated, so that the quality of the fried food is influenced; is a catalyst poison in the hydrogenation reaction process, can cause the hydrogenation catalyst to coke in a high-temperature and high-pressure state, and leads the catalyst to be deactivated; but is itself a valuable nutrient and emulsifier and is widely used in the food industry. Therefore, the production process conditions can be determined by measuring the content of the phospholipid, and the method has practical significance for the quality of the oil and the comprehensive utilization.
At present, methods suitable for measuring the content of phosphorus/phospholipid in oil mainly comprise gravimetric methods, turbidity methods, High Pressure Liquid Chromatography (HPLC), ultraviolet spectrophotometry (UV), Fourier transform infrared spectroscopy (FTIR), colorimetric methods, plasma emission spectroscopy (ICP) and other measuring methods.
The gravimetric method and the nephelometric method have the advantages of simple operation, but are not applicable to samples with low phospholipid content, and have large errors, thus the analysis requirements cannot be met.
HPLC, UV, FTIR methods use expensive instruments, the cost of analysis is high, need to be with the actual professional knowledge of the operator to complete.
The most used colorimetric method is the molybdenum blue colorimetric method, and the principle of the method is that a sample and metal oxides are ashed, phosphorus in the sample is changed into phosphate, acid is added to dissolve the phosphate to obtain phosphate radical, phosphomolybdate is generated after the molybdate is added, the phosphomolybdate is reduced to generate molybdenum blue, the color shade of the molybdenum blue is in direct proportion to the content of phospholipid, and therefore colorimetric quantification can be carried out. The method is adopted in the national standard GB/T5537-2008. The obvious disadvantages of this method are that it takes a long time, generally takes more than 20 hours to complete an analysis, and the analysis steps are numerous and need a high level of professional skill to complete.
The ICP method is a method in which a sample is completely decomposed to form excited atoms and ions by using a high temperature generated by argon plasma, and outer layer electrons transit from an excited state to a low energy level due to instability of the excited atoms and ions, and emit characteristic spectral lines. Because the light intensity is in direct proportion to the concentration of the element to be detected, after light is split by a grating and the like, the total phosphorus concentration can be obtained by detecting the intensity of the specific wavelength of the total phosphorus by using a detector. The resolution of ICP is highly required when determining total phosphorus concentration. The method has the advantages that the pretreatment process of the sample is complex, and the digestion process of the sample at the early stage also needs to consume a long time. Equivalent such detection methods are adopted by UOP corporation of america.
Disclosure of Invention
The invention mainly aims to provide a method for detecting the content of phosphorus element in grease by utilizing ICP organic sample injection, which can quickly, simply, safely and accurately detect the content of phosphorus/phospholipid in grease.
In order to achieve the purpose, the invention provides a method for detecting the content of phosphorus element in grease by ICP organic sample injection, which comprises the following steps:
step 1, setting working conditions of an inductively coupled plasma spectrometer;
step 2, preparing a series of phosphorus standard solutions with concentration;
step 3, sequentially introducing the phosphorus standard solution obtained in the step 2 into an inductively coupled plasma spectrometer for measurement to obtain a corresponding relation between a spectral line signal value and the concentration of the phosphorus standard solution;
step 4, diluting the oil sample to be detected, and then introducing the diluted oil sample into an inductively coupled plasma spectrometer for measurement to obtain a spectral line signal value of the oil sample to be detected, wherein a diluent for diluting the oil sample to be detected is one or more of biological aviation kerosene, isooctane and xylene;
step 5, obtaining the phosphorus element concentration C of the grease sample to be detected according to the corresponding relation between the spectral line signal value obtained in the step 3 and the concentration of the phosphorus standard solution and the spectral line signal value of the grease sample to be detected, and calculating by using a formula I to obtain the phosphorus element content M in the grease sample to be detected;
wherein V is the volume of the grease sample to be measured after dilution;
and m is the dosage of the grease sample to be detected.
The invention discloses a method for detecting phosphorus element content in grease by ICP organic sample injection, wherein the concentration of phosphorus standard solution in terms of phosphorus element is 0mg/L, 0.5mg/L, 1mg/L, 10mg/L and 20 mg/L.
The method for detecting the content of the phosphorus element in the grease by utilizing ICP organic sample injection is characterized in that the determination conditions of the phosphorus standard solution in the step 3 are the same as the determination conditions of the grease sample to be detected in the step 4.
The invention relates to a method for detecting the content of phosphorus element in grease by ICP organic sample injection, wherein the corresponding relation between the spectral line signal value and the phosphorus standard solution solubility in the step 3 is a linear regression equation: y ═ ax + b, where y denotes the spectral signal value, x denotes the phosphorus standard solution solubility, a is 1 ± 0.001, and b is 0 ± 0.1.
The invention discloses a method for detecting phosphorus content in grease by ICP organic sample injection, wherein the mass ratio of a grease sample to be detected to a diluent is 1:7-1: 12.
The invention relates to a method for detecting the content of phosphorus element in grease by utilizing ICP organic sample injection, wherein the working conditions of an inductively coupled plasma spectrometer are as follows: the power is 1500W, the plasma is 15L/min, the auxiliary gas is 1.2L/min, the atomizing gas is 0.8L/min, the pump speed is 0.8mL/min, and the phosphorus element determination spectral line is 213.62 nm.
The invention relates to a method for detecting phosphorus element content in grease by utilizing ICP organic sample injection, wherein the determination of phosphorus standard solution in step 3 and the determination of grease sample to be detected in step 4 are carried out at least twice in parallel, and an arithmetic mean value is taken.
The invention discloses a method for detecting phosphorus content in grease by utilizing ICP organic sample injection, wherein a grease sample to be detected is jatropha curcas crude oil, jatropha curcas refined oil, palm oil, waste grease, millennium oil or soybean oil.
The invention relates to a method for detecting phosphorus content in grease by ICP organic sample injection, wherein a diluent for diluting a grease sample to be detected is biological aviation kerosene.
The invention has the beneficial effects that:
1. in the invention, the sample is directly diluted by the organic solvent to replace the processing processes of phospholipid dry ashing, microwave digestion and the like, so that the use of high-temperature and high-pressure conditions in the analysis and detection process is reduced, and the safety of the analysis method is greatly improved.
2. In the invention, the sample is directly diluted by the organic solvent, so that the early sample treatment process in phospholipid determination can be completed within 5 minutes, and compared with the pretreatment time of ashing and the like for at least 5 hours in other analysis methods, the whole analysis and detection time is greatly shortened, and the method is more favorable for guiding production.
3. The invention dilutes the sample by using diluents such as biological aviation kerosene and the like, can well dissolve the sample and accurately determine the phosphorus content in the sample.
4. The accuracy, the precision and the standard adding recovery rate of the measuring result of the invention all meet the requirements, and the requirements of phospholipid detection of production enterprises can be met.
Detailed Description
The following examples illustrate the invention in detail: the present example is carried out on the premise of the technical scheme of the present invention, and detailed embodiments and processes are given, but the scope of the present invention is not limited to the following examples, and the experimental methods without specific conditions noted in the following examples are generally performed according to conventional conditions.
The invention provides a method for detecting the content of phosphorus element in grease by ICP organic sample injection, which comprises the following steps:
step 1, setting working conditions of an inductively coupled plasma spectrometer;
step 2, preparing a series of phosphorus standard solutions with concentration;
step 3, sequentially introducing the phosphorus standard solution obtained in the step 2 into an inductively coupled plasma spectrometer for measurement to obtain a corresponding relation between a spectral line signal value and the concentration of the phosphorus standard solution;
step 4, diluting the oil sample to be detected, and then introducing the diluted oil sample into an inductively coupled plasma spectrometer for measurement to obtain a spectral line signal value of the oil sample to be detected, wherein a diluent for diluting the oil sample to be detected is one or more of biological aviation kerosene, isooctane and xylene;
step 5, obtaining the phosphorus element concentration C of the grease sample to be detected according to the corresponding relation between the spectral line signal value obtained in the step 3 and the concentration of the phosphorus standard solution and the spectral line signal value of the grease sample to be detected, and calculating by using a formula I to obtain the phosphorus element content M in the grease sample to be detected;
wherein V is the volume of the grease sample to be measured after dilution;
and m is the dosage of the grease sample to be detected.
The invention does not specially limit the working conditions of the inductively coupled plasma spectrometer, and the instrument uses the instrument to follow the guidance of the instrument manufacturer as much as possible so as to optimally set the parameters of the instrument for the purpose of obtaining the optimal signal-to-noise ratio. The preferred operating conditions are: the power is 1500W, the plasma is 15L/min, the auxiliary gas is 1.2L/min, the atomizing gas is 0.8L/min, the pump speed is 0.8mL/min, and the phosphorus element determination spectral line is 213.62 nm. Under the condition, the phosphorus standard solution and the grease sample to be detected are measured, so that the stability is high and the accuracy is high.
In step 2 of the present invention, a series of concentrations of phosphorus standard solutions are prepared, wherein the concentrations of the phosphorus standard solutions are, for example, 0mg/L, 0.5mg/L, 1mg/L, 10mg/L and 20mg/L, respectively. The form of phosphorus in the pseudo solution is not particularly limited in the present invention, and may be organic phosphorus or inorganic phosphorus, and organic phosphorus is preferred. The concentration of the standard solution is the concentration in terms of phosphorus element.
And 3, sequentially introducing the phosphorus standard solution obtained in the step 2 into an inductively coupled plasma spectrometer for measurement to obtain a corresponding relation between a spectral line signal value and the concentration of the phosphorus standard solution. That is, spectral line signal values of the phosphorus standard solution at concentrations of 0mg/L, 0.5mg/L, 1mg/L, 10mg/L, and 20mg/L are measured, and the obtained spectral line signal values are in one-to-one correspondence with the concentrations of the phosphorus standard solution, thereby creating a corresponding curve or line of the spectral line signal values and concentrations of the phosphorus standard solution.
Wherein, the corresponding relation between the spectral line signal value and the solubility of the phosphorus standard solution is generally a linear regression equation: y ═ ax + b, where y denotes the spectral signal value, x denotes the phosphorus standard solution solubility, a is 1 ± 0.001, and b is 0 ± 0.1.
In a preferred embodiment, the phosphorus standard solution is measured in parallel for a plurality of times, for example, twice, and the arithmetic mean of the measured values of the plurality of times is taken to further improve the accuracy and reliability of the measurement.
And 4, diluting the oil sample to be measured, and then introducing the diluted oil sample to the inductively coupled plasma spectrometer for measurement to obtain a spectral line signal value of the oil sample to be measured, wherein the diluent for diluting the oil sample to be measured is one or more of biological aviation kerosene, isooctane and xylene.
The diluent used by the invention, especially the biological aviation kerosene, has high intersolubility with the grease sample to be measured, so that the interference of organisms can be reduced to the greatest extent, and the measurement accuracy is higher. The mass ratio of the grease sample to be detected to the diluent is preferably 1:7-1:12, and more preferably 1: 9.
The grease sample to be measured is not particularly limited, and is preferably jatropha curcas crude oil, jatropha curcas refined oil, palm oil, waste grease, millennium tung oil or soybean oil.
The specific steps of the preparation of the grease to be detected are as follows: and (3) taking a grease sample to be detected into a 25mL sample bottle, diluting with a diluent, and shaking up for later use.
The measuring conditions of the grease sample to be measured in the invention are the same as those of the phosphorus standard solution as much as possible, so that the comparability of data can be ensured, and the accuracy and the reliability of the measuring result can be further ensured. The measurement result is preferably accurate to 0.1. mu.g/g.
And 5, obtaining the phosphorus element concentration C of the grease sample to be detected according to the corresponding relation between the spectral line signal value obtained in the step 3 and the concentration of the phosphorus standard solution and the spectral line signal value of the grease sample to be detected, and calculating by using a formula I to obtain the phosphorus element content M in the grease sample to be detected.
The invention can accurately measure the phosphorus content of the sample to be measured under the condition of not adding an internal standard because the diluent has better intersolubility with the sample to be measured, and is suitable for preliminary measurement of the phosphorus content of an oil product.
The specific operation of the invention can be referred to as follows:
1) the working conditions of the adjusting instrument are 1500W of power, 15L/min of plasma, 1.2L/min of auxiliary gas, 0.8L/min of atomizing gas, 0.8mL/min of pump speed and 213.62nm of phosphorus element determination spectral line.
2) Respectively weighing 200mg/L standard solutions of 0mL, 0.125mL, 0.25mL, 2.5mL and 5mL into 5 volumetric flasks of 50mL, respectively weighing 10g of base oil into 5 volumetric flasks, diluting the base oil to a scale mark by using diluents such as biological aviation kerosene and the like, shaking up, and calculating the mass concentration of each standard solution.
3) And (4) sequentially introducing the blank solution and the standard solution into an instrument for analysis, and making a corresponding standard curve.
4) 2.5g (to the nearest 0.001g) of the sample was weighed into a 25mL sample bottle, diluted 10-fold with bio-aviation kerosene and shaken up, and the sample solution was introduced into the instrument for analysis as described in 3.
(5) The phosphorus content in the sample is calculated according to the following formula I:
in the formula:
m-the content of phosphorus element in the grease sample to be detected;
v-volume of the grease sample to be measured after dilution, unit: milliliters (mL);
m-amount of grease sample to be measured, unit: grams (g);
c-concentration of phosphorus element in the grease sample to be measured by the instrument, unit: microgram/mL (μ g/mL);
the final result of the phosphorus element of the grease sample to be measured by the instrument is expressed by the arithmetic mean value of a plurality of parallel results, and the accuracy is 0.1 mu g/g.
1. In the invention, the sample is directly diluted by the organic solvent to replace the processing processes of phospholipid dry ashing, microwave digestion and the like, so that the use of high-temperature and high-pressure conditions in the analysis and detection process is reduced, and the safety of the analysis method is greatly improved.
2. In the invention, the sample is directly diluted by the organic solvent, so that the early sample treatment process in phospholipid determination can be completed within 5 minutes, and compared with the pretreatment time of ashing and the like for at least 5 hours in other analysis methods, the whole analysis and detection time is greatly shortened, and the method is more favorable for guiding production.
3. The accuracy, the precision and the standard adding recovery rate of the measuring result of the invention all meet the requirements, and the requirements of phospholipid detection of production enterprises can be met.
The technical solution of the present invention will be further measured by the following specific examples.
Example 1
Accuracy test-comparing Jatropha curcas crude oil with GB/T5537-2008
Weighing 2.5g (accurate to 0.001g) of 5 different jatropha curcas crude oil samples into 25mL sample bottles, diluting 10 times with biological aviation kerosene and shaking up. 5 samples are respectively measured in ICP with a standard curve, and are compared and analyzed with the measurement result of a national standard method, the deviation values are less than 5%, and the average value is 2.27%. The specific results are shown in the following table 1:
TABLE 1 Jatropha curcas crude oil accuracy test results
Example 2
Accuracy test-comparing refined Jatropha curcas oil with GB/T5537-2008
Weighing 2.5g (accurate to 0.001g) of 5 different jatropha curcas refined oil samples into 25mL sample bottles, diluting 10 times with biological aviation kerosene and shaking up. 5 samples are respectively measured in ICP with a standard curve, and are compared and analyzed with the measurement result of a national standard method, the deviation values are less than 5%, and the average value is 3.33%, so that the method has good accuracy adaptability to refined jatropha curcas oil and meets the measurement requirement. The specific results are shown in the following table 2:
TABLE 2 accuracy test results for refined Jatropha curcas oil
Example 3
Accuracy test-palm oil vs. GB/T5537-2008
2.5g (to the nearest 0.001g) of 5 different palm oil samples were weighed into 25mL sample bottles, diluted 10-fold with bio-aviation kerosene and shaken up. 5 samples are respectively measured in ICP with a standard curve, and are compared and analyzed with the measurement result of the national standard method, the deviation values are less than 5%, and the average value is 4.16%, so that the method has good accuracy adaptability to palm oil and meets the measurement requirement. The specific results are shown in the following table 3:
TABLE 3 palm oil accuracy test results
Example 4
Accuracy test-waste grease and GB/T5537-2008 contrast
2.5g (to the nearest 0.001g) of 5 different waste oil samples were weighed into 25mL sample bottles, diluted 10-fold with bio-aviation kerosene and shaken up. 5 samples are respectively measured in ICP with a standard curve, and are compared and analyzed with measurement results of a national standard method, the deviation values are less than 5%, and the average value is 4.22%. The specific results are shown in the following table 4:
TABLE 4 accuracy test results for waste oils and fats
Example 5
Accuracy test-comparison of millennium tung oil with GB/T5537-2008
Weighing 2.5g (to the nearest 0.001g) of 5 different millennia oil samples into 25mL sample bottles, diluting 10 times with biological aviation kerosene and shaking up. 5 samples are respectively measured in ICP with a standard curve, and are compared and analyzed with the measurement result of a national standard method, the deviation values are less than 5%, and the average value is 3.57%. The specific results are shown in the following table 5:
TABLE 5 accuracy test results for millennium tung oil
Example 6
Accuracy test-Soybean oil vs. GB/T5537-2008
Weighing 2.5g (to the nearest 0.001g) of 5 different millennia oil samples into 25mL sample bottles, diluting 10 times with biological aviation kerosene and shaking up. 5 samples are respectively measured in ICP with a standard curve, and are compared and analyzed with the measurement result of a national standard method, the deviation values are less than 5%, and the average value is 2.17%, so that the method has good accuracy adaptability to soybean oil and meets the measurement requirement. The specific results are shown in the following table 6:
TABLE 6 Soybean oil accuracy test results
Example 7
Precision test-Jatropha curcas crude oil
A sample of 1 Jatropha curcas oil 5.0g (to the nearest 0.001g) was weighed into a 50mL sample bottle, diluted 10-fold with bio-aviation kerosene and shaken up. The detection is continuously carried out for 5 times in ICP with a standard curve, and the RSD value is 0.86%, which shows that the method has good accuracy adaptability to the jatropha curcas crude oil and meets the measurement requirement. The specific results are shown in the following table 7:
TABLE 7 precision test results for Jatropha curcas crude oil
Example 8
Precision test-refined Jatropha curcas oil
Weighing 1 jatropha curcas refined oil sample 5.0g (accurate to 0.001g) into a 50mL sample bottle, diluting 10 times with biological aviation kerosene, and shaking up. The method is continuously detected for 5 times in ICP with a standard curve, and the RSD value is 1.61%, which shows that the method has good precision adaptability to the refined jatropha curcas oil and meets the measurement requirement. The specific results are shown in the following table 8:
TABLE 8 precision test results for refined Jatropha curcas oil
Example 9
Precision test-palm oil
Weigh 1 sample of palm oil 5.0g (to the nearest 0.001g) into a 50mL sample bottle, dilute 10-fold with bio-aviation kerosene and shake well. Continuously detecting for 5 times in ICP with a standard curve, wherein the RSD value is 2.65%, which shows that the method has good accuracy adaptability to palm oil and meets the measurement requirement. The specific results are shown in the following table 9:
TABLE 9 palm oil accuracy test results
Example 10
Precision test-waste oil
Weigh 1 sample of waste oil 5.0g (to the nearest 0.001g) into a 50mL sample bottle, dilute 10 times with bio-aviation kerosene and shake well. The detection is continuously carried out for 5 times in ICP with a standard curve, and the RSD value is 4.56%, which shows that the method has good precision adaptability to waste grease and meets the measurement requirement. The specific results are shown in the following table 10:
TABLE 10 precision test results for waste oils and fats
Example 11
Precision test-millennium tung oil
Weigh 1 millennium tung oil sample 5.0g (to the nearest 0.001g) into a 50mL sample bottle, dilute 10 times with biological aviation kerosene and shake well. The method is continuously detected for 5 times in ICP with a standard curve, and the RSD value is 2.07 percent, which shows that the method has good precision adaptability to the millennium tung oil and meets the measurement requirement. The specific results are shown in the following table 11:
TABLE 11 precision test results of Kalopanax pictus oil
Example 12
Precision test-Soybean oil
Weigh 1 soybean oil sample 5.0g (to the nearest 0.001g) into a 50mL sample bottle, dilute 10-fold with bio-aviation kerosene and shake well. The detection is continuously carried out for 5 times in ICP with a standard curve, and the RSD value is 2.42 percent, which shows that the method has good accuracy adaptability to soybean oil and meets the measurement requirement. The specific results are shown in table 12 below:
TABLE 12 detection results of soybean oil accuracy
Example 13
Spiked recovery test
Weighing 2.5g (accurate to 0.001g) of Jatropha curcas crude oil, refined Jatropha curcas oil, palm oil, waste oil, millennium oil and soybean oil samples into 6 25mL sample bottles respectively, diluting by 10 times with biological aviation kerosene, shaking uniformly, adding standard solutions into 6 samples respectively, and measuring 6 samples respectively. The calculation result shows that the recovery rate of each sample is 95-105%, and the standard recovery rate meets the requirement of GB/T27404-. The specific results are shown in the following table 13:
TABLE 13 results of recovery measurements of each oil sample with a standard
In conclusion, the determination method is simple and easy to operate, is suitable for determining the preliminary phosphorus content of the grease, has the determination result accuracy, the accuracy and the standard addition recovery rate meeting the requirements, and can meet the requirement of phospholipid detection of production enterprises.
The present invention is capable of other embodiments, and various changes and modifications may be made by one skilled in the art without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (9)
1. A method for detecting the content of phosphorus element in grease by utilizing ICP organic sample injection is characterized by comprising the following steps:
step 1, setting working conditions of an inductively coupled plasma spectrometer;
step 2, preparing a series of phosphorus standard solutions with concentration;
step 3, sequentially introducing the phosphorus standard solution obtained in the step 2 into an inductively coupled plasma spectrometer for measurement to obtain a corresponding relation between a spectral line signal value and the concentration of the phosphorus standard solution;
step 4, diluting the oil sample to be detected, and then introducing the diluted oil sample into an inductively coupled plasma spectrometer for measurement to obtain a spectral line signal value of the oil sample to be detected, wherein a diluent for diluting the oil sample to be detected is one or more of biological aviation kerosene, isooctane and xylene;
step 5, obtaining the phosphorus element concentration C of the grease sample to be detected according to the corresponding relation between the spectral line signal value obtained in the step 3 and the concentration of the phosphorus standard solution and the spectral line signal value of the grease sample to be detected, and calculating by using a formula I to obtain the phosphorus element content M in the grease sample to be detected;
wherein V is the volume of the grease sample to be measured after dilution;
and m is the dosage of the grease sample to be detected.
2. The method for detecting the content of phosphorus element in grease by utilizing ICP organic sampling according to claim 1, wherein the concentration of the phosphorus standard solution in terms of phosphorus element is 0mg/L, 0.5mg/L, 1mg/L, 10mg/L and 20 mg/L.
3. The method for detecting the content of the phosphorus element in the grease by utilizing ICP organic sampling according to claim 1, wherein the determination conditions of the phosphorus standard solution in the step 3 are the same as the determination conditions of the grease sample to be detected in the step 4.
4. The method for detecting the content of the phosphorus element in the grease by utilizing ICP organic sampling according to claim 1, wherein the corresponding relation between the spectral line signal value and the solubility of the phosphorus standard solution in the step 3 is a linear regression equation: y ═ ax + b, where y denotes the spectral signal value, x denotes the phosphorus standard solution solubility, a is 1 ± 0.001, and b is 0 ± 0.1.
5. The method for detecting the content of the phosphorus element in the grease by utilizing ICP organic sampling according to claim 1, wherein the mass ratio of the grease sample to be detected to the diluent is 1:7-1: 12.
6. The method for detecting the content of phosphorus in grease by utilizing ICP organic sampling according to claim 1, wherein the working conditions of an inductively coupled plasma spectrometer are as follows: the power is 1500W, the plasma is 15L/min, the auxiliary gas is 1.2L/min, the atomizing gas is 0.8L/min, the pump speed is 0.8mL/min, and the phosphorus element determination spectral line is 213.62 nm.
7. The method for detecting the content of the phosphorus element in the grease by utilizing ICP organic sampling according to claim 1, wherein the determination of the phosphorus standard solution in the step 3 and the determination of the grease sample to be detected in the step 4 are performed at least twice in parallel, and an arithmetic mean value is taken.
8. The method for detecting the content of phosphorus in grease by utilizing ICP organic sample injection according to claim 1, wherein the grease sample to be detected is jatropha curcas crude oil, jatropha curcas refined oil, palm oil, waste grease, millennia oil or soybean oil.
9. The method for detecting the content of the phosphorus element in the grease by utilizing ICP organic sampling according to claim 1, wherein a diluent for diluting the grease sample to be detected is biological aviation kerosene.
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