CN204495726U - Measure the reaction, extraction colorimetric device of water base adhesive mesoboric acid content - Google Patents

Measure the reaction, extraction colorimetric device of water base adhesive mesoboric acid content Download PDF

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Publication number
CN204495726U
CN204495726U CN201520177268.2U CN201520177268U CN204495726U CN 204495726 U CN204495726 U CN 204495726U CN 201520177268 U CN201520177268 U CN 201520177268U CN 204495726 U CN204495726 U CN 204495726U
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water base
base adhesive
acid content
reaction
extraction
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邱建华
李国政
宋金勇
张东豫
周浩
田海英
郝辉
李怀奇
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China Tobacco Henan Industrial Co Ltd
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China Tobacco Henan Industrial Co Ltd
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Abstract

The utility model belongs to boric acid detection technique field, is specifically related to a kind of reaction, extraction colorimetric device measuring water base adhesive mesoboric acid content.This device comprises the chromogenic reaction container and liquid-liquid extraction box body that link together, and wherein chromogenic reaction container is funnel-form, and funnel-form bottom is connected with color comparison tube.Measure the method for water base adhesive mesoboric acid content, comprise steps such as measuring solvent preparation, sample pretreatment, reaction, colour developing, extraction, colorimetric.Reaction, extraction colorimetric device provided by the utility model, structure is simple, be easy to make, and practicality is better.The measuring method provided is based on the know-why of methylene blue-ethylene dichloride photometry, is suitable for detecting the water base adhesive sample of boron content at 1 ~ 100mg/g.The utility model has the advantages such as pocket is good, wide accommodation, antijamming capability, can sxemiquantitative water base adhesive sample mesoboric acid content, has and promotes applicability preferably.

Description

Measure the reaction, extraction colorimetric device of water base adhesive mesoboric acid content
Technical field
The utility model belongs to boric acid detection technique field, is specifically related to a kind of reaction, extraction colorimetric device measuring water base adhesive mesoboric acid content.
Background technology
Boric acid is as a kind of industrial chemicals, and in industrial circle is produced, tool has been widely used; Simultaneously boric acid is also a kind of external sterilizing antiseptic and common drug, and in some cases, also can make pesticide and catalyzer uses, thus purposes is comparatively extensive.
Water base adhesive is a kind of adhesive by the filmogen that maybe can be dissolved in the water can be disperseed to make, and in actual use procedure, adds appropriate boric acid and can accelerate its drying, improve sticking efficiency in water base adhesive.Generally speaking, the existence of trace B element can play certain positive effect to human metabolism, but will present borism when boron content is too high.Because boric acid is drained very slow in human body, and the boric acid of people's body accumulation can affect digestive ferment effect, causes multiple physiological maladies.Research shows, if eat 0.5g boric acid every day can cause anorexia, hinders the absorption of nutriment.And if adult's disposable food 1 ~ 3g boric acid material can cause poisoning, its clinical poisoning manifestations mainly contains the gastrointestinal symptoms such as Nausea and vomiting, stomachache, diarrhoea.So detect the boric acid concentration in food or environment fast, timely, have very important significance.
In prior art, conventional boric acid method for quick is turmeric test paper method.Although the method has highly sensitive advantage, but due to operating conditions relative complex, loaded down with trivial details, such as need to dry, drip the operation such as acid-base solution respectively, and there is the drawbacks such as repeatability is poor, be thus badly in need of exploring the detection method of new mensuration boric acid concentration that can be quick, easy.
Summary of the invention
The utility model is according to methylene blue-ethylene dichloride photometry principle, provide the measuring method of a kind of reaction, extraction colorimetric device measuring water base adhesive mesoboric acid content and the measurement water base adhesive mesoboric acid content using this device, the method can be rapid qualitative and semiquantitative determination water base adhesive mesoboric acid content, and the boric acid content be particularly useful in the water base adhesive in cigarette production line measures.
The concrete technical scheme that the present invention takes is as follows.
A kind of reaction, extraction colorimetric device measuring water base adhesive mesoboric acid content, comprise the chromogenic reaction container and liquid-liquid extraction box body that link together, wherein chromogenic reaction container is funnel-form, and namely funnel-form bottom is connected with color comparison tube: this device comprise liquid-liquid extraction box body, with the chromogenic reaction container be connected bottom liquid-liquid extraction box body and the color comparison tube be connected with chromogenic reaction container lower end; Described chromogenic reaction container is funnel-form.
The reaction, extraction colorimetric device of described mensuration water base adhesive mesoboric acid content, liquid-liquid extraction box body top is provided with lid, is convenient to vibrate, mixes, shakes up the operations such as liquid; Chromogenic reaction container is fixedly connected with or the movable connection method such as cutting ferrule, screw thread with adopting bottom liquid-liquid extraction box body, and adopt same with chromogenic reaction container lower end of color comparison tube is fixedly connected with or the movable connection method such as cutting ferrule, screw thread.
The reaction, extraction colorimetric device of described mensuration water base adhesive mesoboric acid content, this device material is preferably polypropylene material, and wherein the capacity of chromogenic reaction container is preferably 50mL, and the capacity of liquid-liquid extraction box body is preferably 50mL, and the capacity of color comparison tube is preferably 5mL.
Adopt the reaction, extraction colorimetric device of described mensuration water base adhesive mesoboric acid content to measure the method for water base adhesive mesoboric acid content, comprise the following steps:
(1) measure solvent to prepare, described measurement solvent comprises sample pre-treatments solution, chromophoric solution, extraction agent, boron standard color range colorimetric solution or boron standard color range colorimetric card;
Described sample pre-treatments solution is the mixed solution of sulphur phosphorus acid mixture, sodium fluoride and sodium sulphate; Concrete employing following steps preparation: to prepare 100mL solution, be added to the water by the 15mL concentrated sulphuric acid, then add 10mL phosphoric acid, 2g sodium fluoride, 10g sodium sulphate, water is diluted to 100mL; The described concentrated sulphuric acid is with the sulphur acid meter of massfraction 98%, and phosphoric acid is the phosphoric acid of 85% in massfraction;
Described chromophoric solution is the methylene blue aqueous solution of 0.01 mol/L; Compound method is, to prepare 1L, take methylene blue 3.73 g with after a small amount of water-soluble solution, thin up is settled to 1 L;
Described extraction agent is: 1,2-ethylene dichloride;
Described boron standard color range colorimetric solution adopts following steps preparation:
A. prepare boron standard color range solution, described boron standard color range solution is the aqueous solution of a series of variable concentrations adopting boric acid preparation, and its mesoboric acid series concentration is preferably followed successively by: 1mg/g, 5mg/g, 10mg/g, 50mg/g and 100mg/g;
B. each 1g of serial boron standard color range solution prepared in steps A is taken, be placed in the reaction, extraction colorimetric device measuring water base adhesive mesoboric acid content respectively, then add 1g respectively without boron water base adhesive standard items, add 5mL sample pre-treatments liquid respectively, mix, under normal temperature, react 1h;
C. after reaction terminates, add 30mL water, 5mL chromophoric solution and 25mL extraction agent respectively, vibration 5min makes aqueous phase and organic phase fully mix, and finally leave standstill 10min, layering obtains organic phase, and wherein part organic phase is arranged in color comparison tube;
D. arrange from low to high or from high to low according to boric acid concentration and namely obtain boron standard color range colorimetric solution, namely the color of the organic phase obtained according to step C can be used for detecting, sxemiquantitative water base adhesive sample mesoboric acid content;
Described boron standard color range colorimetric card, boron standard color range colorimetric solution basis is prepared from, be specially, organic phase color in boron standard color range colorimetric solution is recorded, gathered, carry out replacement with the picture with color gradient and be combined into boric acid standard color range colorimetric card, concrete as: after photographs collection is carried out to the organic phase color digital camera in boron standard color range colorimetric solution, print combination to make boron standard color range colorimetric card or replace with the picture with color gradient the digital photograph printed, boron standard color range colorimetric card is made in combination further;
It should be noted that, during actual detection water base adhesive sample mesoboric acid content, because the color of water base adhesive itself can be disturbed to some extent to reacting the organic phase color after terminating, thus need when preparing boron standard color range colorimetric solution to add 1g without boron water base adhesive sample to correct the impact that in actual testing process, water base adhesive sample contrasts boron standard color range standard colorimetric solution colour;
(2) sample pretreatment, takes 1g water base adhesive testing sample, adds 5mL sample pre-treatments solution, shakes up, and be placed in the reaction, extraction colorimetric device measuring water base adhesive mesoboric acid content, react under normal temperature, mix, the reaction time is 1h;
(3) in the rear solution of step (2) reaction, add 30mL water, 5mL chromophoric solution, vibration 5min, then add 25mL extraction agent, the reaction, extraction colorimetric device measuring water base adhesive mesoboric acid content is left standstill 10min layering and obtains organic phase;
Need to explain and illustrate, the object adding suitable quantity of water in testing process controls the H in solution +concentration range is about 0.8 ± 0.4mol/L, because if acidity is too low in reaction system, complex reaction rate also can be lower, thus extend the reaction time, if acidity is too high in reaction system, then the extraction quantity of methylene blue originally in extraction solvent ethylene dichloride strengthens, thus affects testing result, thus needs in reaction system to add appropriate water to regulate H +concentration; In testing process, the addition of chromophoric solution is then to meet methylene blue and fluoboric acid root anionic reactive aequum, thus can regulate according to actual sample situation;
(4) compare with boron standard color range colorimetric solution or boron standard color range colorimetric card according to the color of organic phase in step (3), thus the roughly content range of acquisition water base adhesive testing sample mesoboric acid.
The present invention is based on the know-why of methylene blue-ethylene dichloride photometry, and concrete operations principle is: water base adhesive is after sodium sulphate breakdown of emulsion, and wherein contained boric acid and hydrofluorite complexing form fluoboric acid root negative ion (BF 4 -), in acidic aqueous solution, methylene blue and fluoboric acid root negative ion form bluish violet complex compound, this complex compound can by 1,2-ethylene dichloride quantified extract enters organic layer.Color and the boric acid content of organic layer are linear, by with standard colorimetric solution or standard color comparison card comparison after can the content of sxemiquantitative determination sample mesoboric acid.
The reaction, extraction colorimetric device of mensuration water base adhesive mesoboric acid content provided by the utility model, structure is simple, be easy to make, and practicality is better.Because the addition of water base adhesive mesoboric acid is usually about 1 ~ 5%, and adopt this method to be suitable for detecting sample (by preparation concentration range more meticulous or more wide in range standard colorimetric solution or the standard color comparison card of boron content at 1 ~ 100mg/g, purposes can be more extensive, but be limited to the difference degree of human eye for organic phase aberration, thus unlimited extension range of application of the present invention is not suitable for, in actual use, the series concentration range effect provided in the present invention is more excellent), be thus suitable for detection, semiquantitative determination water base adhesive mesoboric acid content.In general, based on the mensuration water base adhesive mesoboric acid content assaying method of the reaction, extraction colorimetric device of mensuration water base adhesive mesoboric acid content, simple operating steps, detection time is short, dependency degree for experimental assembly and technician is relatively low, compared with conventional curcumin development process, the method has the advantages such as pocket is good, easy to operate, highly sensitive, wide accommodation, antijamming capability are better, especially can obtain water base adhesive sample mesoboric acid content by semiquantitative determination, thus have and promote applicability preferably.
Accompanying drawing explanation
Fig. 1 is the reaction, extraction colorimetric device structural representation for measuring water base adhesive mesoboric acid content provided by the present invention;
The boron standard color range colorimetric card of Fig. 2 prepared by the present invention;
Fig. 3 is the actual testing result of Boron contents in embodiment 2 in certain sample;
Fig. 4 is the actual testing result of Boron contents in embodiment 3 in certain sample.
Embodiment
Below in conjunction with embodiment, explanation is further explained to the invention.
embodiment 1
As shown in Figure 1, reaction, extraction colorimetric device for measuring water base adhesive mesoboric acid content provided by the present invention, comprise the chromogenic reaction container 1 and liquid-liquid extraction box body 2 that link together, wherein chromogenic reaction container 1 is funnel-form, and funnel-form bottom is connected with color comparison tube 4.
The reaction, extraction colorimetric device of described mensuration water base adhesive mesoboric acid content, liquid-liquid extraction box body 2 top is provided with lid, is convenient to the vibration of liquid, mixes and the operation such as shakes up; Chromogenic reaction container 1 adopts with the junction 3 bottom liquid-liquid extraction box body 2 and is fixedly connected with or the movable connection method such as cutting ferrule, screw thread, and adopt same with chromogenic reaction container 1 of color comparison tube 4 is fixedly connected with or the movable connection method such as cutting ferrule, screw thread.
The reaction, extraction colorimetric device of described mensuration water base adhesive mesoboric acid content, this device material is preferably polypropylene material, wherein the capacity of chromogenic reaction container 1 is preferably 50mL, and the capacity of liquid-liquid extraction box body 2 is preferably 50mL, and the capacity of color comparison tube 4 is preferably 5mL.
During concrete use, first water base adhesive testing sample is placed in chromogenic reaction container 1, then adds sample pre-treatments solution and react, after reaction terminates, add water, chromophoric solution and extraction agent, fully shake, mix, shake up.Colour developing, extracted after, stratification, organic phase is separated with aqueous phase, because organic phase to be observed is positioned at bottom, wherein part organic phase is arranged in color comparison tube 4, thus is convenient to further than colour contrast, thus can boric acid content in sxemiquantitative water base adhesive sample.
Require emphasis and illustrate, in actual use procedure, in order to Reaction time shorten, other equipment external for this device can be carried out stirring, the operation such as heating is with Reaction time shorten.Such as, can chromogenic reaction container 1 be placed in water-bath, impel completing fast of reaction by heating water bath mode.Thus this device also has good equipment epitaxy advantage.
embodiment 2
Adopt the reaction, extraction colorimetric device measuring water base adhesive mesoboric acid content described in embodiment 1 to measure the method for water base adhesive mesoboric acid content, comprise the following steps.
(1) measure solvent to prepare, described measurement solvent comprises sample pre-treatments solution, chromophoric solution, extraction agent, boron standard color range colorimetric solution or boron standard color range colorimetric card.
Described sample pre-treatments solution is the mixed solution of sulphur phosphorus acid mixture, sodium fluoride and sodium sulphate; Concrete employing following steps preparation: to prepare 100mL solution, be added to the water by the 15mL concentrated sulphuric acid, then add 10mL phosphoric acid, 2g sodium fluoride, 10g sodium sulphate, water is diluted to 100mL.
Described chromophoric solution is the methylene blue aqueous solution of 0.01 mol/L; Compound method is, to prepare 1L, take methylene blue 3.73 g with after a small amount of water-soluble solution, thin up is settled to 1 L.
Described extraction agent is: 1,2-ethylene dichloride.
Described boron standard color range colorimetric solution adopts following steps preparation:
A. prepare boron standard color range solution, described boron standard color range solution is the aqueous solution of a series of variable concentrations adopting boric acid preparation, and its mesoboric acid series concentration is preferably followed successively by: 1mg/g, 5mg/g, 10mg/g, 50mg/g and 100mg/g;
B. each 1g of serial boron standard color range solution prepared in steps A is taken, be placed in the reaction, extraction colorimetric device measuring water base adhesive mesoboric acid content respectively, then add 1g respectively without boron water base adhesive standard items, add 5mL sample pre-treatments liquid respectively, mix, under normal temperature, react 1h;
C. after reaction terminates, add 30mL water, 5mL chromophoric solution and 25mL extraction agent respectively, vibration 5min makes aqueous phase and organic phase fully mix, and finally leave standstill 10min, layering obtains organic phase, and wherein part organic phase is arranged in color comparison tube;
D. arrange from low to high or from high to low according to boric acid concentration and namely obtain boron standard color range colorimetric solution, namely the color of the organic phase obtained according to step C can be used for detecting, sxemiquantitative water base adhesive sample mesoboric acid content.
Described boron standard color range colorimetric card, boron standard color range colorimetric solution basis is prepared from, be specially, record is carried out to the organic phase color in boron standard color range colorimetric solution, gather, carry out replacement with the picture with color gradient and be combined into boric acid standard color range colorimetric card, concrete as: after photographs collection is carried out to the organic phase color digital camera in boron standard color range colorimetric solution, print combination to make boron standard color range colorimetric card or replace with the picture with color gradient the digital photograph printed, boron standard color range colorimetric card is made in further combination, prepared colorimetric card as shown in Figure 2.
Require emphasis and illustrate, when adopting boron standard color range colorimetric solution to carry out color comparison, comparison effect is comparatively accurate, and error is relatively little, but pocket is poor, or needs in situ preparation, thus inconvenience relatively in operation; And adopt boron standard color range colorimetric card pocket better, and colorimetric card can be reused, but error is then larger comparatively speaking.In general, because the present invention is only limitted to the boric acid content in sxemiquantitative water base adhesive, thus corresponding error is also that within the scope that can allow, when specifically using, those skilled in the art can suitably select as required.
Need in addition explain and illustrate be, during actual detection water base adhesive sample mesoboric acid content, because the color of water base adhesive itself can be disturbed to some extent to reacting the organic phase color after terminating, thus need when preparing boron standard color range colorimetric solution to add 1g without boron water base adhesive sample to correct the impact that in actual testing process, water base adhesive sample contrasts boron standard color range standard colorimetric solution colour.
(2) sample pretreatment, takes 1g water base adhesive testing sample, adds 5mL sample pre-treatments solution, shakes up, and be placed in the reaction, extraction colorimetric device measuring water base adhesive mesoboric acid content, react under normal temperature, mix, the reaction time is 1h;
(3) in the rear solution of step (2) reaction, add 30mL water, 5mL chromophoric solution, vibration 5min, then add 25mL extraction agent, the reaction, extraction colorimetric device handstand measuring water base adhesive mesoboric acid content is left standstill 10min layering and obtains organic phase;
Need to explain and illustrate, the object adding suitable quantity of water in testing process controls the H in solution +concentration range is about 0.8 ± 0.4mol/L, because if acidity is too low in reaction system, complex reaction rate also can be lower, thus extend the reaction time, if acidity is too high in reaction system, then the extraction quantity of methylene blue originally in extraction solvent ethylene dichloride strengthens, thus affects testing result, thus needs in reaction system to add appropriate water to regulate H +concentration; In testing process, the addition of chromophoric solution is then to meet methylene blue and fluoboric acid root anionic reactive aequum, thus can regulate according to actual sample situation;
(4) compare with boron standard color range colorimetric solution or boron standard color range colorimetric card according to the color of organic phase in step (3), thus the roughly content range of acquisition water base adhesive testing sample mesoboric acid.
Adopt said method, the boric acid content that the high speed that inventor produces Beijing Chemical Co., Ltd. used in production of cigarettes line process connects in mouth glue sample (in water base adhesive a type) detects, pass through colorimetric, testing result shows (as shown in Figure 3), the content of the boric acid in this sample between 10 ~ 50mg/g, but is more partial to 50mg/g.
For checking the reliability of this result, adopt ICPMS calibration curve method to detect to this water base adhesive sample, testing result shows that the boric acid actual content in this sample is 32mg/g.
The above results shows, detection method provided by the present invention is accurately with reliably for the semi-quantitative results of water base adhesive sample mesoboric acid content, consider its simplicity, low cost feature simultaneously, because of but be suitable for actual Test Field use, thus there is good using value.
embodiment 3
The present embodiment adopts and embodiment 2 same procedure, and the boric acid content in a kind of high speed overlapping glue (type of the water base adhesive) sample produce Beijing Chemical Co., Ltd. used in production of cigarettes detects.After reaction terminates, Colorimetric results shows (as shown in Figure 4), and the boric acid content in this sample, at detection limit about 1mg/g, tends to lower than detection limit 1mg/g.
Same employing ICPMS calibration curve method has carried out detecting quantitatively to the boric acid content in sample, and result shows, the boric acid content in this sample is 5 μ g/g.
The above results shows again, and detection method provided by the present invention is comparatively accurately with reliably, is also consistent with existing testing result.

Claims (3)

1. measure a reaction, extraction colorimetric device for water base adhesive mesoboric acid content, it is characterized in that, this device comprise liquid-liquid extraction box body, with the chromogenic reaction container be connected bottom liquid-liquid extraction box body and the color comparison tube be connected with chromogenic reaction container lower end; Described chromogenic reaction container is funnel-form.
2. measure the reaction, extraction colorimetric device of water base adhesive mesoboric acid content as claimed in claim 1, it is characterized in that, liquid-liquid extraction box body top is provided with lid; Chromogenic reaction container is fixedly connected with or movable connection method with adopting bottom liquid-liquid extraction box body, and color comparison tube adopts with chromogenic reaction container lower end and is fixedly connected with or movable connection method.
3. measure the reaction, extraction colorimetric device of water base adhesive mesoboric acid content as claimed in claim 1, it is characterized in that, this device material is polypropylene material, and wherein the capacity of chromogenic reaction container is 50mL, the capacity of liquid-liquid extraction box body is 50mL, and the capacity of color comparison tube is 5mL.
CN201520177268.2U 2015-03-27 2015-03-27 Measure the reaction, extraction colorimetric device of water base adhesive mesoboric acid content Active CN204495726U (en)

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Address after: 450000 Yulin South Road, Henan, Zheng Dong, No. 16 South Road, Zhengzhou

Patentee after: China Tobacco Henan Industrial Co., Ltd.

Address before: 450000 Zhengzhou agricultural road, Henan, No. 29

Patentee before: China Tobacco Henan Industrial Co., Ltd.