CN109342645A - A method of measurement heavy bio oil moisture content - Google Patents
A method of measurement heavy bio oil moisture content Download PDFInfo
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- CN109342645A CN109342645A CN201811245576.9A CN201811245576A CN109342645A CN 109342645 A CN109342645 A CN 109342645A CN 201811245576 A CN201811245576 A CN 201811245576A CN 109342645 A CN109342645 A CN 109342645A
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- 238000005259 measurement Methods 0.000 title claims abstract description 34
- 238000000034 method Methods 0.000 title claims abstract description 34
- 239000012075 bio-oil Substances 0.000 title claims abstract description 32
- 239000002904 solvent Substances 0.000 claims abstract description 28
- 239000003921 oil Substances 0.000 claims abstract description 23
- 239000000203 mixture Substances 0.000 claims abstract description 18
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
- 238000012937 correction Methods 0.000 claims description 14
- 102000016550 Complement Factor H Human genes 0.000 claims description 3
- 108010053085 Complement Factor H Proteins 0.000 claims description 3
- 238000004364 calculation method Methods 0.000 claims description 3
- 239000003960 organic solvent Substances 0.000 claims 1
- 235000019441 ethanol Nutrition 0.000 abstract description 7
- 230000008569 process Effects 0.000 abstract description 7
- 230000008901 benefit Effects 0.000 abstract description 3
- 239000000463 material Substances 0.000 abstract description 2
- 238000007781 pre-processing Methods 0.000 abstract description 2
- 238000005303 weighing Methods 0.000 abstract 1
- 235000019198 oils Nutrition 0.000 description 17
- 238000001514 detection method Methods 0.000 description 9
- 238000005516 engineering process Methods 0.000 description 6
- 235000019498 Walnut oil Nutrition 0.000 description 5
- 239000000839 emulsion Substances 0.000 description 5
- 239000008170 walnut oil Substances 0.000 description 5
- 241000758789 Juglans Species 0.000 description 4
- 235000009496 Juglans regia Nutrition 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 4
- 235000020234 walnut Nutrition 0.000 description 4
- 239000010779 crude oil Substances 0.000 description 3
- 238000013332 literature search Methods 0.000 description 3
- 238000004566 IR spectroscopy Methods 0.000 description 2
- 238000013475 authorization Methods 0.000 description 2
- 239000004519 grease Substances 0.000 description 2
- 239000002023 wood Substances 0.000 description 2
- 239000002028 Biomass Substances 0.000 description 1
- 238000005481 NMR spectroscopy Methods 0.000 description 1
- 206010044565 Tremor Diseases 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000012417 linear regression Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000005311 nuclear magnetism Effects 0.000 description 1
- 238000011017 operating method Methods 0.000 description 1
- 238000000643 oven drying Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000001373 regressive effect Effects 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 230000009466 transformation Effects 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
- G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
- G01N31/16—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using titration
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- Biochemistry (AREA)
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- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The present invention provides a kind of methods for measuring heavy bio oil moisture content.This method comprises the following steps: (1) using karl Fischer moisture teller, measure the moisture content of solvent (such as ethyl alcohol or methanol);(2) the heavy bio oil for weighing certain mass, then mixes with solvent by a certain percentage, forms the mixture of stable homogeneous;(3) using the moisture content of karl Fischer moisture teller measurement mixture;(4) moisture content of heavy biology oil samples is calculated.Advantages of the present invention is that the characteristics such as unstable, sticky for overcoming sample are directly measured by a step preprocessing process.Experimental implementation is simple, as a result accurate reliable, has application and reference value in terms of sticky unstable material measurement of water-content coefficient.
Description
Technical field
The present invention provides a kind of methods for measuring heavy bio oil moisture content, belong to detection method field.
Background technique
Moisture content is an important characteristic of bio oil, and it is other special to influence viscosity, calorific value, solid content of bio oil etc.
Property, under normal circumstances, the moisture content of bio oil is lower, and the quality of bio oil is better.The moisture content of bio oil is measured frequently with card
Er Feixiu moisture teller, but the large viscosity of heavy bio oil, directly use karl Fischer analyzer, it is difficult to be precisely weighed and
Sample-adding.The present invention is a kind of method for measuring heavy bio oil moisture content, is diluted using solvent, is sticky biomass processes
Then the mixture of stable homogeneous is measured using karl Fischer moisture teller, measuring method is easy, as a result accurately, solution
Sticky Unstable Sample of having determined can not correct amount and sample-adding problem.
Literature search discovery by the prior art, Chinese patent Authorization Notice No. are as follows: CN106970005A, title are as follows:
Crude oil water content measuring method.The readme of the patent are as follows: the embodiment of the present invention provides a kind of crude oil water content measuring method, packet
Include: sample is stood the predetermined time so that grease is sufficiently separated by step 1, to form the oil emulsion at top and the free water of bottom,
Wherein the oil emulsion is the mixture of crude oil and emulsified water;Step 2, the density p for obtaining sampleLWith volume VL, obtain free water
Density pWWith volume VW, obtain the density p of oil emulsionEMOWith volume VEMO;Obtain scene temperature;Step 3, according in laboratory
The density p of the moisture content of the oil emulsion measured, sampleLWith volume VL, the density p of free waterWWith volume VW, oil emulsion it is close
Spend ρEMOWith volume VEMO, take scene temperature, calculate the overall moisture content of sample.This technology is disadvantageous in that: experiment consumption
When it is longer, need the standing of sample and the time of layering, step is relatively complicated, needs repeatedly to measure density, volume and temperature, more
Secondary measurement and calculating increase experimental error.The present invention only needs the pre-treatment step of primary sample, just by one-shot measurement
It can obtain the moisture content of sample.
Literature search discovery by the prior art, Chinese patent Authorization Notice No. are as follows: CN201410634685.5, title
Are as follows: the moisture content detection method based on Subtractive Infrared Spectroscopy.The readme of the patent are as follows: the invention discloses one kind based on red
The moisture content detection method of outer difference spectrum technology chooses the balance sample that absolutely dry sample and different relative humidity is made in timber to be measured
Product;The infrared spectrogram I of absolutely dry sample is measured using infrared spectrometer0With the infrared spectrogram I of balance sampleW;Use balance sample
Infrared spectrogram IWSubtract the infrared spectrogram I of absolutely dry sample0, obtain Infrared Difference spectrogram IW-0;It acquires in Infrared Difference spectrogram
2900-3750cm-1Area A in rangeW-0;The moisture content W of different relative humidity wood samples is measured using traditional oven drying method;
By the moisture content W and area A of each sampleW-0Contained using least square method linear regression building Subtractive Infrared Spectroscopy detection timber
The model of water rate.The model can be used for the batch measurement of wood sample to be measured, and each sample time-consuming 1s substantially reduces timber and contains
The detection time of water rate.The present invention has the advantages that the period is short, detection is quick, sample requirement is micro or even trace, is a kind of nothing
Detection technique is damaged, can be applied to timber evaluation field.This technology is disadvantageous in that: needing repeatedly measurement building aqueous
The model of rate, then could be according to the moisture content of model determination sample.It is complex to construct model step, and model is not general
It needs to rebuild model when replacing sample type all over applicability.
Literature search discovery by the prior art, Chinese Patent Application No. are as follows: CN201410775532.2, title are as follows:
A kind of measuring method of walnut oil-containing moisture content.The readme of the patent are as follows: the present invention provides a kind of low-field nuclear magnetic resonance technologies
The method for measuring walnut oil-containing moisture content.Its operating procedure specifically includes that 1. preparation samples and weighs;2. total using low field nuclear-magnetism
Vibration technology quickly measures the relaxation signals of sample;3. measuring sample moisture content;4. extracting the grease and measurement sample oil-containing of sample
Rate;5. analysis and processing data.The value of the oil-containing moisture content of the transverse relaxation data of walnut sample and practical measurement is tied jointly
It closes partial least-squares regressive analysis method to be analyzed, obtains the regression equation of walnut oil-containing moisture content, establish the survey of oil-containing moisture content
Try database;Quality Detection is carried out to unknown walnut sample using the database of foundation, realizes the fast of walnut oil-containing moisture content
Speed prediction.Operation of the present invention is easy, works well, and the quick detection of prediction walnut oil-containing moisture content may be implemented, and is applicable in walnut
Quality preferred area, for walnut quality detect work lay the foundation.This technology is disadvantageous in that: needing early period to establish
Water cut test database needs mathematical analysis process, operates relatively complicated time-consuming, and database is just for single kind
Sample lacks applicability.
Summary of the invention
Exist when it is an object of the invention to solve the problems, such as the sticky unstable material measurement of water-content coefficient such as heavy bio oil,
And provide a kind of method for measuring heavy bio oil moisture content.
Technical scheme is as follows
A method of measurement heavy bio oil moisture content, it includes the following steps:
(1) determination of moisture instrument is used, the moisture content W of solvent is measured1;
(2) heavy biology oil samples to be measured are taken, are then mixed with solvent, uniform mixture is formed;
(3) using the moisture content W of determination of moisture instrument measurement mixture2;
(4) the moisture content W of heavy biology oil samples is calculated3, calculation formula is as follows:
W3=[(1+M) W2-MW1]×H
Wherein: H is the measurement result correction factor of the determination of moisture instrument, and M is heavy bio oil sample and solvent
Mixing mass ratio.
Further, the determination of moisture instrument uses karl Fischer moisture teller, has reproducibility good, accuracy
High advantage can accurately measure the moisture content in sample.
Further, the correction factor determines that method is as follows, utilizes the moisture content of determination of moisture instrument measurement pure water
For W4, then correction factor H is 1/W4。
Further, the solvent be ethyl alcohol, methanol or other can be with miscible organic molten of biological oil samples to be measured
Agent.
Further, it need to determine the mixed proportion of suitable biological oil samples and solvent according to bio oil sample characteristics of for example, increase
Sample-adding product mobility and stability, are convenient for measuring, and generally mix with ratio between 1-20.
Further, the W1、W2、W3、W4It is required to be measured in parallel repeatedly, to reduce error.
The method that the present invention designs can overcome the characteristics such as unstable, sticky of sample, by a step preprocessing process, directly
It connects and measures, it is easy to operate, mathematical analysis and the modeling knowledge of profession are not needed, and result is accurately reliable, in sticky shakiness
There is application and reference value in terms of earnest matter measurement of water-content coefficient.
Specific embodiment
The method that heavy bio oil moisture content is measured designed by the present invention, core is by complicated, unstable, sticky
Sample is handled by solvent, forms the mixture of stable homogeneous, conveniently measures the moisture content of heavy bio oil.It is specific
Steps are as follows:
(1) karl Fischer moisture teller is used, (such as ethyl alcohol, methanol can be uniform with heavy bio oil for measurement solvent
Mixed reagent) moisture content W1;
(2) certain mass heavy biology oil samples to be measured are weighed, is then mixed with solvent, forms uniform mixture;
Mixed proportion is bio oil: solvent=1:M (M=1,2,3 ..., 20);
(3) using the moisture content W of karl Fischer moisture teller measurement mixture2;
(4) the moisture content W of heavy biology oil samples is calculated3, calculation formula is as follows:
W3=[(1+M) W2-MW1] × H formula (1)
Wherein: H is the measurement result correction factor of karl Fischer moisture teller, and M is heavy bio oil sample and solvent
Mixing mass ratio.
In practical measurement process, in order to reduce measurement error, W1、W2、W3、W4It can be measured in parallel repeatedly.
Before said determination process starts, need to calibrate karl Fischer moisture teller, the method is as follows: measure first pure
The moisture content of water, theoretically the moisture content of pure water is 100%, but the numerical value of practical measurement has certain deviation, therefore needs
Correction factor is determined first.Correction factor determines that method is as follows, and the moisture content using determination of moisture instrument measurement pure water is W4,
Then correction factor H is 1/W4.Certainly, in the calculating process of above-mentioned formula (1), W1、W2It can be modified to obtain with correction factor in advance
Revised moisture content W5And W6, then calculated again with revised coefficient:
W3=(1+M) W6-MW5Formula (2)
Wherein W5For the moisture content of solvent after amendment, W is equal in quantity1×H;W6For solvent after amendment and bio oil mixing
The moisture content of liquid is equal to W in quantity2×H。
Present invention is further elaborated in following combination specific embodiment and explanation.
Embodiment one:
1. utilizing karl Fischer tester for water ratio, the moisture content of pure water is measured.Measurement three times, be respectively as follows: 104.4%,
106.67%, 105.57%, being averaged is 105.55%, and obtaining correction factor (H) is 1/105.55%=0.95.
2. using industrial alcohol as solvent, the moisture content of solvent is measured.Measurement is respectively as follows: 6.13% three times, 7.13%,
7.11%, it is averaged (W1) it is 6.79%.
3. using beaker, heavy bio oil 2.7604g is weighed, 2.7592g alcohol is then weighed, mass ratio is about 1:1, then
Mixed proportion (M) is 1.It is thoroughly mixed, forms the mixture of stable homogeneous.
4. utilizing karl Fischer tester for water ratio, the moisture content of mixture is measured.Three times, moisture content is respectively as follows: for measurement
9.66%, 9.44%, 10.17%, it is averaged (W2) it is 9.76%.
5. moisture content (the W of heavy biology oil samples is calculated by formula (1)3) are as follows: 12.09%.
Embodiment two:
1. using the correction factor (H) of embodiment one for 0.95.
2. using the identical solvent of embodiment one, the moisture content (W of solvent1) it is 6.79%, the moisture content of solvent after amendment
(W5) it is 6.45%.
3. using beaker, heavy bio oil 2.8339g being weighed, 28.7476g alcohol is then weighed, mass ratio is about 1:10,
Then mixed proportion (M) is 10.It is thoroughly mixed, is formed with stable mixture.
4. utilizing karl Fischer moisture content, analyzer measures the moisture content of mixture.It measures three times, moisture content (W2) are as follows:
7.16%, 7.20%, 7.21%, moisture content (W after amendment6) are as follows: 6.80%, 6.84%, 6.85%.
5. moisture content (the W of heavy biology oil samples is calculated by formula (2)3) are as follows: 10.63 ± 0.23%.
Embodiment three:
1. using the correction factor (H) of embodiment one for 0.95.
2. using the identical solvent of embodiment one, the moisture content (W of solvent1) it is 6.79%, the moisture content of solvent after amendment
(W5) it is 6.45%.
3. using beaker, heavy bio oil 2.8374g is weighed, 57.4074g alcohol is then weighed, mixed proportion is about 1:
20, then mixed proportion (M) is 20.It is thoroughly mixed, is formed with stable mixture.
4. being measured three times, moisture content (W using the moisture content of karl Fischer tester for water ratio measurement mixture2) respectively
Are as follows: 6.99%, 7.02%, 6.96%, moisture content (W after amendment6) are as follows: 6.64%, 6.67%, 6.61%.
5. moisture content (the W of heavy biology oil samples is calculated by formula (2)3) are as follows: 10.45 ± 0.49%.
Above-mentioned embodiment is only a preferred solution of the present invention, so it is not intended to limiting the invention.Have
The those of ordinary skill for closing technical field can also make various changes without departing from the spirit and scope of the present invention
Change and modification.Therefore all mode technical solutions obtained for taking equivalent substitution or equivalent transformation, all fall within guarantor of the invention
It protects in range.
Claims (5)
1. a kind of method for measuring heavy bio oil moisture content, which comprises the steps of:
(1) determination of moisture instrument is used, the moisture content W of solvent is measured1;
(2) heavy biology oil samples to be measured are taken, are then mixed with solvent, uniform mixture is formed;
(3) using the moisture content W of determination of moisture instrument measurement mixture2;
(4) the moisture content W of heavy biology oil samples is calculated3, calculation formula is as follows:
W3=[(1+M) W2-MW1]×H
Wherein: H is the measurement result correction factor of the determination of moisture instrument, and M is the mixing of heavy bio oil sample and solvent
Mass ratio.
2. the method for measurement heavy bio oil moisture content as described in claim 1, which is characterized in that the moisture teller
Device uses karl Fischer moisture teller.
3. the method for measurement heavy bio oil moisture content as described in claim 1, which is characterized in that the correction factor is true
Determine that method is as follows, the moisture content using determination of moisture instrument measurement pure water is W4, then correction factor H is 1/W4。
4. the method for measurement heavy bio oil moisture content as described in claim 1, which is characterized in that the solvent is second
Alcohol, methanol or other can be miscible with biological oil samples to be measured organic solvent.
5. the method for measurement heavy bio oil moisture content as described in claim 1, which is characterized in that special according to biological oil samples
Property, it determines the mixing mass ratio of suitable biological oil samples and solvent, generally mixes with mass ratio M between 1-20.
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Cited By (1)
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CN113970500A (en) * | 2021-10-27 | 2022-01-25 | 北京新风航天装备有限公司 | Method for rapidly measuring oil content of oil stain solid waste |
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