CN108195970B - The detection method of australene content in a kind of alkaline pulping black liquor - Google Patents
The detection method of australene content in a kind of alkaline pulping black liquor Download PDFInfo
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- CN108195970B CN108195970B CN201810111756.1A CN201810111756A CN108195970B CN 108195970 B CN108195970 B CN 108195970B CN 201810111756 A CN201810111756 A CN 201810111756A CN 108195970 B CN108195970 B CN 108195970B
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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Abstract
The present invention relates to detection technique field, a kind of detection method of australene content in alkaline pulping black liquor is disclosed.This method uses ethyl alcohol or methanol to pre-process sample to be tested first, prevent other black liquor components to the australene influence that distribution coefficient generates in liquid phase, then the sample to be tested bottle of testing sample solution is prepared, the air in pyrogallol solution removing sample bottle is added simultaneously, sealing, which is placed in automatic headspace sample injector, to be balanced, then it uses and is detected in the gas chromatograph equipped with flame ionization detector, the equilibrium condition of head-space sampler are as follows: 50 ~ 90 DEG C of furnace temperature, equilibration time is 15 ~ 60min, and it is calculated by standard curve and obtains testing result.The detectable concentration range of the present invention includes 0.4 ~ 1000mg/L, and for relative standard deviation less than 5%, concentration range is wide, and detection method is simple, and the accuracy of testing result is high.
Description
Technical field
The present invention relates to detection technique fields, more particularly in a kind of alkaline pulping black liquor australene content inspection
Survey method.
Background technique
During soda pulping process, in certain temperature and time range, alkali can by extracts most in wood chip, lignin and
Hemicellulose is dissolved in lye, and since lignin shows black liquor after chemical processing, the liquid being discharged after slurrying is black, that is, is referred to as
Black liquor.Contain a certain amount of grease in softwood wood chip (the especially wood chip of pine class) black liquor caused by pulping and digesting
Matter, referred to as crude turpentine.Currently, 1 ton of pine class wood chip about can produce the crude turpentine of 1kg after alkaline cooking, China
Crude turpentine yield is about at 80000 tons/year.Terpenoid substance and organic sulfur compound are mainly contained in crude turpentine；And terpenes
Substance is mainly the monoterpene based on australene.After removing organic sulfur compound and other impurity, australene can be used for closing
At high value added products such as spice additive, borneol, terpenic oil, terpene resin or gasoline additives, before there is extensive market
Scape.
China is pulping and paper-making big country, and the yield of produced crude turpentine occupies first five position of the world.Due to different factory's alkaline process
Chip raw material used in slurrying and process conditions are different, and the ingredient of produced crude turpentine is also complex changeable, except thick pine
Fuel-economizing purifying and refining techniques more lack outer, and the quantitative detecting method of australene also rarely has exploitation, cause to crude turpentine into
The value of row purifying and refining is also difficult to evaluate, and part crude turpentine then enters the alkali collection workshop section of calcining with black liquor, sternly
The high-valued conversion for affecting China's crude turpentine product again, causes the serious wasting of resources.
Currently, the detection method of australene has not been reported substantially in the included crude turpentine of black liquor.Although part researcher
Using gas chromatography measurement seed oil, (Xue Yizhe, Lu Shaorong, Wei Xiying gas chromatography measure Forsythia Suspensa Seeds oil nanometer
The Asia-Pacific nopinene determination study [J] traditional medicine, 2017,13 (6): 38-40. in cream) and and Brazilian orange oil (Liu Bing,
Chen Lizhou, Liu Huachen wait GC-MS combination retention index to analyze volatile component [J] food industry in Brazilian orange oil,
2017 (7): 309-311.) etc. the content of australene in samples, but contain high concentration alkali and lignin macromolecule in black liquor, directly
Heavy corrosion and blocking can be generated to instrument by carrying out gas chromatographic detection, lead to instrument damage.
The present invention is removed in sample bottle using the solubility of ethyl alcohol or methanol solution raising firpene, pyrogallol as a result,
Oxygen aoxidizes influence to measurement result to avoid firpene, head-space sampler avoids firpene volatilization in pre-treatment sample to reach
Harm of the alkali to gas-chromatography, the comprehensive top for proposing australene content in a kind of alkaline pulping black liquor based on sample pre-treatments
Sky-gas-chromatography detection method, to the content of australene in accurate quantitative analysis crude turpentine, be crude turpentine efficiency refining high and
High-valued conversion provides theoretical foundation.
Summary of the invention
The technical problem to be solved in the present invention is that overcome drawbacks described above, australene in a kind of alkaline pulping black liquor is provided and is contained
The detection method of amount.
The invention is realized by the following technical scheme:
The detection method of australene content in a kind of alkaline pulping black liquor, comprising the following steps:
S1. sample pretreatment: alkaline pulping black liquor is shaken up and removes the bubble in sample to be tested, by what is be uniformly mixed
Black liquor is added in ethyl alcohol or methanol solution, obtains the testing sample solution methanol that ethyl alcohol or methanol concentration are 5 ~ 45%；
S2. the preparation of sample: volume V is taken1Step S1 preparation testing sample solution, be added in ml headspace bottle, then
The oxygen in ml headspace bottle is removed, and seals and obtains sample to be tested bottle, the volume V1For 0.5 ~ 15mL；
S3. the balance and detection of sample: sample to be tested bottle obtained by step S2 is placed in automatic headspace sample injector carry out it is flat
Weighing apparatus records the α-of ml headspace bottle to be measured then using being detected in the gas chromatograph equipped with flame ionization detector respectively
Firpene gas-chromatography signal value A1；
Wherein, the equilibrium condition of head-space sampler are as follows: 50 ~ 90 DEG C of furnace temperature, equilibration time are 15 ~ 60min；
S4. it the foundation of standard curve: according to proportion of ethanol described in step S1, is prepared using australene ethanol solution
Know that the australene standard solution of concentration, australene are added quality and are denoted as m, sample to be tested bottle will be prepared according to step S2, and use
Condition described in step S3 detects its signal value A, using linear fit establish shaped likeCalibration curve equation, wherein
M-μ g, a-μ g-1, b-dimensionless；
S5. in sample australene content calculating: according to the australene signal value of the resulting black liquor sample to be tested of step S3
A1And calibration curve equation obtained by step S4, the content of australene in sample to be tested is calculated using following formula, wherein X is single
The volume fraction of black liquor in the volume testing sample solution of position,
Wherein, C-μ g/mL.
Since solubility is not high in water for firpene, present invention firstly provides first need to surpass to sample to be tested in sample pretreatment
On the other hand the means such as sound play the role of mixing on the one hand for removing the bubble in sample.The sample only mixed,
Sampling is dissolved in the sampling process of ethyl alcohol or methanol that sample is just uniform, and just to representativeness, this also just further ensures that testing result
Accuracy.
Preferably, use 1 ~ 3min of ultrasound to remove the bubble in sample to be tested in step S1；By uniformly mixed black liquor
It is added in ethyl alcohol or methanol solution.
Preferably, it is used in step S2 and pyrogallol is added into container to remove the oxygen in ml headspace bottle；It is described to be measured
The concentration of pyrogallol is 10 ~ 100g/L in sample solution.
Preferably, the concentration of ethyl alcohol or methanol is 30 ~ 45% in the testing sample solution.
Preferably, in step S3 head-space sampler other operating conditions are as follows: assist gas pressure 1.5 ~ 5bar of power, nebulizer gas pressure
10 ~ 20psi, quantitative loop 0.5 ~ 3.0mL of volume, pressing time, quantitative loop inflationtime, 5 ~ 20s of sample injection time.
Preferably, in step S3 head-space sampler other operating conditions are as follows: assist gas pressure 2.5 ~ 4bar of power, nebulizer gas pressure
15 ~ 20psi, quantitative loop 0.8 ~ 1.5mL of volume, pressing time, quantitative loop inflationtime, 10 ~ 15s of sample injection time.
Preferably, the operating condition of gas chromatograph are as follows: injection port use Splitless injecting samples, inlet pressure be 10 ~
30psi, post case temperature are 30 ~ 60 DEG C, and retention time is 5 ~ 15min, and injector temperature is 220 ~ 240 DEG C, and detector temperature is
330~350℃。
Preferably, the operating condition of gas chromatograph are as follows: injection port use Splitless injecting samples, inlet pressure be 20 ~
25psi, post case temperature are 40 ~ 60 DEG C, and retention time is 10 ~ 15min, and injector temperature is 220 ~ 230 DEG C, and detector temperature is
340~350℃。
Compared with now with technology, the invention has the following advantages:
Prepared by ethyl alcohol or methanol 5 ~ 45% testing sample solution is added in the present invention in black liquor, can prevent other
Component (mainly lignin and alkali) is to the australene influence that distribution coefficient generates in liquid phase.
Australene is easily oxidized in air, is had a significant impact to testing result, and the present invention is using in removing ml headspace bottle
Air (into ml headspace bottle plus pyrogallol) is detected, and the accuracy of detection is effectively raised.
The detectable concentration range of the present invention is wide, and concentration range includes 0.4 ~ 1000mg/L, and the accuracy of testing result is high,
Relative standard deviation is less than 5%.
Detailed description of the invention
Fig. 1 is the chromatogram of firpene in Headspace Gas Chromatography black liquor.
Specific embodiment
The present invention is further illustrated combined with specific embodiments below.Unless stated otherwise, it is used in the embodiment of the present invention
The raw material and conventional use of method of raw material and method for this field regular market purchase.
Embodiment 1
For the wood chip that the present embodiment uses for masson pine, soda pulping process prepares the condition of black liquor are as follows: over dry masson pine wood chip
1kg, NaOH dosage 22%, sulphidity 40%, solid-to-liquid ratio 4:1 are started to warm up from 25 DEG C, heating rate 1 DEG C/min, and 123 DEG C of whens put
Black liquor in boiling vessel out.
The detection method of australene content in a kind of alkaline pulping black liquor, comprising the following steps:
S1. sample pretreatment:
Alkaline pulping black liquor is shaken up, and ultrasound 3min removes the bubble in sample to be tested, it is a certain amount of by what is be uniformly mixed
Black liquor is added in ethanol solution, obtains the testing sample solution that concentration of alcohol is 40%.
S2. the preparation of sample: volume V is taken1For testing sample solution prepared by the step S1 of 15mL, it is added to ml headspace bottle
In, pyrogallol is then added into ml headspace bottle, makes pyrogallol concentration 20g/L, and seal ml headspace bottle, obtains sample to be tested
Bottle；
S3. the balance and detection of sample: sample to be tested bottle obtained by step S2 is placed in automatic headspace sample injector carry out it is flat
Weighing apparatus removes the oxygen in ml headspace bottle, then using being detected in the gas chromatograph equipped with flame ionization detector, respectively
Record the australene gas-chromatography signal value A of ml headspace bottle to be measured1；
Wherein, the equilibrium condition of head-space sampler are as follows: 50 DEG C of furnace temperature, equilibration time 30min；
Other operating conditions of head-space sampler are as follows: assist gas pressure power 2.5bar, nebulizer gas pressure 15psi, quantitative loop volume
1.0mL, pressing time, quantitative loop inflationtime, sample injection time 10s.
The operating condition of gas chromatograph are as follows: injection port uses Splitless injecting samples, inlet pressure 20psi, post case temperature
Degree is 50 DEG C, retention time 10min, and injector temperature is 220 DEG C, and detector temperature is 330 DEG C.
S4. the foundation of standard curve: serial australene ethyl alcohol standard solution is prepared to head space according to step S1 the method
In bottle, and ml headspace bottle is sealed rapidly.Above-mentioned solution is placed into headspace autosampler 80oIt is balanced under conditions of C
After 45min, the accurate signal value of australene is detected and recorded.The australene liquor capacity of addition is molten multiplied by australene standard
The concentration of liquid obtains accurate additional amount m(μ g of australene), and as independent variable, using australene signal value as dependent variable, adopt
The correction equation of australene content detection in black liquor is established with linear fitting, it may be assumed that A=32197m+7.892；
S5. in sample australene content calculating: according to the australene signal value of the resulting black liquor sample to be tested of step S3
A1And calibration curve equation obtained by step S4, the content of australene in sample to be tested is calculated using following formula, wherein X is single
The volume fraction of black liquor in the volume testing sample solution of position,
Wherein, C-μ g/mL.
The present embodiment tests 3 samples under the same conditions, and being computed and measuring the average value of australene content is 6.92g/
L, relative standard deviation 4.63%.
Embodiment 2
For the sample that the present embodiment uses for larch, soda pulping process prepares the condition of black liquor are as follows: over dry larch wood chip
1kg, NaOH dosage 20%, sulphidity 30%, solid-to-liquid ratio 4:1 are started to warm up from 25 DEG C, heating rate 1 DEG C/min, and 123 DEG C of whens put
Black liquor in boiling vessel out.
The detection method of australene content in a kind of alkaline pulping black liquor, comprising the following steps:
S1. sample pretreatment:
Alkaline pulping black liquor is shaken up, and ultrasound 1min removes the bubble in sample to be tested, it is a certain amount of by what is be uniformly mixed
Black liquor is added in ethanol solution, obtains the testing sample solution that concentration of alcohol is 30%.
S2. the preparation of sample: volume V is taken1For testing sample solution prepared by the step S1 of 15mL, it is added to ml headspace bottle
In, pyrogallol is then added into ml headspace bottle, makes pyrogallol concentration 80g/L, and seal ml headspace bottle, obtains sample to be tested
Bottle；
S3. the balance and detection of sample: sample to be tested bottle obtained by step S2 is placed in automatic headspace sample injector carry out it is flat
Weighing apparatus removes the oxygen in ml headspace bottle, then using being detected in the gas chromatograph equipped with flame ionization detector, respectively
Record the australene gas-chromatography signal value A of ml headspace bottle to be measured1；
Wherein, the equilibrium condition of head-space sampler are as follows: 50 DEG C of furnace temperature, equilibration time 50min；
Other operating conditions of head-space sampler are as follows: assist gas pressure power 3.0bar, nebulizer gas pressure 15psi, quantitative loop volume
1.5mL, pressing time, quantitative loop inflationtime, sample injection time 15s.
The operating condition of gas chromatograph are as follows: injection port uses Splitless injecting samples, inlet pressure 25psi, post case temperature
Degree is 60 DEG C, retention time 12min, and injector temperature is 220 DEG C, and detector temperature is 340 DEG C.
S4. the foundation of standard curve: serial australene ethyl alcohol standard solution is prepared to head space according to step S1 the method
In bottle, and ml headspace bottle is sealed rapidly.Above-mentioned solution is placed into headspace autosampler 80oIt is balanced under conditions of C
After 45min, the accurate signal value of australene is detected and recorded.The australene liquor capacity of addition is molten multiplied by australene standard
The concentration of liquid obtains accurate additional amount m(μ g of australene), and as independent variable, using australene signal value as dependent variable, adopt
The correction equation of australene content detection in black liquor is established with linear fitting, it may be assumed that A=32197m+7.892；
S5. in sample firpene content calculating: according to the firpene signal value A of the resulting black liquor sample to be tested of step S31With
And calibration curve equation obtained by step S4, the content of firpene in sample to be tested is calculated using following formula, wherein X is unit volume
The volume fraction of black liquor in testing sample solution,
Wherein, C-μ g/mL.
The present embodiment tests 3 samples under the same conditions, and being computed and measuring the average value of australene content is 2.14g/
L, relative standard deviation 3.65%.
Embodiment 3
The sample that the present embodiment uses for pine, soda pulping process prepares the condition of black liquor are as follows: over dry radiate pine sheet
1kg, NaOH dosage 18%, sulphidity 45%, solid-to-liquid ratio 6:1 are started to warm up from 25 DEG C, heating rate 1 DEG C/min, and 123 DEG C of whens put
Black liquor in boiling vessel out.
The detection method of australene content in a kind of alkaline pulping black liquor, comprising the following steps:
S1. sample pretreatment:
Alkaline pulping black liquor is shaken up, and ultrasound 3min removes the bubble in sample to be tested, it is a certain amount of by what is be uniformly mixed
Black liquor is added in methanol solution, obtains the testing sample solution that methanol concentration is 35%.
S2. the preparation of sample: volume V is taken1For testing sample solution prepared by the step S1 of 15mL, it is added to ml headspace bottle
In, pyrogallol is then added into ml headspace bottle, makes pyrogallol concentration 20g/L, and seal ml headspace bottle, obtains sample to be tested
Bottle；
S3. the balance and detection of sample: sample to be tested bottle obtained by step S2 is placed in automatic headspace sample injector carry out it is flat
Weighing apparatus removes the oxygen in ml headspace bottle, then using being detected in the gas chromatograph equipped with flame ionization detector, respectively
Record the firpene gas-chromatography signal value A of ml headspace bottle to be measured1；
Wherein, the equilibrium condition of head-space sampler are as follows: 60 DEG C of furnace temperature, equilibration time 45min；
Other operating conditions of head-space sampler are as follows: assist gas pressure power 2.5bar, nebulizer gas pressure 20psi, quantitative loop volume
1.0mL, pressing time, quantitative loop inflationtime, sample injection time 20s.
The operating condition of gas chromatograph are as follows: injection port uses Splitless injecting samples, inlet pressure 22psi, post case temperature
Degree is 40 DEG C, retention time 10min, and injector temperature is 220 DEG C, and detector temperature is 350 DEG C.
S4. the foundation of standard curve: serial australene methanol standard solution is prepared to head space according to step S1 the method
In bottle, and ml headspace bottle is sealed rapidly.Above-mentioned solution is placed into headspace autosampler 80oIt is balanced under conditions of C
After 45min, the accurate signal value of australene is detected and recorded.The australene liquor capacity of addition is molten multiplied by australene standard
The concentration of liquid obtains accurate additional amount m(μ g of australene), and as independent variable, using australene signal value as dependent variable, adopt
The correction equation of australene content detection in black liquor is established with linear fitting, it may be assumed that A=32197m+7.892；
S5. in sample australene content calculating: according to the australene signal value of the resulting black liquor sample to be tested of step S3
A1And calibration curve equation obtained by step S4, the content of australene in sample to be tested is calculated using following formula, wherein X is single
The volume fraction of black liquor in the volume testing sample solution of position,
Wherein, C-μ g/mL.
The present embodiment tests 3 samples under the same conditions, and being computed and measuring the average value of australene content is 1.26g/
L, relative standard deviation 4.34%.
Embodiment 4 ~ 7
Embodiment 4 ~ 7 and the detecting step and process conditions of embodiment 1 are essentially identical, in place of main difference are as follows:
The detectable concentration range of detection method is wide known in summary, and concentration range includes 0.4 ~ 1000mg/
The accuracy of L, testing result are high, and relative standard deviation is less than 5%.
Obviously, the above embodiment of the present invention be only to clearly illustrate example of the present invention, and not be pair
The restriction of embodiments of the present invention.For those of ordinary skill in the art, may be used also on the basis of the above description
To make other variations or changes in different ways.There is no necessity and possibility to exhaust all the enbodiments.It is all this
Made any modifications, equivalent replacements, and improvements etc., should be included in the claims in the present invention within the spirit and principle of invention
Protection scope within.
Claims (5)
1. the detection method of australene content in a kind of alkaline pulping black liquor, which comprises the following steps:
S1. sample pretreatment: alkaline pulping black liquor is shaken up and removes the bubble in sample to be tested, by uniformly mixed black liquor
It is added in ethyl alcohol or methanol solution, obtains the testing sample solution that ethyl alcohol or methanol concentration are 5 ~ 45%；
S2. the preparation of sample: the testing sample solution for taking the step S1 of volume V1 to prepare is added in ml headspace bottle, then uses
Pyrogallol is added into ml headspace bottle to remove the oxygen in ml headspace bottle, and seals and obtain sample to be tested bottle, the volume V1 is
0.5~15mL；The concentration of pyrogallol is 10 ~ 100g/L in the testing sample solution；
S3. the balance and detection of sample: sample to be tested bottle obtained by step S2 being placed in automatic headspace sample injector and is balanced,
Then using being detected in the gas chromatograph equipped with flame ionization detector, the australene of ml headspace bottle to be measured is recorded respectively
Gas-chromatography signal value A1；
Wherein, the equilibrium condition of head-space sampler are as follows: 50 ~ 90 DEG C of furnace temperature, equilibration time are 15 ~ 60min；
S4. according to ethyl alcohol described in step S1 or methanol ratio, australene ethanol solution or methanol the foundation of standard curve: are used
Solution prepares the australene standard solution of known concentration, and australene is added quality and is denoted as m, will prepare according to step S2 to test sample
Product bottle, and its signal value A is detected using condition described in step S3, using linear fit establish shaped likeStandard it is bent
Line equation, wherein m-μ g, a-μ g-1, b-dimensionless；
S5. in sample australene content calculating: according to the australene signal value A1 of the resulting black liquor sample to be tested of step S3 with
And calibration curve equation obtained by step S4, the content of australene in sample to be tested is calculated using following formula, wherein X is unit body
The volume fraction of black liquor in product testing sample solution,
Wherein, C-μ g/mL.
2. according to claim 1 in alkaline pulping black liquor australene content detection method, which is characterized in that in step S1
Use 1 ~ 3min of ultrasound to remove the bubble in sample to be tested；Uniformly mixed black liquor is added in ethyl alcohol or methanol solution.
3. according to claim 1 in alkaline pulping black liquor australene content detection method, which is characterized in that it is described to be measured
The concentration of ethyl alcohol or methanol is 30 ~ 45% in sample solution.
4. according to claim 1 in alkaline pulping black liquor australene content detection method, which is characterized in that in step S3
Other operating conditions of head-space sampler are as follows: assist gas pressure 1.5 ~ 5bar of power, 10 ~ 20psi of nebulizer gas pressure, quantitative loop volume 0.5 ~
3.0mL, pressing time, quantitative loop inflationtime, 5 ~ 20s of sample injection time.
5. according to claim 4 in alkaline pulping black liquor australene content detection method, which is characterized in that in step S3
Other operating conditions of head-space sampler are as follows: assist gas pressure 2.5 ~ 4bar of power, 15 ~ 20psi of nebulizer gas pressure, quantitative loop volume 0.8 ~
1.5mL, pressing time, quantitative loop inflationtime, 10 ~ 15s of sample injection time.
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