CN105403556B - The assay method of chloride ion content in a kind of field engine coolant - Google Patents
The assay method of chloride ion content in a kind of field engine coolant Download PDFInfo
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Abstract
The invention belongs to harmful element chemical composition analysis technical field of measurement and test in coolant, the assay method of chloride ion content in a kind of disclosed field engine coolant, detection sample is made to digest completely using concentrated nitric acid and hydrogen peroxide, add in excessive silver-colored standard solution, in a heated state, chlorination silver sol is made to form cotton-shaped silver nitride precipitation, liquid to be determined is formed after filtering precipitation, under ICP inductively coupled plasma atomic emission spectrometer best operating conditions, measure the excessive silver ion content in liquid to be determined, chloride ion content to be determined is calculated according to measured silver ion content；This invention removes the physics and chemistry disruption when precipitation interference and equipment detection；More accurate compared with flame atomic absorption spectrometry result, with the advantages of structure favorable reproducibility, precision is high, and method is easy to operate, stable, quick, environmental protection, reliable and practical.
Description
Technical field
The invention belongs to harmful element chemical composition analysis technical field of measurement and test in coolant, are related to a kind of measure tractor
With chloride ion content in the method for chloride ion content in engine coolant more particularly to a kind of field engine coolant
ICP Inductively coupled plasma atomic emission spectrometry technologies.
Background technology
The working condition of farm tractor is heavy load state, and engine should belong to heavy load diesel engine.Weight
Load diesel engine is in peak load or the internal combustion engine operated for a long time close under peak load, and output power generates after burning
Heat it is also big, the 33% of the general calory burning, which will pass through coolant, radiates, and coolant is the normal work of engine-cooling system
One of key factor of work.The working environment of tractor is severe, working frequency is high, and reliability and life requirement are high, therefore, weight
Requirement of the load diesel engine to coolant is stringenter, it is desirable that coolant used should have cooling, antifreeze, boiling protection, prevent
The cavitation pitting and anticorrosion to various metals, good antiscale property and anti-mildew effect.
Common heavy load diesel engine coolant is generally 1) ethylene glycol concentrate both at home and abroad at present；2) propylene glycol
Base concentrate；3) ethylene glycol dilution (50% volume fraction)；4) propylene-glycol-based dilution (50% volume fraction), at these
It is anti-cavitation pitting on the basis of solution, usually adds in some supplement additives, such as phosphate, borate, molybdate, nitrite
Deng.Chlorion can be brought into while various supplement additives are added in basal liquid, and water used can also bring chlorine into when preparing solution
Ion.Existing on a small quantity for chlorion is possible to generate corruption to metals such as the iron, aluminium, copper of cooling system when coolant works
Erosion.When coolant thermal concentration reaches a certain level, chloride ion content can accordingly increase, chlorion be easy to be attracted to iron,
The metals such as aluminium, copper are passivated film surface, react generation chlorine with the oxide passivation film cation of the metal surfaces such as iron, aluminium, copper
Compound, and the chloride generated is easily dissolved in coolant, promotes destruction of the chlorion to passivating film, forms local spot corrosion
Afterwards, with metal intercrystalline corrosion and breakaway corrosion can also further occur for chlorion.Micro chlorion is cooling down in coolant
The metal surface of system forms spot corrosion, and then causes stress corrosion, can make water tank wall erosion saturating when serious, radiator leak occurs and show
As the trace chlorine in coolant can even corrode the components such as cylinder sleeve, the water pump vane of cooling system, the corrosion production of generation
Object enters cooling system, and water tank is caused to block, and cylinder sleeve is stuck, and pump impeller blade fracture etc. in turn results in cooling system event
Barrier, influences machine normal operation.Therefore chloride ion content in coolant must be strictly controlled, cooling system could be reduced
Failure, it is ensured that engine work.
At present, the method for measuring chloride ion content also has much, such as at present：
1) SH/T0621-95 engine coolants chloride content determination method, the standard at reflux, are dripped using current potential
Determine method and measure chloride ion content, it is relatively large to the detection error of Micro Amounts of Chlorine and cumbersome, while some additive capacities are high
When, measurement result is seriously affected, the additive interference in Condition of Engine Coolant for Heavy Duty Engines can not be eliminated.Also heavy burden cannot be used for
The measure of chloride ion content in lotus engine coolant.
2) Yao Yongsheng " chloride ion content in flame atomic absorption spectrometry indirect determination lime " (《Metallurgical analysis》2011
1 phase of year) using Dissolving Simple with Nitric Acid, the chlorion of equivalent is added in sample and curve, excessive silver ion is added and forms silver chlorate
Saturated solution, after filtering silver nitride precipitation, the silver ion of flame atomic absorption spectrometry excess.Since atomic absorption method is examined in itself
Survey the restriction of range, it is desirable that could be measured to measuring after solution is diluted, dilution has been introduced while increasing operating procedure and has been missed
Difference.
3) indirect determination of the flame atomic absorption spectrometrys such as Wang Yajian, Zhang Libo oxidation flue dust in chlorine (《Metallurgical analysis》
7 phases in 2013), using the molten sample of dust technology, add in excessive silver ion and form silver chlorate saturated solution, filter silver nitride precipitation
Afterwards, the silver ion of flame atomic absorption spectrometry excess.Equally there is also the restriction due to atomic absorption method detection range itself,
It is required that could be measured to measuring after solution is diluted, dilution error has been introduced while increasing operating procedure.
4) Qian Chuhong, the skilful English of beam etc. in atomic absorption method indirect determination ethanedioic acid ammonium Micro Amounts of Chlorine (《Using chemical industry》
6th phase in 2003), nitric acid treatment sample adds standard silver nitrate a certain amount of, curve be in different Chloride Solutions add in
The silver nitrate solution of sample same amount after being centrifuged at a high speed, measures the silver ion content of supernatant liquor, is converted to and is equivalent to measure
The chloride ion content gone out, this method is complicated for operation, and silver nitrate addition can not be complete when chlorinity is higher in unknown sample
Full precipitation chlorion.
5) Wang Chuanhua, Micro Amounts of Chlorine in atomic absorption spectrophotometry indirect determination phosphoric acid by wet process (《Phosphate fertilizer and compound fertilizer》2006
The 4th phase of year), silver nitrate standard liquid is added in nitric acid environment, adds ethanol solution, precipitates Isolating chlorinated silver, atomic absorption spectrometry is surveyed
Fixed remaining silver content, calculates chloride ion content, this method with 4) there are it is similary the problem of.
6) Ye Xiaoping, Indirect Determination of Trace Chlorine in High-valence Rare Earth Oxide by GFAAS Method (《Rare earth》2006
The 2nd phase of year), hydrogen peroxide and nitric acid treatment sample add in silver-colored standard solution precipitation chlorion, live in ethyl alcohol-gelatin and surface
Property agent in the presence of, centrifugation separation, the silver ion of graphite furnace atomic absorption spectrometry excess is converted into chloride ion content.
7) Wei Wenye, Chloride selective electrode directly measure chloride ion content in zinc indium electrolyte (《Metallurgical analysis》2011
Year 8 phases), this method is measured using single-minded chlorinity meter, and equipment determines resultant error relatively using single-minded to Micro Amounts of Chlorine
Greatly.
Method 1) and 7) be it is direct measure chloride ion content, but to Micro Amounts of Chlorine measurement result can error it is larger.Method 2),
3) it is, 4), 5) He 6) chloride ion content in atomic absorption spectrometry indirect determination different material.Above-mentioned 1) SH/T0621-95 hairs
Motivation coolant chloride content determination method, the coolant that defining can measure must satisfy mercaptobenzothiazoler content and be no more than
0.6%, otherwise measurement result deviation is larger.Method 2), 3), 4), 5), 6) He 7) be not measure coolant in Micro Amounts of Chlorine from
Son, method can't be directly used in the measure of chloride ion content in coolant.Since heavy load diesel engine coolant is situated between
Matter is different from general fluid dielectric coolant, and interference component is not quite similar, and has company to be limited in the checking and accepting technology standard of oneself enterprise
Determine chloride ion content to be allowed to be no more than 20mg/kg in coolant, well below the 60mg/kg of chemical industry standard.Above-mentioned chlorine
The assay method of ion concentration can not meet the measure of trace chlorine in used with tractor heavy-duty diesel engine coolant.
Therefore, these above-mentioned methods cannot be directly used to measure the chloride ion content in heavy load diesel engine coolant.
How the chloride ion content in Accurate Determining field engine coolant becomes a urgent problem to be solved.
Invention content
In order to solve the above technical problems, the present invention provides chloride ion contents in a kind of field engine coolant
Assay method, measurement result can chloride ion content in accurate response field engine coolant, have that precision is high, weight
The advantages that existing property is good, and measurement result is accurate.
To achieve these goals, the present invention adopts the following technical scheme that：
The assay method of chloride ion content, material therefor are in a kind of field engine coolant：Concentrated nitric acid, peroxide
Change hydrogen, chlorine standard solution, silver-colored standard solution, coolant to be detected, device therefor is ICP inductively coupled plasma atomic emissions
Spectrometer；
Detection sample is made to digest completely using concentrated nitric acid and hydrogen peroxide, add in excessive silver-colored standard solution, in heating shape
Under state, chlorination silver sol is made to form cotton-shaped silver nitride precipitation, liquid to be determined is formed after filtering precipitation, ICP inductive couplings etc. from
Under daughter atom emission spectrometer best operating condition, the excessive silver ion content in liquid to be determined is measured, i.e., measured by
Silver ion content calculates chloride ion content to be determined；It is as follows：
1), experiment condition is determining：
1.1 treatments of the sample acid：The reagent used is 25mL, hydrogen peroxide 10mL for concentrated nitric acid dosage；
1.2 inductively coupled plasma atomic emission spectrometer ICP measure the operating condition of silver content：Including：Plasma
Body atomic emissions power, peristaltic pump sample lifting capacity, atomizer and atomizing pressure, analysis spectral line selection, cooling gas, auxiliary gas,
Carrier gas, best observation position, the selection of time of integration setting；
2), analyzing detecting method：
The resolution processing of 2.1 samples：Coolant sample 5.0000g to be determined is weighed in 250mL beakers, enriching nitric acid
Sample is placed on hot digestion on electric furnace by 25mL, and after treatments of the sample is complete, hydrogen peroxide 10mL is added dropwise, and treats that reaction is not fierce
Afterwards, continue to be heated to hydrogen peroxide decomposition completely, remove and be cooled to room temperature；
2.2, which measure liquid, prepares：The chlorion standard solution of 0.01mg/mL is accurately added in the solution produced to 2.1 steps
10mL, the accurate silver ion standard solution 10mL for adding in 1.0mg/mL, makes it generate silver nitride precipitation, to make silver chlorate sol form
Precipitation is converted into the flocculent deposit easily filtered, and low-temperature heat boils solution 30min, removes and be cooled to room temperature, with slow filter paper mistake
It filters in 100mL volumetric flasks, rinses beaker and precipitation for several times with nitric acid washing lotion, be diluted with water to scale, shake up, this liquid is sample
Liquid to be determined；
The preparation of 2.3 working curves：The accurate silver ion standard solution for drawing 1.0mg/mL respectively, 0,1.0mL, 2.0mL,
4.0mL, 6.0mL, 8.0mL, 10.0mL are simultaneously respectively placed in seven 100mL volumetric flasks, are added nitric acid 5mL, are diluted with water to
100mL shakes up, this group of liquid is working curve liquid to be determined；
The operating condition of 2.4 determining inductively coupled plasma atomic emission spectrometer ICP：
Inductively coupled plasma atomic emission spectrometer ICP operating conditions and running parameter are as follows：RF power：1.1KW；
Cooling gas flow：18mL/min, secondary air amount 0.5mL/min, nebulizer gas pressure, that is, atomizing pressure 40pis；Time of integration 30s；
Peristaltic pump sample lifting capacity 1.9mL, best observation position be 5.0mm, analysis spectral line：328.068nm；
The measure of 2.5 samples：It is to be determined with the working curve of step 2.3 under the instrument operating condition selected in step 2.4
First point of (0.0) suppressed zero of liquid, measures the luminous intensity of working curve liquid silver ion to be determined, and instrument contains according to silver ion
Amount and the corresponding luminous intensity values drawing curve measured；Instrument working curve under the conditions of measure liquid to be determined silver from
Sub- content；
The calculating of 2.6 chloride ion contents：
Chlorion is with reacting for silver ion：Cl-1+Ag+1=AgCl ↓ it is reaction with same mole, chloride ion content to be determined
Calculation formula is as follows：
In formula：C is the excessive silver ion amount determined, unit mg；M is sample weighting amount, unit g；ω for measure liquid in chlorine from
Son amount, unit mg/kg.
The assay method of chloride ion content in a kind of field engine coolant, the reagent of the method is excellent
Grade pure reagent, the guaranteed reagent used for concentrated nitric acid, hydrogen peroxide, concentrated nitric acid, hydrogen peroxide dosage be respectively 25mL,
10mL；Four parts of 5.0000g coolants sample is weighed in 4 250mL beakers, it is dense to be separately added into 15mL, 20mL, 25mL, 30mL
After treatments of the sample is complete, hydrogen peroxide 5,8,10,15mL, sample is added dropwise in nitric acid acid, the hot digestion sample on low-temperature furnace
Resolution is very fast and resolution be completely addition be concentrated nitric acid acid is 25mL, 30mL, hydrogen peroxide 10mL, 15mL, and ICP is wriggled
When pump promotes sample solution, the acid in sample liquid can influence the atomizing effect of sample introduction speed and atomizer, select as far as possible it is relatively low and
It is proper amount of acid processing sample, the addition for selecting concentrated nitric acid acid is 25mL, hydrogen peroxide 10mL, hydrogen peroxide heat resolve into
Water does not influence the atomizing effect of sample introduction speed and atomizer.
The assay method of chloride ion content in a kind of field engine coolant, described with water is ultra-pure water.
The assay method of chloride ion content in a kind of field engine coolant, the inductively coupled plasma are former
The RF power of sub- emission spectrometer ICP determines：2mL silver standard solution is taken to be placed in a 100mL volumetric flask, adds in concentrated nitric acid
5mL is settled to 100mL scales with water, shakes up, measures the luminous intensity values of silver ion；Different RF watt levels are adjusted to carry out
Experiment, RF power increases so that the intensity of spectral line enhancing, but background is increased faster simultaneously, thus signal-to-background ratio increase with RF power and
Decline；Experiment is shown to be conducive to obtain big signal-to-background ratio and Detection capability, but matrix effect is heavier when RF power is low；RF is using big
Power can mitigate matrix effect, but signal-to-background ratio and detection limit are damaged, and when RF power is excessive easily burns out quarter bend, reduces quarter bend
Service life；Experiment selects RF power as 1.1KW.
The assay method of chloride ion content in a kind of field engine coolant, the inductively coupled plasma are former
Sub- emission spectrometer ICP gases used is high-purity argon gas, and argon flow amount determines：2mL silver standard solution is taken to be placed in a 100mL
In volumetric flask, concentrated nitric acid 5mL is added in, 100mL scales is settled to water, shakes up, measure the light intensity value of silver, adjust plasma
Gas, cooling gas and secondary air amount measure the light intensity value of silver；Experiment it is selected wait nebulizer gas pressures for nebulizer pressure 40pis,
Cool down gas 20L/min and secondary air amount 0.5L/min.
The assay method of chloride ion content in a kind of field engine coolant, the inductively coupled plasma are former
The best observation position of sub- emission spectrometer ICP determines：2mL silver standard solution is taken to be placed in a 100mL volumetric flask, is added in dense
Nitric acid 5mL is settled to 100mL scales with water, shakes up, and measures the light intensity value of silver.The different location of quarter bend is adjusted, measures silver
Luminous intensity values, torch pipe central tube and the distance of coil lower edge should be suitably increased at about 5.0mm, measure the absorbance value of silver
Maximum is tested and determines that best observation position is 5.0mm.
The assay method of chloride ion content in a kind of field engine coolant, the inductively coupled plasma are former
The selection of the analysis spectral line wavelength of sub- emission spectrometer ICP：Instrument use silver analysis spectral line for：328.068nm、
224.643nm, 241.323nm, 338.289nm, wherein, the signal-to-noise ratio of 224.643nm is 230, and existing interference element is Sn
And Pb；241.323nm signal-to-noise ratio is 150, and there are chaff elements to be known as：Co Mo Hf Eu Ir Th Se；338.289nm make an uproar than for
2300, there are chaff elements to be known as：Mo Ti Cr Pu Sb；328.068nm makes an uproar than being 3800, without common element disturbance；From these
Spectral line interference sees that the analysis spectral line wavelength that can be used is determining according to signal-to-noise ratio and experiment for 328.068nm, use wavelength for
328.068nm spectral line is the analysis spectral line of this method.
The assay method of chloride ion content in a kind of field engine coolant, the method experimental result accuracy
Verification --- the measure of the rate of recovery：It is using reagent：Concentrated nitric acid, hydrogen peroxide, chlorine standard solution：0.01mg/mL, silver label are accurate
Solution：1.0mg/mL；The reagent is top pure grade, and water used is ultra-pure water；It weighs coolant 5.0000g 4 and is respectively placed in 4
In a 150mL beakers, not chlorination standard solution in a beaker, another 3 are separately added into reagent 0.01mg/mL chlorine solution amounts and are
5.0mg, 10.0mg, 15.0mg, formed Standard entertion liquid, by the operating procedure in 2 analyzing detecting method of above-mentioned steps survey this four
Chloride ion content in a coolant, the measured value of mark-on liquid subtract the measured value for being not added with standard liquid, are recycled rate measurement result.
The assay method of chloride ion content in a kind of field engine coolant, the method experimental result reproducibility
Verification --- the measure of precision：The digestion of sample：With step 1, wherein step 1.2, which uses, adds in concentrated nitric acid amount as 25mL；
Working curve is prepared, ICP inductively coupled plasma atomic emission spectrometers operating condition is the same as chloride ion content in coolant
Determination step；The measure of sample：Under the instrument operating condition selected, with first point in working curve liquid to be determined
(0.0) suppressed zero measures the luminous intensity values of working curve liquid silver to be determined, according to silver content and corresponding luminous intensity values
Drawing curve.Measuring the luminous intensity of submitted sample liquid excess silver ion to be determined is worth corresponding excessive silver ion to contain
Amount, calculates chloride ion content.
By adopting the above-described technical solution, the present invention has the advantages that：
1) in field engine coolant of the present invention chloride ion content assay method, due in coolant
There are many organic matter and inorganic additive, preservative etc., experiment can be disappeared completely using nitric acid, hydrogen peroxide treatment sample
Organic matter is solved, and the element of the generations such as the sulphur in a small amount of preservative interference can be aoxidized, sulphur etc. has been eliminated and has been generated with silver and sunk
The interference of the coexistence elements in shallow lake.On the analysis spectral line of the selected wavelength of analysis, ICP inductively coupled plasma atomic emission spectrums
When method measures silver ion, matrix can be ignored with oligo-element interference coexists, that is to say, that dry this invention removes precipitation
Disturb the physics and chemistry disruption when being detected with equipment；
2) in field engine coolant of the present invention chloride ion content assay method, using ICP inductance
Excessive silver ion content contains to calculate chlorion after coupled plasma-atomic emission spectrographic determination generation silver nitride precipitation
Amount, easy to operate, quick, environmentally friendly, measurement result is more accurate, and method is stablized, reliable and practical；
3) in field engine coolant of the present invention chloride ion content assay method, sunk using silver ion
Trace chlorine in the coolant of shallow lake actively with the concentration effect of chlorion and silver ion, promotes the generation of silver nitride precipitation,
Reduce the solubility of silver nitride precipitation so that chlorion precipitation to be determined is complete, and does not have to dilution during measure excess silver ion, can
Directly upper machine measures, and reduces the error that dilution operation is brought repeatedly, measurement result is more accurate；
4) in field engine coolant of the present invention chloride ion content assay method, using ICP inductance couplings
It closes plasma atomic emission spectrometry and measures micro and trace chloro ion in field engine coolant, compared with technical background
In flame atomic absorption spectrometry detection limit it is lower, detection range is broader, and measurement result is more accurate.
Specific embodiment
The purpose of the assay method of chloride ion content in a kind of open field engine coolant of the present invention, it is intended to protect
All changes and improvements in the scope of the invention are protected, embodiment below is not limitation of the invention.By following
The present invention can be explained in more detail in embodiment：
The assay method of chloride ion content, material therefor are in a kind of field engine coolant：Concentrated nitric acid；Peroxide
Change hydrogen；Silver-colored standard solution：1.0mg/mL；Chlorine standard solution：0.01mg/mL；Device therefor is former for ICP inductively coupled plasmas
Sub- emission spectrometer.Sample product to be determined is made to be digested to sample liquid to be determined completely using concentrated nitric acid, hydrogen peroxide, in ICP inductance
Under coupled plasma-atomic emission spectrometer best operating condition, the silver ion measured in sample to be determined liquid to be determined contains
Amount；It is as follows：
1st, experiment condition is determining：
1.1 treatments of the sample acid：The reagent used is concentrated nitric acid, hydrogen peroxide, concentrated nitric acid, hydrogen peroxide
Dosage be respectively 25mL, 10mL；
1.2 inductively coupled plasma atomic emission spectrometer ICP measure the operating condition of chloride ion content：Including：Deng
Gas ions transmission power, peristaltic pump sample lifting capacity, atomizer and atomizing pressure, analysis spectral line selection, cooling gas, auxiliary gas,
Carrier gas, best observation position, the selection of time of integration setting；
2nd, analyzing detecting method：
2.1 Specimen eliminating：It accurately weighs coolant 5.0000g to be placed in 250mL beakers, adds in concentrated nitric acid low-temperature digestion sample
After treatments of the sample is complete, hydrogen peroxide 10mL is added dropwise in product, after reacting not fierce, continues to be heated to hydrogen peroxide to have decomposed
Entirely, it removes and is cooled to room temperature；
The preparation of 2.2 liquid to be determined：The chlorion standard of 0.01mg/mL is accurately added in the solution produced to 2.1 steps
Solution 10mL, the accurate silver ion standard solution 10mL for adding in 1.0mg/mL, makes it generate silver nitride precipitation in nitric acid medium,
For silver chlorate sol form precipitation is made to be converted into the flocculent deposit easily filtered, low-temperature heat boils solution 30min, removes and be cooled to room
Temperature with slow filter paper filtering in 100mL volumetric flasks, rinses beaker and precipitation for several times with nitric acid washing lotion, is diluted with water to scale,
It shakes up, this liquid is the liquid to be determined of sample to be determined；
The preparation of 2.3 working curves：The silver ion standard solution of absorption 1.0mg/ respectively, 0,1.0mL, 2.0mL, 4.0mL,
6.0mL, 8.0mL, 10.0mL are simultaneously respectively placed in seven 100mL volumetric flasks, are added nitric acid 5mL, are diluted with water to 100mL, shake up,
This group of liquid is working curve liquid to be determined；
The operating condition of 2.4 determining inductively coupled plasma atomic emission spectrometer ICP：
Inductively coupled plasma atomic emission spectrometer ICP operating conditions and running parameter are as follows：RF power：1.1KW；
Cooling gas flow：18mL/min, secondary air amount 0.5mL/min, nebulizer gas pressure (atomizing pressure) 40pis；Time of integration 30s；
Peristaltic pump sample lifting capacity 1.9mL, best observation position be 5.0mm, analysis spectral line：328.068nm；
The measure of 2.5 samples：Under selected instrument operating condition, with first point (0.0) of working curve liquid to be determined
Suppressed zero measures the luminous intensity of working curve liquid silver element to be determined, and instrument is according to silver ion content and corresponds to what is measured
Luminous intensity values drawing curve；Instrument measures the excessive silver ion content of liquid to be determined in working curve under the conditions of；
The calculating of 2.6 chloride ion contents
Chlorion is with reacting for silver ion：Cl-1+Ag+1=AgCl ↓ it is reaction with same mole, chloride ion content to be determined
Calculation formula is as follows：
In formula：
C --- the excessive silver ion amount determined, mg；
M --- sample weighting amount, g；
ω --- measure amount of chloride ions in liquid, mg/kg；
The assay method of chloride ion content, the method are top grade with reagent in a kind of field engine coolant
Pure, water used is ultra-pure water.The reagent used for concentrated nitric acid, hydrogen peroxide, concentrated nitric acid, hydrogen peroxide dosage be respectively
25mL、10mL；Four parts of 5.0000g coolants sample is weighed in 4 250mL beakers, be separately added into 15mL, 20mL, 25mL,
30mL concentrated nitric acids acid, the hot digestion sample on low-temperature furnace, after treatments of the sample is complete, be added dropwise hydrogen peroxide 5,8,10,
15mL, Specimen eliminating is very fast and resolution be completely addition be concentrated nitric acid acid is 25mL, 30mL, hydrogen peroxide 10mL,
When 15mL, ICP peristaltic pump promote sample solution, the acid in sample liquid can influence the atomizing effect of sample introduction speed and atomizer, to the greatest extent may be used
Relatively low and proper amount of acid processing sample can be selected, the addition for selecting concentrated nitric acid acid is 25mL, hydrogen peroxide 10mL, peroxidating
Hydrogen heat resolve Cheng Shui does not influence the atomizing effect of sample introduction speed and atomizer；
ICP radio-frequency generator RF power determines：2mL silver standard solution is taken to be placed in a 100mL volumetric flask, adds in dense nitre
Sour 5mL is settled to 100mL scales with water, shakes up, measures the luminous intensity values of silver ion；Adjust different RF watt levels into
Row experiment, RF power increases so that the intensity of spectral line enhances, but background is increased faster simultaneously, therefore signal-to-background ratio increases with RF power
And decline.Experiment is shown to be conducive to obtain big signal-to-background ratio and Detection capability, but matrix effect is heavier when RF power is low；RF is used
It is high-power to mitigate matrix effect, but signal-to-background ratio and detection limit are damaged, and when RF power is excessive easily burn out quarter bend, reduce square
Pipe service life.Experiment selects RF power as 1.1KW；
The ICP gases used is high-purity argon gas, and argon flow amount determines：2mL silver standard solution is taken to be placed in a 100mL
In volumetric flask, concentrated nitric acid 5mL is added in, 100mL scales is settled to water, shakes up, measure the light intensity value of silver, adjust plasma
Gas, cooling gas and secondary air amount measure the light intensity value of silver.Experiment is selected to wait nebulizer gas pressures (nebulizer pressure) 40pis, cold
But gas 20L/min and secondary air amount 0.5L/min；
The best observation position determines：2mL silver standard solution is taken to be placed in a 100mL volumetric flask, adds in dense nitre
Sour 5mL is settled to 100mL scales with water, shakes up, and measures the light intensity value of silver.The different location of quarter bend is adjusted, measures the hair of silver
Light intensity value, torch pipe central tube and the distance of coil lower edge should be suitably increased at about 5.0mm, measure the absorbance value of silver most
Greatly.Experiment determines that best observation position is 5.0mm；
The selection of the analysis spectral line wavelength：Since the analysis spectral line of silver that instrument is recommended is：328.068nm、
224.643nm, 241.323nm, 338.289nm, wherein, the signal-to-noise ratio of 224.643nm is 230, and existing interference element is Sn
And Pb；241.323nm signal-to-noise ratio is 150, and there are chaff elements to be known as：Co Mo Hf Eu Ir Th Se；338.289nm make an uproar than for
2300, there are chaff elements to be known as：Mo Ti Cr Pu Sb；328.068nm makes an uproar than being 3800, without common element disturbance.From these
Spectral line interference see, adoptable analysis spectral line wavelength be 328.068nm, according to signal-to-noise ratio and experiment determine, use wavelength for
328.068nm spectral line is the analysis spectral line of this method.
Embodiment one
1. add in influence of the different nitric acid amounts to the measurement result of chloride ion content in coolant sample liquid to be determined；
1.1 Specimen eliminating：It is accurate to weigh coolant 5.0000g and be placed in 250mL beakers, add in concentrated nitric acid 15,20,25,
30mL low-temperature digestion samples after treatments of the sample is complete, are added dropwise hydrogen peroxide 10mL, after reacting not fierce, continue to be heated to
Hydrogen peroxide decomposes completely, removes and is cooled to room temperature；
The preparation of 1.2 liquid to be determined：The chlorion standard of 0.01mg/mL is accurately added in the solution produced to 1.1 steps
Solution 10mL adds in the silver ion standard solution 10mL of 1.0mg/mL, it is made to generate silver nitride precipitation, to make silver chlorate sol form
Precipitation is converted into the flocculent deposit easily filtered, and low-temperature heat coctoprecipitinogen solution 30min is removed and is cooled to room temperature, with filtering at a slow speed
Paper is filtered in 100mL volumetric flasks, is rinsed beaker and precipitation for several times with nitric acid washing lotion, is diluted with water to scale, shakes up, this liquid is
Sample liquid to be determined；
The preparation of 1.3 working curves：The silver ion standard solution of absorption 1.0mg/ respectively, 0,1.0mL, 2.0mL, 4.0mL,
6.0mL, 8.0mL, 10.0mL are simultaneously respectively placed in seven 100mL volumetric flasks, are added nitric acid 5mL, are diluted with water to 100mL, shake up,
This group of liquid is working curve liquid to be determined；
The operating condition of 1.4 determining inductively coupled plasma atomic emission spectrometer ICP：
Inductively coupled plasma atomic emission spectrometer ICP operating conditions and running parameter are as follows：
The measure of 1.5 samples：Under selected instrument operating condition, with first point (0.0) of working curve liquid to be determined
Suppressed zero measures the luminous intensity of working curve liquid silver element to be determined, and instrument is according to silver ion content and corresponds to what is measured
Luminous intensity values drawing curve；Instrument measures the excessive silver ion content of liquid to be determined in working curve under the conditions of.Point
The measurement result that chloride ion content is not calculated is as shown in table 1 below：
1 different solutions acid of table clears up sample, gained chlorine ion content determination result
Conclusion：As can be seen from the above table, the difference of sample concentrated nitric acid amount is cleared up, complete degree is not to sample treatment
It is different with the measurement result obtained.Only when the sour dosage of resolution reaches enough, sample could be cleared up completely, could Accurate Determining
Chloride ion content in coolant.
Embodiment two
The measure of the verification of experimental result accuracy --- the rate of recovery：
It is using reagent：Concentrated nitric acid, hydrogen peroxide, chlorine standard solution：0.01mg/mL, silver-colored standard solution：1.0mg/mL；
The reagent is top pure grade, and water used is ultra-pure water；Coolant 5.0000g 4 is weighed to be respectively placed in 4 150mL beakers,
Not chlorination standard solution in one beaker, another 3 be separately added into reagent 0.01mg/mL chlorine solutions amount for 5.0mg, 10.0mg,
15.0mg forms Standard entertion liquid, the chlorine in this four coolants is surveyed by the operating procedure in 2 analyzing detecting method of above-mentioned steps
Ion concentration, the measured value of mark-on liquid subtract the measured value for being not added with standard liquid, and it is as shown in table 2 below to be recycled rate measurement result：
Table 2：Determination of recovery rates result
The rate of recovery of measurement result illustrates that this method accuracy of measurement is higher in table, meets field engine coolant
Middle chloride ion content accuracy requirement.
Embodiment three
The measure of the verification of experimental result reproducibility --- precision：
The digestion of sample：With the step 1 of embodiment one, wherein step 1.2, which uses, adds in concentrated nitric acid amount as 25mL；
The step of working curve is prepared, ICP inductively coupled plasma atomic emission spectrometers operating condition is with embodiment 1
2、3；
The measure of sample：Under the instrument operating condition selected, with first point (0.0) in working curve liquid to be determined
Suppressed zero measures the luminous intensity values of working curve liquid silver to be determined, is drawn according to silver content and corresponding luminous intensity values
Working curve.Measuring the luminous intensity of submitted sample liquid excess silver ion to be determined is worth corresponding excessive silver ion content, meter
Calculate chloride ion content such as the following table 3：
By this instance analysis assay method step operation, 7 replications, measurement result such as the following table 3 are carried out：
Table 3:7 replication results
It is as shown in the table, measurement result relatively, illustrate in field engine coolant of the present invention chlorine from
The advantages of assay method of sub- content has structure favorable reproducibility, and precision is high.
Therefore, pass through the verification of above-mentioned embodiment, it can be seen that field engine coolant of the present invention
The assay method of middle chloride ion content has the advantages that precision is high, favorable reproducibility, measurement result is accurate.
Claims (9)
1. the assay method of chloride ion content in a kind of field engine coolant, it is characterized in that：Material therefor is：Dense nitre
Acid, hydrogen peroxide, chlorine standard solution, silver-colored standard solution, coolant to be detected, device therefor are ICP inductively coupled plasmas
Atomic Emission Spectrometer AES；
Detection sample is made to digest completely using concentrated nitric acid and hydrogen peroxide, add in excessive silver-colored standard solution, in a heated state,
Chlorination silver sol is made to form cotton-shaped silver nitride precipitation, liquid to be determined is formed after filtering precipitation, in ICP inductively coupled plasmas original
Under sub- emission spectrometer best operating condition, the excessive silver ion content in liquid to be determined is measured, i.e., according to measured silver ion
Content meter calculates chloride ion content to be determined；It is as follows：
1), experiment condition is determining：
1.1 treatments of the sample acid：The reagent used is 25mL, hydrogen peroxide 10mL for concentrated nitric acid dosage；
1.2 inductively coupled plasma atomic emission spectrometer ICP measure the operating condition of silver content：Including：Plasma is former
Sub- transmission power, peristaltic pump sample lifting capacity, atomizer and atomizing pressure, analysis spectral line selection, cooling gas, auxiliary gas, carrier gas,
Best observation position, the selection of time of integration setting；
2), analyzing detecting method：
The resolution processing of 2.1 samples：Coolant sample 5.0000g to be determined is weighed in 250mL beakers, enriching nitric acid 25mL,
Sample is placed on hot digestion on electric furnace, after treatments of the sample is complete, hydrogen peroxide 10mL is added dropwise, after reacting not fierce, after
The continuous hydrogen peroxide that is heated to decomposes completely, removes and is cooled to room temperature；
2.2, which measure liquid, prepares：The chlorion standard solution 10mL of 0.01mg/mL is accurately added in the solution produced to step 2.1,
The accurate silver ion standard solution 10mL for adding in 1.0mg/mL, makes it generate silver nitride precipitation, to precipitate silver chlorate sol form
Be converted into the flocculent deposit easily filtered, low-temperature heat boils solution 30min, removes and be cooled to room temperature, with slow filter paper filtering in
In 100mL volumetric flasks, rinse beaker and precipitation for several times with nitric acid washing lotion, be diluted with water to scale, shake up, this liquid is to be measured for sample
Determine liquid；
The preparation of 2.3 working curves：The accurate silver ion standard solution for drawing 1.0mg/mL respectively, 0,1.0mL, 2.0mL,
4.0mL, 6.0mL, 8.0mL, 10.0mL are simultaneously respectively placed in seven 100mL volumetric flasks, are added nitric acid 5mL, are diluted with water to
100mL shakes up, this group of liquid is working curve liquid to be determined；
The operating condition of 2.4 determining inductively coupled plasma atomic emission spectrometer ICP：
Inductively coupled plasma atomic emission spectrometer ICP operating conditions and running parameter are as follows：RF power：1.1KW；Cooling
Throughput：18mL/min, secondary air amount 0.5mL/min, nebulizer gas pressure, that is, atomizing pressure 40pis；Time of integration 30s；It wriggles
Pump sample lifting capacity 1.9mL, best observation position be 5.0mm, analysis spectral line：328.068nm；
The measure of 2.5 samples：Under the instrument operating condition selected in step 2.4, with the working curve of step 2.3 liquid to be determined
1: 0.0 suppressed zero measures the luminous intensity of working curve liquid silver ion to be determined, and instrument is according to silver ion content and right
The luminous intensity values drawing curve that should be measured；The silver ion that instrument measures liquid to be determined in working curve under the conditions of contains
Amount；
The calculating of 2.6 chloride ion contents：
Chlorion is with reacting for silver ion：Cl-1+Ag1+=AgCl ↓ and for reaction with same mole, the calculating of chloride ion content to be determined
Formula is as follows：
In formula：C is the excessive silver ion amount determined, unit mg；M is sample weighting amount, unit g；ω is amount of chloride ions in measure liquid,
Unit mg/kg.
2. the assay method of chloride ion content, feature in a kind of field engine coolant as described in claim 1
It is：The reagent of the method is guaranteed reagent, and the guaranteed reagent used is concentrated nitric acid, hydrogen peroxide, concentrated nitric acid, mistake
The dosage of hydrogen oxide is respectively 25mL, 10mL；Four parts of 5.0000g coolants sample is weighed in 4 250mL beakers, is added respectively
Enter 15mL, 20mL, 25mL, 30mL concentrated nitric acid acid, the hot digestion sample on low-temperature furnace after treatments of the sample is complete, is added dropwise
Hydrogen peroxide 5,8,10,15mL, Specimen eliminating is very fast and resolution be completely addition be concentrated nitric acid acid is 25mL, 30mL, mistake
Hydrogen oxide 10mL, 15mL, when ICP peristaltic pumps promote sample solution, the acid in sample liquid can influence the mist of sample introduction speed and atomizer
Change effect, select relatively low and proper amount of acid processing sample as far as possible, the addition for selecting concentrated nitric acid acid is 25mL, hydrogen peroxide
10mL, hydrogen peroxide heat resolve Cheng Shui do not influence the atomizing effect of sample introduction speed and atomizer.
3. the assay method of chloride ion content, feature in a kind of field engine coolant as described in claim 1
It is：Described with water is ultra-pure water.
4. the assay method of chloride ion content, feature in a kind of field engine coolant as described in claim 1
It is：The RF power of the inductively coupled plasma atomic emission spectrometer ICP determines：2mL silver standard solution is taken to be placed in one
In 100mL volumetric flasks, concentrated nitric acid 5mL is added in, 100mL scales is settled to water, shakes up, measure the luminous intensity values of silver ion；
Different RF watt levels are adjusted to be tested, RF power increases so that the intensity of spectral line enhances, but background is increased fast simultaneously, because
This signal-to-background ratio increases with RF power and is declined；Experiment, which is shown, to be conducive to increase signal-to-background ratio and Detection capability when RF power reduces, but
Matrix effect weight；Matrix effect can be mitigated, but signal-to-background ratio and detection limit are damaged, and RF power increased using increase RF power
Quarter bend is easily burnt out when big, reduces quarter bend service life；Experiment selects RF power as 1.1KW.
5. the assay method of chloride ion content, feature in a kind of field engine coolant as described in claim 1
It is：The inductively coupled plasma atomic emission spectrometer ICP gases used is high-purity argon gas, and argon flow amount determines：It takes
2mL silver standard solution is placed in a 100mL volumetric flask, is added in concentrated nitric acid 5mL, is settled to 100mL scales with water, shakes up, and is surveyed
The light intensity value of fixed silver adjusts plasma (orifice) gas, cooling gas and secondary air amount, measures the light intensity value of silver；What experiment was selected etc.
Nebulizer gas pressure is nebulizer pressure 40pis, cooling gas 20L/min and secondary air amount 0.5L/min.
6. the assay method of chloride ion content, feature in a kind of field engine coolant as described in claim 1
It is：The best observation position of the inductively coupled plasma atomic emission spectrometer ICP determines：2mL silver standard solution is taken to put
In a 100mL volumetric flask, concentrated nitric acid 5mL is added in, 100mL scales is settled to water, shakes up, measure the light intensity value of silver；
The different location of quarter bend is adjusted, measures the luminous intensity values of silver, torch pipe central tube and the distance of coil lower edge should be suitably increased to
At about 5.0mm, the absorbance value for measuring silver is maximum；Experiment determines that best observation position is 5.0mm.
7. the assay method of chloride ion content, feature in a kind of field engine coolant as described in claim 1
It is：The selection of the analysis spectral line wavelength of the inductively coupled plasma atomic emission spectrometer ICP：In instrument using point of silver
Analysing spectral line is：328.068nm, 224.643nm, 241.323nm, 338.289nm, wherein, the signal-to-noise ratio of 224.643nm is 230,
Existing interference element is Sn and Pb；241.323nm signal-to-noise ratio is 150, and there are chaff elements to be known as：Co Mo Hf Eu Ir Th
Se；338.289nm signal-to-noise ratio is 2300, and there are chaff elements to be known as：Mo Ti Cr Pu Sb；328.068nm signal-to-noise ratio is 3800,
Without common element disturbance；From these spectral lines interfere, the analysis spectral line wavelength that can be used for 328.068nm, according to signal-to-noise ratio with
Experiment determines, uses wavelength as analysis spectral line that 328.068nm spectral lines are this method.
8. the assay method of chloride ion content, feature in a kind of field engine coolant as described in claim 1
It is：The verification of the method experimental result accuracy --- the measure of the rate of recovery：It is using reagent：Concentrated nitric acid, hydrogen peroxide, chlorine
Standard solution：0.01mg/mL, silver-colored standard solution：1.0mg/mL；The reagent is top pure grade, and water used is ultra-pure water；It weighs
Coolant 5.0000g 4 is respectively placed in 4 150mL beakers, and not chlorination standard solution in a beaker, another 3 are separately added into
Reagent 0.01mg/mL chlorine solutions amount is 5.0mg, 10.0mg, 15.0mg, forms Standard entertion liquid, analyzes and examines by above-mentioned steps 2
Operating procedure in survey method surveys the chloride ion content in this four coolants, and the measured value of mark-on liquid subtracts the survey for being not added with standard liquid
Definite value is recycled rate measurement result.
9. the assay method of chloride ion content, feature in a kind of field engine coolant as described in claim 1
It is：The verification of the method experimental result reproducibility --- the measure of precision：The digestion of sample：With the step 1 of method, wherein
Step 1.2, which uses, adds in concentrated nitric acid amount as 25mL；Working curve is prepared, ICP inductively coupled plasma atomic emission spectrometers
Operating condition is the same as the determination step of chloride ion content in coolant；The measure of sample：Under the instrument operating condition selected, use
The 1: 0.0 suppressed zero in working curve liquid to be determined measures the luminous intensity values of working curve liquid silver to be determined, foundation
Silver content and corresponding luminous intensity values drawing curve measure the luminous intensity of submitted sample liquid excess silver ion to be determined
It is worth corresponding excessive silver ion content, calculates chloride ion content.
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