CN102393466B - Primary amino radical tester - Google Patents
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- CN102393466B CN102393466B CN201110249480.1A CN201110249480A CN102393466B CN 102393466 B CN102393466 B CN 102393466B CN 201110249480 A CN201110249480 A CN 201110249480A CN 102393466 B CN102393466 B CN 102393466B
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Abstract
The invention discloses a primary amino radical tester, which is obtained by improving a paradigm amino acid tester, is mainly used for measuring the primary amino radical content of proteins, and is popularized and application to the measurement of the primary amino radical content of various organic compounds. The tester mainly comprises a reaction part, a gas measuring part, a gas washing part and a recovering part, and has the characteristics of rapidness, accuracy, cleanliness and the like.
Description
Technical field:
The invention belongs to chemical analysis test instrument and equipment field, relate to a kind of protein primary amino radical content instrument---primary amino radical tester of (comprising collagen polypeptide, each seed amino acid) that is mainly used in measuring.
Background technology:
At present for measuring the method for protein primary amino radical group content, there are ninhydrin colorimetry, TNBS colourimetry, Micellar Electrokinetic Chromatography, formaldehyde method, Van Slyke's method, vapor-phase chromatography.Wherein, triketohydrindene hydrate colorimetric and TNBS colorimetric belong to spectrophotometric method, all have instrument error.In addition, in ninhydrin colorimetry, after the time length of heating colour developing and colour developing, the depth of color all can cause error; TNBS colourimetry selectivity is very strong, and main and lysine epsilon-amino reacts, can not quantitatively whole primary amino radicals.In formaldehyde method, also there is further the subsidiary reaction with primary amino radical condensation in methylol compound, affects accuracy of measurement.In addition, formaldehyde, due in depositing process, is easily subject to the impact generation oxidation of external environment to become formic acid, and in titration process, formic acid can additionally consume NaOH, thereby makes measurement result higher.For example, though chromatography so has high sensitivity, but instrument and equipment is had relatively high expectations: in vapor-phase chromatography, required stainless steel reaction device processing request is high and involve great expense.In Van Slyke's method use procedure measuring period long, experimental implementation is complicated, it is larger that experiment is affected by ambient temperature.
Existing normal form amino acid determining instrument, is mainly comprised of reaction unit, amount device of air and air-washer three parts.Wherein reaction unit and air-washer are respectively integral structure, to cleaning, bring much inconvenience.Former normal form amino acid determining instrument needs special-purpose support to be fixed, and takes up room large.Test is subject to surrounding environment influence larger, under low temperature, can not measure.Normal form amino acid determining instrument is not unified to process to waste gas, waste liquid, and environmental pollution is serious.
Summary of the invention:
For the deficiencies in the prior art, the object of this invention is to provide a kind of primary amino radical acidity test instrument with and using method.
The present invention be take Van Slyke's method as principle, on the basis of normal form amino acid determining instrument, designs a kind of quick, simple, accurate, clean primary amino radical tester.The reactive moieties of analyzer (I) includes magneton (9), and with water-bath chuck (4) and magnetic agitation (10), reactor (1) bottom is flat design.The gas washing part (III) of analyzer includes magneton (29), is furnished with magnetic agitation (30), and gas washing hemisphere (27) bottom is flat design.This device can be used for the measurement of primary amino radical group in protein, gelatin and micro-amino acid.
A kind of primary amino radical tester, by reaction unit (I), amount device of air (II), air-washer (III), retracting device (IV), formed, it is characterized in that, reaction unit (I), amount device of air (II), air-washer (III), retracting device (IV) connect successively, and exhausr port and the leakage fluid dram of reaction unit (I), amount device of air (II), air-washer (III) are all connected in recovery section (IV).
Preferably, described reaction unit (I) comprises reactor (1), charge pipe (2) and three-limb tube (14).Preferably, three-limb tube (14) is with cock (15), and cock (15) is positioned at three-limb tube (14) intersection, the trend for adjustments of gas in three-limb tube (14).
Preferably, described reactor (1) top is ground (12), and bottom is flat, with water-bath chuck (4), as shown in Figure 1.Thin neck glass tube (7) and a downward drainage conduit (11) upwards arranged at reactor (1) bottom; One end of thin neck glass tube (7) connects charge pipe (2), and the other end is connected through chuck (4) and reactor wall (5); Drainage conduit (11) is connected through chuck (4) and reactor wall (5), for the discharge of reactor (1).Preferably, on reactor jacket (4) outer wall, contain two interfaces (6), for communication loop water-bath.Preferably, reactor (1) contains magneton (9), the supporting magnetic agitation in bottom (10).
Preferably, described reaction unit (I) comprises two charge pipes---the first charge pipe (2) and the second charge pipe (3).Preferably, the first charge pipe (2) and the second charge pipe (3) bottom are thin neck glass tube, and the first charge pipe (2) is 25～35ml, and the second charge pipe (3) is about 10～20ml.Reaction unit (I) comprises two thin neck glass tubes, and the first thin neck glass tube (7) and the second thin neck glass tube (8), connect respectively the first charge pipe (2) and the second charge pipe (3).
Preferably, three-limb tube (15) is connected with reactor top ground (12) by the grinding port plug (13) of thin neck glass tube one end, and the other end of three-limb tube (15) is connected with inclined hole stop,threeway (19) by thin neck bend pipe (17).
Air-washer (III) comprises gas washing hemisphere (27) and buffering ball (26); Gas washing hemisphere (27) and buffering ball (26) are connected with inclined hole stop,threeway (19) through thin neck glass connecting pipe (23).Preferably, gas washing hemisphere (27) radius is 100～150mm, and buffering ball (26) radius is 80～100mm.
Preferably, gas washing hemisphere (27) top connects thin neck glass tube (24), for gas, passes in and out; Bottom with a downward glass tube (25) for discharge opeing, and with one 90 ° upwards bend pipes (28) for connecting buffering ball (26).Gas washing hemisphere (27) is flat, includes magneton (29), supporting magnetic stirring apparatus (30).
Described retracting device (IV) comprises four-way connecting pipe (31) and returnable bottle (33).Preferably, returnable bottle (33) is furnished with the plug (36) containing two glass tubes (34), (35).
Reactor of the present invention (1) is furnished with water-bath chuck (4), bottom connects two charge pipes, the first charge pipe (2) and the second charge pipe (3), top ground (12) is connected with three-limb tube (14) by the grinding port plug (13) of thin neck glass tube one end, three-limb tube (14) other end is connected with inclined hole stop,threeway (19) by thin neck bend pipe (17), eudiometer tube (20) bottom connects level ball (21) (emulsion tube (22) length is 1.5 times of eudiometer tube (20)) by emulsion tube (22), eudiometer tube (20) top straight tube (18) connects gas washing hemisphere (27) by connecting pipe (23), 90 ° of gas washing hemisphere (27) the lower ends bend pipe (25) that makes progress connects buffering ball (26).Three-limb tube gas outlet (16), reactor discharging tube (11), gas washing hemisphere discharging tube (25) are all connected with four-way connecting pipe (31) by silicone tube (on the silicone tube of discharging tube (11), (25) mouthful with tongs), then are connected on retracting device (IV) by silicone tube (32).
The water-bath chuck (4) of reactor of the present invention (1) connects constant temperature water bath, in order to regulate temperature of reaction; Reactor (1) includes magneton (9), and bottom is furnished with magnetic agitation (10), can reaction speed by adjusting stirring rate.Gas washing hemisphere of the present invention (27) includes magneton (29), and bottom is furnished with magnetic agitation (30), by regulating stirring rate to regulate gas washing speed.
The present invention also provides the using method of described uncle's ammonia quantitative instrument, comprises the following steps:
Before use of the present invention, first carry out preliminary work, each interface of good seal, reactor discharging tube (11) and gas washing hemisphere discharging tube (25) clip with tongs.First from level ball (21), inject deionized water, eudiometer tube (20) is filled with after deionized water, turn eudiometer tube cock maintenance dose tracheae (20) is full of water state.Then by gas washing liquid (potassium permanganate 20～40g, NaOH 20～40g, deionized water 200～400ml), from surge flask (26), pour into, when filling with gas washing hemisphere (27) to eudiometer tube cock (19) and locating, turn eudiometer tube cock (19), makes eudiometer tube (20) communicate with three-limb tube (14).Improve level ball (21), eudiometer tube (20) is filled with to deionized water to three-limb tube cock (15) and locate.Turn three-limb tube cock (15), makes reactor (1) communicate with retracting device (IV) by three-limb tube gas outlet (11), and simultaneously turn eudiometer tube cock (19) is to horizontal direction, closing capacity tracheae.Level ball (21) is put in to lower, now in gas washing hemisphere (27) and eudiometer tube (20), is all full of liquid, and and isolate from outer air.Open circulator bath and magnetic agitation (10).
During test sample of the present invention, first from the first charge pipe (2), add approximately 20～30ml of glacial acetic acid, then add approximately 20～30ml of 40% sodium nitrite in aqueous solution, closed the first charge pipe (2) and the second charge pipe (3).In reactor (1), reaction generates NO or NO
2gas, keeps 5～8min, the interior air of emptying reactor (1).Turn three-limb tube cock (15), closed reactor (1).Open the first charge pipe (2) and the second charge pipe (3), in reactor (1), produce gas drives liquid out of from the first charge pipe (2) and the second charge pipe (3), after gas is driven out of completely in the thin neck of the first charge pipe (2) and the second charge pipe (3) bottom, closed the first charge pipe (2) and the second charge pipe (3).Turn three-limb tube cock (15) and eudiometer tube cock (19), only communicate reactor (1) with eudiometer tube (20), keep reactor (1) interior gas inlet tracheae (20).In the first charge pipe (2), fill with deionized water, fluid-tight.In the second charge pipe (3), add testing protein solution, slowly open charge pipe (3) cock, make the slow inflow reactor of liquid to be measured (1), and with a small amount of deionized water rinsing the second charge pipe (3), with n-amyl alcohol fluid-tight.Closed the second charge pipe (3) during reinforced end.In course of reaction, when gas surpasses eudiometer tube venturi portion in eudiometer tube (20), improve rapidly level ball (21), turn eudiometer tube cock (19), catches up with gas into gas washing hemisphere (27).After gas is caught up with only, turn eudiometer tube cock (19), closed gas washing hemisphere (27), makes eudiometer tube (20) communicate with reactor (1).Level ball (21) is put in to lower, continues to keep reactor (1) interior gas inlet tracheae (20).Reactor (1) stops reaction from adding liquid to be measured to start clock reaction 30min～60min.Open respectively the first charge pipe (2) and the second charge pipe (3), the first charge pipe (2) and the interior liquid of the second charge pipe (3) are entered in reactor (1).Catch up with after the interior gas of most reactor (1) turn eudiometer tube cock (19), closing capacity tracheae (20).Open reactor leakage fluid dram (11) tongs, make waste reaction solution all flow into returnable bottle (33).Mention level ball (21), turn eudiometer tube cock (19), all catches up with gas into gas washing hemisphere (27).Turn eudiometer tube cock (19), closing capacity tracheae (20).Open the stirring rate of the interior magneton of large gas washing hemisphere (27) (29), keep 2～5min.The stop magnetic agitation (30) of gas washing hemisphere (27), cock on turn eudiometer tube (19), reduce level ball (21), the interior gas of gas washing hemisphere (27) is caught up with into eudiometer tube (20), when gas washing liquid flow to eudiometer tube cock (19) and locates, turn eudiometer tube cock (19), closing capacity tracheae (20).Improve level ball (21), make the interior liquid levels of level ball (21) and the interior liquid surface level of eudiometer tube (20), read eudiometer tube (20) scale, recording volume V records now air pressure and temperature, for later calculating simultaneously.
The present invention compares original technology tool and has the following advantages:
1, reaction is not subject to external environmental condition variable effect, compares normal form amino acid determining instrument and can under low temperature, measure in winter.Determination data is stable, and average error reduces half compared with normal form amino acid determining instrument.
2, by circulator bath, can regulate temperature of reaction, sense cycle is short, and the reaction time shortens 1/3 compared with normal form amino acid determining instrument.
3, gas washing hemisphere (27) is furnished with magnetic agitation (10), automatically gas washing.Reactor (1) is furnished with magnetic agitation (30), can react fully and carry out, and regulates reaction process.
4, easy to clean, after each part detachable, clean respectively, and reactor (1) and gas washing hemisphere (27) all can carry out self-cleaning by the magnetic agitation (10) of reactor (1) and the stirrer (30) of gas washing hemisphere (27).
5, make course of reaction cleaner adding of recovery section (IV), waste reaction solution (mixed liquor of sodium nitrite, glacial acetic acid and liquid to be measured) and gas washing waste liquid (potassium permanganate, NaOH mixed liquor) can directly enter returnable bottle by silicone tube (32), and self-cleaning can react to each other between waste liquid, reaction produces waste gas and all by recovery section (IV) is unified, discharges, and keeps clean environment.
6, volume is little, is convenient to place, and except retracting device (IV), all can be positioned on experiment table and operate.
Accompanying drawing explanation:
Fig. 1 primary amino radical tester schematic diagram of the present invention.Wherein:
1, reactor 2, the first charge pipe 3, the second charge pipe 4, water-bath chuck 5, reactor wall 6, circulator bath interface 7, the first thin neck feed pipe 8, the second thin neck feed pipe 9, magneton 10, magnetic agitation 11, discharging tube 12, reactor ground 13, grinding port plug 14, three-limb tube 15, three-way cock 16, gas outlet 17, thin neck bend pipe 18, thin neck straight tube 19, inclined hole stop,threeway 20, eudiometer tube 21, level ball 22, emulsion tube 23, thin neck connecting pipe 24, thin neck separator tube 25, discharging tube 26, buffering ball 27, gas washing hemisphere 28, feed tube 29, magneton 30, magnetic agitation 31, four-way connecting pipe 32, silicone tube 33, returnable bottle 34, feed tube 35, gas outlet 36, plug
Specific embodiments:
Following examples are to further illustrate of the present invention, but the present invention is not limited thereto.
Embodiment 1
Primary amino radical acidity test instrument of the present invention, is comprised of reaction unit (I), amount device of air (II), air-washer (III), retracting device (IV).
Preferably, reaction unit (I) comprises reactor (1), the first charge pipe (2), the second charge pipe (3) and three-limb tube (14).Wherein reactor, containing water-bath chuck (4), contains two interfaces (6) on water-bath chuck (4) outer wall, for connecting circulator bath.Preferably, reactor bottom is flat, contains the first thin neck glass tube (7), the second thin neck glass tube (8) and a downward drainage conduit (11).Wherein first thin neck glass tube (7) one end connects the first charge pipe (2), and the other end is connected through water-bath chuck (4) and reactor wall (5), for adding of reactant liquor; Second thin neck glass tube (8) one end connects the second charge pipe (3), and the other end is connected through water-bath chuck (4) and reactor wall (5), for adding of liquid to be measured; Drainage conduit (11) is connected through water-bath chuck (4) and reactor wall (5), for the discharge of reactor (1).Drainage conduit (11) is connected with the four-way connecting pipe (31) in retracting device (IV) by silicone tube, and drainage conduit (11) is furnished with tongs.Preferably, reactor (1) contains magneton (9), the supporting magnetic agitation in bottom (10).Reactor (1) top is ground (12), is connected with the ground piston of three-limb tube.Three-limb tube (14) institute band glass tube is thin neck glass tube, and intersection is three hole cocks (15).One end (13) with grinding port plug in three ends of three-limb tube is connected with reactor ground (12), one end of exhausr port (16) is connected with the four-way connecting pipe (31) in retracting device (IV) by silicone tube, and last one end is connected with inclined hole stop,threeway (19) by thin neck bend pipe (17).
Preferably, amount device of air (II) comprises eudiometer tube (20) and level ball (21).Wherein inclined hole three-way cock (19) is contained in eudiometer tube upper end, and cock upper end is two thin neck glass tubes; Bend pipe (17) connecting tee connecting pipe wherein, thin neck straight tube (18) is connected with gas washing hemisphere (27) by the thin neck connecting pipe (23) in air-washer (III).Preferably, in eudiometer tube, venturi portion is amount gas part, scale range 10～15ml, minimum scale 0.05ml; Eudiometer tube bottom is gas buffer part (effect is to prevent that gas from too much causing gas to overflow from level ball (21)), and buffer portion volume is about 150～200ml, and interface is contained in bottom, by emulsion tube, is connected with level ball (21).Preferably, level sphere volume is about 200～250ml, is positioned over lower.
Preferably, air-washer (III) comprises thin neck connecting pipe (23), gas washing hemisphere (27) and buffering ball (26).Wherein thin neck connecting pipe one end is connected with eudiometer tube (20) by thin neck straight tube (18), and the other end is connected with gas washing hemisphere (27) by separator tube (24).Preferably, gas washing hemisphere (27) is flat, and radius is about 100～150mm, includes magneton (29), supporting magnetic stirring apparatus (30).Two glass tubes are contained in gas washing hemisphere bottom, and wherein downward-sloping is discharging tube (25), for the discharge of gas washing liquid, by silicone tube, is connected with the four-way connecting pipe (31) in retracting device (IV); 90 ° of bend pipes (28) that make progress are connected with buffering ball (26) lower end.Preferably, buffering ball (26) radius is about 80～120mm, and top is funnel-form inlet, and bore is about 50～70mm, is convenient to adding of gas washing liquid.
Preferably, retracting device (IV) comprises four-way connecting pipe (31) and returnable bottle (33).Wherein three interfaces of four-way connecting pipe (31) one end connect respectively exhausr port (16), reactor leakage fluid dram (11) and gas washing hemisphere leakage fluid dram (25), and the interface of the other end is connected with feed tube (34) by silicone tube.Preferably, returnable bottle (33) volume is 10-20L, for the recovery of waste reaction solution and deposit; Returnable bottle (33) is suitable for reading is furnished with plug (36), contains feed pipe (34) and escape pipe (35) on plug, and escape pipe (35) is directly connected in hood or fuming cupboard gas outlet by silicone tube, prevents gas dissipation.
Primary amino radical acidity test instrument of the present invention, its reaction unit (I), amount device of air (II), air-washer (III) can be positioned on experiment table, fixing with iron stand.Retracting device (IV) is positioned over horizontal level lower than the place of reaction unit (I) and air-washer (III), and processes at any time.
Embodiment 2
1. Preparatory work of experiment:
During use of the present invention, first carry out preliminary work, first to prepare gas washing liquid (potassium permanganate 20～40g, NaOH 20～40g, deionized water 200～400m1), then each piston is wiped to vacuum grease, reactor (12) suitable for reading twines sealed membrane and fixes with clip, and reactor discharging tube (11) and gas washing hemisphere discharging tube (25) clip with tongs, and reactor jacket (4) communicates with circulator bath.Three-limb tube cock (15) is revolved into
" " (as eudiometer tube cock (19) in figure mono-) revolved in eudiometer tube cock (19), and guaranteed discharge tracheae (20) communicates with retracting device (IV) by three-limb tube gas outlet (11).From level ball (21), inject deionized water, improve level ball (21) (higher than eudiometer tube cock (19)), gas is driven out of from three-limb tube gas outlet (11), eudiometer tube (20) is filled with after deionized water, (19) 90 ° of one-tenth horizontal directions of turn eudiometer tube cock, closing capacity tracheae (20), maintenance dose tracheae (20) is full of water state.Finally from surge flask (26), pour gas washing liquid into half bottle of gas washing (27), cock on turn eudiometer tube (19) becomes " // ", maintenance dose tracheae (20) communicates with gas washing hemisphere (27), reduce level ball (21), gas washing hemisphere (27) interior gas soakage tracheae (20), when gas washing liquid flow to eudiometer tube cock (19) and locates (guarantee that leakage fluid dram (25) locate not deposit gas).(19) 180 ° of one-tenth of turn eudiometer tube cock " ", make eudiometer tube (20) and gas washing hemisphere (27) closure, and communicate with three-limb tube (14).Improve level ball (21), gas is driven out of from three-limb tube gas outlet (11), eudiometer tube (20) is filled with to deionized water (three-way pipe (14) be connected with eudiometer tube (20) thin neck in without gas residue), turn eudiometer tube cock (19) is to horizontal direction, closing capacity tracheae (20).(15) 180 ° of one-tenth of turn three-limb tube cock
reactor (1) communicates with retracting device (IV) by three-limb tube gas outlet (11).Level ball (21) is put in to lower, now in gas washing hemisphere (27) and eudiometer tube (20), is all full of liquid, and and isolate from outer air.Open circulator bath and magnetic agitation (10) (in level experiment, circulator bath temperature constant, reactor (1) lower magnetic force stirring (10) invariablenes turning speed).
2. test sample:
During test sample of the present invention, first from the first charge pipe (2), add approximately 20～30ml of glacial acetic acid, then add approximately 20～30ml (the interior liquid of reactor (1) reaches reactor more than 3/4) of 40% sodium nitrite in aqueous solution, turn the first charge pipe (2) and the second charge pipe (3) cock, make the first charge pipe (2) and the second charge pipe (3) closure, reactor (1) is only connected with retracting device (IV) by three-limb tube gas outlet (11).In reactor (1), reaction generates NO or NO
2gas, more than keeping 2～5min, guarantees the interior air of reactor (1) all to discharge.Turn three-limb tube cock (15) becomes
make reactor (1) sealing, eudiometer tube (20) does not communicate with the external world yet simultaneously.Turn the first charge pipe (2) and the second charge pipe (3) cock, the first charge pipe (2) and the second charge pipe (3) are opened, in reactor (1), producing gas drives liquid out of from the first charge pipe (2) and the second charge pipe (3), after gas is driven out of completely in the thin neck of the first charge pipe (2) and the second charge pipe (3) bottom, turn the first charge pipe (2) and the second charge pipe (3) cock, make the first charge pipe (2) and the second charge pipe (3) closure.Turn eudiometer tube cock cock (19) becomes " ", reactor (1) is only communicated with eudiometer tube (20), be hedged off from the outer world, (now reactor (1) is only to react NO or the NO producing with the interior gas of eudiometer tube (20) to keep reactor (1) interior gas inlet tracheae (20)
2gas).In charge pipe (2), add deionized water (account for volume 3/4, play fluid-tight effect, simultaneously for experiment is prepared) below.In the second charge pipe (3), add testing protein solution (as needs, please heat maintenance protein solution is working fluid), slowly open the second charge pipe (3) cock, making liquid to be measured slowly enter reactor (1) (did not add, leave trace, prevent that air from entering reactor (1)).Closed the second charge pipe (3) cock, with a small amount of deionized water rinsing the second charge pipe (3) (5ml～10ml), add again approximately 1～2ml n-amyl alcohol (n-amyl alcohol and solution layering, in solution top), slowly open the second charge pipe (3) cock, make solution slowly enter reactor (1), closed cock when n-amyl alcohol arrives the second charge pipe (3) cock place, add deionized water (to account for volume 3/4, play fluid-tight effect, simultaneously for experiment is prepared below).In course of reaction, when in eudiometer tube (20), gas surpasses eudiometer tube venturi portion, improve rapidly level ball (21), (19) 180 ° of one-tenth of turn eudiometer tube cock " // ", maintenance dose tracheae (20) communicates with gas washing hemisphere (27), gas is caught up with into gas washing hemisphere (27) and (opened gas washing hemisphere (27) magnetic agitation (9) below, make NO and NO
2gas is washed Gas-Liquid Absorption rapidly), after in eudiometer tube (20), gas is caught up with only, (19) 180 ° of one-tenth of turn eudiometer tube cock " ", make eudiometer tube (20) and gas washing hemisphere (27) closure, and communicate with reactor (1), level ball (21) is put in to lower, continues to keep reactor (10) interior gas inlet tracheae (20).Reactor (1), from adding liquid to be measured to start clock reaction 30～60min (process domestic demand is repeatedly caught up with gas into gas washing hemisphere (27)), stops reaction.Open respectively the first charge pipe (2) and the second charge pipe (3) cock, the first charge pipe (2) and the interior liquid of the second charge pipe (3) are entered in reactor (1), air in the thin neck of the first charge pipe (2) and the second charge pipe (3) bottom is caught up with in reactor (1), closed the second charge pipe (3) cock, keeps the first charge pipe (2) cock to open.Along with liquid continuous, add, the interior gas of reactor (1) is all caught up with into eudiometer tube (20).When liquid is arrived in three-limb tube cock (15) while locating, (19) 90 ° of turn eudiometer tube cocks become horizontal directions, closing capacity tracheae (20), simultaneously closed the first charge pipe (2) cock.Turn three-limb tube cock (15) becomes
open reactor leakage fluid dram (11) tongs, make waste reaction solution all flow into returnable bottle (33).Close tongs, open the first charge pipe (2) cock, add deionized water to reactor (1) to be full of, closed the first charge pipe (2) cock, with the automatic cleaning reaction device (1) (unlatching that keeps reactor (1) circulator bath and magnetic agitation (10) in course of reaction) of magnetic agitation (10).Mention level ball (21), turn eudiometer tube cock (19) becomes " // ", gas is all caught up with into gas washing hemisphere (27) (gas washing hemisphere (27) above narrower neck tube (24) without gas residue), (19) 90 ° of one-tenth horizontal directions of turn eudiometer tube cock, closing capacity tracheae (20).Open the stirring rate of the interior magneton of large gas washing hemisphere (27) (29), keep 2～5min.The stop magnetic agitation (30) of gas washing hemisphere (27), cock on turn eudiometer tube (19) becomes " // ", maintenance dose tracheae (20) communicates with gas washing hemisphere (27), reduce level ball (21), gas washing hemisphere (27) interior gas soakage tracheae (20), when gas washing liquid flow to eudiometer tube cock (19) and locates, (19) 90 ° of turn eudiometer tube cocks become horizontal directions, closing capacity tracheae (20).Improve level ball (21), make the interior liquid levels of level ball (21) and the interior liquid surface level of eudiometer tube (20), read eudiometer tube (20) scale, recording volume V records now air pressure and temperature, for later calculating simultaneously.
3. experiment aftertreatment:
Turn eudiometer tube cock (19) becomes " ", and turn three-limb tube cock (15) becomes
maintenance dose tracheae (20) is connected with retracting device (IV) by three-limb tube gas outlet (16).Mention level ball (21), gas is driven out of from three-limb tube gas outlet (16), eudiometer tube (20) is filled with to deionized water, (19) 90 ° of one-tenth horizontal directions of turn eudiometer tube cock, closing capacity tracheae (20), maintenance dose tracheae (20) is full of water state (between three-way cock (15) and inclined hole three-way cock (19), thin neck glass tube is interior without gas residue).Turn three-limb tube cock (19) becomes
make eudiometer tube (20) and three-limb tube (14) closure, reactor (1) communicates with retracting device (IV) by three-limb tube gas outlet (16).Level ball (21) is put in to lower, opens reactor leakage fluid dram (11) tongs, the interior liquid of emptying reactor (1), closes leakage fluid dram (11) tongs, prepares the next test for the treatment of test sample.In test sample process, gas washing liquid is become when dark blue from dark purple, opens leakage fluid dram (25) tongs, emptying gas washing hemisphere (27) liquid.Close leakage fluid dram (25) tongs, rejoin new gas washing liquid.After test reaction is all complete, open reactor leakage fluid dram (11) and gas washing hemisphere leakage fluid dram (25) tongs, emptying reactor (1) and the interior waste liquid of gas washing hemisphere (27).From buffering ball (26), add glacial acetic acid and sodium nitrite mixed liquor to gas washing hemisphere (27), open the interior magneton of large gas washing hemisphere (27) (29) rotating speed, the gas washing liquid of washing off on gas washing hemisphere (27) inwall is residual.After effluent discharge, use washed with de-ionized water one time again.In retracting device (IV), be potassium permanganate, NaOH, glacial acetic acid and the sodium nitrite mixed liquor that reactor (1) and gas washing hemisphere (27) are discharged, self-absorption reacts to each other.The NO and the NO that produce
2gas is processed by unified discharge of exhausr port (35).As treated, test sample easily produces a large amount of bubbles, need in reactor (1), add a small amount of n-amyl alcohol before adding liquid to be measured, for froth breaking.
4. calculate
Following formula the computing formula of primary amino radical tester and the setting method of relevant parameters.
Note n
samplefor sample primary amino radical molar weight, n
n2by being surveyed nitrogen molar weight, the mol ratio that generates nitrogen by the known primary amino radical reaction of reaction principle is 1: 1, and this equation can be expressed as:
N
sample=n
n2(1)
Note c is sample molar content (mol/g), and m is sample quality (m), and equation can be expressed as:
N
sample=cm (2)
The note ρ mass density (g/ml) that is nitrogen, the ambient temperature during according to amount gas and atmospheric pressure are tabled look-up and are obtained, V is for measuring the volume (ml) of nitrogen, M be nitrogen molecule amount (mol/g) equation can be expressed as:
n
N2＝ρV/M (3)
Formula (2), (3) are brought in (1), and arrangement obtains:
By formula (4), can calculate the primary amino radical content of sample.
Claims (6)
1. a primary amino radical tester, by reaction unit (I), amount device of air (II), air-washer (III), retracting device (IV), formed, reaction unit (I), amount device of air (II), air-washer (III), retracting device (IV) connect successively, it is characterized in that, described reaction unit (I) comprises reactor (1), charge pipe (2) and three-limb tube (14), wherein reactor (1) top is ground (12), magneton (9) is contained in inside, bottom is flat and supporting magnetic agitation (10), outside with water-bath chuck (4); Air-washer (III) comprises gas washing hemisphere (27) and buffering ball (26), and wherein gas washing hemisphere (27) is flat, includes magneton (29), supporting magnetic stirring apparatus (30); Retracting device (IV) comprises four-way connecting pipe (31) and returnable bottle (33), and exhausr port and the leakage fluid dram of reaction unit (I), amount device of air (II), air-washer (III) are all connected on retracting device (IV).
2. primary amino radical tester as claimed in claim 1, it is characterized in that, described reaction unit (I) comprises the first charge pipe (2) and the second charge pipe (3), wherein the bottom of the first charge pipe (2) connects the first thin neck glass tube (7), the bottom of the second charge pipe (3) connects the second thin neck glass tube (8), the volume of the first charge pipe (2) is 25～35ml, and the volume of the second charge pipe (3) is 10～20ml.
3. primary amino radical tester as claimed in claim 1, it is characterized in that, in described reaction unit (I), a thin neck glass tube (7) making progress and a downward drainage conduit (11) are arranged at reactor (1) bottom, one end of thin neck glass tube (7) connects charge pipe (2), and the other end is connected through chuck (4) and reactor wall (5); Drainage conduit (11) is connected through chuck (4) and reactor wall (5), for the discharge of reactor (1); On reactor jacket (4) outer wall, contain two interfaces (6), for communication loop water-bath.
4. primary amino radical tester as claimed in claim 1, it is characterized in that, in described reaction unit (I), three-limb tube (14) is connected with reactor top ground (12) by the grinding port plug (13) of thin neck glass tube one end, the other end of three-limb tube (14) is connected with inclined hole stop,threeway (19) by thin neck bend pipe (17), wherein three-limb tube (14) is with cock (15), cock (15) is positioned at three-limb tube (14) intersection, the trend for adjustments of gas in three-limb tube (14).
5. primary amino radical tester as claimed in claim 1, is characterized in that, gas washing hemisphere (27) and buffering ball (26) are connected with inclined hole stop,threeway (19) through thin neck glass connecting pipe (23); Gas washing hemisphere (27) top connects thin neck glass tube (24), for gas, passes in and out; Bottom with a downward glass tube (25) for discharge opeing, and with the upwards bend pipe (28) of 90 ° for connecting buffering ball (26); The radius of gas washing hemisphere (27) is 100～150mm, and the radius of buffering ball (26) is 80～100mm.
6. the using method of primary amino radical tester as claimed in claim 1, comprises the following steps:
1) preliminary work: preparation gas washing liquid, fill with gas washing hemisphere (27), again eudiometer tube (20) is filled with to deionized water, and keep being all full of liquid in gas washing hemisphere (27) and eudiometer tube (20), with isolate from outer air, wherein gas washing liquid principal ingredient comprises potassium permanganate 20～40g, NaOH 20～40g, deionized water 200～400ml; Open circulator bath and magnetic agitation (10);
2) test sample: add glacial acetic acid 20～30ml to the first charge pipe (2) successively, sodium nitrite in aqueous solution 20～30ml of 40%, chemical reaction occurs in reactor (1), generates NO or NO
2gas, the interior air of emptying reactor (1); Drive gas in the thin neck of the first charge pipe (2) and the second charge pipe (3) bottom out of, by adjusting cock, keep reactor (1) only to communicate with eudiometer tube (20), isolated with ambient atmosphere; In the second charge pipe (3), add testing protein solution, with n-amyl alcohol fluid-tight, stop reaction after 30～60 minutes, the gas of generation is caught up with into gas washing hemisphere (27) from eudiometer tube (20), opens magnetic agitation, absorbs NO
2gas, after 10～30 minutes catches up with residual gas into eudiometer tube (20), reads eudiometer tube (20) scale, and recording volume V records now air pressure and temperature simultaneously.
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| CN201110249480.1A CN102393466B (en) | 2011-08-29 | 2011-08-29 | Primary amino radical tester |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201110249480.1A CN102393466B (en) | 2011-08-29 | 2011-08-29 | Primary amino radical tester |
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| CN102393466B true CN102393466B (en) | 2014-10-08 |
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| CN102794442A (en) * | 2012-07-23 | 2012-11-28 | 宁夏共享集团有限责任公司 | Liquid material device for preventing contact of liquid material and air to react for casting |
| CN103018077A (en) * | 2012-12-28 | 2013-04-03 | 河南师范大学 | Leakage detection sampler |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5528923A (en) * | 1992-12-21 | 1996-06-25 | Ledez; Kenneth M. | Gas amount and solubility investigation apparatus |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5528923A (en) * | 1992-12-21 | 1996-06-25 | Ledez; Kenneth M. | Gas amount and solubility investigation apparatus |
Non-Patent Citations (7)
| Title |
|---|
| Donald D. Van Slyke.Manometric Determination of Primary Amino Nitrogen and its Application to Blood Analysis.《Journal of Biological Chemistry》.1929,第83卷 |
| einige Anwendungen derselben in der Chemie der Proteine, des Harns und der Enzyme.《Berichte der deutschen chemischen Gesellschaft》.1910, * |
| einigeAnwendungenderselbeninderChemiederProteine des Harns und der Enzyme.《Berichte der deutschen chemischen Gesellschaft》.1910 |
| Manometric Determination of Primary Amino Nitrogen and its Application to Blood Analysis;Donald D. Van Slyke;《Journal of Biological Chemistry》;19291231;第83卷;第425-447页 * |
| van Slyke D D.Eine Methode zur quantitativen Bestimmung der aliphatischen Aminogruppen * |
| 张志贤.实用有机定量分析.《实用有机定量分析》.1965, * |
| 郑燕龙,潘子昂.范氏氨基酸测定器.《实验室玻璃仪器手册》.2007, * |
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