CN106769274A - A kind of preparation method of the ABS standard samples for X-ray fluorescence spectra analysis - Google Patents
A kind of preparation method of the ABS standard samples for X-ray fluorescence spectra analysis Download PDFInfo
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/38—Diluting, dispersing or mixing samples
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/44—Sample treatment involving radiation, e.g. heat
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—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
- G01N23/22—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
- 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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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/38—Diluting, dispersing or mixing samples
- G01N2001/386—Other diluting or mixing processes
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2223/00—Investigating materials by wave or particle radiation
- G01N2223/07—Investigating materials by wave or particle radiation secondary emission
- G01N2223/076—X-ray fluorescence
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2223/00—Investigating materials by wave or particle radiation
- G01N2223/10—Different kinds of radiation or particles
- G01N2223/101—Different kinds of radiation or particles electromagnetic radiation
- G01N2223/1016—X-ray
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2223/00—Investigating materials by wave or particle radiation
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Abstract
The invention provides a kind of preparation method of the ABS standard samples for X-ray fluorescence spectra analysis.Methods described comprises the following steps:S1. the powder stock containing metal target element is prepared, the size of the powder stock was 400 mesh sieves;S2. ABS resin of the metal target constituent content less than instrument test limit is chosen, and confirms wherein to be free of antioxidant, plasticizer;S3. lubricant is added in the ratio relative to ABS resin quality 2 ‰ ~ 3 ‰, ABS resin is uniform with mix lubricant;S4. according to standard sample tenor demand, according to it is following rule confirm metal addition;S5. powder stock and the mixed ABS resins of S3. are put into high mixer, first time mixing is carried out at lower speeds;A small amount of lubricant is subsequently adding, second mixing is carried out at the higher speeds;S6. the mixed materials of S5. are heated into melting, extrusion moulding, granulation in an extruder;Standard sample is made by pellet.Method in accordance with the present invention, be obtained in that with the hand-to-hand standard sample of target content, and sample preparation is visibly homogeneous, favorable reproducibility.
Description
Technical field
The invention belongs to analyze with the preparation method of standard sample, and in particular to a kind of for X-ray fluorescence spectra analysis
ABS standard samples preparation method.
Background technology
European Union disclosed WEEE instructions and ROHS instructions in 2003, prohibits the use of or limits using leaded(Pb), mercury,
The electronic electric equipment product of the harmful substances such as cadmium, Cr VI, the foreign trade restriction to China in the field is on the rise.How to have
The problem that effect is seriously paid close attention to the producer that the instruction has crossed production electric equipment products as me.Therefore, be badly in need of it is a kind of quick,
The method for accurately testing electric middle harmful substance.Analyzed using ion emission spectroscopy more than current analysis method, but this side
Pre-treatment of the method to sample is relatively complicated, and exists because the factors such as matrix difference, concentration gradient can cause detection data difference
Problem.Xray fluorescence spectrometer nondestructive can carry out multielement analysis, with quick, accurate, easy, accuracy
High the advantages of, but in discrimination process, the acquisition of standard sample costly, because in the preparation process of sample, loss is difficult
To avoid, it is very big or situations such as there is uneven, poor reproducibility that the actual sample for often occurring preparing deviates standard sample.
The content of the invention
The invention aims to overcome the deficiencies in the prior art, there is provided it is a kind of for X-ray fluorescence spectra analysis
The preparation method of ABS standard samples.Satisfactory ABS standard samples can be readily available by methods described.
Above-mentioned purpose of the invention is achieved by following technical solution:
A kind of preparation method of ABS standard samples for X-ray fluorescence spectra analysis, comprises the following steps:
S1. the powder stock containing metal target element is prepared, the size of the powder stock was 400 mesh sieves;
S2. ABS resin of the metal target constituent content less than instrument test limit is chosen, and is confirmed wherein without antioxidant, plasticising
Agent;
S3. lubricant is added in the ratio relative to ABS resin quality 2 ‰ ~ 3 ‰, ABS resin is uniform with mix lubricant;
S4. according to standard sample tenor demand, according to it is following rule confirm metal addition:
A. cadmium element:When in ABS standard samples, the target content of cadmium element<During 100ppm, the addition=target of cadmium element contains
Amount ×(1.1±5%);
When in ABS standard samples, during the target content≤3000ppm of 100ppm≤cadmium element, the addition=target of cadmium element contains
Amount ×(1.05±5%);
B. lead element:When in ABS standard samples, during the target content≤3000ppm of lead element, the addition=target of lead element
Content ×(1.05±5%);
C. mercury element:When in ABS standard samples, during the target content≤3000ppm of mercury element, the addition=target of mercury element
Content ×(1.2±5%);
D. chromium:When in ABS standard samples, the target content of chromium<During 1000ppm, the addition=target of chromium contains
Amount ×(1.05±5%);
When in ABS standard samples, during the target content≤3000ppm of 1000ppm≤chromium, the addition=target of chromium
Content ×(1.1±5%);
S5. according to S4. rule conversion powder stock addition, and powder stock is put into the mixed ABS resins of S3.
In high mixer, first time mixing is carried out under the mixing speed of 100 ~ 400r/min;After well mixed, add relative to ABS
The lubricant of resin quality 0.5 ‰ ~ 1.5 ‰, carries out second mixing under the mixing speed of 500 ~ 1200r/min;
S6. the mixed materials of S5. are heated into melting, extrusion moulding, granulation in an extruder;Standard sample is made by pellet.
Can be containing any one or a few in cadmium, lead, mercury or chromium in the standard sample.
Preferably, in S2., detect that the content for confirming object element in ABS resin is less than test limit by ICP-AES.
Preferably, in S2., detected by GC/MS and confirm to be free of antioxidant, plasticizer in ABS resin.
Preferably, in S3., ABS resin and lubricant are placed in sealing space, it is multi-party with the frequency of 20 ~ 40 times/min
Mix to vibration, incorporation time is no less than 5min.
Lubricant used can be lubricant commonly used in the art, preferably White Mineral Oil.
Preferably, in S3., it was processed in 2 hours after ABS resin is uniform with mix lubricant.
Inventor has found, metal dust is mixed at twice with ABS resin, is even more important to well mixed, mixed for the first time
Control is closed in relatively low rotating speed, lubricant can be made more uniformly to infiltrate ABS, and make ABS preferably preliminary with metal dust
Mixing.Mix for second, filled into the lubricant of appropriate amount, and under mixing speed higher, metal dust is mixed with ABS
Obtain more full and uniform.Preferably, in S5., the mixing velocity of mixing is 200 ~ 300r/min for the first time;Second mixing of mixing
For 700 ~ 1000r/min preferably, in S5., the time of mixing is 3 ~ 5min to speed every time.Preferably, in S6., pellet passes through
The mode of injection moulding is made standard sample;The temperature for being molded melting is 170 ~ 190 DEG C.
Preferably, in S6., obtained standard sample is sheet.
Preferably, in S6., the thickness of obtained standard sample is 1 ~ 5mm.
Preferably, in S6., the extruder is preferably double screw extruder.It is highly preferred that extrusion heating melt temperature is
180~210℃。
Preferably, the powder stock containing metal target element is selected from the inorganic salts containing metal target element or oxidation
Thing.For example, cadmium can be with selective oxidation cadmium, lead is selected from lead orthoplumbate, and mercury is selected from mercury oxide, and chromium is selected from potassium bichromate.
Preferably, in S5., other auxiliary agents during second mixing also in addition to lubricant.Described other auxiliary agents include but not
It is limited to stabilizer, antioxidant etc..
Compared with prior art, the present invention has following Advantageous Effects:
Method in accordance with the present invention, be obtained in that with the hand-to-hand standard sample of target content, sample preparation is visibly homogeneous, and
Favorable reproducibility.Method of the present invention is easy to operate, can be realized using conventional equipment.The standard that the method is prepared
Sample provides magnitude tracing material for daily electric plastic product detection, solves matrix difference, concentration gradient etc.
Factor can cause detection data difference problem, accurately ensure that the monitoring of the heavy metal element concentration in electronic and electrical equipment, no
The health of environment and the people is only protected, and the skill for making China's Related product squeeze into the international market, breaking in international trade
Art barrier has cleared away obstacle, and standard substance is reliably detected for the import and export of National Electrical electric equipment products are provided.
Specific embodiment
With reference to specific embodiment and comparative example, the present invention is described in further detail, but the present invention is not limited to
Following embodiments.
In embodiment, raw material used is commercial goods.
Embodiment:Standard sample is prepared by the demand of table 1, according to dependency rule, the addition of the respective element that converts, conversion
Notional result is as shown in table 2:
Table 1
The standard sample metal target of embodiment 1 contains Amount(mg/kg) | The standard sample metal target of embodiment 2 contains Amount(mg/kg) | The standard sample metal target of embodiment 3 Content(mg/kg) | The standard sample metal target of embodiment 4 contains Amount(mg/kg) | |
Cadmium(Cd) | 13 | 130 | 1300 | 2600 |
Lead(Pb) | 10 | 100 | 1000 | 2000 |
Mercury(Hg) | 9.5 | 95 | 950 | 1900 |
Chromium(Cr) | 5 | 50 | 500 | 1500 |
Table 2
Embodiment 1 adds metal concentration(mg/kg) | Embodiment 2 adds metal concentration(mg/kg) | Embodiment 3 adds metal concentration(mg/kg) | Embodiment 4 adds metal concentration(mg/kg) | |
Cadmium(Cd) | 14.3 | 136.5 | 1365 | 2730 |
Lead(Pb) | 10.5 | 105 | 1050 | 2100 |
Mercury(Hg) | 11.4 | 114 | 1140 | 2280 |
Chromium(Cr) | 5.25 | 52.5 | 525 | 1650 |
In embodiment, cadmium oxide, lead orthoplumbate, mercury oxide, potassium bichromate are selected in each metallic element source respectively.According to each gold
In category compound, the content of metal, the actual interpolation amount of the metallic compound that converts, as a result as shown in table 3:
Table 3
Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | |
ABS/g | 1000 | 1000 | 1000 | 1000 |
Cadmium oxide/g | 0.0163 | 0.156 | 1.56 | 3.12 |
Lead orthoplumbate/g | 0.0116 | 0.116 | 1.16 | 2.32 |
Mercury oxide/g | 0.0123 | 0.123 | 1.23 | 2.46 |
Potassium bichromate/g | 0.0297 | 0.297 | 2.97 | 8.91 |
S1. cadmium oxide, lead orthoplumbate, mercury oxide, potassium bichromate are ground with ball mill respectively, mistake respectively after grinding
400 mesh stainless steels are sieved;
S2. ABS resin of the metal target constituent content less than instrument test limit is chosen, and is confirmed wherein without antioxidant, plasticising
Agent;
S3.1000g ABS resins quality adds 2mL White Mineral Oils, and ABS resin and lubricant are placed in hermetic bag, with 30 times/
The multi-direction vibrations of frequency of min, mix 7min, are well mixed;
S4. the content according to metal target element in standard sample, the addition of the needs that convert, obtain the formula of table 3;
S5. according to the formula of table 3, take powder stock and be put into high mixer with the mixed ABS resins of S3., 250r/min's
First time mixing is carried out under mixing speed, after mixing 3 minutes, the White Mineral Oil relative to ABS resin quality 1mL is added,
Second mixing is carried out under the mixing speed of 850r/min, incorporation time is also 3 minutes.
S6. by the mixed materials of S5. at 190 DEG C, melting is heated in double screw extruder so that powdered heavy metal fills
Divide and be evenly dispersed into ABS masterbatch, granulated by ABS extrusion moulding, in comminutor with extruder, at a temperature of 180 DEG C, use
ABS injection mouldings are made standard sample by injection machine.
In the standard sample that embodiment 1 ~ 4 is prepared, the measured value of each element is as shown in table 4:
Table 4
Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | |
Cadmium element(mg/kg) | 12.87 | 130.85 | 1314.44 | 2651.76 |
Lead element(mg/kg) | 10.93 | 101.92 | 1029.01 | 2032.62 |
Mercury element(mg/kg) | 9.79 | 98.21 | 966.89 | 1979.90 |
Chromium(mg/kg) | 4.90 | 49.53 | 502.15 | 1511.96 |
Contrasted from the target standard specimen of the measured result of table 4 and table 1, according to measurement error scope major part in the range of 3.5%, with
Desired value is sufficiently close to.
Standard sample uniformity 1:
According to the aimed concn of embodiment 1,10 batches are repeated, two parallel standards samples are made per batch products, test each standard
Metal element content in sample, as a result as shown in table 5:
Table 5
Note:Using:《CNAS-GL03 proficiency testings sample homogeneity and estimation of stability guide》The requirement of 4.1 uniformity testings
With the uniformity that method, 4.2 one-factor analysis of variance methods carry out sample, as a result as shown in table 6.
The finished product uniformity of table 6(Interpretation of result)
F critical values F0.05 (9,10)=3.02
The F value < F critical values of calculating, this shows in 0.05 significance, with sample room without significant difference, sample in sample
It is uniform.
Standard sample uniformity 2:
According to the aimed concn of embodiment 2,10 batches are repeated, two parallel standards samples are made per batch products, test each standard
Metal element content in sample, as a result as shown in table 7:
Table 7
Note:Using:《CNAS-GL03 proficiency testings sample homogeneity and estimation of stability guide》The requirement of 4.1 uniformity testings
With the uniformity that method, 4.2 one-factor analysis of variance methods carry out sample, as a result as shown in table 8.
The finished product uniformity of table 8(Interpretation of result)
F critical values F0.05 (9,10)=3.02
The F value < F critical values of calculating, this shows in 0.05 significance, with sample room without significant difference, sample in sample
It is uniform.
Standard sample uniformity 3:
According to the aimed concn of embodiment 3,10 batches are repeated, two parallel standards samples are made per batch products, test each standard
Metal element content in sample, as a result as shown in table 9:
Table 9
Note:Using:《CNAS-GL03 proficiency testings sample homogeneity and estimation of stability guide》The requirement of 4.1 uniformity testings
With the uniformity that method, 4.2 one-factor analysis of variance methods carry out sample, as a result as shown in table 10.
The finished product uniformity of table 10(Interpretation of result)
F critical values F0.05 (9,10)=3.02
The F value < F critical values of calculating, this shows in 0.05 significance, with sample room without significant difference, sample in sample
It is uniform.
Standard sample uniformity 4:
According to the aimed concn of embodiment 4,10 batches are repeated, two parallel standards samples are made per batch products, test each standard
Metal element content in sample, as a result as shown in table 11:
Table 11
Note:Using:《CNAS-GL03 proficiency testings sample homogeneity and estimation of stability guide》The requirement of 4.1 uniformity testings
With the uniformity that method, 4.2 one-factor analysis of variance methods carry out sample, as a result as shown in table 12.
The finished product uniformity of table 12(Interpretation of result)
F critical values F0.05 (9,10)=3.02
The F value < F critical values of calculating, this shows in 0.05 significance, with sample room without significant difference, sample in sample
It is uniform.
Be can be seen that in sample from the checking of table 5 ~ 12 and sample room is without significant difference, sample is uniform.Result has
Repeatability.
Comparative example:
According to the aimed concn of embodiment 4, sample preparation is carried out as follows:
S1. cadmium oxide, lead orthoplumbate, mercury oxide, potassium bichromate are ground with ball mill respectively, 400 mesh is crossed after grinding
Stainless steel sieves above-mentioned material;
S2. ABS resin of the metal target constituent content less than instrument test limit is chosen, and is confirmed wherein without antioxidant, plasticising
Agent;
S3.1000g ABS resins quality adds 2mL White Mineral Oils, and ABS resin and lubricant are placed in hermetic bag, with 30 times/
The multi-direction vibrations of frequency of min, mix 7min, are well mixed;
S4. according to the formula of table 3, take powder stock and be put into high mixer with the mixed ABS resins of S3., add relative to ABS
The White Mineral Oil of resin quality 1mL, under the mixing speed of 600r/min, mixes 6 minutes.
S5. by the mixed materials of S4. at 190 DEG C, melting is heated in double screw extruder so that powdered heavy metal fills
Divide and be evenly dispersed into ABS masterbatch, granulated by ABS extrusion moulding, in comminutor with extruder, at a temperature of 180 DEG C, use
ABS injection mouldings are made comparative example standard sample by injection machine.
10 batches are repeated, two parallel comparative example standard samples are made per batch products, the metal unit tested in each standard sample
Cellulose content, as a result as shown in table 13:
Note:Using:《CNAS-GL03 proficiency testings sample homogeneity and estimation of stability guide》The requirement of 4.1 uniformity testings
With the uniformity that method, 4.2 one-factor analysis of variance methods carry out sample, as a result as shown in table 14.
The finished product uniformity of table 14(Interpretation of result)
F critical values F0.05 (9,10)=3.02
Far more than F critical values, this shows in 0.05 significance the F values of calculating, has significantly with sample room in sample
Difference, sample is uneven.Result is without repeatability.
From the above, it can be seen that by method of the present invention, being obtained in that uniform sample, and the standard being made
Very close to theoretical value, accuracy is much higher than 20 ~ 30% error models of common customer requirements to the content of metal target element in sample
Enclose.
Claims (10)
1. the preparation method of a kind of ABS standard samples for X-ray fluorescence spectra analysis, it is characterised in that including following step
Suddenly:
S1. the powder stock containing metal target element is prepared, the size of the powder stock was 400 mesh sieves;
S2. ABS resin of the metal target constituent content less than instrument test limit is chosen, and is confirmed wherein without antioxidant, plasticising
Agent;
S3. lubricant is added in the ratio relative to ABS resin quality 2 ‰ ~ 3 ‰, ABS resin is uniform with mix lubricant;
S4. according to standard sample tenor demand, according to it is following rule confirm metal addition:
A. cadmium element:When in ABS standard samples, the target content of cadmium element<During 100ppm, the addition=target of cadmium element contains
Amount ×(1.1±5%);
When in ABS standard samples, during the target content≤3000ppm of 100ppm≤cadmium element, the addition=target of cadmium element contains
Amount ×(1.05±5%);
B. lead element:When in ABS standard samples, during the target content≤3000ppm of lead element, the addition=target of lead element
Content ×(1.05±5%);
C. mercury element:When in ABS standard samples, during the target content≤3000ppm of mercury element, the addition=target of mercury element
Content ×(1.2±5%);
D. chromium:When in ABS standard samples, the target content of chromium<During 1000ppm, the addition=target of chromium contains
Amount ×(1.05±5%);
When in ABS standard samples, during the target content≤3000ppm of 1000ppm≤chromium, the addition=target of chromium
Content ×(1.1±5%);
S5. according to S4. rule conversion powder stock addition, and powder stock is put into the mixed ABS resins of S3.
In high mixer, first time mixing is carried out under 100 ~ 400r/min mixing speeds;After well mixed, add relative to ABS trees
The lubricant of lipid amount 0.5 ‰ ~ 1.5 ‰, carries out second mixing under the mixing speed of 500 ~ 1200r/min;
S6. the mixed materials of S5. are heated into melting, extrusion moulding, granulation in an extruder;Standard sample is made by pellet.
2. the preparation method of the ABS standard samples of X-ray fluorescence spectra analysis is used for according to claim 1, and its feature exists
In in S2., the content for detecting metal target element in confirmation ABS resin by ICP-AES is less than test limit.
3. the preparation method of the ABS standard samples of X-ray fluorescence spectra analysis is used for according to claim 1, and its feature exists
In in S2., by being free of antioxidant, plasticizer in GC/MS detection confirmation ABS resins.
4. the preparation method of the ABS standard samples of X-ray fluorescence spectra analysis is used for according to claim 1, and its feature exists
In, in S3., ABS resin and lubricant are placed in sealing space, with the multi-direction vibration mixing of the frequency of 20 ~ 40 times/min, mix
The conjunction time is no less than 5min.
5. the preparation method of the ABS standard samples of X-ray fluorescence spectra analysis is used for according to claim 1, and its feature exists
In in S3., being processed in 2 hours after ABS resin is uniform with mix lubricant.
6. the preparation method of the ABS standard samples of X-ray fluorescence spectra analysis is used for according to claim 1, and its feature exists
In in S5., the mixing velocity of mixing is 200 ~ 300r/min for the first time;Second mixing velocity of mixing is 700 ~ 1000r/
min。
7. the preparation method of the ABS standard samples of X-ray fluorescence spectra analysis is used for according to claim 1, and its feature exists
In in S5., the time of mixing is 3 ~ 5min every time.
8. the preparation method of the ABS standard samples of X-ray fluorescence spectra analysis is used for according to claim 1, and its feature exists
In in S6., pellet is made standard sample by way of injection moulding;The temperature for being molded melting is 170 ~ 190 DEG C.
9. the preparation method of the ABS standard samples of X-ray fluorescence spectra analysis is used for according to claim 1, and its feature exists
In in S5., second is additionally added other auxiliary agents in addition to lubricant when mixing.
10. the preparation method of the ABS standard samples of X-ray fluorescence spectra analysis is used for according to claim 1, and its feature exists
In in S6., the extruder is double screw extruder.
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CN109100383A (en) * | 2018-08-31 | 2018-12-28 | 深圳市必发达科技有限公司 | Standard sample is used in a kind of RoHS detection |
CN110819059A (en) * | 2019-11-04 | 2020-02-21 | 安徽建筑大学 | Preparation method of ABS plastic standard sample containing trace lead |
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