CN106290632A - The detection method of chloride ion content in paper pulp - Google Patents
The detection method of chloride ion content in paper pulp Download PDFInfo
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- CN106290632A CN106290632A CN201610643039.4A CN201610643039A CN106290632A CN 106290632 A CN106290632 A CN 106290632A CN 201610643039 A CN201610643039 A CN 201610643039A CN 106290632 A CN106290632 A CN 106290632A
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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- G01N30/02—Column chromatography
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- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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Abstract
The invention discloses the detection method of chloride ion content in a kind of paper pulp, belong to the quantitative detection field of chloride ion content in paper pulp.The detection method of chloride ion content in paper pulp of the present invention, comprises the following steps: extracts the chloride ion in pulp sample to be measured, obtains extracting solution；After being filtered by extracting solution, chromatography of ions is used to quantitative determine.The present invention during chloride ion, is reduced chloride ion loss in heating process by adding sodium hydroxide solution, is made by supersound extraction the chloride ion of pulp sample surface and inside thereof fully be extracted in extracting pulp sample to be measured.The detection method of chloride ion content in paper pulp of the present invention, not only in pulp sample, the extraction ratio of chloride ion is high, and the accuracy of measurement of chloride ion content and highly sensitive, reproducible, simple to operate, testing cost is low.
Description
Technical field
The present invention relates to the detection method of chloride ion content in a kind of paper pulp, particularly relate to chloride ion in a kind of mensuration paper pulp
The ion chromatographic method of content, belongs to the quantitative detection field of chloride ion content in paper pulp.
Background technology
Association with pulp bleaching is one important procedure of pulp and paper industry, it is therefore an objective to the whiteness and the whiteness that improve paper pulp are stable
Property.And along with the development in epoch, the most green paper pulp increasingly comes into one's own.Tradition has the technique of pollution by two to environment
Chlorine monoxid sterilization is replaced.During using chlorine dioxide to bleach paper pulp, chlorine element is reduced into as chloride ion.Chlorine
Ion is one of them source of anionic trash in paper technology, and the existence of anionic trash can affect the wet end shape of paper machine
Condition, thus reduce paper machine can behavior in service and production efficiency, improve chemical wear, affect the economic benefit of enterprise；In addition
Some special paper usings, need special pulps to do raw material such as electric elements packaging Paper or cardboard etc..Therefore, measure in paper pulp chlorine from
The content of son is most important.Traditional method uses pure water to extract or vapor distillation is during extracting chloride ion, paper pulp meeting
Hydrolysis produces substantial amounts of polysaccharide, and polysaccharide exists absorption on anion chromatographic column, gradually occupies the merit on anion chromatographic column
Energy group, and cause chromatographic peak deformation and chromatographic column pressure to raise, affecting the accuracy of determination of chloride ion, chromatographic column pressure raises
The damage causing chromatographic column will improve the operating cost of enterprise again.Therefore, pre-treating method is simple, reproducibility is strong to set up one
And the new method of chloride ion in the ion-chromatographic determination paper pulp of low cost, will have great importance.
Summary of the invention
The technical problem to be solved is to provide the detection method of chloride ion content in a kind of paper pulp, and the method carries
Taking the simple to operate of chloride ion in pulp sample to be measured, the extraction ratio of chloride ion is high, and assay accuracy is high, reproducible.
For solving above-mentioned technical problem, the technical solution used in the present invention is:
The invention discloses the detection method of chloride ion content in a kind of paper pulp, comprise the following steps: (1) extracts paper to be measured
Chloride ion in slurry samples, obtains extracting solution；(2), after being filtered by extracting solution, chromatography of ions is used to quantitative determine.
Wherein, the chloride ion in step (1) described extraction pulp sample to be measured includes: add hydrogen in pulp sample to be measured
Sodium hydroxide solution and deionized water, seal, carry out supersound extraction；The sample solution obtained after supersound extraction is heated, so
Rear cooling, obtains extracting solution.Wherein, described deionized water is preferably secondary deionized water；Carrying after can also including cooling
Take liquid secondary deionized water and be settled to the cumulative volume of added sodium hydroxide solution and deionized water, in order to follow-up determines
Amount detection.
In chloride ion in step (1) described extraction pulp sample to be measured, count according to g/ml, pulp sample to be measured: hydrogen-oxygen
Change the cumulative volume=1-5:10-100 of sodium solution and deionized water；Preferably, count according to g/ml, pulp sample to be measured: hydroxide
Sodium solution and the cumulative volume=2:50 of deionized water.Wherein sodium hydroxide solution is 1-7:43-49 with the volume ratio of deionized water,
It is preferably 5:45.The concentration of described sodium hydroxide solution is 10-50mol/L, preferably 30mol/L.Described supersound extraction time
Between be 100-130min, preferably 120min；The power of described supersound extraction is 50-150W, preferably 100W.Described heating
Power is 1000-1500W, and the time of heating is 10-30min；Preferably, the power of described heating is 1200W, the time of heating
For 20min；After heating, pulp sample becomes black.Described heating can use electric furnace or other firing equipments；The process of heating
In the volatilization of sample solution to be avoided, such as can cover the vessel port filling pulp sample to be measured with surface plate.Described sealing
Can seal with preservative film, or adopt and seal in other ways.
The detection method of chloride ion content in paper pulp of the present invention, was filtered into the disposable pin of 0.22 μm described in step (2)
Formula filter；Preferably, the front 3mL discarding syringe filter extracts solution.The condition of described chromatography of ions includes: ion color
Spectrometer is WY-IC6200 type ion chromatograph；Chromatographic column is ShodexSI 52-4E anion chromatographic column；Leacheate is
The sodium carbonate leacheate of 3.6mmol/L；Flow velocity: 0.8mL/min；Electric conductivity detector temperature: 40 DEG C；Column temperature: 50 DEG C；Suppression electricity
Stream: 30mA；Sample size: 25 μ L.Described quantitative determination uses external standard method, including: according to chloride ion in chloride ion standard solution
Concentration and peak area drawing curve (concrete, such as with the concentration of chloride ion in chloride ion standard solution as abscissa, with
The peak area of chloride ion standard solution is vertical coordinate drawing curve), obtain linear equation；By chlorine in pulp sample to be measured from
The peak area of son brings linear equation into, calculates the respective concentration of chloride ion in pulp sample to be measured.
During the present invention extracts the chloride ion in pulp sample to be measured, addition sodium hydroxide solution can reduce chloride ion and exist
Heating process is lost, uses supersound extraction fully to extract with the chloride ion to pulp sample surface and inside thereof.This
Bright sodium hydroxide solution volume and the supersound extraction time to extracting in pulp sample to be measured during chloride ion is optimized.
Result shows, under conditions of other parameters are consistent, for 2g pulp sample, along with 30mol/L sodium hydroxide solution volume
Increasing, the extraction ratio of chloride ion also presents raising trend, during until sodium hydroxide solution addition volume is 5.0mL, chloride ion
Extraction ratio tends towards stability.Therefore the addition volume that present invention determine that sodium hydroxide solution is: every 2g pulp sample adds 30mol/L
Sodium hydroxide solution 5.0mL.The optimum results of supersound extraction time shows, under conditions of other parameters are consistent, and supersound extraction
In the range of time 100-130min, along with the increase of supersound extraction time, the extraction ratio of chloride ion presents raising trend, ultrasonic
During extraction time 120min, the extraction ratio of chloride ion tends towards stability.Therefore the time that present invention determine that supersound extraction is 120min.
In paper pulp of the present invention, chloride ion content detection method is reproducible, and the accuracy of mensuration is high.To same concentration
Chloride ion standard solution continuous sample introduction 6 times, the retention time of chloride ion chromatographic peak and the relative standard deviation of peak area are respectively
0.08% and 0.25%.Measuring the content of chloride ion in actual paper slurry samples by detection method is 38.06mg/kg；
The response rate that actual sample carries out recovery of standard addition test is 105.0%.
The detection method of chloride ion content in paper pulp of the present invention, kind or source for pulp sample do not have special limit
System.
Technical solution of the present invention compared with prior art, has the advantages that
The present invention uses the content of chloride ion in ion chromatography paper pulp, the process of chloride ion in extracting pulp sample
In, reduce chloride ion loss in heating process by adding sodium hydroxide solution, make pulp sample table by supersound extraction
The chloride ion of face and inside thereof is fully extracted, and not only in pulp sample, the extraction ratio of chloride ion is high, simple to operate, and chlorine
The accuracy of determination of ion content, highly sensitive, reproducible, testing cost is low.Therefore, chloride ion content in paper pulp of the present invention
Detection method be applicable to pulp product technology controlling and process in process of production.
Accompanying drawing explanation
Fig. 1 is the chromatogram of chloride ion standards solution analysis；Wherein, chromatographic peak is Cl-(2.50mg/L)；
Fig. 2 is the chromatogram of actual paper slurry samples chloride test；Wherein, chromatographic peak is Cl-；
Fig. 3 is that sodium hydroxide solution volume is to the influence curve figure of determination of chloride ion in pulp sample；
Fig. 4 is that the supersound extraction time is to the influence curve figure of determination of chloride ion in pulp sample.
Detailed description of the invention
Below in conjunction with specific embodiment further describe the present invention, advantages of the present invention and feature will be with describe and
Apparent.It should be understood that described embodiment is only exemplary, the scope of the present invention is not constituted any restriction.This area
Skilled artisans appreciated that, lower without departing from the spirit and scope of the present invention can to the details of technical solution of the present invention and
Form is modified or replaces, but these amendments or replacement each fall within protection scope of the present invention.
1, instrument and reagent
WY-IC6200 type ion chromatograph (Anhui Wanyi Science and Technology Co., Ltd.)；Anion suppressor (ASRS, peace
Hui Wan instrument Science and Technology Co., Ltd.)；Electric conductivity detector (CD 6000, Anhui Wanyi Science and Technology Co., Ltd.)；Anion color
Spectrum post (Shodex SI 52-4e, Japan Showa electrician)；The 0.22 disposable syringe filter of μm (Qingdao Ai Li analysis experiment science and technology
Company limited)；Pulp sample (Shandong Yinying Co., Ltd.)；Sodium carbonate (standard reagent)；Sodium hydroxide (top grade is pure)；Chlorine
Ion quasi-stock solution 1000mg/L.
Ultrasonic extractor (KQ2200E, Kunshan Shu Mei).
The assay of chloride ion in embodiment 1 pulp sample
1, experimental technique
1.1 leacheates, the preparation of anion standard solution
1.1.1 the preparation of leacheate
Accurate weighing 0.3816g sodium carbonate standard reagent, is placed in 1000mL volumetric flask, dissolves also by secondary deionized water
It is settled to scale, obtains the sodium carbonate leacheate of 3.6mmol/L.
1.1.2 the preparation of standard working solution
Accurately pipette 1.0mL Cl-In Standard Stock solutions 100mL volumetric flask, it is settled to scale by secondary deionized water,
Obtain Cl-Concentration is 10.0mg/L.
1.1.3 the preparation of working curve solution
Accurately pipette 0.5,1.0,2.5mL, 5.0mL standard working solution be respectively placed in 10mL volumetric flask, go with secondary
Ionized water is settled to scale, obtain concentration be respectively 0.5,1.0,2.5, the working curve solution of 5.0mg/L.
1.1.4 the preparation of repeatability solution
Accurately pipette 2.5mL standard working solution, be placed in 10mL volumetric flask, be settled to scale by secondary deionized water,
Obtaining concentration is 2.5mg/L Cl-Solution, as the solution of precision test.
The preparation of 1.2 sample solutions
(1) accurately weigh specification after cutting be the quality of 5 × 5mm pulp sample be 2.0000g, be placed in 200mL burn
In Bei；
(2) sodium hydroxide solution and the 45mL secondary deionized water beaker in (1) of 5mL 30mol/L it are separately added into
In, after beaker mouth being sealed with the preservative film of specialty, it is transferred in ultrasonic extractor, to the ion in sample with ultrasonic
The mode extracted extracts 120min, and wherein ultrasonic power is 100W.
(3) after ultrasonic 120min, it is transferred on electric furnace heating by the beaker containing sample solution, adjusts electric furnace
Heating power is 1200W, covers beaker mouth with surface plate in heating process, when the pulp sample in beaker becomes black, closes
Closing electric furnace, the time that this heating process needs is about 20min；
(4) after beaker cools down, it is added thereto to secondary deionized water and uses a small amount of repeatedly by the dissolving of sample residue, and turn
Move to, in 50mL volumetric flask, finally be settled to scale by secondary deionized water；
(5) take sample solution and cross the disposable syringe filter of 0.22 μm, enter ion chromatography system and be analyzed, cross pin
Before formula filter, 3mL sample solution to discard.
The analysis of 1.3 standard solution
(1) repeatability
Chloride ion standard solution continuous sample introduction 6 times to same concentration 2.5mg/L, obtains chloride ion ion standard solution and divides
The chromatogram of analysis, and calculate the retention time of chloride ion chromatographic peak and the relative standard deviation of peak area.
(2) linear relationship
Linear solvent to the standard solution of preparation, carries out sample introduction according to the Loading sequence from low concentration to high concentration and divides
Analysis, obtains the peak area of chloride ion under variable concentrations, with the concentration (mg/L) of chloride ion as abscissa, with its peak area for vertical seat
Mark and draw working curve processed.
The mensuration of the content of chloride ion and recovery of standard addition in 1.4 pulp sample
Using WY-IC6200 type ion chromatograph, ShodexSI 52-4E anion chromatographic column, flow velocity is 0.8mL/min；
Electric conductivity detector temperature: 40 DEG C；Column temperature: 50 DEG C；Suppression electric current: 30mA；Sample size: 25 μ L, 3.6mmol/L sodium carbonate sample is molten
Liquid detects, and carries out the chloride ion in actual sample quantitatively according to external standard method simultaneously.
Actual sample is carried out recovery of standard addition test, and processing method is with the process of 1.2 pulp sample, and adding target content is
50mg/kg, calculates the response rate.
2, experimental result
The analysis of 2.1 standard solution
2.1.1 it is repeated
Chloride ion standard solution continuous sample introduction 6 times to same concentration 2.5mg/L, obtains chloride ion standards solution analysis
Chromatogram (Fig. 1), the relative standard deviation of the retention time and peak area that obtain chloride ion chromatographic peak is respectively 0.08% He
0.25%.
2.1.2 linear relationship
With the concentration (mg/L) of chloride ion as abscissa, with its peak area for vertical coordinate drawing curve, obtain chlorine from
The linear equation of son is Y=13181X-1230.6, and its correlation coefficient is 0.9997.
The mensuration of the content of chloride ion and recovery of standard addition in 2.2 pulp sample
The sample solution handled well 1.2 detects, and obtains the chromatogram (Fig. 2) of actual sample detection, basis simultaneously
Chloride ion in actual sample is carried out quantitatively by external standard method, and obtaining the content of chloride ion in actual sample is 38.06mg/kg.Right
Actual sample carries out recovery of standard addition test, and the rate of being recycled is 105.0%.
The optimization of parameter in experimental example 1 pulp sample pretreatment process
1, the optimization of sodium hydroxide solution volume
Pulp sample pretreatment process adds sodium hydroxide solution to reduce chloride ion and lose in heating process.This
The bright sample to identical sample weighting amount (quality of pulp sample is 2.0000g) is separately added into 1.0,2.0,3.0,4.0,5.0,
6.0 and 7.0mL 30mol/L sodium hydroxide solutions, and it is separately added into 49.0,48.0,47.0,46.0,45.0,44.0 accordingly
With 43.0 secondary deionized water, through the supersound extraction (ultrasonic 120min, ultrasonic power 100W) of identical time, heating power
1200W, heats 20min, and the chloride ion in the testing sample solution after cooling constant volume is measured (the same enforcement of concrete grammar
Example 1), obtain adding the impact on determination of chloride ion result of the different volumes sodium hydroxide solution.
By the volume of sodium hydroxide solution, the concentration of chloride ion being drawn curve, result is shown in Fig. 3, can from curve
Going out, along with the increase of 30mol/L sodium hydroxide solution volume, the extraction ratio of chloride ion also presents raising trend, until hydroxide
When sodium solution volume is 5mL, the extraction ratio of chloride ion tends towards stability；Continue to increase the volume of sodium hydroxide solution, carrying of chloride ion
The rate that takes no longer improves.Therefore, present invention determine that in 2.0000g pulp sample, the addition volume of 30mol/L sodium hydroxide solution
For 5.0mL.
2, the optimization of supersound extraction time
In pulp sample pretreatment process, the purpose of supersound extraction is that the chloride ion to pulp sample surface and inside thereof enters
Row extracts.The present invention is to a sample solution, (it is 5 × 5mm paper that sample solution prepares 1.2 in same embodiment 1, i.e. specification
Quality 2.0000g of slurry samples, adds sodium hydroxide solution and the 45mL secondary deionized water of 5mL 30mol/L), ultrasonic power
For 100W, respectively through 100,105,110,115,120,125 and the sample solution of the supersound extraction of 130min, through adding hot merit
Rate 1200W, heats 20min, and the chloride ion in the sample solution of cooling constant volume is measured (the same embodiment of concrete grammar
1), the different supersound extraction time impact on determination of chloride ion result is obtained.
By the supersound extraction time, the concentration of chloride ion being drawn curve, result is shown in Fig. 4.Can from the curve drawn
Going out, along with the increase of supersound extraction time, the extraction ratio of chloride ion also presents raising trend, the chloride ion when ultrasonic 120min
Extraction ratio tends towards stability；Continuing to increase the supersound extraction time, the extraction ratio of chloride ion no longer improves.Therefore, present invention determine that super
The time that sound extracts is 120min.
Claims (10)
1. the detection method of chloride ion content in a paper pulp, it is characterised in that comprise the following steps: (1) extracts paper pulp to be measured
Chloride ion in sample, obtains extracting solution；(2), after being filtered by extracting solution, chromatography of ions is used to quantitative determine.
2. according to the detection method described in claim 1, it is characterised in that in step (1) described extraction pulp sample to be measured
Chloride ion includes: adds sodium hydroxide solution and deionized water in pulp sample to be measured, seals, carry out supersound extraction；Will be super
The sample solution that sound obtains after extracting heats, and then cools down, obtains extracting solution.
3. according to the detection method described in claim 2, it is characterised in that: count according to g/ml, pulp sample to be measured: sodium hydroxide
Solution and the cumulative volume=1-5:10-100 of deionized water；
Preferably, count according to g/ml, pulp sample to be measured: sodium hydroxide solution and the cumulative volume=2:50 of deionized water.
4. according to the detection method described in Claims 2 or 3, it is characterised in that: sodium hydroxide solution and the volume of deionized water
Ratio is 1-7:43-49, preferably 5:45.
5. according to the detection method described in Claims 2 or 3, it is characterised in that: the concentration of described sodium hydroxide solution is 10-
50mol/L, preferably 30mol/L.
6. according to the detection method described in claim 2, it is characterised in that: the time of described supersound extraction is 100-130min,
It is preferably 120min；
The power of described supersound extraction is 50-150W, preferably 100W.
7. according to the detection method described in claim 2, it is characterised in that: the power of described heating is 1000-1500W, heating
Time be 10-30min；Preferably, the power of described heating is 1200W, and the time of heating is 20min.
8. according to the detection method described in claim 1, it is characterised in that the condition of step (2) described chromatography of ions includes:
Ion chromatograph is WY-IC6200 type ion chromatograph；Chromatographic column is ShodexSI 52-4E anion chromatographic column；Drip washing
Liquid is the sodium carbonate leacheate of 3.6mmol/L；Flow velocity: 0.8mL/min；Electric conductivity detector temperature: 40 DEG C；Column temperature: 50 DEG C；Suppression
Electric current: 30mA；Sample size: 25 μ L.
9. according to the detection method described in claim 1, it is characterised in that: step was filtered into 0.22 μm once described in (2)
Property syringe filter.
10. according to the detection method described in claim 1, it is characterised in that: step (2) described quantitative determination includes: according to chlorine
In ion standard solution, the concentration of chloride ion and peak area drawing curve, obtain linear equation；By in pulp sample to be measured
The peak area of chloride ion brings linear equation into, calculates the respective concentration of chloride ion in pulp sample to be measured.
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Cited By (1)
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| CN110879261A (en) * | 2019-11-29 | 2020-03-13 | 安徽皖维高新材料股份有限公司 | Method for detecting content of chloride ions in PVB resin by adopting ion chromatography |
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