CN109459340A - A kind of aqueous absorption medicine flash baking on-Line Monitor Device - Google Patents

Abstract

The invention discloses a kind of aqueous absorption medicine flash baking on-Line Monitor Devices, include work station, tension sensor, baking oven, connecting rod, luggage carrier, sample disc.Tension sensor is fixed in the dust cover on baking oven top, and quality signal passes to work station.Inside from baking oven, it is connected above connecting rod with tension sensor, is connected below with luggage carrier.When test, sample be packed into reticulated samples disk, be put into the cavity ring of luggage carrier and dry, when Mass lost arrive threshold value when work station alarm, taking-up sample disc.Not only drying rate is fast by the present invention, and avoids the volatilization of the nitroglycerine in sample, improves the accuracy and safety of detection.

Description

A kind of aqueous absorption medicine flash baking on-Line Monitor Device

Technical field

The invention belongs to explosive wastewater Physico-chemical tests fields, are mainly used in online prison when aqueous absorption medicine flash baking It surveys, is determined by tracking quality variation and stop heating time, the nitroglycerine in sample will not be made to volatilize or decompose, guarantee inspection The accuracy of result is surveyed, the security risk of test process is excluded.

Technical background

It absorbs medicine and refers to the substance made of nitrocellulose (NC) absorption nitroglycerine (NG).

The NG that Nobel in 1888 absorbs 40% with 60% NC should be traced back to first, biradical bolus has been made, then use Calender used in rubber industry rolled in flakes at that time, was then cut into certain shapes and size, became double-base propellant for sending out Penetrate shell.This technique was transformed later, and explosive and non-explosivity substance is added in formula in order to improve performance, It continues up so far.

NC and NG is the main component of double-base powder.NC is high molecular polymer, its plasticizing must be by means of low molecule Solution, NG are the low molecule solution plasticizer of NC.The addition of NG increases the intermolecular distance of NC, improves its strand Flexibility and the intermolecular Van der Waals force of reduction, make it dissolve plasticizing, become the concentrated solution of polymer.This solution improves glass Glass temperature and flow temperature are conducive to machine-shaping under certain external force.

Arms attached explosive wastewater product is all the mixture being made of various ingredients.Consider for safety, economy, Each war production enterprise will not produce all raw material, wherein many substances are obtained by buying.Usually it is biradical, change it is biradical, Triple-base propellant or propellant manufacturing enterprise require to purchase absorption medicine.

NC and NG is explosibility substance.NC is the fibre solid object of cotton shape, the pole under friction condition dry NC Easy static electrification assembles negative electrical charge, at this point, high to shock, friction, heat and electric spark sensitivity.Dry NC easily catches fire, combustion It burns and generates bulk gas, while releasing big calorimetric, therefore NC requires that water is added in storage and transport.NG is colourless or yellowish Color liquid, 145 DEG C of boiling point (decomposition), friction sensitivity 100% is very sensitive to impact, showing tremendous enthusiasm Huadu, cannot individually transport.

Absorb the classical manufacturing process of medicine are as follows: NC suspends in a dispersion medium, makes each group by the methods of spraying, stirring Divide and macroscopically uniformly mix in accurate measurement, and be firmly combined, this process is known as absorbing.

Contain 90% or so moisture in the medicine slurry of good absorbing.Moisture in medicine slurry can be divided into free water, physical bond water and Materialization combination water.Free water refers to be not bound between spice, is suspended in surface layer after spice sedimentation, can be with simple method It filters.Physical bond water refers to the moisture infiltrated in medicine slurry hole or capillary, this part water just can be big under certain extruding Part squeezes out.Materialization combination water refers to the absorption water combined by hydrogen bond or other molecular separating force.Expelling water process make free water, Most of water drive of physical bond water is removed.A general expelling water machine drives away the moisture in medicine slurry to 20%~40%.At this time Medicine slurry can be used as absorb medicine product transported.The enterprise for absorbing medicine is purchased, medicine will be absorbed as production propellant powder or is pushed away Into one of the raw material of agent, need to measure the moisture absorbed in medicine, calculating according to absorption medicine siccative needs other components to be added Quality, after all components are mixed, can just produce it is biradical, change biradical, triple-base propellant or propellant product.

Aqueous absorption medicine uses oven method measuring moisture content, since NG has low volatility, so oven temperature controls At 55 DEG C, and it cannot use and vacuumize baking oven.Detection process are as follows: by whole material multiple sample quarterlies about 500g, then It is 3mm and 2mm double deck screen that quick rubbing, which crosses sieve pore,；2mm oversize about 10g is taken, is put into aluminium box or glass culture dish, in sample Litmus blue test paper is put above product (to examine the chemical stability of drying sample: test paper color is observed at regular intervals, if test paper Color reddens, and illustrates that NG starts to decompose at this time, should immediately take out sample out of baking oven), it is put into 55 DEG C of baking ovens and dries 5 hours, Taking-up lets cool weighing.

Litmus paper metachromatic principle: NG decomposition produces-NO₂, in conjunction with aqueous vapor after in acidity, litmus blue test paper meet acid Become red.

In aqueous absorption medicine, NG is close with NC structure, is tightly combined, and forms small " micelle " one by one.The knot of water and NC Close it is relatively weak, so water is in the outside of " micelle ".Water in sample, which is heated, to volatilize, gradually decreases, and " micelle " gradually exposes Come, continue to heat at this time, NG can be made to start to volatilize or decompose.

It can be seen that test paper discoloration illustrates that NG is decomposed in sample.But the volatility of NG is greater than decomposability at same temperature, i.e., When detecting that NG is decomposed, there is considerable degree of NG to be volatilized out sample, the reduction of NG can make water content detection value higher.It is another Aspect, NG volatilization gas are mixed with the air in baking oven, are equivalent to fuel-air explosive, and baking oven charges, so security risk It is larger.

Furthermore aluminium box or glass culture dish fill aqueous absorption medicine 10g, and sample layer is thicker, and steam can only be waved from upper surface Hair forms " crust layer " after the sample drying of upper surface, stops the drying of moisture in bottom sample, water content detection value can be made inclined It is low.On the other hand, the NG in " crust layer " is in the case where no moisture wraps up, heated to start to volatilize and decompose, not only have compared with Big security risk can also make water content detection result higher.Therefore it needs during the drying process, to open oven door, claimed with stainless steel Measuring spoon " stirring " sample destroys " crust layer ".But this operation is less reproducible, cannot be intuitive: or " stirring " is not enough also It does not volatilize compared with juicy or moisture has been evaporated completely and has not taken out sample in time but, caused heating that NG is caused to volatilize.

Have the shortcomings that in a word with the moisture content that Oven Method detects aqueous absorption medicine following:

(1) drying efficiency is low, and detection time is long；

(2) accuracy is poor；

(3) there is security risk.

Therefore Oven Method is improved to " Oven Method+Karl_Fischer method ": sample, which is only dried at 55 DEG C 3 hours, just to be taken out (at this time In sample also contain about 4% moisture), let cool, weigh, calculate drying after reduction moisture；Then the sample of the baking is set In in 100mL volumetric flask, extractant constant volume is added, shakes frequently about 0.5 hour, makes in sample water transport into extractant, Standing makes to extract solution clarification, and accurate 5mL sample of drawing extracts solution, detects moisture with Karl_Fischer method.By each sample Weighing method is added as the sample moisture content test value with Karl_Fischer method water content detection value.

" Oven Method+Karl_Fischer method " although avoiding the volatilization of NG, safety and accuracy are improved, and there are following two A disadvantage:

(1) detection cycle is long；

(2) operating procedure is more；

(3) Karl_Fischer method is increased, testing staff is required to improve；

(4) Karl_Fischer method produces more spent organic solvent.

Summary of the invention

It the shortcomings that in order to correct two Geju City detection methods (Oven Method, " Oven Method+Karl_Fischer method "), has invented one kind and has contained Water absorbs medicine flash baking on-Line Monitor Device.

A kind of aqueous absorptions medicine flash baking on-Line Monitor Device, include work station, tension sensor, baking oven, connecting rod, Luggage carrier, sample disc.It is characterized by: tension sensor is fixed on the dust cover that length × width × height is 500 × 500 × 300mm Interior, dust cover bottom four corners install the stabilizer blade of 4 high 20mm, diameter 20mm；Dust cover is placed on baking oven top, and bottom surface center is cut One weighing hole；The preformed hole that thermometer was originally put in center at the top of baking oven is opened, the weighing hole face preformed hole of dust cover is made, Weighing hole is identical with reserved bore dia；Between dust cover and baking oven, there is the protection sleeve pipe of a high 20mm by weighing hole and pre- It boxes out connected, the diameter of protection sleeve pipe is 10mm bigger than weighing hole；The quality signal transmission that tension sensor detects is to work station； Connecting rod is made of upper hook, heat insulation, bottom dog；Heat insulation is the cylindrical body of 130~150mm of height, upper hook and bottom dog Construct similar, total length is 40~50mm, and the length of screw wimble fraction is 10~20mm；Respectively by upper hook and bottom The gimlet of hook is screwed into inside heat insulation upper end and inside lower end, is assembled into connecting rod；Inside from baking oven, by the upper extension of connecting rod Hook passes through preformed hole and weighing hole, is connected with tension sensor, and the gap between heat insulation and reserved hole wall is 1~2mm；Loading Frame is made of fixed ring, connection chain, guard bar and cavity ring；Cavity ring outer diameter 110mm, internal diameter 80mm, hollow area are welded with two The fixed wire of root right-angled intersection, 3 guard bars holded up upwards of the equidistant welding in cavity ring outer, 3 guard bar height are 50mm, The connection chain of 80mm long is respectively welded in upper end, and 3 connection chains, which are topmost got together, to be welded in the fixed ring of outer diameter 10mm；Gu Determine ring to be suspended on the bottom dog of connecting rod；Sample disc is that 1mm sieve is made by sieve pore, and chassis diameter is 90mm, and outer wall height is The intersection of 40mm, chassis and outer wall is retainer plate, and outer wall is topmost guard ring.When test, sample disc in advance 55 DEG C dry, Cooling, weighing, obtains original quality；Work station is opened, sets oven temperature as 55 DEG C；It, will after oven temperature reaches 55 DEG C The aqueous rapid rubbing of medicine that absorbs crosses the double deck screen that sieve pore is 3mm and 2mm, and the oversize 10g for taking 2mm to sieve is accurate to 0.0001g, Loose tiling is put into sample disc, is put into cavity ring together, is shut oven door, is started monitoring after ten minutes and is absorbed medicine and sample The quality resultant of disk, every 10 minutes 1 inferior quality values of record；Quality resultant can continue to reduce, in quality resultant 0.5 hour The absolute value of reduction amount is alarmed no more than 0.01g work station, is taken out from baking oven containing the sample disc for absorbing medicine.

In the present invention, dries and taken out the sample disc containing medicine is absorbed, be put into drier after being cooled to room temperature and weigh, subtract sample The original quality of product disk obtains drying the quality for absorbing medicine, and according to the quality for absorbing medicine before drying, it is aqueous to calculate absorption medicine Amount.

In the present invention, upper hook, bottom dog, fixed ring, guard bar, retainer plate, material used in guard ring are 316 stainless steel wires, directly Diameter is about 2~3mm；Material used in connection chain is 316 stainless steels, the chain being made of the thick steel wire of 1mm；Dust cover, cavity ring Material used is 316 stainless steel plates, and thickness is about 2mm；Stabilizer blade, protection sleeve pipe, material used in heat insulation are polytetrafluoroethylene (PTFE).

The invention has the following advantages that

(1) detection time is shortened this is because reticulated samples disk, increases the moisture evaporation face 2 times or more in sample.

(2) detection accuracy is improved this is because taking out sample before NG volatilization, guarantee will not by on-line monitoring Because the loss of NG influences water content detection result；It dries water efficiency to improve, the moisture in sample can dry completely.

(3) operating procedure it is few, it is easy to operate this is because without Karl_Fischer method survey moisture the step of, operation threshold it is low, The universality of method is strong.

(4) volatilization of the safety due to avoiding NG is improved, security risk is eliminated.

(5) environmentally protective not generate spent organic solvent.

Detailed description of the invention

Fig. 1 is aqueous absorption medicine flash baking on-Line Monitor Device schematic diagram.1. work station in figure, 2. dust covers, 3. dry Case, 4. stabilizer blades, 5. protection sleeve pipes, 6. connecting rods, 7. luggage carriers.

Fig. 2 is the component diagram of connecting rod.8. upper hook in figure, 9. heat insulation sections, 10. bottom dogs.

Fig. 3 is assembled connecting rod.

Fig. 4 is luggage carrier schematic diagram.11. fixed ring in figure, 12. connection chains, 13. guard bars, 14. cavity rings.

Fig. 5 is cavity ring top view.13 guard bar in figure, 15. fixed wires.

Fig. 6 is sample disc perspective view.16. retainer plate in figure, 17. guard rings.

Fig. 7 is certain batch of aqueous medicine sample that absorbs with the quality-monitoring value of heating time.

Specific embodiment

With reference to the accompanying drawing and preferred embodiment the present invention is described in further detail.

Embodiment 1

1. design principle

Quasi- aqueous absorption in S type pulling force bridge-type resistance strain type sensor (abbreviation tension sensor) real-time monitoring baking oven The mass change of medicine sample stops heating when the drying of sample moisture in time.The volatilization that NG in medicine is absorbed due to avoiding, disappears The influence to testing result is lost in addition to security risk and NG.

It is accurate with testing result, detection is time-consuming short for target, specific design principle is as follows:

(1) safeguard measure appropriate should be fixed and be had to tension sensor, be not easy exposed be placed on baking oven top.

(2) calibration and calibrating of tension sensor are completed at normal temperature, and baking oven heat should not be transmitted to pull sensing Device is equivalent to tension sensor and still weighs at normal temperature.

(3) after sample drying, device should be able to pass through warning note testing crew.

(4) vessel for absorbing medicine sample are held, sample can be allowed to have more moisture evaporation face, while also to guarantee sample Not during the drying process to scaling-off in baking oven.

(5) component of load-bearing, material should have certain intensity.

(6) sample disc floor space is sufficiently large；Sample disc is matched with luggage carrier, should be easily put into luggage carrier.

2. specific invention detail

(1) tension sensor is fixed in dust cover, and dust cover is placed on baking oven top.

(2) 4 solid cylinder polytetrafluoroethylene (PTFE) stabilizer blades are installed in dust cover bottom；The upper hook and bottom dog of connecting rod exist It is not attached to inside heat insulation, the gap between heat insulation and reserved hole wall is 1~2mm, and most of heat in baking oven is prevented to pass To sensor.A small amount of heat can be passed in dust cover by the gap of heat insulation and preformed hole in baking oven, these heats can quilt The cold air dilution of surrounding, influences the weighing of sensor little.

(3) alarm threshold value is set in work station, (quality started subtracts quality reduced value within 0.5 hour in 0.5 hour 0.5 hour quality) be less than threshold value when, work station instruction alarm, prompt testing crew.

(4) size of medicine is absorbed between 2~3mm, therefore sample disc is designed to mesh-like, screen size 1mm, so both It can guarantee that moisture evaporation face is big, while sample will not scaling-off influence accuracy.

(5) supporting part all uses 316 stainless steels.

(6) sample disk diameter 90mm, height 40mm, for laboratory baking test level, sample disc floor space is sufficiently large. Luggage carrier cavity ring outer diameter 110mm, thimble outer it is equidistant welding 3 height holded up upwards be 50mm guard bar (calculating can Know that guard bar spacing is 95mm).Such design has achieved the purpose that sample disc can be easily put into the cavity ring of luggage carrier.

3. a kind of aqueous absorption medicine flash baking on-Line Monitor Device introduction

A kind of aqueous absorption medicine flash baking on-Line Monitor Device includes work station 1, tension sensor, baking oven 3, connection Bar 6, luggage carrier 7, sample disc.According to Fig. 1, it is the dust-proof of 500 × 500 × 300mm that tension sensor, which is fixed on length × width × height, In cover 2,2 bottom four corners of dust cover install the stabilizer blade 4 of 4 high 20mm, diameter 20mm；Dust cover 2 is placed on the top of baking oven 3, bottom surface Center cuts a round weighing hole；The preformed hole for originally putting thermometer will be hit exactly at the top of baking oven 3 to open, and makes the title of dust cover 2 Metering-orifice face preformed hole, weighing hole are identical with reserved bore dia；Between dust cover 2 and baking oven 3, there is the protection of a high 20mm Weighing hole is connected by casing 5 with preformed hole, and the diameter of protection sleeve pipe 5 is 10mm bigger than weighing hole；The matter that tension sensor detects Amount signal is transferred to work station 1.According to fig. 2, connecting rod 6 is made of upper hook 8, heat insulation 9, bottom dog 10；Heat insulation 9 is height The cylindrical body of 130~150mm, upper hook 8 is similar with the construction of bottom dog 10, and total length is 40~50mm, screw tapering The length divided is 10~20mm.According to Fig. 3, the gimlet of upper hook 8 and bottom dog 10 is screwed into inside 9 upper end of heat insulation respectively Inside lower end, it is assembled into connecting rod 6；From 3 the inside of baking oven, the upper hook 8 of connecting rod 6 is passed through into preformed hole and weighing hole, with Tension sensor is connected, and the gap between heat insulation 9 and reserved hole wall is 1~2mm.According to Fig. 4, luggage carrier 7 by fixed ring 11, Connection chain 12, guard bar 13 and cavity ring 14 form.According to Fig. 5,14 outer diameter 110mm of cavity ring, internal diameter 80mm, hollow area welding There is the fixed wire 15 of two right-angled intersections；Equidistant welding 3 guard bars holded up upwards, 13,3 guard bars 13 in 14 outer of cavity ring Height is 50mm, and 12,3 12 the tops of connection chain of connection chain that 80mm long is respectively welded in upper end, which are got together, is welded to outer diameter In the fixed ring 11 of 10mm.Fixed ring 11 is suspended on the bottom dog 10 of connecting rod 6.According to Fig. 6, sample disc is 1mm sieve by sieve pore It is made, chassis diameter is 90mm, and outer wall height is 40mm, and the intersection of chassis and outer wall is retainer plate 16, and outer wall is topmost Guard ring 17.

Upper hook 8, bottom dog 10, fixed ring 11, guard bar 13, retainer plate 16, material used in guard ring 17 are 316 stainless steel wires, Diameter is about 2~3mm；Material used in connection chain 12 is 316 stainless steels, the chain being made of the thick steel wire of 1mm；Dust cover 2, sky Material used in thimble 14 is 316 stainless steel plates, and thickness is about 2mm；Stabilizer blade 4, protection sleeve pipe 5, material used in heat insulation 9 are poly- four Vinyl fluoride.

4. application method introduction

When test, sample disc in 55 DEG C of drying, cooling, weighing, obtains original quality in advance；Open work station 1, setting is dried 3 temperature of case is 55 DEG C；After 3 temperature of baking oven reaches 55 DEG C, it is the double of 3mm and 2mm that the aqueous absorption rapid rubbing of medicine, which is crossed sieve pore, Layer sieve, the oversize 10g for taking 2mm to sieve are accurate to 0.0001g, and loose tiling is put into sample disc, are put into cavity ring 14 together On, oven door is shut, starts the quality resultant that monitoring absorbs medicine and sample disc after ten minutes, every 10 minutes 1 inferior qualities of record Value；Quality resultant can continue reduce, by 0.5 hour in Mass lost amount absolute value be not more than 0.01g when work station alarm, It takes out from baking oven containing the sample disc for absorbing medicine, is put into drier after being cooled to room temperature and weighs, subtract the original matter of sample disc Amount obtains the quality that drying absorbs medicine, according to the quality for absorbing medicine before drying, calculates and absorbs medicine water content.

5. investigating apparatus of the present invention quality testing data

5.1 use 10g standard test weight to be investigated as sample

When baking oven is in 55 DEG C of constant temperature, using 10g standard test weight as sample, is monitored on-line with the present invention, recorded every 1 hour The quality of a counterweight is recorded, daily monitoring 14 hours, monitored 5 days altogether, data are shown in Table 1.

The apparatus of the present invention of table 1 monitor quality of the 10g standard test weight in 55 DEG C of constant temperature

1 data of table explanation:

(1) monitoring quality is 0.11%~0.12% more than actual mass, this is because the density of gas molecule is small at 55 DEG C At room temperature, so that gas reduces the buoyancy of counterweight, and terrestrial gravitation does not change, so weighing numerical value greatly at room temperature Numerical value (mass value of standard test weight is examined and determine in room temperature)；

(2) convection current of hot and cold air is smaller in baking oven, the influence very little of weighing device, so the repeatability of detection data Preferably, precision is high.

Can be speculated according to the above analysis result: apparatus of the present invention are after 55 DEG C are stablized, the monitoring mass ratio of sample to be tested Actual mass can be stable always more 0.1% or so.So if monitoring quality changes with the extension of heating time, just It is that sample itself quality is changed.

5.2 use 20g standard test weight to be investigated as sample

Using 20g standard test weight as sample, its quality is monitored with the present invention, in 55 DEG C of constant temperature, every 1 hour record 1 The monitoring quality of secondary counterweight is 20.0265 respectively, 20.0268,20.0270,20.0264,20.0270,20.0271, 20.0267,20.0265,20.0266,20.0270,20.0268,20.0269,20.0266,20.0267,20.0268g, it is average Quality is 20.0277g, RSD=0.001% (n=15).These data explanation:

(1) monitoring quality is 0.14% more than actual mass, this is because the density of gas molecule is small at room temperature at 55 DEG C, So that gas reduces the buoyancy of counterweight, and terrestrial gravitation does not change, so weighing the numerical value (standard of numerical value greatly at room temperature The mass value of counterweight is examined and determine in room temperature)；

(2) convection current of hot and cold air is smaller in baking oven, the influence very little of weighing device, so the repetition of detection data Property is preferable, precision is high.

It may be speculated that the monitoring quality of sample can be always about 0.14% more than real quality after baking oven heating.With the time Increase, if monitoring quality change, be that sample itself quality is changed, that is, monitor quality reduction, exactly inhale Medicine sample quality is received to reduce.

5.3 use 5g standard test weight to be investigated as sample

When baking oven is in 55 DEG C of constant temperature, using 5g counterweight as sample, every 1 hour record, 1 monitoring quality, respectively 5.0035、5.0035、5.0035、5.0035、5.0035、5.0035、5.0035、5.0035、5.0035、5.0034、5.0035、 5.0035,5.0035,5.0035,5.0035g, average quality 5.0035g, RSD=0.0004% (n=15).It can be seen that

(1) counterbalance mass is greater than actual mass about 0.07%, this is because the density of gas molecule subtracts after temperature increases Small, so that gas reduces the buoyancy of counterweight, and terrestrial gravitation does not change, so weighing the numerical value of numerical value greatly at room temperature (counterweight actual mass is demarcated in room temperature)；

(2) influence of the convection current weighing device of hot and cold air is smaller in baking oven, and the repeatability of detection data is preferable, accurate Degree is high.

Equally, can be speculated according to the above analysis result: apparatus of the present invention are after 55 DEG C are stablized, the monitoring matter of sample to be tested Measure can be stable always than actual mass more 0.1% or so.So if monitoring quality becomes with the extension of heating time Change, is exactly that sample itself quality is changed.

6. the determination of alarm threshold value

By in above-mentioned " 5 " 3 test as can be seen that apparatus of the present invention monitoring quality can characterize absorb medicine sample be heated after The variation of quality.It, should be in time by sample from baking oven for the volatilization for avoiding NG in sample after absorbing the moisture in medicine sample and volatilizing Middle taking-up.In order to remind testing crew, design monitoring station has warning function, i.e., when monitor value reaches threshold value, software is mentioned Show alarm.Therefore it needs to determine suitable alarm threshold value by actual monitoring result.

Sample disc is dried at 55 DEG C in advance, is put into present apparatus baking oven (in 55 DEG C of constant temperature), is monitored after ten minutes Value.Weighing plate is taken out, let cool, is weighed, ready aqueous absorption medicine 10.0235g is put into, is then put into togerther in the present apparatus (55 DEG C of constant temperature) starts to monitor quality after ten minutes, then every the quality resultant of 10 minutes records samples and weighing plate. The detected value of weighing plate is subtracted from the quality resultant of each time point, just obtains the quality of the sample of each time point.With sample Quality is ordinate, the time is that abscissa makees Fig. 7.

From figure 7 it can be seen that the weighing value 0.11% of the monitoring initial value of sample greatly at room temperature, when then as heating Between extension, quality-monitoring value starts to be decreased obviously, and stops decline when by 130 minutes.When illustrating to be heated to 130 minutes, moisture Volatilize completely.

From Fig. 7 it can also be seen that continuing after being heated to 180 minutes, sample monitoring mass figures start to become smaller again, this is Since NG starts caused loss of volatilizing.Illustrate if not stopping also within 180 minutes heating sample, the NG in sample can volatilize into Enter in the small space of baking oven, increases risk.

In Fig. 7: heating time, the quality of sample was reduced to 7.9421g from 8.1183g from 100 minutes to 130 minute, Reduction amount is 0.1762g；Heating time, the quality of sample was reduced to 7.9412g from 7.9421g from 130 minutes to 160 minute, Reduction amount is 0.009g；From 160 minutes to 190 minute, the quality of sample is reduced to 7.8798g from 7.9412g, and reduction amount is 0.0614g.Primarily determine alarm threshold value are as follows: quality reduction amount is not more than 0.01g alarm in 0.5 hour.

It resamples and uses present apparatus flash baking, take out sample in time when Mass lost amount is less than (in 0.5 hour) 0.01g Product cool in drier to room temperature, are subsequently placed in 100mL volumetric flask, and extractant constant volume is added, shakes about 0.5hr frequently, Make in sample water transport into extractant, standing makes to extract solution clarification, and accurate 5mL sample of drawing extracts solution, uses karr It is 0.1% that Fei Xiufa, which detects water content in A,.Illustrate that (quality before 0.5 hour subtracts 0.5 using quality reduction amount in 0.5 hour Quality after hour) it is not more than 0.01g as threshold value, stop heating sample at this time, can guarantee that the moisture in sample dries completely It is dry, and NG will not volatilize in sample.

7 the method for the present invention are compared with old detection method

The comparison of 7.1 detection times

There are two the aqueous old detection methods for absorbing medicine moisture content: Oven Method and " Oven Method+Karl_Fischer method ".This hair It is bright because of 2 reasons, detection time is significantly faster than 2 aging methods: first is that using the weighing plate in sieve face, moisture evaporation face being increased Big 2 times or more；Second is that on-line monitoring, stops heating when moisture evaporation is complete in time.

The drying time of 3 methods be relatively shown in Table 2 (preparation of samples all be that crossing sieve method rubs, the time used is identical, It therefore does not include time when 3 methods compare).

Drying time used in 2 three kinds of furnace drying methods of table

As can be seen from Table 2, the method for the present invention detection time is far smaller than 2 aging methods.

7.2 the method for the present invention are compared with old detection method testing result accuracy

It is 2~3mm double deck screen that certain batch of quick rubbing of aqueous absorption medicine, which is crossed sieve pore, takes 2mm oversize about 50g, uses respectively The method of the present invention, Oven Method and " Oven Method+Karl_Fischer method " detect moisture content.

The method of the present invention detection: it weighs 10.1056g and is put into drier with present invention drying moisture, after being cooled to room temperature It weighs and (is labeled as A), calculating water content is 23.5%.Then A is placed in 100mL volumetric flask, extractant constant volume is added, frequently Shaking about 0.5 hour makes in sample water transport into extractant, and standing 0.5 hour makes to extract solution clarification, accurate to draw 5mL sample extracts solution, is 0.1% with water content in Karl_Fischer method detection A, illustrates that aqueous absorption medicine can be complete with the present invention Full drying.

Oven Method detection: weighing 10.1123g in glass culture dish, is put into 55 DEG C of baking ovens and dries 5 hours (for observation The influence of " crust layer " to water content detection value, unused metal sample spoon stirred sample in drying course), taking-up is put into drier In, it is weighed after cooling and (is labeled as B), calculating water content is 22.7%.Then B is placed in 100mL volumetric flask, extractant is added Constant volume shakes about 0.5 hour frequently, makes in sample water transport into extractant, and standing makes to extract solution clarification, accurate to draw 5mL sample extracts solution, is 2.3% with water content in Karl_Fischer method detection B.Illustrate the medicinal Oven Method drying of aqueous absorption Afterwards, also remaining has 2.3% water in sample.In addition, 22.7%+2.3%=25.0%, 23.5% surveyed greater than the present invention, Illustrate that NG has a small amount of volatilization.When due to this method practical application, residual moisture no longer is detected with karl Fischer, so water content detection As a result quoting value is exactly 22.7%.For other 2 methods, Oven Method testing result accuracy is lower.Furthermore due to This method has a small amount of NG to volatilize when detecting, and baking oven charges, and has some potential safety problems.If using metal sample in drying course Spoon stirred sample destroy " crust layer ", will increase moisture and volatilize face, can preferably dry moisture completely, but due to cannot and When take out sample in moisture drying, also resulted in a small amount of NG volatilization, security risk can not rule out.The reduction amount of NG at this time It can be incorporated in the reduction amount of moisture, testing result can be made higher.

" Oven Method+Karl_Fischer method " detection: 10.0517g is weighed in glass culture dish, is put into 55 DEG C of baking ovens and dries 3 hours, taking-up was put into drier, is weighed after cooling and (is labeled as C), and calculating water content is 20.1%.Then C is placed in In 100mL volumetric flask, extractant constant volume is added, shakes frequently about 0.5 hour, keeps water transport in sample quiet into extractant Setting makes to extract solution clarification, and accurate 5mL sample of drawing extracts solution, is 3.6% with water content in Karl_Fischer method detection C.It should The water content detection that method is finally quoted is the result is that 20.1%+3.6%=23.7%.Since this method drying time is shorter, avoid The volatilization of NG, so with the aqueous moisture content for absorbing medicine of " Oven Method+Karl_Fischer method " detection, accuracy is higher.

From the above test results, it can be seen that the present invention can to avoid the volatilization of NG, and due to volatilization face increase, do not generate " hard shell " stops the volatilization of internal moisture, therefore testing result accuracy of the invention is high.The accuracy of the method for the present invention is higher than Oven Method is suitable with " Oven Method+Karl_Fischer method " accuracy.

8 summarize

From the test of the above standard test weight as can be seen that apparatus of the present invention are in 55 DEG C of constant temperature, since molecule subtracts in hot-air It is few, the buoyancy of counterweight is reduced, and terrestrial gravitation does not change, so the numerical value of numerical value greatly at room temperature is weighed, the matter exceeded Amount is about the 0.1% of proper mass.The influence of the convection current weighing result of hot and cold air is smaller in baking oven, and detection data is stable, again Renaturation is good.When being specifically used for the aqueous drying monitoring for absorbing medicine, it can determine that sample stops heating by mass change inflection point Time.

Due to drying the moisture in aqueous absorption medicine with the method for the present invention, it can be avoided the volatilization of NG, be also avoided that drying " hard shell " formed is to the obstruction of internal moisture, the accuracy height of institute's testing result in the process of the present invention.The present apparatus is due to avoiding The volatilization of NG, eliminates security risk, increases intrinsic safety.Invention increases moisture evaporation faces, so moisture is waved Dry speed significantly improves.

In short, the method for the present invention and device can improve the accuracy in detection of moisture content and the peace of detection in aqueous absorption medicine Quan Xing, and substantially reduce detection time.

Claims (3)

1. a kind of aqueous absorption medicine flash baking on-Line Monitor Device comprising work station [1], tension sensor, baking oven [3], connects Extension bar [6], luggage carrier [7], sample disc.It is characterized by: tension sensor be fixed on length × width × height be 500 × 500 × In the dust cover [2] of 300mm, dust cover [2] bottom four corners install the stabilizer blade [4] of 4 high 20mm, diameter 20mm；Dust cover [2] It is placed on baking oven [3] top, bottom surface center cuts a round weighing hole；The pre- of thermometer is originally put into center at the top of baking oven [3] It boxes out opening, makes the weighing hole face preformed hole of dust cover [2], weighing hole is identical with reserved bore dia；In dust cover [2] and dry Between case [3], there is the protection sleeve pipe [5] of a high 20mm that weighing hole is connected with preformed hole, the diameter of protection sleeve pipe [5] is than claiming The big 10mm of metering-orifice；The quality signal transmission that tension sensor detects is to work station [1]；Connecting rod [6] by upper hook [8], every Heat block [9], bottom dog [10] composition；Heat insulation [9] is the cylindrical body of 130~150mm of height, upper hook [8] and bottom dog [10] Construct similar, total length is 40~50mm, and the length of screw wimble fraction is 10~20mm；Respectively by upper hook [8] It is screwed into inside heat insulation [9] upper end and inside lower end with the gimlet of bottom dog [10], is assembled into connecting rod [6]；It is inner from baking oven [3] Face, by the upper hook [8] of connecting rod [6] pass through preformed hole and weighing hole, be connected with tension sensor, heat insulation [9] with reserve Gap between hole wall is 1~2mm；Luggage carrier [7] is by fixed ring [11], connection chain [12], guard bar [13] and cavity ring [14] Composition；Cavity ring [14] outer diameter 110mm, internal diameter 80mm, hollow area is welded with the fixed wire [15] of two right-angled intersections, hollow 3 guard bars [13] holded up upwards of the equidistant welding in ring [14] outer, 3 guard bars [13] are highly 50mm, and upper end is welded respectively The connection chain [12] of 80mm long is connect, 3 connection chains [12], which are topmost got together, to be welded in the fixed ring [11] of outer diameter 10mm； Fixed ring [11] is suspended on the bottom dog [10] of connecting rod [6]；Sample disc is that 1mm sieve is made by sieve pore, and chassis diameter is 90mm, Outer wall height is 40mm, and the intersection of chassis and outer wall is retainer plate [16], and outer wall is topmost guard ring [17].When test, sample Product disk in 55 DEG C of drying, cooling, weighing, obtains original quality in advance；It opens work station [1], sets baking oven [3] temperature as 55 ℃；After baking oven [3] temperature reaches 55 DEG C, the aqueous absorption rapid rubbing of medicine is crossed into the double deck screen that sieve pore is 3mm and 2mm, takes 2mm The oversize 10g of sieve, is accurate to 0.0001g, and loose tiling is put into sample disc, is put on cavity ring [14] together, shuts baking Chamber door starts the quality resultant that monitoring absorbs medicine and sample disc, every 10 minutes 1 inferior quality values of record after ten minutes；Quality is closed Amount can continue reduce, by 0.5 hour in reduction amount absolute value be not more than 0.01g when work station alarm, taken out from baking oven Containing the sample disc for absorbing medicine.

2. the aqueous absorption medicine flash baking on-Line Monitor Device of one kind according to claim 1, it is characterised in that: dried and taken Out containing the sample disc for absorbing medicine, it is put into drier after being cooled to room temperature and weighs, subtract the original quality of sample disc, dried The quality for absorbing medicine calculates according to the quality for absorbing medicine before drying and absorbs medicine water content.

3. the aqueous absorption medicine flash baking on-Line Monitor Device of one kind according to claim 1, it is characterised in that: upper hook [8], bottom dog [10], fixed ring [11], guard bar [13], retainer plate [16], material used in guard ring [17] are 316 stainless steel wires, directly Diameter is about 2~3mm；Material used in connection chain [12] is 316 stainless steels, the chain being made of the thick steel wire of 1mm；Dust cover [2], Material used in cavity ring [14] is 316 stainless steel plates, and thickness is about 2mm；Stabilizer blade [4], protection sleeve pipe [5], heat insulation [9] are used Material is polytetrafluoroethylene (PTFE).