CN110320167A - The denier analysis and diagnosis method of atom extinction photometer and atom extinction photometer - Google Patents
The denier analysis and diagnosis method of atom extinction photometer and atom extinction photometer Download PDFInfo
- Publication number
- CN110320167A CN110320167A CN201910247666.XA CN201910247666A CN110320167A CN 110320167 A CN110320167 A CN 110320167A CN 201910247666 A CN201910247666 A CN 201910247666A CN 110320167 A CN110320167 A CN 110320167A
- Authority
- CN
- China
- Prior art keywords
- pollution
- analysis
- atom extinction
- cup
- extinction photometer
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/01—Arrangements or apparatus for facilitating the optical investigation
- G01N21/15—Preventing contamination of the components of the optical system or obstruction of the light path
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/3103—Atomic absorption analysis
Landscapes
- Physics & Mathematics (AREA)
- Biochemistry (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Spectroscopy & Molecular Physics (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analysing Materials By Optical Means (AREA)
- Automatic Analysis And Handling Materials Therefor (AREA)
Abstract
The denier analysis and diagnosis method of the present invention offer atom extinction photometer and atom extinction photometer.In the case where carrying out denier analysis in electric heating atom extinction, when polluted influence, it is unable to get correct assay value.In the past, the measurement in advance for determining pollution sources was rule of thumb repeated in measurement person, needed time and labor.Analysis beginner can not carry out the judgement for pollution, the result that must be made mistake sometimes.The present invention completed to solve the above problems is the device and system with " denier analysis and diagnosis system ", it automates the sequence for the pollution for determining the liquor charging path comprising electric furnace, Autosampler including reaction cup, specimen cup and measurement solvent etc. with atom extinction photometer main body, Autosampler and operation PC.
Description
Technical field
The present invention relates to the pollution situation diagnostic methods and device of measurement system when progress denier analysis.
Background technique
In general, the metal of electric heating atom light absorption method measurement μ g/L rank.According to the difference of determination condition, additionally it is possible to
Carry out the denier Elements of ng/L rank.In the case where carrying out denier Elements, when electric furnace,
When sample liquor charging system has the pollution based on measure object element, it is unable to get correct assay value.Describe " data exception
The reason of caused mostly by pollution, therefore, will be because being managed to these." (non-patent literature 1).
When pollution confirmation before measurement is insufficient or does not determine pollution sources and is directly measured, it can not obtain sometimes
To high-precision analysis as a result, therefore, the pollution of reaction cup, the pollution of specimen cup, sample is examined successively before measurement starts
The pollution of liquor charging system is transferred to the measurement of sample after there is no problem in confirmation.
Patent document 1 discloses following technology: in order to carry out the judgement for pollution in electric heating atom extinction, simultaneously
It measures two or more metals and monitors from external pollution.Patent document 2, which discloses, efficiently cleans Autosampler
The technology of nozzle.Patent document 3 describes the technology of the clean method of the influence of the hydrofluoric acid after removal hydrofluoric acid solution measurement.
Here, pollution refers to, the object that residue of environment or measure object element etc. is generated due to the sample of pervious measurement
Matter remains in measurement system and impacts to the value of new measurement.
Existing technical literature
Patent document
Patent document 1: Japanese Unexamined Patent Publication 04-307353
Patent document 2: Japanese Unexamined Patent Publication 08-075756
Patent document 3: Japanese Unexamined Patent Publication 08-261917
Non-patent literature
Non-patent literature 1: clear department (2012) of horizontal well facilitates practice！Analytical chemistry natsume company from being learned basis
Summary of the invention
Subject to be solved by the invention
In the case where carrying out denier analysis in electric heating atomic absorption, when polluted influence, nothing
Method obtains correct assay value.Therefore, in the past, the measurement in advance for determining pollution sources is rule of thumb repeated in measurement person,
Need time and labor.Additionally, there are following projects: analysis beginner can not carry out malfunctioning sometimes for the judgement of pollution
Result accidentally.
In accordance with the invention it is possible to provide the beginner of analysis also without mistakenly progress micro-analysis without contaminated
Influence denier analytical equipment and denier analysis and diagnosis method.
Means for solving the problems
In order to solve the above problems, atomic absorption spectrum analysing arrangement of the invention has the atom for being able to carry out electric heating measurement
Extinction photometer main body, Autosampler and operation computer, have following micro-analysis diagnostic function: determining comprising anti-
Answering electric furnace including cup, the liquor charging path of Autosampler and specimen cup, whether there is or not the micro dirts based on measure object element
Dye.
The micro-analysis diagnostic function of atomic absorption spectrum analysing arrangement according to the present invention has following function: atom extinction
The measurement of photometric noise level；The reaction cup, the heating furnace, the liquor charging path comprising the Autosampler, institute
State the pollution evaluation of specimen cup, measurement solvent；And the evaluation of the reproducibility based on titer.
According to the micro-analysis diagnostic function, there is the function that diagnosis rank can be selected when micro-analysis diagnoses and starts
Energy.
In addition, atomic absorption analysis method according to the present invention, in the atom extinction photometer for being able to carry out electric heating measurement
Measurement start before determine the liquor charging path comprising electric furnace, Autosampler including reaction cup and specimen cup whether there is or not be based on
The micropollution of measure object element, wherein the method includes the following process: noise level sets process, measures the original
The noise level of sub- extinction photometer main body, sets it to the threshold value of the noise level；Reaction cup is polluted whether there is or not judgment process,
The heating that the reaction cup is carried out with the maximum temperature in the atom extinction photometer main body, according to the signal strength of detector
The signal strength for finding out the measure object element of the reaction cup, determines whether pollution；Furnace interior is polluted whether there is or not judgment process,
The defined heating and cooling in the atom extinction photometer main body are carried out, institute is found out according to the signal strength of the detector
The signal strength for stating the measure object element of electric furnace, determines whether pollution；Liquor charging system is polluted whether there is or not judgment process,
Pure water is imported into the detector via the Autosampler, according to the signal strength of the measure object element of detector
Determine comprising the Autosampler liquor charging system pollution whether there is or not；Whether there is or not judgment process for specimen cup pollution, via described automatic
Diluted acid in specimen cup is imported the detector by sampler, is sentenced according to the signal strength of the measure object element of detector
The pollution of the fixed specimen cup whether there is or not；And reproducibility confirms process, in reaction cup pollution, whether there is or not judgment process, furnace interior are dirty
Be infected with no judgment process, liquor charging system pollution whether there is or not judgment process, specimen cup pollution whether there is or not after judgment process, utilize measurement
The determination condition of object elements repeatedly measures standard sample, calculates standard deviation.
Invention effect
According to the present invention, it carries out the judgement polluted caused by device and environment and independent of the measurement of experience person and sentences
It is disconnected, it can be measured the cleaning or replacement of system as needed.The beginner of analysis be also able to carry out micro-analysis without
Make the misjudgment for pollution.
Detailed description of the invention
Fig. 1 is the figure for showing an example of the structure of atom extinction photometer of embodiments of the present invention.
Fig. 2 is the knot for showing the atomization portion and Autosampler portion of the atom extinction photometer of embodiments of the present invention
The figure of an example of structure.
Fig. 3 is the figure for showing an example of input picture of the atom extinction photometer of embodiments of the present invention.
Fig. 4 is figure the step of showing micro-analysis diagnostic system of the invention.
Fig. 5 is the figure for showing the setting procedure of noise level of micro-analysis diagnostic system of the invention.
The figure for the step of Fig. 6 is the reaction cup pollution judgment process for showing micro-analysis diagnostic system of the invention.
The figure for the step of Fig. 7 is the furnace interior pollution judgment process for showing micro-analysis diagnostic system of the invention.
The figure for the step of Fig. 8 is the liquor charging path pollution judgment process for showing micro-analysis diagnostic system of the invention.
Fig. 9 is figure the step of showing the specimen cup judgment process of micro-analysis diagnostic system of the invention.
Figure 10 is figure the step of showing the mensuration operation of the reproducibility of micro-analysis diagnostic system of the invention.
Figure 11 is figure the step of showing the mensuration operation of micro-analysis diagnostic system of the invention.
Label declaration
100: atom extinction photometer main part；110: light source portion；120: atomization portion；125: electric furnace；126: anti-
Answer cup；130: spectrum part；140: test section；200: sample injection unit (Autosampler: AS)；210: specimen cup；220: sample
Frame；230: nozzle；300: operation portion computer (PC)；310: control unit；320: record portion；330: data processing division；340:
Determination unit；350: input unit；360: display unit；410: measure object element sets window；420: the specimen cup confirmed
Quantity and setting place set window；430: the pollution criteria of specimen cup set window；440: the setting of titer reproducibility benchmark
Window.
Specific embodiment
In the following, the embodiments of the present invention will be described with reference to the drawings.
Fig. 1 is the structure chart of " denier analysis and diagnosis system " of the invention, by the atom for being able to carry out electric heating measurement
Extinction photometer main body 100, sample injection unit (Autosampler: AS) 200 and operation are constituted with portion computer (PC) 300.It is former
Sub- extinction photometer main body 100 for example polarizes Zeeman atomic extinction using new and high technology section, (Co., Ltd.) Hitachi length of schooling ZA3000
Photometer, as shown in Fig. 2, existing in atomization portion 120 comprising the electric furnace 125 including reaction cup 126, in automatic sampling
The specimen holder 220 for being provided with specimen cup 210 and the nozzle 230 for dispensing sample are provided in device 200.When 126 He of reaction cup
When there is the pollution of measurement element etc. in electric furnace 125, specimen cup 210 and nozzle 230, it is unable to get correctly measurement knot
Fruit.Therefore, the confirmation that do not polluted by each process of " denier analysis and diagnosis system " as shown below.Operation is used tricks
Calculation machine portion 300 has the control unit 310 controlled the movement of atom extinction main part 100；Store atom extinction main part
The record portion 320 of 100 determination condition, measurement result, preset threshold value etc.；To preset threshold value etc. and carry out self-test
The data processing division 330 that the signal strength in survey portion 140 is compared etc.；And the determination unit 340 of the judgement of pollution situation is carried out,
Input unit 350 has an input units such as mouse, keyboard, and display unit 360 shows the result of aftermentioned each process, mistake and for operation
The instruction etc. of member.
As shown in figure 11, in atomic absorption spectrum analysing arrangement, it is however generally that, after selection measurement element and condition
(S1120), operator whether there is according to regulation step sequentially determining comprising the electric furnace 125, automatic including reaction cup 126
The pollution of liquor charging path, specimen cup 210 and the measurement solvent of sampler 200 etc., determines dirty according to obtained signal strength etc.
Dye situation after the replacement or cleaning that carry out pollution portion, starts to carry out standard sample and unknown sample in polluted situation
Measurement.
Denier analyzing and diagnosing in the denier analyzing and diagnosing in atom extinction photometer of the invention, in Figure 11
In S1130 step, each process shown in Fig. 4 is carried out.Fig. 4 is process the step of showing " denier analyzing and diagnosing " of the invention
Figure.
Initially, operator selects a pollution determination step (S405) from following items.
あ: the pollution situation of decision analysis device entirety
い: there is no pollutions, therefore are only simply determined
う: suspecting there is pollution, and therefore, it is desirable to be cleaned (it is desirable that the shadow for the High concentration samples being measured before excluding tightly
It rings)
According to the selection project of operator, control unit 310 shows following instruction in display unit 360, is transferred to corresponding work
Sequence.
Select " あ ": the message of display [executing whole projects of denier analyzing and diagnosing] starts to carry out process A.
Select " い ": the message of display [carrying out the process A and step D of denier analyzing and diagnosing] starts to carry out process A.
Selection " う ": display [please remove reaction cup/ring, to cleaning in furnace.Please assembling new ring/reaction cup simultaneously
" あ " is selected after carrying out nozzle rinse.] message, carry out it is standby, until from input unit 350 input be ready to complete until.
At this point, selection " い ", in the case where being determined to be NG, passes through the finger of control unit 310 in the step D of following records
Show, atom extinction photometer main part 100 executes aftermentioned process A~step D.
In addition, about " denier analyzing and diagnosing ", as shown in figure 3, can before measurement starts in advance from input unit 350 into
Row setting below.
I: measure object element
II: the quantity of the specimen cup confirmed and setting place
III: process B, the pollution criteria value of C, D, E
IV: the regulation absorbance value of each element
Then, each process of denier analysis and diagnosis method is described in detail.
The setting process of A noise level
Fig. 5 is flow chart the step of showing " the setting process of A noise level " (S430) of the invention.
Operator implements nozzle check in 120 assembly reaction cup 126 (S510) of the atomization portion of atomic absorption spectrum analysing arrangement
(S520), the beginning of " denier analyzing and diagnosing " is indicated.Then, the letter after condition setting (S540), during 3 measurements 10 seconds
Number, value (a) (S560) of 3 average value as noise level of maximum absorbance is calculated, the value that setup algorithm goes out is used as and makes an uproar
Sound level (a) (S570).Here, nozzle check refers to that carrying out position is set so that nozzle enters the inlet of reaction cup, item
Part setting refer to the lamp for being measured element light/wavelength be aligned and set measure used in other conditions.
The pollution judgment process of B reaction cup
Fig. 6 is flow chart the step of showing " the pollution judgment process of B reaction cup " (S435) of the invention.
The 1st heating in atomization portion 120 is carried out with the maximum temperature that can be set in atomic absorption spectrum analysing arrangement 100
(S610), signal strength indication (b1) is obtained.Then, the 2nd heating (S630) in atomization portion 120 is equally carried out with the 1st time,
It obtains signal strength indication (b2).Determine after the 2nd heating obtained signal strength indication (bn) whether become noise level (a) with
Under (S650), display determine result.It is more than the noise water set in noise level setting process (S430) in signal strength indication (b)
In the case where flat (a), the heating (S660) in atomization portion 120 is carried out with maximum temperature again, confirmation signal intensity value (bn) is
It is no to become noise level (a) below (S650).At this point, if signal strength indication (bn) do not become noise level (a) hereinafter, if more
Reaction cup (S690) is changed, the pollution judgment process for carrying out B reaction cup is started again at.
In the device with automatic reaction cup replacement function, the replacement of reaction cup position of readiness will be previously positioned at instead
It answers cup to be replaced with the reaction cup 126 being arranged in electric furnace 125, thus carries out the replacement of reaction cup.
C furnace interior pollutes judgment process
Fig. 7 is flow chart the step of showing " C furnace interior pollutes judgment process " (S440) of the invention.
In atomic absorption spectrum analysing arrangement 100, " atomized stage+cooling stage " (S710) of selection setting element, with
Impact missing mode executes the heating (S720) in atomization portion 120.Determine whether signal strength indication (c1) becomes noise level (a) below
(S740).In the case where signal strength indication (c1) is more than the noise level (a) set in noise level setting process (S430),
1 maximum heating (S750) is carried out again, executes " atomized stage+cooling stage " of setting element in a manner of impact missing again
(S760), determine whether signal strength indication (c2) becomes noise level (a) below (S770).At this point, if signal strength indication
(c2) noise level (a) is not become hereinafter, then replacing reaction cup (S780).After reaction cup replacement, starts again at and carry out in C furnace
Pollute judgment process in portion.
Here, atomized stage is heated to the process for being able to detect the temperature of Atomic absorption signal of measurement element, cold
But the stage is to flow through argon gas on the reaction cup periphery being heated and carry out cooling process to reaction cup, and impact missing, which refers to, not to be infused
Enter the process of the heating in the atomization portion in the state of sample.
Pollute judgment process in D liquor charging path
Fig. 8 is flow chart the step of showing " polluting judgment process in D liquor charging path " (S445) of the invention.
The pure water for entering specimen cup 210 is measured using the temperature program(me) of setting element, determines signal strength indication
(dn) whether become the noise level (a) set in noise level setting process (S430) below.
Initially, implement 1 nozzle rinse (S810), then, 1 measurement is respectively carried out to the pure water entered in 3 pure water cups
(S830).If the signal strength indication (d1~d3) of any one pure water cup in 3 pure water cups become noise level (a) with
Under, then enter next process (S840).It is more than noise level (a) in the signal strength indication (d1~3) of whole pure water cups
In the case of, after carrying out nozzle rinse (S850), pure water measurement (S860) is executed again.Whether determine signal strength indication (d4~d6)
Below (S870) as noise level (a).At this point, if signal strength indication (d4~6) do not become noise level (a) hereinafter, if
It carries out the cleaning (nozzle rinse) in liquor charging path and specifies the pure water sample cup (S890) of preparation, start again at and carry out D liquor charging road
Diameter pollutes judgment process.
Here, nozzle rinse refers to that cleaning solution is flowed through in nozzle to be cleaned.
E specimen cup judgment process
Fig. 9 is flow chart the step of showing " E specimen cup judgment process " (S450) of the invention.
The specimen cup 210 for being put into dilute acid soln is placed on specimen holder 220 (S910).Utilize preset element
Temperature program(me) respectively measure 1 time (S920), determine signal strength indication (f) whether become regulation absorbance (e) below (S930).?
Signal strength indication (f) be more than regulation absorbance (e) when, there may be pollutions for dilute acid soln, therefore, replacement dilute acid soln again into
Row measurement (S950).At this point, " specimen cup is contaminated for progress when signal strength indication (f2) is more than regulation absorbance (e).Measurement
Preliminary sample cup." display.The specimen cup (S970) for specifying preparation starts again at and carries out the judgement of E specimen cup.
Regulation absorbance (e) refers to be preset in the range of not impacting to later denier analysis result
, absorption photometric value as background.
The mensuration operation of F reproducibility
Figure 10 is flow chart the step of showing " measurement of F reproducibility " (S485) of the invention.
2 measurements are carried out to the titer of the object element entered in specimen cup 210 using the temperature program(me) of setting element
(S1010, S1020) is calculated standard deviation (S1040), is compared with preset threshold value (S1050), carry out reproducibility
Judgement.If the reproducibility of absorbance become defined value (such as 3%) hereinafter, if terminate denier analysis and diagnosis system,
Start the measurement (S1060) of progress standard sample.If the reproducibility of absorbance do not become as defined in value hereinafter, if execute again
Measurement, carries out the judgement of reproducibility.At this point, if the reproducibility of absorbance do not become as defined in value hereinafter, if " be transferred to
" temperature program(me) automatic generation function "." display, be transferred to " temperature program(me) automatic generation function ", optimize and terminate
(S1070)。
Here, " temperature program(me) automatic generation function " is following function: changing drying/ashing/original of object sample on one side
Sonization temperature is measured on one side, sets the optimal temperature program(me) of reproducibility.
Then, the denier analyzing and diagnosing function in atom extinction photometer portion of the invention is illustrated.
Initially, operator is from the project below shown in display unit 360, by the input from input unit 350 from
Pollution determination step chosen below.
あ: the pollution situation of decision analysis device entirety
い: there is no pollutions, therefore are only simply determined
う: suspecting there is pollution, and therefore, it is desirable to be cleaned (it is desirable that the shadow for the High concentration samples being measured before excluding tightly
It rings)
According to the selection project of operator, control unit 310 shows following instruction in display unit 360, and control unit 310 shifts
To corresponding process.
Select " あ ": the message of display [executing whole projects of " denier analyzing and diagnosing "] starts to carry out process A.
Select " い ": the message of display [carrying out the process A and step D of " denier analyzing and diagnosing "] starts to carry out process
A。
Selection " う ": [reaction cup/ring please be remove, to cleaning in furnace.Please is assembling new ring/reaction cup and carrying out
" あ " is selected after nozzle rinse.].
At this point, selection " い ", in the step D of following records in the case where being determined to be NG, executes process A~step D.
In addition, as shown in figure 3, denier analysis diagnostic device can be preset in display unit 360 before measurement starts
Projects of display.
I: measure object element (is indicated the measurement masurium of periodic table by input unit 350, is thus shown in measure object
Element is set in window 410)
II: the quantity of the specimen cup confirmed and setting place (indicate sample injection unit layout by input unit 350
(not shown) be numbered and finish number, be thus shown in measure object element setting window 410 in)
III: the pollution determinating reference (being inputted from input unit 350) of specimen cup
In the following, describing denier analysis diagnostic device in detail.
The set-up function of A noise level
Operator is in 120 assembly reaction cup 126 of the atomization portion of atom extinction photometer main part 100, from input unit 350
Indicate nozzle check.Control unit 310 implements the nozzle check of the nozzle 230 of sample injection unit 200 according to the instruction of operator,
Result is shown in display unit 360.
Then, operator is according to operation PC300, since input unit 350 indicates denier analyzing and diagnosing.According to this
Instruction, operation use the control unit 310 of PC300 after the condition setting in light source portion 110, during 10 seconds of 3 secondary light source portions 110 of measurement
Test section 140 signal strength, in data processing division 330 calculate maximum absorbance 3 average value as noise water
Flat value (a), is stored in calculated value as noise level (a) in record portion 320.
The pollution decision-making function of B reaction cup
Control unit 310 carries out the of atomization portion 120 with the maximum temperature that can set in atomic absorption spectrum analysing arrangement 100
1 heating obtains the signal strength indication (b1) of test section 140.Then, the 2nd of atomization portion 120 is equally carried out with the 1st time
Secondary heating obtains signal strength indication (b2).Control determines the signal obtained after the 2nd heating with the determination unit 340 of PC300
Whether intensity value (bn) becomes noise level (a) hereinafter, will determine that result is stored in record portion 320, and be shown in display
In portion 360.In the case where signal strength indication (b) is more than noise level (a), atomization portion is equally carried out with maximum temperature again
120 heating, determines whether signal strength indication (bn) becomes noise level (a) below.At this point, if signal strength indication (bn) not
As noise level (a) hereinafter, then carrying out " reaction cup please being replace in display unit 360." display, carry out it is standby.Operator
Reaction cup 126 is replaced, determines function in the pollution for after the input that input unit 350 carries out replacement end, starting again at B reaction cup
Energy.In addition, after replacement reaction cup automatically, starting again at B reaction cup in the device for replacing function automatically with reaction cup
Pollute decision-making function.
C furnace interior pollutes decision-making function
In atomic absorption spectrum analysing arrangement 100, as " atomized stage+cooling stage " of setting element, control unit 310
(state of unimplanted sample) executes the heating in atomization portion 120 in a manner of impact missing, obtains the signal strength indication of test section 140
(c1).Determination unit 340 determines whether acquired signal strength indication becomes noise level (a) hereinafter, storing the result into record
In portion 320, and it is shown in display unit 360.In the case where signal strength indication (c1) is more than noise level (a), according to next
From the instruction of control unit 310, atomization portion 120 carries out 1 maximum heating again, and " the atom of setting element is executed in a manner of impact missing
Change stage+cooling stage ", determination unit 340 determine whether signal strength indication (c2) becomes noise level (a) below.At this point, if
Signal strength indication (c2) does not become noise level (a) hereinafter, then display " please replace reaction cup in display unit 360." carry out to
Machine.After operator replaces reaction cup 126, after the input replacement of input unit 350, starts again at the pollution of C furnace interior and determine function
Energy.In addition, after replacement reaction cup automatically, it is dirty to start again at C furnace interior in the device for replacing function automatically with reaction cup
Contaminate decision-making function.
D liquor charging system pollutes decision-making function
By setting the temperature program(me) of element, entered in specimen cup 210 using 100 Duis of atom extinction photometer main part
Pure water is measured, and determines whether the signal strength indication (dn) of acquired test section 140 becomes noise water using determination unit 340
Put down (a) below.
Initially, implement the nozzle rinse of the nozzle 230 of 1 sample injection unit 200, then, be put into from display shown in Fig. 3
The measurement for the pure water in 3 pure water cups that each setting window in portion 360 pre-enters is each to be carried out 1 time.Utilize 340 pairs of institutes of determination unit
The noise level (a) stored in the signal strength indication and record portion 320 of obtained detector 140 is compared judgement, if 3
The signal strength indication (d1~d3) of any one pure water cup in pure water cup becomes noise level (a) hereinafter, then depositing the result
Storage is shown in display unit 360 in record portion 320, and control unit 310 carries out the instruction into next process.?
In the case that the signal strength indication (d1~3) of whole pure water cups is more than noise level (a), after carrying out nozzle rinse again, execute
Pure water measurement.Determination unit 340 determines whether signal strength indication (d4~d6) becomes noise level (a) below.At this point, if signal
Intensity value (d4~6) does not become noise level (a) hereinafter, the then measurement of the pure water cup of the specified preparation of control unit 310, carries out again
D liquor charging system pollutes decision-making function.
E specimen cup decision-making function
The specimen cup 210 for being put into dilute acid soln is placed on specimen holder 220.Control unit 310 utilizes atom extinction light
Degree meter main part 100, the temperature program(me) by setting element respectively measure 1 time, to the signal strength indication (f) of test section 140 and pre-
The regulation absorbance (e) being first stored in record portion 320 is compared, using determination unit 340, according to the signal strength after comparison
Value determines whether pollution.When signal strength indication (f) is more than regulation absorbance, there may be pollutions for dilute acid soln, it is therefore intended that
The measurement of prepared dilute acid soln cup, executes measurement again.It is more than regulation extinction at signal strength indication (f2) after measuring again
In the case where spending (e), after specimen cup replacement, starts again at and carry out the judgement of E specimen cup, similarly handled.
The measurement function of F reproducibility
2 measurements are carried out to the titer of the object element entered in specimen cup 210 using the temperature program(me) of setting element,
The signal strength indication for obtaining test section 140, stores it in record portion 320.Data processing division 330 is according in record portion 320
The signal strength indication of storage calculates standard deviation, in determination unit 340 with the threshold value that presets and be stored in record portion 320
It is compared, carries out the good no judgement of reproducibility.In determination unit 340, it is less than record portion in the standard deviation of signal strength indication
In the case where the threshold value stored in 320, if the reproducibility of absorbance become defined value (such as 3%) hereinafter, if terminate pole
Micro-analysis diagnosis.
In the case where being judged to not polluting in each process of the denier analyzing and diagnosing, shown in display unit 360
Show the measurement starting image of standard sample.If value as defined in the reproducibility of absorbance does not become hereinafter, if same execution again
Measurement, carries out the confirmation of reproducibility.At this point, if the reproducibility of absorbance do not become as defined in value hereinafter, if " be transferred to
" temperature program(me) automatic generation function "." display, optimize, terminate denier analyzing and diagnosing function.
Record portion 320 has the result for each process for being able to record denier analyzing and diagnosing function and carries out as needed
The function of recalling confirmation, when generating the unfavorable condition in process, display produces the work of unfavorable condition in display unit 360
Sequence.
In denier analysis and diagnosis system of the invention, operator initially enters measurement element/determination condition
(S1120), automatic to carry out atom extinction photometer main part 100 and liquor charging system after selecting a pollution determination step (S405)
The pollution in system portion 200 determines, pollution situation and the game method as measurement preparation hereafter are shown in display unit 360, but
It is the judgement of the determination unit 340 from the operation portion PC 300 can also to be shown in display unit 360 and from control unit 310
Instruction, operator carry out pollution judgement according to the step.
In addition it is also possible to there is timer function in control unit 310, and on the basis of setting measures start time, choosing
Denier analyzing and diagnosing function is selected, as a result, before measuring start time, control unit 310 terminates denier analyzing and diagnosing function,
Its result is shown in display unit 360.
Claims (7)
1. a kind of atom extinction photometer, which is characterized in that
The atom extinction photometer have be able to carry out electric heating measurement atom extinction photometer main body, Autosampler and
Operation computer,
The atom extinction photometer has micro-analysis diagnostics division, which determines comprising including reaction cup
Whether there is or not the micropollutions based on measure object element for electric furnace, the liquor charging path of Autosampler and specimen cup.
2. atom extinction photometer according to claim 1, which is characterized in that
The micro-analysis diagnostics division carries out the following processing:
The measurement of the noise level of the atom extinction photometer；
The reaction cup, the heating furnace, the liquor charging path comprising the Autosampler, the specimen cup, measurement solvent
Pollution determine；And
The judgement of reproducibility based on titer.
3. atom extinction photometer according to claim 1, which is characterized in that
The micro-analysis diagnostics division selects diagnosis rank when micro-analysis diagnoses and starts, as a result, the micro-analysis diagnosis
Portion can to measure whether there is or not the electric furnace comprising the reaction cup of the micropollution based on the measure object element, from
The liquor charging path of dynamic sampler and specimen cup are selected.
4. atom extinction photometer according to claim 1, which is characterized in that
The micro-analysis diagnostics division determines the electricity comprising the reaction cup using the noise level determined as a reference value
Whether there is or not the micropollutions based on the measure object element for heating furnace, the liquor charging path of Autosampler and specimen cup.
5. atom extinction photometer according to claim 1, which is characterized in that
The micro-analysis diagnostics division executes processing relevant to the judgement by selection pollution determination step automatically.
6. atom extinction photometer according to claim 1, which is characterized in that
The micro-analysis diagnostics division is by setting measurement start time, thus before the set measurement start time
Terminate.
7. a kind of micro-analysis diagnostic method of atom extinction photometer, in the atom extinction light for being able to carry out electric heating measurement
Degree meter measurement start before determine include reaction cup including electric furnace, Autosampler liquor charging path and specimen cup whether there is or not
Micropollution based on measure object element, which is characterized in that the micro-analysis diagnostic method includes the following process:
Noise level sets process, measures the noise level of the atom extinction photometer main body, sets it to the noise water
Flat threshold value；
Whether there is or not confirmation judgment process for reaction cup pollution, carry out the reaction with the maximum temperature of the atom extinction photometer main body
The heating of cup, the signal strength of the measure object element of the reaction cup is found out according to the signal strength of detector；
Whether there is or not judgment process for furnace interior pollution, carry out the defined heating and cooling of the atom extinction photometer main body, according to
The signal strength of the detector finds out the signal strength of the measure object element of the electric furnace；
Whether there is or not processes for liquor charging system pollution, pure water are imported the detector via the Autosampler, according to the detector
The measure object element signal strength determine comprising the Autosampler liquor charging system have it is pollution-free；
Whether there is or not judgment process for specimen cup pollution, and the diluted acid in the specimen cup is imported the detection via the Autosampler
It is pollution-free to determine that the specimen cup has according to the signal strength of the measure object element of detector for device；And
Reproducibility confirm process, the reaction cup pollution whether there is or not judgment process, furnace interior pollution whether there is or not judgment process, liquor charging system
Whether there is or not processes and specimen cup pollution for system pollution whether there is or not after judgment process, is repeatedly surveyed using the determination condition of measure object element
Determine standard sample.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2018-063600 | 2018-03-29 | ||
| JP2018063600A JP7211616B2 (en) | 2018-03-29 | 2018-03-29 | Ultratrace analysis diagnostic method in atomic absorption spectrophotometer |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN110320167A true CN110320167A (en) | 2019-10-11 |
Family
ID=68112844
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910247666.XA Pending CN110320167A (en) | 2018-03-29 | 2019-03-29 | The denier analysis and diagnosis method of atom extinction photometer and atom extinction photometer |
Country Status (2)
| Country | Link |
|---|---|
| JP (1) | JP7211616B2 (en) |
| CN (1) | CN110320167A (en) |
Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH04307353A (en) * | 1991-04-03 | 1992-10-29 | Hitachi Ltd | Atomic absorption analysis method and apparatus |
| JPH08219985A (en) * | 1995-02-14 | 1996-08-30 | Shimadzu Corp | Atomic absorption spectrophotometer |
| JPH08261917A (en) * | 1995-03-28 | 1996-10-11 | Hitachi Ltd | Cleaning method, cleaning device, and instrument for analysis having it |
| CN102834708A (en) * | 2010-04-12 | 2012-12-19 | 株式会社日立高新技术 | Elementary analysis device and method |
| CN103994982A (en) * | 2014-05-28 | 2014-08-20 | 河北三九爱德福药业有限公司 | Method for detecting calcium carbonate residue after cleaning of calcium preparation production line |
| CN104246489A (en) * | 2012-04-23 | 2014-12-24 | 株式会社日立高新技术 | Mass analyzer and mass analysis method |
| CN104395733A (en) * | 2012-06-19 | 2015-03-04 | 株式会社日立高新技术 | Method of atomic absorption analysis and atomic absorption photometer |
| CN107255729A (en) * | 2017-06-12 | 2017-10-17 | 合肥市第二人民医院 | A kind of automatic clinical chemistry analyzer and its method of work |
| CN107449742A (en) * | 2016-05-31 | 2017-12-08 | 株式会社岛津制作所 | Online heavy metal monitor and the detection method using the online heavy metal monitor |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS61107161A (en) * | 1984-10-31 | 1986-05-26 | Hitachi Ltd | Automatic analyser |
| JP3587899B2 (en) * | 1995-01-30 | 2004-11-10 | トキコテクノ株式会社 | Underground tank leak inspection system |
| JP3300213B2 (en) * | 1995-11-29 | 2002-07-08 | 松下電器産業株式会社 | Aerial impurity monitoring device and aerial impurity monitoring method |
| JP6110697B2 (en) * | 2013-03-15 | 2017-04-05 | 株式会社日立ハイテクノロジーズ | Automatic analyzer, nozzle cleaning method, and cleaning member holder |
-
2018
- 2018-03-29 JP JP2018063600A patent/JP7211616B2/en active Active
-
2019
- 2019-03-29 CN CN201910247666.XA patent/CN110320167A/en active Pending
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH04307353A (en) * | 1991-04-03 | 1992-10-29 | Hitachi Ltd | Atomic absorption analysis method and apparatus |
| JPH08219985A (en) * | 1995-02-14 | 1996-08-30 | Shimadzu Corp | Atomic absorption spectrophotometer |
| JPH08261917A (en) * | 1995-03-28 | 1996-10-11 | Hitachi Ltd | Cleaning method, cleaning device, and instrument for analysis having it |
| CN102834708A (en) * | 2010-04-12 | 2012-12-19 | 株式会社日立高新技术 | Elementary analysis device and method |
| CN104246489A (en) * | 2012-04-23 | 2014-12-24 | 株式会社日立高新技术 | Mass analyzer and mass analysis method |
| CN104395733A (en) * | 2012-06-19 | 2015-03-04 | 株式会社日立高新技术 | Method of atomic absorption analysis and atomic absorption photometer |
| CN103994982A (en) * | 2014-05-28 | 2014-08-20 | 河北三九爱德福药业有限公司 | Method for detecting calcium carbonate residue after cleaning of calcium preparation production line |
| CN107449742A (en) * | 2016-05-31 | 2017-12-08 | 株式会社岛津制作所 | Online heavy metal monitor and the detection method using the online heavy metal monitor |
| CN107255729A (en) * | 2017-06-12 | 2017-10-17 | 合肥市第二人民医院 | A kind of automatic clinical chemistry analyzer and its method of work |
Non-Patent Citations (1)
| Title |
|---|
| 李清禄: "《简明化学实验教程 第2版》", vol. 2017, 厦门大学出版社, pages: 294 * |
Also Published As
| Publication number | Publication date |
|---|---|
| JP2019174315A (en) | 2019-10-10 |
| JP7211616B2 (en) | 2023-01-24 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| JP6735655B2 (en) | Methods for generating input information for electronic laboratory journals | |
| JP5164388B2 (en) | Sample measuring device | |
| JP6208127B2 (en) | Automatic analyzer | |
| CN101118245A (en) | Automatic analyzer | |
| JP6368067B2 (en) | Mass spectrometer and mass spectrometry method | |
| JP2009216705A (en) | Automatic analyzer | |
| WO2009145251A1 (en) | Method for assisting judgment of abnormality of reaction process data and automatic analyzer | |
| JP6234812B2 (en) | Automatic analyzer | |
| JP2019219228A (en) | Autoanalyzer and automatic analysis method | |
| CN101344530A (en) | Automatic analyzer and analysis method using the same | |
| CN110320167A (en) | The denier analysis and diagnosis method of atom extinction photometer and atom extinction photometer | |
| CN113358885B (en) | Automatic analysis device | |
| JP2009281802A (en) | Autoanalyzer and specimen searching system | |
| JP2000266754A (en) | Automatic chemical analyzer | |
| CN113406038A (en) | Optical detection method and device for pH value of water | |
| JP2604043B2 (en) | Automatic analyzer | |
| EP4267974A1 (en) | Calibration and validation of cuvettes in automated chemical analyzers | |
| CN110542670B (en) | Realize online near-infrared analyzer of many indexes simultaneous detection | |
| CN113447478A (en) | Detection method for pesticide residue detector and pesticide residue detector | |
| JP2016170075A (en) | Automatic analyzer and method for automatic analysis | |
| JPH02287260A (en) | Automatic analyzer | |
| JP2010276568A (en) | Automated analyzer for clinical inspection | |
| JP5414286B2 (en) | Automatic analyzer | |
| JP3078403B2 (en) | Automatic chemical analyzer | |
| TWI797787B (en) | Device for controlling raman spectrometer |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |