CN106940325B - The detection method of heat exchange equipment dirt sample - Google Patents
The detection method of heat exchange equipment dirt sample Download PDFInfo
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- CN106940325B CN106940325B CN201710238266.3A CN201710238266A CN106940325B CN 106940325 B CN106940325 B CN 106940325B CN 201710238266 A CN201710238266 A CN 201710238266A CN 106940325 B CN106940325 B CN 106940325B
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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- G01N23/223—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material by irradiating the sample with X-rays or gamma-rays and by measuring X-ray fluorescence
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Abstract
The present invention provides a kind of detection methods of heat exchange equipment dirt sample.The detection method includes the dirty sample for acquiring heat exchange equipment；Dirty sample is roasted, product of roasting is obtained；It is measured using ingredient and content of the Xray fluorescence spectrometer to product of roasting, obtains measurement result.On the one hand the detection method of heat exchanger dirt sample can analyze heat exchange equipment dirt sample in the case where Unmarked word, and seventies kinds of elements can be analyzed in the case where standard sample lacks, content range can be from trace to 100%, to solve the problems, such as that heat exchanger dirt sample is caused to be difficult to analyze without standard sample in the prior art.On the other hand the detection method has also widened the application range of Xray fluorescence spectrometer, and analyzes that speed is fast, feature easy to operate, saves testing cost.
Description
Technical field
The present invention relates to equipment dirt sample detection fields, in particular to a kind of detection method of heat exchange equipment dirt sample.
Background technique
Dirt is had on heat exchange equipment wall surface, very big on heat transfer property and pressure drop influence, thermal resistance can reach sometimes and start to control
The order of magnitude of production.For specific heat exchange equipment, the factors such as structure, material, dirt type, fluid properties and use condition
Have an impact to the ingredient and content of dirty sample, and then influences its descaling method.
When analyzing totally unknown heat exchange equipment dirt sample, the main component and content of sample are obtained, the prior art is logical
Qualitative and quantitative analysis is carried out frequently with chemical method.Using the qualitative carbonate of hydrochloric acid solution, iron ion；Using the qualitative sulphur of barium chloride
Hydrochlorate；Using the qualitative silicon ion of sodium fluoride；Using the qualitative chloride ion of silver nitrate solution；After hydrochloric acid is added, test tube mouth side one
Be added 1 drop acetic acid lead solution and 1~2 drop sodium hydroxide solution filter paper item, by the test tube under alcolhol burner micro emulsion, if test paper become
Black, then the dirt sample includes sulfide.Qualitative substance is quantified using corresponding national standard or professional standard.Using chemistry
Method analyzes dirty sample and is difficult to obtain whole compositions of dirty sample.
There is also utilize x ray fluorescence spectrometry test sample ingredient and content in the prior art, it is common practice to
Information of the relevant data acquisition about sample composition is consulted first；Suitable standard sample is found further according to the information of sample composition
Product；The information of according to standard sample selects suitable method for making sample sample preparation: including standard sample and to test sample；According to standard sample
Calibration curve is drawn after information setting measuring condition, then measurement standard sample；It finally measures to test sample, to obtain to test sample
Analyze result.
But due to the complexity of heat exchange equipment scale sample ingredient and content, it is difficult to find suitable standard sample, thus very
Hardly possible obtains the information about sample composition and content.
Summary of the invention
The main purpose of the present invention is to provide a kind of detection methods of heat exchange equipment dirt sample, difficult in the prior art to solve
The problem of being detected is formed with heat exchanging equipment dirt sample.
To achieve the goals above, this application provides a kind of detection method of heat exchange equipment dirt sample, the detection method packets
It includes: acquiring the dirty sample of heat exchange equipment；Dirty sample is roasted, product of roasting is obtained；Roasting is produced using Xray fluorescence spectrometer
The ingredient and content of object are measured, and obtain measurement result.
Preferably, before being roasted to dirty sample, detection method further include: dirty sample is dried and to drying before
The step of dirty sample afterwards is weighed；It is preferred that the dirty sample before drying is placed in vacuum drying oven and is dried in drying steps.
Preferably, before being measured using Xray fluorescence spectrometer to the ingredient and content of product of roasting, detection side
Method further includes the steps that product of roasting being ground into powder.
Preferably, when being measured using ingredient and content of the Xray fluorescence spectrometer to product of roasting, Unmarked word is selected
Analysis program is measured.
Preferably, Xray fluorescence spectrometer has built-in standard items, is selected from standard sample using standard specimen as inspection
Sample carries out standardlcss analysis.
It preferably, is analysis in helium to the step of ingredient and content of product of roasting using Xray fluorescence spectrometer
It is carried out in medium.
Preferably, in the step of being measured using ingredient and content of the Xray fluorescence spectrometer to product of roasting, control
The product of roasting of detection is the≤powder of 3g.
Preferably, when being measured using ingredient and content of the Xray fluorescence spectrometer to product of roasting, using scanning mould
Formula measures product of roasting.
Preferably, being measured the step of obtaining measurement result to the ingredient of product of roasting and content includes: using X-ray
Fluorescence Spectrometer is measured the ingredient and content of product of roasting, obtains PRELIMINARY RESULTS；Verification calibration is carried out to PRELIMINARY RESULTS,
Obtain measurement result.
Preferably, the step of carrying out verification calibration to PRELIMINARY RESULTS includes any one or more of following a into i:
A. according to the content of ingredient each in PRELIMINARY RESULTS, verifying evaluation profile selected in Xray fluorescence spectrometer is
No is interactive evaluation mode, if not interactive evaluation mode, then be changed to interactive evaluation mode and redeterminate；
B. whether the characteristic of dirty sample is powder defined in verifying, and is redeterminated if it is not, being adjusted to powder；
C. check whether the highest K alpha ray spectrum line in the ingredient of product of roasting has overlapping, if lap is more than half peak height
When, then select K β line；If K α line and K β line are overlapped simultaneously, L α line is selected to be redeterminated；
D. it checks whether the intensity of spectral line exceeds the range of linearity of detector, if exceeding the range of linearity of detector, selects
Time sensitive spectral line is selected to redeterminate；
Whether the molecular formula for e. verifying compound is accurate, if inaccurate, redeterminates after being changed to accurate molecular formula；
If f. a certain ingredient in known dirty sample it is known that and without corresponding ingredient in PRELIMINARY RESULTS, in PRELIMINARY RESULTS
Measurement is re-started after adding corresponding ingredient；
If g. in known dirty sample a certain ingredient content, and inconsistent to the content of ingredient corresponding in PRELIMINARY RESULTS, then general
The content of corresponding ingredient in PRELIMINARY RESULTS re-starts measurement after being changed to known content；
H. each ingredient verified in dirty sample is measured, and confirmation carries out normalization to measurement result after being measured；
I. theoretical Compton line intensity is calculated according to the densimeter of ingredient each in PRELIMINARY RESULTS, by theoretical Compton line intensity
It is compared with practical Compton line intensity, obtains ratio, and when ratio is 0.7~1.4, then PRELIMINARY RESULTS is to measure knot
Fruit.
It applies the technical scheme of the present invention, the detection method of the heat exchanger dirt sample on the one hand can be in the case where Unmarked word
Heat exchange equipment dirt sample is analyzed, and seventies kinds of elements can be analyzed in the case where standard sample lacks, content range can be with
From trace to 100%, to solve the problems, such as that heat exchanger dirt sample is caused to be difficult to analyze without standard sample in the prior art.Separately
On the one hand the detection method has also widened the application range of Xray fluorescence spectrometer, and analyzes that speed is fast, spy easy to operate
Point saves testing cost.
Detailed description of the invention
The accompanying drawings constituting a part of this application is used to provide further understanding of the present invention, and of the invention shows
Examples and descriptions thereof are used to explain the present invention for meaning property, does not constitute improper limitations of the present invention.In the accompanying drawings:
Fig. 1 shows the detection method process signal of heat exchange equipment dirt sample in a kind of preferred embodiment according to the application
Figure.
Include with lower label in above-mentioned attached drawing:
1, balance；2, crucible；3, vacuum drying oven；4, drier；5, Muffle furnace；6, mortar；7, fluid sample cup；8, X is penetrated
Line Fluorescence Spectrometer.
Specific embodiment
It should be noted that in the absence of conflict, the features in the embodiments and the embodiments of the present application can phase
Mutually combination.Below in conjunction with embodiment, the present invention will be described in detail.
As background technique is previously mentioned, due to the complexity of heat exchange equipment scale sample ingredient and content, it is difficult to obtain about sample
The information of product composition, and find that suitable standard sample is also highly difficult, the scale sample ingredient of such heat exchanger is difficult to use
Existing method carries out quantitative and semi-quantitative.In order to detect the ingredient and relative amount of such heat exchanger dirt sample, in the application one
In the typical embodiment of kind, a kind of detection method of heat exchange equipment dirt sample is provided, which includes: that acquisition heat exchange is set
Standby dirty sample；Dirty sample is roasted, product of roasting is obtained；To the ingredient of product of roasting and contained using Xray fluorescence spectrometer
Amount is measured.
On the one hand the detection method of the above-mentioned heat exchanger dirt sample of the application can analyze heat exchange in the case where Unmarked word and set
Standby dirt sample, and seventies kinds of elements can be analyzed in the case where standard sample lacks, content range can from trace to
100%, to solve the problems, such as that heat exchanger dirt sample is caused to be difficult to analyze without standard sample in the prior art.On the other hand should
Detection method has also widened the application range of Xray fluorescence spectrometer, and analyzes that speed is fast, feature easy to operate, saves
Testing cost.
The detection method of above-mentioned heat exchange equipment dirt sample has been able to the ingredient to certain dirty samples for being difficult to find that standard sample
It is detected with relative amount.In order to improve the relative precision of dirty sample detection, in a preferred embodiment of the present application, In
Before being roasted to dirty sample, above-mentioned detection method further include: dirty sample is dried and the dirty sample of dry front and back is carried out
The step of weighing.
It weighs by the way that dirty sample is dried, and to the weight of the dirty sample before drying and after dry, so as to
Enough accurate water contents obtained in dirty sample.
In above-mentioned the step of dirty sample is dried, it is dried using existing drying mode.In the application one
In kind preferred embodiment, the dirty sample before drying is placed in vacuum drying oven and is dried.Claim to the dirty sample before drying
It after weight, is placed in a vacuum drying oven and is dried, can physically or chemically be reacted to avoid external environment with dirty sample generation and cause
Its ingredient changes, so that testing result is relatively accurate.
In above-mentioned sintering step, used container is sintered also without particular/special requirement, as long as can be realized the sintering to dirty sample
Ashing.Preferably dirty sample is placed in Muffle furnace in this application and is sintered.
The step of being measured using ingredient and content of the Xray fluorescence spectrometer to product of roasting, according to specifically being made
The nuance of Xray fluorescence spectrometer model and performance, concrete operation step can be adjusted slightly.In order to make to examine
It is relatively more accurate to survey result, in a preferred embodiment of the present application, in use Xray fluorescence spectrometer to product of roasting
Before the step of ingredient and content are measured, above-mentioned detection method further includes the steps that product of roasting being ground into powder.
In above preferred embodiment, it is ground into Xray fluorescence spectrometer on powder and carries out ingredient and assay, measurement knot
Fruit is more acurrate.
The above-mentioned detection method of the application surveys the ingredient and content of product of roasting using Xray fluorescence spectrometer
Periodically, selection standardlcss analysis program is measured.Point of the ingredient of heat exchanging equipment dirt sample and content compared to the prior art
Analysis method, the application are measured the quantitative and semi-quantitative inspection for not only realizing Unmarked word dirt sample using standardlcss analysis program
It surveys, and analyzes fast, the easy to operate feature of speed, save testing cost.
Above-mentioned detection method selection standardlcss analysis program, which measures, can obtain reliable measurement intensity, can automatic seeking
Peak is not influenced by chemical shift, and background is based on a large area scanning, will not be influenced by neighbouring Overlapped spectral line, and work as
Measuring signal intensity has reached a certain limit value, and the electric current of high pressure generator lowers automatically, is more than detector to avoid measurement intensity
The range of linearity.
It is above-mentioned to be measured using ingredient and content of the Xray fluorescence spectrometer to product of roasting, according to specifically used X
The performance difference appropriate adjustment of ray fluorescence spectrometer can be realized.In a preferred embodiment of the present application, x-ray fluorescence
Spectrometer has built-in standard items, selects to carry out standardlcss analysis using standard specimen as sample is checked from standard sample.Specifically
Ground stores the Standard Curve Database of apparatus manufacturer measurement standard sample in the system of Xray fluorescence spectrometer.It is to be measured measuring
When sample, full spectrum scanning is carried out to sample to be tested, the signal strength of sample is obtained, it is accordingly dense that sample is obtained in Standard Curve Database
Degree.
In above preferred embodiment, built-in standard items can be what instrument carried, be also possible to operator for a long time to not
The standard items for being detected and being accumulated with dirt sample.Although by selecting the standard items built in these to examine the content of dirty sample to be measured
Survey accuracy it is relatively low, but compared with the existing technology in there is no appropriate criteria sample that can not detect for, have can be qualitative
With the advantage of half-quantitative detection, in order to formulate corresponding descaling method.
It is in a preferred embodiment of the present application, glimmering using X-ray in order to further increase the relative precision of detection
Photothermal spectroscopic analyzer to the step of ingredient and content of product of roasting is carried out in the analysis medium of helium.By above-mentioned product of roasting
Analysis is carried out in the analysis medium of helium, helps avoid the interference of other impurities, improves the opposite of detection
Accuracy.
In above-mentioned detection method, when using Xray fluorescence spectrometer to the detection of the ingredient of product of roasting and content, specifically
Applied sample amount depending on the detection range of instrument.In the application, the product of roasting for controlling detection is the≤powder of 3g.
In another preferred embodiment, carried out using ingredient and content of the Xray fluorescence spectrometer to product of roasting
When measurement, product of roasting is measured using scan pattern.Using scan pattern measurement product of roasting can automatic peak-seeking, not by chemical potential
The influence of shifting, background are based on a large area scanning, will not be influenced by neighbouring Overlapped spectral line, and when measuring signal intensity reaches
A certain limit value is arrived, the electric current of high pressure generator lowers automatically, is more than the range of linearity of detector to avoid measurement intensity.
In order to further increase the accuracy of measurement result, in a kind of preferred embodiment, to the ingredient of product of roasting
And it includes: to the ingredient of product of roasting and to be contained using Xray fluorescence spectrometer that content, which is measured the step of obtaining measurement result,
Amount is measured, and obtains PRELIMINARY RESULTS；Verification calibration is carried out to PRELIMINARY RESULTS, obtains measurement result.According to the shape of specific sample
Principal component in state, sample and the content etc. of principal component, verify PRELIMINARY RESULTS, so that measurement result is more
Accurately.
In the application another kind preferred embodiment, carrying out the step of verification is calibrated to PRELIMINARY RESULTS includes following a to i
In any one or more:
A. according to the content of ingredient each in PRELIMINARY RESULTS, verifying evaluation profile selected in Xray fluorescence spectrometer is
No is interactive evaluation mode, if not interactive evaluation mode, then be changed to interactive evaluation mode and redeterminate；
B. whether the characteristic of dirty sample is powder defined in verifying, and is redeterminated if it is not, being adjusted to powder；
C. it checks whether highest spectral line has overlapping, if overlapping, non-overlapping time high spectral line is selected to be redeterminated；
D. check whether the intensity of K α spectral line exceeds the range of linearity of detector, if exceeding the range of linearity of detector,
Selection K β spectral line redeterminates；If the intensity of K β spectral line also exceeds the range of linearity of detector, L α spectral line is selected to redeterminate；
Whether the molecular formula for e. verifying compound is accurate, if inaccurate, redeterminates after being changed to accurate molecular formula；
If f. a certain ingredient in known dirty sample it is known that and without corresponding ingredient in PRELIMINARY RESULTS, in PRELIMINARY RESULTS
Measurement is re-started after adding corresponding ingredient；
If g. in known dirty sample a certain ingredient content, and inconsistent to the content of ingredient corresponding in PRELIMINARY RESULTS, then general
The content of corresponding ingredient in PRELIMINARY RESULTS re-starts measurement after being changed to known content；
H. each ingredient verified in dirty sample is measured, and confirmation carries out normalization to measurement result after being measured；
I. theoretical Compton line intensity is calculated according to the densimeter of ingredient each in PRELIMINARY RESULTS, by theoretical Compton line intensity
It is compared with practical Compton line intensity, obtains ratio, and when ratio is 0.7~1.4, then PRELIMINARY RESULTS is to measure knot
Fruit.
The detailed step of the detection method of the application is described below.
X-ray fluorescence analysis: also known as X-ray secondary emission spectrum analysis.This law utilizes simple x-ray photon or other micro-
The atom in particle excitated test substance is seen, is allowed to generate secondary characteristic X-ray (X-ray fluorescence) and carry out elemental analysis
With the method for chemical state research.
The principle of x-ray fluorescence analysis are as follows: sample is after x-ray bombardment, due to the atomic energy level knot of each element
Structure be all it is specific, the energy for the X-ray released when transition after it is excited is also specific, referred to as characteristic X-ray.Pass through
The energy for measuring characteristic X-ray, can determine the presence of respective element, and the power of characteristic X-ray, then represents the element
Content.
Specific detecting step and material therefor are as shown in Figure 1.Wherein, 1, balance (precision 0.0001g)；2, crucible；3, true
Empty baking oven；4, drier；5, Muffle furnace；6, mortar；7, fluid sample cup；8, Xray fluorescence spectrometer.
Method operating process is as follows:
(1) take a certain amount of dirty sample first, weighed and (be accurate to 0.0001), be then dried, later again into
Row weighing (being accurate to 0.0001), the difference of the dirty sample quality of dry front and back are the quality of moisture content in dirty sample；Then by dirty sample into
Row roasting is weighed after cooling to the dirty sample after roasting.
(2) X-ray fluorescence spectra analysis standardlcss analysis is carried out after then grinding sample.Xray fluorescence spectrometer is matched
It sets as follows: end window Rh target metal ceramics light pipe, the design of light pipe cerebral cryotherapy；Analyze the helium system of fluid sample；Two detections
Device: 1 flow counter, 1 scintillation counter；Analyzing crystal: XS-55, PETHE LiF200；Two kinds of specification collimators
0.23 ° and 0.46 °.
The determination of Xray fluorescence spectrometer measurement parameter: weighing the powdered dirty sample of 3g or so, and helium condition is depressurized in selection,
Sample is measured using scan pattern, selects standardlcss analysis.
The appraisal procedure of result after dirty sample analysis:
(1) according to analyze come each ingredient content, judge whether selected evaluation profile file suitable, for changing
Hot device dirt sample is typically chosen interaction qualitative assessment mode.The interaction of interaction qualitative assessment mode fingering row standardlcss analysis result is commented
Estimate, shows that content, interactive evaluation refer to the assessment mode for considering the absorption enhancement effect between element.
(2) whether the characteristic of sample defined in checking is accurate, and such as method for making sample, adjustment in time is not allowed in sample size etc..
Powder is generally for heat exchanger dirt sample, if the characteristic of display sample is not powder, is adjusted to powder in time.
(3) it checks whether spectral line has obvious overlapping, if overlapping is very serious, nonoverlapping spectral line is selected to be assessed.Usually
The sequence of spectral line is selected as by highly sensitive line to low sensitive line, when the α line overlap part K of even two kinds ingredients is more than half peak height,
K β line is then selected, selects L α line if K α line and K β line are overlapped seriously simultaneously.
(4) range of linearity for checking the whether super detector of intensity of spectral line will consider to replace spectral line, the sensitive spectrum of selection time
Line re-measures.
(5) check whether the molecular formula of compound is accurate, inaccuracy is modified in time.
(6) content of known compound is defined, if certain ingredients are for known in dirty sample (for example use chemical determination
Cross), then it can define, assessment result can be made more acurrate.
(7) molecular formula and content of compound that insertion XRF (x ray fluorescence spectrometry) is not analyzed, in sample
Know containing and XRF does not analyze compound and needs to be inserted into, click " quantitative ", selection " adds sample ".
(8) judging whether can be with normalizing.Normalizing refers to the institute when result resultant is not 100%, but in confirmatory sample
When having compound to be measured or define, 100% processing is carried out to result resultant.Note: only all in confirmatory sample
When compound is measured or defines, normalizing could be carried out to result.When general default resultant is between 99.5%-100.5%
To carry out normalizing.
(9) it checks Compton line ratio, i.e., theoretical Compton line intensity is calculated by the densimeter of each element in sample, it will
Theoretical strength is compared with actual strength, if ratio close to 1, illustrates that this standardlcss analysis result is more accurate.More than one
Secondary test result show when ratio between 0.7-1.4 when, measurement result and actual result error in allowed limits, because
And the ratio relatively 1 is thought in the case of this.
Further illustrate the beneficial effect of the application below in conjunction with specific embodiments.
A certain amount of dirty sample is taken, is weighed, quality 10.3564g, then by the dirty sample after weighing at 110 DEG C ± 2
DEG C vacuum oven in dry 2 hours, then take out and be put into drier to its cooling, weigh again later, matter
Amount is 10.1035g, and the difference of the dirty sample quality after drying is 0.2529g, i.e., the quality of moisture content in dirty sample；By the dirt after drying
Sample is roasted at 900 DEG C, is put into cooling in drier to the dirty sample after roasting and is weighed again, quality 6.5307g,
After sample is ground, 3.0912g sample is taken to carry out X-ray fluorescence spectra analysis.
Start instrument and carry working software, before measurement, will analyze medium becomes the parameters of helium inspection apparatus, opens
After machine is stablized, start standardlcss analysis program, selects to carry out Unmarked word point using standard specimen as sample is checked from standard sample
Analysis, analysis the results are shown in Table 1, learn that measured value and standard value object significant difference, instrument are used directly for analyzing by table 1.
Table 1: the standard value and measured value of standard sample compare
| Substance title | Standard value (%) | Measured value | Tolerance |
| SiO2 | 71.43 | 71.7 | ±2.0 |
| Na2O | 13.52 | 14.3 | ±1.0 |
| Al2O3 | 0.95 | 0.879 | ±0.15 |
| SO3 | 0.61 | 0.538 | ±0.06 |
| Cl | 0.26 | 0.214 | ±0.04 |
| K2O | 5.54 | 4.10 | ±1.85 |
| CaO | 4.80 | 4.30 | ±1.00 |
| Fe2O3 | 0.04 | 0.0320 | ±0.0100 |
| SrO | 1.99 | 1.75 | ±0.40 |
| Sb2O3 | 0.75 | 0.719 | ±0.070 |
Heat exchanging device dirt sample is analyzed again, and analysis the results are shown in Table 2.
Table 2: dirty sample analyzes result
The Compton line ratio of the analysis result is 1.06, and ratio illustrates that this standardlcss analysis result is calibrated close to 1
Really.
It can be seen from the above description that the above embodiments of the present invention realized the following chievements: the heat exchanger
On the one hand the detection method of dirty sample can analyze heat exchange equipment dirt sample in the case where Unmarked word, and can lack in standard sample
Seventies kinds of elements are analyzed in the case where few, content range can be from trace to 100%, to solve in the prior art without mark
Quasi- sample and cause heat exchanger dirt sample to be difficult to the problem of analyzing.On the other hand the detection method has also widened X-ray fluorescence spectra
The application range of instrument, and analyze that speed is fast, feature easy to operate saves testing cost.
The foregoing is only a preferred embodiment of the present invention, is not intended to restrict the invention, for the skill of this field
For art personnel, the invention may be variously modified and varied.All within the spirits and principles of the present invention, made any to repair
Change, equivalent replacement, improvement etc., should all be included in the protection scope of the present invention.
Claims (6)
1. a kind of detection method of heat exchange equipment dirt sample, which is characterized in that the detection method includes:
Acquire the dirty sample of heat exchange equipment；
The dirty sample is roasted, product of roasting is obtained；
It is measured using ingredient and content of the Xray fluorescence spectrometer to the product of roasting, obtains measurement result；
Before being roasted to the dirty sample, the detection method further include: the dirty sample is dried and to drying
The step of dirty sample of front and back is weighed；
When being measured using ingredient and content of the Xray fluorescence spectrometer to the product of roasting, standardlcss analysis journey is selected
Sequence is measured；
In the step of being measured using ingredient and content of the Xray fluorescence spectrometer to the product of roasting, detection is controlled
The product of roasting is the≤powder of 3g；
Ingredient and content to the product of roasting are measured the step of obtaining the measurement result and include:
It is measured using ingredient and content of the Xray fluorescence spectrometer to the product of roasting, obtains PRELIMINARY RESULTS；
Verification calibration is carried out to the PRELIMINARY RESULTS, obtains the measurement result；
The step of carrying out verification calibration to the PRELIMINARY RESULTS includes any one or more of following a into i:
A verifies assessment mould selected in the Xray fluorescence spectrometer according to the content of ingredient each in the PRELIMINARY RESULTS
Whether formula is interactive evaluation mode, if not interactive evaluation mode, then be changed to interactive evaluation mode and redeterminate；
B, whether the characteristic for verifying defined dirty sample is powder, is redeterminated if it is not, being adjusted to powder；
C, checks whether the highest K α spectral line in the ingredient of the product of roasting has overlapping, if lap is more than half peak height,
Then select K β spectral line；If K α spectral line and K β spectral line are overlapped simultaneously, L α spectral line is selected to be redeterminated；
D, checks whether the intensity of K α spectral line exceeds the range of linearity of detector, if exceeding the range of linearity of detector, selects K
β spectral line redeterminates；If the intensity of K β spectral line also exceeds the range of linearity of detector, L α spectral line is selected to redeterminate；
E, whether the molecular formula for verifying compound is accurate, if inaccurate, redeterminates after being changed to accurate molecular formula；
F, if a certain ingredient in the known dirty sample it is known that and without corresponding ingredient in the PRELIMINARY RESULTS, it is described just
Measurement is re-started after adding corresponding ingredient in step result；
G, if in the known dirty sample a certain ingredient content, and it is inconsistent to the content of corresponding ingredient in the PRELIMINARY RESULTS,
Then it is changed to the content of the corresponding ingredient in the PRELIMINARY RESULTS to re-start measurement after known content；
H, each ingredient verified in the dirty sample are measured, and confirmation carries out at normalizing the measurement result after being measured
Reason；
I calculates theoretical Compton line intensity according to the densimeter of ingredient each in the PRELIMINARY RESULTS, by the theoretical Compton line
Intensity is compared with practical Compton line intensity, obtains ratio, and when the ratio is 0.7~1.4, then the preliminary knot
Fruit is the measurement result.
2. detection method according to claim 1, which is characterized in that in the drying steps, described in front of drying
Dirty sample, which is placed in vacuum drying oven, to be dried.
3. detection method according to claim 1, which is characterized in that in use Xray fluorescence spectrometer to the roasting
Before the ingredient and content of product are measured, the detection method further includes that the product of roasting is ground into the step of powder
Suddenly.
4. detection method according to claim 1, which is characterized in that the Xray fluorescence spectrometer has built-in mark
Quasi- product select to carry out standardlcss analysis using standard specimen as sample is checked from standard sample.
5. detection method according to claim 1, which is characterized in that produced using Xray fluorescence spectrometer to the roasting
The step of ingredient and content of object, is carried out in the analysis medium of helium.
6. detection method according to claim 1, which is characterized in that produced using Xray fluorescence spectrometer to the roasting
When the ingredient and content of object are measured, the product of roasting is measured using scan pattern.
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