CN108931606A - A kind of method of pair of magnesium chloride hydrate crystallization water detection - Google Patents

A kind of method of pair of magnesium chloride hydrate crystallization water detection Download PDF

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Publication number
CN108931606A
CN108931606A CN201810552612.XA CN201810552612A CN108931606A CN 108931606 A CN108931606 A CN 108931606A CN 201810552612 A CN201810552612 A CN 201810552612A CN 108931606 A CN108931606 A CN 108931606A
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China
Prior art keywords
sample
solvent
reagent
titration
titer
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CN201810552612.XA
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Inventor
哈权章
祝甲财
张学鹏
黄丽萍
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Qinghai Salt Lake Industry Co Ltd
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Qinghai Salt Lake Industry Co Ltd
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Priority to CN201810552612.XA priority Critical patent/CN108931606A/en
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N31/00Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
    • G01N31/16Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using titration
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N5/00Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid
    • G01N5/02Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid by absorbing or adsorbing components of a material and determining change of weight of the adsorbent, e.g. determining moisture content
    • G01N5/025Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid by absorbing or adsorbing components of a material and determining change of weight of the adsorbent, e.g. determining moisture content for determining moisture content

Abstract

A kind of method of pair of magnesium chloride hydrate crystallization water detection, including:First operation S1, provides titer reagent and solvent, carries out pre- titration balance, measures the titer of the titer reagent;Second operation S2, emptying titration waste liquid simultaneously rejoin solvent, obtain the first solvent, carry out titration balance to first solvent;Third operates S3, provides the sample of magnesium chloride hydrate, weighs the sample in sealed states, obtains the first sample;4th operation S4, first sample is added in first solvent, is titrated with the titer reagent, titration numerical value and the first mixed solvent are obtained;5th operation S5, sealing weigh the sample and obtain the second sample, and the second sample is added to first in the mixed solvent, titer reagent is supplemented, is titrated again.On-line analysis and batch quantity analysis are realized, detection efficiency is improved;It is easy to operate, avoid operating error;Reduce ambient enviroment measurement error caused by the influence of sample;Operator will not directly contact reagent, solvent, waste liquid, avoid the injury of poisonous and harmful reagent.

Description

A kind of method of pair of magnesium chloride hydrate crystallization water detection
Technical field
The present invention relates to the crystallizations water in a kind of detection method of crystallization water more particularly to a kind of hydrate of metallic compound Detection method.
Background technique
There are many kinds of the methods of determination of moisture, common determination of moisture method:
Seasoning is mainly used in the measurement of solid sample moisture, so that sample is dried out by heating, generallys use often Press seasoning and chemical seasoning method.Atmosphere pressure desiccation refers generally under atmospheric pressure, and sample is lost after measuring 100 DEG C or so heating Substance, but actually at this temperature sample lost be volatile materials total amount, without being entirely water.In addition usually Sample is dried using baking oven, the influence of ambient enviroment is highly prone in operating process, drying terminates to absorb water again also can Cause error;Chemical seasoning method is exactly to have the chemicals of strong adsorption effect and aqueous specimen same water vapour certain It is packed into a drier (glass or vacuum desiccator), so that sample is reached dry constant weight by isothermal diffusion and suction-operated, Then its moisture content can be calculated according to the weight difference of dry front and back sample, this method is dried at room temperature for, when needing longer Between, several days, tens days or even some months.
The way of distillation is put into organic solvent and sample not soluble in water in distillation type moisture content determining device and heats, makes sample In moisture separate, according to the water distilled out, moisture content can be calculated.The equipment of this method is simple, price It is cheap, but have following several disadvantages:Emulsion easily occurs for water and organic solvent;Moisture may be volatilized absolutely not in sample Come;Moisture is attached to sometimes on condensation tube wall, causes error in reading;Outside moisture removal, there are also a large amount of volatile materials.So precision compared with It is low, error is larger, and minute is very long, suitable for not high to moisture content precise requirements and measure the sample of frequency very little Product.
Infrared absorption spectroscopy, the degree of absorption according to moisture to the infrared light of a certain wavelength with it deposit in the sample by content The fact certain relationship, infrared spectrum measurement moisture method is established.The method detection time is long, and higher cost is unfavorable In batch quantity analysis.
Dew point method, dew point method is easy to operate, and instrument is uncomplicated, is usually used in the measurement of micro-moisture in permanent gases.But The interference of this method is more, and some easily cold ventilation bodies especially can first condense when concentration is higher than vapor generates interference.
Seasoning is generally used in the method for the detection magnesium chloride hydrate crystallization water, mainly utilizes baking oven or other bakings The crucible of sample and splendid attire sample is dried in dry equipment.The method is disadvantageous in that:In operation, sample All in air, easily water suction causes measurement error for exposure after before it is dried;Dried crucible using the desiccant such as silica gel into Row constant weight, constant weight can not accomplish closed-loop operation in the process, equally will receive the influence of environment;Institute is dried using drying equipment Time is longer, and workload is many and diverse when measure batch, reduces detection efficiency and cannot achieve on-line measurement.
Summary of the invention
It is an object of the present invention to solve in magnesium chloride hydrate crystallization water detection process, existing following problems:It is extraneous Disturbing factor influence it is big, take a long time, higher cost, workload is many and diverse, is easy to make work in continuous mode when measure batch Human contact is to volatile chemical and cannot achieve on-line measurement.
The present invention provides a kind of methods of magnesium chloride hydrate crystallization water detection, wherein including:First operation (S1), Titer reagent and solvent are provided, pre- titration balance is carried out, so that the solvent and titer reagent is in titration equilibrium state, measure institute The titer for stating titer reagent obtains the numerical value and titration waste liquid of the titer;Second operation S2, emptying titration waste liquid are laid equal stress on It is new that solvent is added, the first solvent is obtained, titration balance is carried out to first solvent, is made at first solvent and titer reagent In titration equilibrium state;Third operates S3, provides the sample of magnesium chloride hydrate, weighs the sample in sealed states, obtain To the first sample;4th operation S4, first sample is added in first solvent, is dripped with the titer reagent It is fixed, obtain titration numerical value and the first mixed solvent;5th operation S5, sealing weighs the sample and obtains the second sample, by second Sample is added to first in the mixed solvent, supplements titer reagent, is titrated again.
According to embodiment of the present invention, wherein use standard water sample titration, measure the drop of the titer reagent It is fixed to spend, in titration process, the standard water sample is kept to be isolated from the outside.
According to embodiment of the present invention, wherein the sample terminates to being added to used in solvent from weighing Time≤30 second, sample is in closed state during sample-adding.
According to embodiment of the present invention, wherein the replacement of the sample, reagent and/or solvent uses automatically more Change mode.
According to embodiment of the present invention, wherein repeat the 5th operation S5, to realize that batch measures.
According to embodiment of the present invention, wherein the reagent uses nothing using karl Fischer reagent, the solvent Water methanol.
According to another aspect of the present invention, a kind of system for the detection of the magnesium chloride hydrate crystallization water is provided, In, including titration vessel 1, buret 2, the pump housing 3, closed title sample device 4, sample more changing device 5, reagent more changing device 6, the drop Constant volume device 1 is for accommodating the solvent;The buret 2 is used for titration operation for accommodating the reagent;The pump housing 3 It is placed in inside the titration vessel 1, for emptying the raffinate in the titration vessel 1 and rejoining solvent;The closed title Sample device 4 weighs sample for being in sample under air-tight state;The sample more changing device 5, which receives, comes from the closed title sample The sample of device, and cooperate with the titration vessel 1, for replacing sample;The reagent more changing device 6 and the buret 2 connect It connects, for supplementing titer reagent.
According to embodiment of the present invention, wherein further include isolating pad, the isolating pad was measured for titer Cheng Zhong makes the standard water sample and extraneous holding isolation.
According to embodiment of the present invention, wherein the closed title sample device 4 includes weighing part and accommodating portion, The weighing part is for showing weighing result, housing section, for accommodating the sample, so that sample is weighing and adding During sample, closed state is kept.
According to embodiment of the present invention, wherein the sample more changing device 5, the reagent more changing device 6 or/ The function of replacing automatically is had with the pump housing 3.
The beneficial effects of the invention are as follows batch quantity analysis is realized, detection efficiency is improved;Stream easy to operate, not complicated Journey avoids operating error;It is swift to operate, it can satisfy the needs of on-line analysis;Reduce influence of the ambient enviroment to sample Caused by measurement error;Karl Fischer reagent and dehydrated alcohol are prepared without testing staff, discharge waste liquid and replacement reagent also not It can directly contact, avoid the injury of poisonous and harmful reagent.
Detailed description of the invention
Fig. 1 is the schematic diagram of system provided by the present invention;And
Fig. 2 is the schematic diagram of detection method of the invention;
Wherein, 1 titration vessel, 2 burets, 3 pump housings, 4 closed title sample devices, 5 samples more changing device, 6 reagents more changing device.
Specific embodiment
The preferred embodiments of the present invention will be described in detail with reference to the accompanying drawing, and reference label refers to the group in the present invention Part, technology, realizing under appropriate circumstances so as to advantages and features of the invention can be easier to be understood.Following description is pair The materialization of the claims in the present invention, and other specific implementations not clearly stated relevant to claim also belong to power The range that benefit requires.
Fig. 1 shows the schematic diagram of system provided by the present invention.
As shown in Figure 1, a kind of system for the detection of the magnesium chloride hydrate crystallization water, wherein including titration vessel 1, drop Determine pipe 2, the pump housing 3, closed title sample device 4, sample more changing device 5, reagent more changing device 6, the titration vessel 1 is described for accommodating Solvent;The buret 2 is used for titration operation for accommodating the reagent;The pump housing 3 is placed in the titration vessel 1 Portion, for emptying the raffinate in the titration vessel 1 and rejoining solvent;The closed title sample device 4 is for being in sample Under air-tight state, sample is weighed;The sample more changing device 5 receive from it is described it is closed claim sample device sample, and with the drop Constant volume device 1 cooperates, for replacing sample;The reagent more changing device 6 is connect with the buret 2, for supplementing titer reagent.
The process of titration includes:Solvent is injected into the titration vessel 1 first, uses the titer reagent pair in buret 2 The solvent carries out pre- titration balance, after reaching pre- titration balance, injects standard water sample to the solvent, continues with the titration Reagent is titrated, to measure the titer of titer reagent.Titer measurement finishes, residual titration in the titration vessel 1 Raffinate, the titration raffinate are the mixtures of the product of the solvent, titer reagent and titer reagent and standard water sample reaction, The titration raffinate cannot be used continuously, and need that titration system is discharged.It will be described in titration raffinate discharge using the pump housing 3 Titration vessel 1 rejoins the solvent, obtains the first solvent, after carrying out titration balance to first solvent, passes through sample The sample weighed by closed title sample device 4 is added in more changing device 5, is titrated using the titer reagent, until titration terminates. After sample titrates, the first mixed solvent is obtained in the titration vessel 1, first mixed solvent is solvent, is dissolved in The mixed solution for the product that sample and titer reagent in the solvent are reacted with the crystallization water in sample, first mixing are molten It is not aqueous in agent, it can be continued to use also in titration equilibrium state so not influencing the titration of subsequent sample.Again by The sample weighed by closed title sample device 4 is added to first in the mixed solvent for sample more changing device 5, is more changed the outfit by reagent It sets to the buret 2 and supplements the titer reagent, continue to titrate.Sample and institute are replaced by the sample more changing device 5 It states reagent more changing device 6 and supplements the titer reagent, realize and the batch of sample is measured.When to same sample progress METHOD FOR CONTINUOUS DETERMINATION When, titration, which finishes, every time can all reach titration equilibrium state, so not having to each sample does titration balance, process is saved, Reagent is saved.In addition, every time titration finish after, the solution in titration vessel, there is no influence it is subsequent titration precision because Element, so, the solution in the titration vessel can continue to use, and save the step of replacing solvent, further save molten Agent and titer reagent.Since this method is easy to operate, on-line measurement can be applied to.The on-line measurement refers to for production line Carry out real-time measurement.
Before titration, first confirm that the titer reagent and solvent have sufficient preparation amount.The titer reagent refers to can To react with the crystallization water being distributed in the solvent, and the reagent of reaction end can be determined accurately.It is preferred that reaction is fast, eventually The apparent reagent of point, in the present invention, it is preferred to karl Fischer reagent.The karl Fischer reagent refer to using iodine and water reaction come The finished product reagent for measuring water content has many advantages, such as that reaction is fast and terminal is obvious.The solvent, which refers to, can quickly dissolve sample Product make the moisture in sample be in the solvent of discrete state in the solvent.The solvent will select water content as low as possible, And the solvent with magnesium chloride without side reaction.In the present invention, it is preferred to anhydrous methanol, because of anhydrous methanol dissolution magnesium chloride hydration Object process will not influence measurement result without side reaction.The titration vessel 1 can use existing various titration vessels 1 with And the titration vessel of invention, function need to meet the requirement for not influencing titration results in the future.The titration vessel 1 was titrating It needs to keep good closed state in journey, enters titration vessel 1, interference drop to avoid the moisture of external environment in titration process Determine result.The selection of buret 2 and the selection of titration vessel 1 are required to make titration operation linking to keep coherent, and buret 2 can be with Using semi-automatic buret 2 or full-antomatic buret 2.
Before titration, need to solvent by pre- titration balancing run, the pre- titration balance refers to using titer reagent The solvent is titrated, keeps the solvent anhydrous, and measures the drift value of the solvent.The drift value referred in the unit time Into the amount of the moisture in titration vessel 1.The drift value is one of the parameter when calculating sample moisture content, so that calculating knot Fruit is more accurate.When titration balance, the titer reagent is constantly titrating the solvent, but the usage amount of this titer reagent, It is not calculated in actual use amount when measurement titer and titration sample, to guarantee the accurate of titration results.
Before titration, it is also necessary in the state of keeping titration balance, be measured to the titer of the titer reagent. Titer refers to the amount of water consumed by unit titer reagent.The titer for measuring the titer reagent, can be used standard water sample into Row measurement can also be measured using anti-coulomb method or other methods, and selection standard water sample of the present invention is measured, convenient fast Victory, device requirement are simple.
The pump housing 3 refers to the pump with suction function, effect be when needing replacing solvent, will be in titration vessel 1 Waste liquid discharge, and new solvent is injected into the titration vessel 1.The pump housing 3 is built in the titration vessel 1, so that The discharge and implant operation be not by the interference of external environment.In addition, discharge waste liquid and supplementing solvent do not need operator Contact chemical substance.
The closed title sample device 4 refers to when weighing sample, sample can be made to be in the weigher of air-tight state, the present invention is not Its specific specification is limited, the various existing or following invention, title sample device with the above function can be used.
The sample more changing device 5, which refers to, to be had after each titration, and new sample is launched into new solvent The device of function.The sample more changing device 5 receives sample from the closed title sample device 4, and sample is launched to the drop In constant volume device 1.The concrete model of the unlimited sample preparation product more changing device 5 of the present invention, existing 814 sample processor, 815 sample treatments Device can be used in the present invention, it is possible to use other sample processors with replacement sample function.Made using this device The replacement of sample meets the needs of METHOD FOR CONTINUOUS DETERMINATION, to realize that batch titrates.
The reagent more changing device 6 is connect with the buret 2, according to titer reagent surplus in buret 2, to the drop Determine pipe 2 and supplement titer reagent, guarantee the needs of Continuous Titration, to realize that batch titrates.Also, during replacing titer reagent, It avoids operator and contacts the titer reagent, operator is protected.
It according to embodiment of the present invention, further include isolating pad, the isolating pad is used in titer continuous mode, Make the standard water sample and extraneous holding isolation.
The isolating pad is measuring the titer reagent using standard water sample for titration vessel 1 and external environment to be isolated Titer when, standard water sample is injected by isolating pad, keep standard water sample be isolated from the outside, avoid the shadow of outside moisture It rings, keeps injected water volume accurate, it is more accurate to be further able to the titer for making finally to measure.
According to embodiment of the present invention, the closed title sample device includes weighing part and accommodating portion, the title Amount part is for showing weighing result, housing section, for accommodating the sample, so that sample is weighing and be loaded process In, keep closed state.
The combination of the gentle crucible with a lid in day can be used to realize in the closed title sample device, uses the crucibles Sample weighs the sample of certain mass so that sample be made to be in air-tight state in the crucible, then will be in the crucible Sample is injected into the solvent, and the crucible is put back to balance and is weighed again, and the quality that sample is added is acquired with minusing, whole A sample-adding process control is within 30 seconds.The interference of samples weighing process environment moisture is avoided, so that the sample quality of weighing It is more accurate.
According to embodiment of the present invention, the sample more changing device 5, the reagent more changing device 6 or/and described The pump housing 3 has the function of replacing automatically.
The function with automatic replacement sample refers to through procedural setting, so that the replacing construction of sample, quality, speed The various parameters such as degree can be according to the operation adjust automatically of titration, to meet the needs of Continuous Titration of the present invention.The present invention is not right The sample more specific structure of changing device 5, model, brand do any restriction, and the sample more changing device 5 can be used existing 814 sample processors and/or 815 sample processors.
Function of the reagent more changing device 6 with automatic replacement reagent, for titrating every time at the end of replace institute automatically Reagent is stated, enables the reagent more changing device 6 in various parameters such as replacing construction, quality, speed, it can be according to the needs of titration Adjust automatically, to meet the needs of Continuous Titration.The present invention is not to the reagent more specific structure of changing device 6, program, model Etc. any restriction is done, existing charger of thinking much is can be used in the reagent more changing device 6.
Function of the pump housing 3 with automatic replacement solvent, for titrating every time at the end of empty raffinate and rejoin Solvent.Enable the pump housing 3 that the raffinate in the titration vessel 1 to be accurately discharged at the end of each titration, is added new Solvent.
The sample replaces function, reagent automatically and replaces the realization that function and solvent replace function automatically automatically, can Meet the needs of batch titration, also, avoids making operator touch chemicals in replacement titer reagent and dissolving agent process Matter.
Fig. 2 shows the flow charts of method of the present invention.
As shown in Fig. 2, according to an aspect of the invention, there is provided the side of a kind of pair of magnesium chloride hydrate crystallization water detection Method, wherein the first operation S1 provides titer reagent and solvent, carries out pre- titration balance, is in the solvent and titer reagent Equilibrium state is titrated, the titer of the titer reagent is measured, obtains the numerical value and titration waste liquid of the titer;Second operation S2, emptying titration waste liquid simultaneously rejoin solvent, obtain the first solvent, carry out titration balance to first solvent, make described First solvent and titer reagent are in titration equilibrium state;Third operates S3, the sample of magnesium chloride hydrate is provided, in seal shape Sample described in state lower-weighing obtains the first sample;4th operation S4, first sample is added in first solvent, It is titrated with the titer reagent, obtains titration numerical value and the first mixed solvent;5th operation S5, sealing weigh the sample The second sample is obtained, the second sample is added to first in the mixed solvent, titer reagent is supplemented, is titrated again.
According to embodiment of the present invention, wherein use standard water sample titration, measure the drop of the titer reagent It is fixed to spend, in titration process, the standard water sample is kept to be isolated from the outside.
According to embodiment of the present invention, the sample from weigh terminate to be added to the time used in solvent≤ 30 seconds, sample was in closed state during sample-adding.
According to embodiment of the present invention, wherein the replacement of the sample, reagent and/or solvent uses automatically more Change mode.
According to embodiment of the present invention, wherein repeat the 5th operation (S5), to realize that batch is surveyed It is fixed.
According to embodiment of the present invention, wherein the reagent uses nothing using karl Fischer reagent, the solvent Water methanol.
Embodiment:
In the present embodiment, instrument uses karl Fischer moisture teller, and reagent uses karl Fischer reagent, and solvent uses The mixed solution of anhydrous methanol and karl Fischer.
Preparation before titration:Confirm that karl Fischer reagent and anhydrous methanol are sufficient, instrument connection is intact, opens power supply and opens It closes, instrument starts to measure after preheating 30 minutes.
Start pre- titration balance:
It is operated on karl Fischer moisture tester control panel, calls in method, selection is loaded into, selects on interface Unit μ l, numeral input 10;
Click starts, and balance display can be done always, until reaching terminal, terminal drift≤20 μ l/min.
Measure titer:
10 μ l standard water samples are first pumped into syringe with microsyringe, it is ensured that there is no bubble in syringe, then click out Begin, will stop balancing, inject standard water sample in titration cup by isolating pad in 30s, during injecting standard water sample The syringe needle of syringe is immersed in solution.After time to be implanted, titration.Titer survey three times is carried out with same method It is fixed, it after the completion of the measurement of the last one titer, is counted, display statistics general view shows average value, absolute and relative standard Deviation.
Sample moisture content measurement:
Before measurement, the raffinate in titration vessel is discharged by built-in suction pump, 25ml anhydrous methanol is then added, opens Magnetic stirrer.Method KF is called in, is loaded into, clicks and starts to carry out titration balance again, balance proceeds to drift value≤20 μ l/ After min, beginning is again tapped on, injection length is shown, sample is added in 30s.It is to be implanted after injecting 0.6~0.8g sample After time, weighed sample size is inputted on the control panel, measurement result is calculated.
Moisture is recorded, titration is terminated.
The titer, sample moisture content calculation are as follows:
Titer C0, unit mg/ml, calculating:
m0:When calibration, the amount of water, unit mg is added
v1:When calibration, the amount of reagent, units/ml are consumed
Sample water content C:
m:When measurement, the quality of sample, unit g
v2:When measurement, the amount of reagent, units/ml are consumed
When carrying out batch measurement, 814 and 815 sample processors are connected, replace sample automatically, realize sample crystallization water content The batch quantity analysis of measurement;With liquid feeding unit is thought much or charger is automatically replenished titer reagent, avoid with it is poisonous and harmful The contact of reagent.
The method that above-mentioned detection magnesium chloride closes the object crystallization water, measuring accuracy can reach ± 0.2mv, moisture measurement range 10ppm to 100%, ± 20 μ l of liquid feeding error;When carrying out the measurement of the magnesium chloride conjunction object crystallization water, Ipol mode (pole can be used Galvanic current) and two kinds of measurement patterns of Upol mode (polarizing voltage), time of measuring is short, accuracy is high, and emptying waste liquid and addition are molten Agent it is easy to operate, reduce workload, improve detection efficiency;Operator does not have to directly contact when replacing titer reagent, Avoid the injury of poisonous and harmful reagent;Sample claims the influence avoided during sample environment to sample and causes error.
It should be noted that the above-mentioned embodiments illustrate rather than limit the invention, and this Field technical staff can be designed alternative embodiment without departing from the scope of the appended claims.In claim In, any reference symbol between parentheses should not be configured to limitations on claims.

Claims (10)

1. the method for a kind of pair of magnesium chloride hydrate crystallization water detection, wherein including:
First operation (S1), provides titer reagent and solvent, carries out pre- titration balance, the solvent and titer reagent is made to be in drop Determine equilibrium state, measure the titer of the titer reagent, obtains the numerical value and titration waste liquid of the titer;
Second operation (S2), emptying titration waste liquid simultaneously rejoin solvent, obtain the first solvent, drip to first solvent Weighing apparatus is allocated, first solvent and titer reagent is made to be in titration equilibrium state;
Third operates (S3), provides the sample of magnesium chloride hydrate, weighs the sample in sealed states, obtains the first sample Product;
4th operation (S4), first sample is added in first solvent, is titrated, is obtained with the titer reagent To titration numerical value and the first mixed solvent;
5th operation (S5), sealing weigh the sample and obtain the second sample, and it is molten that the second sample is added to first mixing In agent, titer reagent is supplemented, is titrated again.
2. according to the method described in claim 1, wherein, using standard water sample titration, measuring the titration of the titer reagent It spends, in titration process, the standard water sample is kept to be isolated from the outside.
3. according to the method described in claim 1, wherein, the sample terminates to being added to the time used in solvent from weighing ≤ 30 seconds, sample was in closed state during sample-adding.
4. according to the method described in claim 1, wherein, the replacement of the sample, reagent and/or solvent is using automatic replacement side Formula.
5. according to the method described in claim 1, wherein, repeating the 5th operation (S5), to realize that batch measures.
6. according to the method described in claim 1, wherein, the reagent is using karl Fischer reagent, the solvent using anhydrous Methanol.
7. a kind of system for the detection of the magnesium chloride hydrate crystallization water, wherein including titration vessel (1), buret (2), pump Body (3), closed title sample device (4), sample more changing device (5), reagent more changing device (6),
The titration vessel (1) is for accommodating the solvent;
The buret (2) is used for titration operation for accommodating the reagent;
The pump housing (3) is placed in that the titration vessel (1) is internal, for emptying raffinate in the titration vessel (1) and again Solvent is added;
The closed title sample device (4) weighs sample for being in sample under air-tight state;
The sample more changing device (5) receives from the closed sample for claiming sample device, and cooperates with the titration vessel (1), For replacing sample;
The reagent more changing device (6) is connect with the buret (2), for supplementing titer reagent.
8. system according to claim 7, wherein further include isolating pad, the isolating pad is used for titer continuous mode In, make the standard water sample and extraneous holding isolation.
9. system according to claim 7, wherein the closed title sample device (4) includes weighing part and accommodating portion, institute Weighing part is stated for showing weighing result, housing section, for accommodating the sample, so that sample is being weighed and is being loaded In the process, closed state is kept.
10. system according to claim 7, wherein the sample more changing device (5), the reagent more changing device (6) Or/and the pump housing (3) has the function of replacing automatically.
CN201810552612.XA 2018-05-31 2018-05-31 A kind of method of pair of magnesium chloride hydrate crystallization water detection Pending CN108931606A (en)

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