CN114166828A - Experimental method for detecting sulfur element in industrial hydrofluoric acid - Google Patents
Experimental method for detecting sulfur element in industrial hydrofluoric acid Download PDFInfo
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- CN114166828A CN114166828A CN202111364881.1A CN202111364881A CN114166828A CN 114166828 A CN114166828 A CN 114166828A CN 202111364881 A CN202111364881 A CN 202111364881A CN 114166828 A CN114166828 A CN 114166828A
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- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 title claims abstract description 87
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 title claims abstract description 73
- 229910052717 sulfur Inorganic materials 0.000 title claims abstract description 70
- 239000011593 sulfur Substances 0.000 title claims abstract description 70
- 238000002474 experimental method Methods 0.000 title claims abstract description 28
- 230000003595 spectral effect Effects 0.000 claims abstract description 30
- 238000004458 analytical method Methods 0.000 claims abstract description 28
- 239000000243 solution Substances 0.000 claims abstract description 28
- 238000000034 method Methods 0.000 claims abstract description 25
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims abstract description 23
- 239000004327 boric acid Substances 0.000 claims abstract description 23
- 239000012086 standard solution Substances 0.000 claims abstract description 18
- 238000001514 detection method Methods 0.000 claims abstract description 13
- 238000009616 inductively coupled plasma Methods 0.000 claims abstract description 12
- 239000000126 substance Substances 0.000 claims abstract description 6
- 239000000523 sample Substances 0.000 claims description 57
- 238000012360 testing method Methods 0.000 claims description 29
- 238000011084 recovery Methods 0.000 claims description 14
- 239000011550 stock solution Substances 0.000 claims description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- 239000012153 distilled water Substances 0.000 claims description 13
- 238000005303 weighing Methods 0.000 claims description 10
- 239000012482 calibration solution Substances 0.000 claims description 8
- 238000012546 transfer Methods 0.000 claims description 8
- -1 polytetrafluoroethylene Polymers 0.000 claims description 5
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 5
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 5
- 239000012496 blank sample Substances 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 4
- 238000007689 inspection Methods 0.000 abstract description 9
- 238000006243 chemical reaction Methods 0.000 abstract description 5
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 6
- RAHZWNYVWXNFOC-UHFFFAOYSA-N Sulphur dioxide Chemical compound O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 description 4
- 238000003556 assay Methods 0.000 description 4
- AKEJUJNQAAGONA-UHFFFAOYSA-N sulfur trioxide Chemical compound O=S(=O)=O AKEJUJNQAAGONA-UHFFFAOYSA-N 0.000 description 4
- 241001061225 Arcos Species 0.000 description 3
- 239000012491 analyte Substances 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- WUKWITHWXAAZEY-UHFFFAOYSA-L calcium difluoride Chemical compound [F-].[F-].[Ca+2] WUKWITHWXAAZEY-UHFFFAOYSA-L 0.000 description 1
- 229910001634 calcium fluoride Inorganic materials 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229910000040 hydrogen fluoride Inorganic materials 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
Classifications
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- 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
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/71—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited
- G01N21/73—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited using plasma burners or torches
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- Chemical & Material Sciences (AREA)
- Plasma & Fusion (AREA)
- Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
Abstract
The invention relates to the field of chemical inspection, in particular to an experimental method for inspecting sulfur element in industrial hydrofluoric acid, which adopts an inductively coupled plasma atomic emission spectrometer for inspection, utilizes a 2% boric acid solution to carry out a complex reaction with the industrial hydrofluoric acid, avoids the damage of the hydrofluoric acid to equipment and inspection personnel in the inspection process, uses a sulfur standard solution as a working curve, selects a proper spectral line, avoids spectral line interference, and adopts the optimal inspection condition to carry out experiments; the method is suitable for rapid and accurate analysis of the sulfur content in the industrial hydrofluoric acid; has the advantages of simple operation and reliable result, and the detection of sulfur element in industrial hydrofluoric acid is the first initiative in China.
Description
Technical Field
The invention relates to the field of chemical examination, in particular to an experimental method for examining sulfur element in industrial hydrofluoric acid.
Background
The most classical method for preparing industrial hydrofluoric acid is to heat calcium fluoride and concentrated sulfuric acid to a certain temperature to generate hydrofluoric acid steam, generate a mixture of hydrogen fluoride, sulfuric acid and other byproducts in the reaction process, and then purify the mixture by distillation, wherein the concentrated sulfuric acid used in the preparation of the industrial hydrofluoric acid directly burns sulfur to generate sulfur dioxide, the sulfur dioxide is oxidized to generate sulfur trioxide, and the sulfur trioxide is dissolved in water to generate the industrial sulfuric acid, so that the industrial hydrofluoric acid contains a certain content of sulfur elements, and the sulfur elements are meaningless for the use of the industrial hydrofluoric acid and can be called as impurity elements. At present, no method for detecting sulfur element in industrial hydrofluoric acid exists in China, and related contents are difficult to be found in literatures and data.
Disclosure of Invention
The invention aims to provide an experimental method for detecting sulfur in industrial hydrofluoric acid, which avoids the damage of hydrofluoric acid to equipment and analysts, has the advantages of simple operation, good precision and accurate experimental result, provides a certain data support for evaluating the quality of the industrial hydrofluoric acid, and fills the gap of detecting sulfur in industrial hydrofluoric acid in China.
In order to achieve the technical effects, the experimental method for detecting sulfur in industrial hydrofluoric acid comprises the following steps:
s1, sample moving: using a liquid transfer gun or a polytetrafluoroethylene dropper to transfer 0.2g of industrial hydrofluoric acid sample to be accurate to 0.01g, adding the industrial hydrofluoric acid sample into a 100mL volumetric flask which is previously filled with 10mL of 2% boric acid solution, using distilled water to fix the volume, and carrying out blank experiments along with batches;
s2, preparing a primary stock solution, namely selecting 1000ug/mL of sulfur standard solution, transferring 1mL of the standard solution into a 1000mL volumetric flask for constant volume to serve as the primary stock solution with the concentration of 1 ug/mL;
s3, respectively transferring 0mL, 1mL, 2mL, 3mL, 4mL and 5mL of the primary stock solution prepared in the step S2 into a 100mL volumetric flask which is previously filled with 10mL of 2% boric acid solution, and fixing the volume by using distilled water;
s4, detecting the six solutions in the step S3 by using an inductively coupled plasma atomic emission spectrometer, drawing a standard curve, and selecting a spectral line suitable for sulfur element analysis;
and S5, detecting the sulfur content of the sample according to the sulfur analysis spectral line obtained in the step S4.
Further, the elemental sulfur analysis line obtained in step S4 uses a 180.731nm analysis line.
The spectral lines of sulfur elements are detected to be 166.668nm, 182.034nm and 180.731nm, wherein the spectral line 166.668nm has a relatively strong interference spectral line, the spectral line 182.034nm is poor in linearity, and the spectral line 180.731nm is recommended.
Further, determining the detection limit of the sulfur element detected by the method, and performing sample blank measurement; and repeating the blank test for 7 times, wherein in the blank test, 10mL of 2% boric acid solution is added into a 100mL volumetric flask, the volume is constant, a blank sample is prepared, the standard deviation is determined according to the detection result of the sulfur element in the blank test for 7 times, and the detection limit of the sulfur element method is calculated.
Further, the linear correlation coefficient of the curve of the sulfur element analysis line obtained in step S4 must be greater than 0.999.
The closer the curve linear correlation coefficient of the analysis spectral line is to 1, the closer the correlation among the explanatory variables is, and the better the linear relation is.
Further, 0.1g of sample, 0.2g of sample and 0.3g of sample are respectively weighed, a method linear experiment is carried out, the signal response value of the instrument is ensured to be in a direct proportional relation with the concentration content of the sample, the test results of the same sample under different sample weighing amounts are close to each other and are smaller than the method allowable error, and the linear experiment meets the requirements; respectively weighing 0.1g, 0.2g and 0.3g of the same sample to be accurate to 0.01g, adding the sample into a 100mL volumetric flask which is filled with 10mL of 2% boric acid solution in advance, carrying out constant volume by using distilled water to obtain a linear analysis sample, and inspecting the analysis sample at a spectral line of 180.731nm by using an inductively coupled plasma atomic emission spectrometer.
The concentration range mentioned in the 5.3 linear range in the national standard GB/T27417-~150%, 0.2g of sample was removed in step S1, and 0.1g, 0.2g, 0.3g of sample was weighed to cover 50% of the concentration of interest~150 percent, and the test result meets the requirement, which indicates that the test result with the content (concentration) in the linear range meets the requirement. The development of the linear assay in determining the linear range of the assay indicates good stability of the target analyte in the sample and in the matrix components.
Further, weighing six equal-quantity 0.2g industrial hydrofluoric acid samples, accurately measuring the samples to 0.01g, adding the samples into a 100mL volumetric flask which is filled with 10mL of 2% boric acid solution in advance, selecting 1000ug/mL of sulfur standard solution, preparing a calibration solution with the concentration of 0.01ug/mL, adding the calibration solution into the six volumetric flasks respectively by taking 0mL, 0.2mL, 0.4mL, 0.6mL, 0.8mL and 1.0mL, respectively analyzing the six volumetric flasks according to the steps S2-S5, subtracting the result of the nonstandard test from the result of the sulfur element test after adding the standard, and obtaining the ratio of the difference value to the theoretical value of the added standard substance, namely the formula:
and calculating the standard adding recovery rate of the five samples according to a formula, wherein the standard adding recovery rate range is required to be 93.5-103.5%.
The standard addition recovery rate range is required to be 93.5-103.5%, which shows that the standard addition recovery rate is better, and the accuracy and precision of the real reaction determination result are better.
The invention has the beneficial effects that: the method comprises the steps of using a pipette or a polytetrafluoroethylene dropper to pipette 0.2g of industrial hydrofluoric acid sample, accurately measuring the sample to 0.01g, adding the sample into a 100mL volumetric flask which is previously filled with 10mL of 2% boric acid solution, using distilled water to fix the volume, and carrying out blank experiments along with batches; selecting 1000ug/mL of sulfur standard solution, wherein the sulfur standard solution is commercially available, transferring 1mL of standard solution into a 1000mL volumetric flask for constant volume, and taking the standard solution as primary stock solution with the concentration of 1 ug/mL; respectively transferring 0mL, 1mL, 2mL, 3mL, 4mL and 5mL of the primary stock solution prepared in the step S2 into a 100mL volumetric flask which is previously filled with 10mL of 2% boric acid solution, and fixing the volume by using distilled water; detecting the six solutions in the step S3 by using an inductively coupled plasma atomic emission spectrometer, and drawing a standard curve; selecting a proper sulfur element analysis spectral line; and detecting the sulfur content of the sample according to the sulfur analysis spectral line obtained in the step S4.
The method adopts an inductively coupled plasma atomic emission spectrometer for inspection, utilizes 2% boric acid solution and industrial hydrofluoric acid to carry out complex reaction, avoids the damage of the hydrofluoric acid to equipment and inspection personnel in the inspection process, uses sulfur standard solution as a working curve, selects proper spectral lines, avoids spectral line interference, and adopts the best inspection condition to carry out experiments; the method is suitable for rapid and accurate analysis of the sulfur content in the industrial hydrofluoric acid; has the advantages of simple operation and reliable result, and the detection of sulfur element in industrial hydrofluoric acid is the first initiative in China.
Detailed Description
The experimental method for detecting sulfur element in industrial hydrofluoric acid comprises the following steps:
s1, sample moving: using a liquid transfer gun or a polytetrafluoroethylene dropper to transfer 0.2g of industrial hydrofluoric acid sample to be accurate to 0.01g, adding the industrial hydrofluoric acid sample into a 100mL volumetric flask which is previously filled with 10mL of 2% boric acid solution, using distilled water to fix the volume, and carrying out blank experiments along with batches;
s2, preparing a primary stock solution, namely selecting 1000ug/mL of sulfur standard solution, transferring 1mL of the standard solution into a 1000mL volumetric flask for constant volume to serve as the primary stock solution with the concentration of 1 ug/mL;
s3, respectively transferring 0mL, 1mL, 2mL, 3mL, 4mL and 5mL of the primary stock solution prepared in the step S2 into a 100mL volumetric flask which is previously filled with 10mL of 2% boric acid solution, and fixing the volume by using distilled water;
s4, detecting the six solutions in the step S3 by using an inductively coupled plasma atomic emission spectrometer, drawing a standard curve, and selecting a spectral line suitable for sulfur element analysis;
and S5, detecting the sulfur content of the sample according to the sulfur analysis spectral line obtained in the step S4.
Further, the elemental sulfur analysis line obtained in step S4 uses a 180.731nm analysis line.
The spectral lines of sulfur elements are detected to be 166.668nm, 182.034nm and 180.731nm, wherein the spectral line 166.668nm has a relatively strong interference spectral line, the spectral line 182.034nm is poor in linearity, and the spectral line 180.731nm is recommended.
Further, determining the detection limit of the sulfur element detected by the method, and performing sample blank measurement; and repeating the blank test for 7 times, wherein in the blank test, 10mL of 2% boric acid solution is added into a 100mL volumetric flask, the volume is constant, a blank sample is prepared, the standard deviation is determined according to the detection result of the sulfur element in the blank test for 7 times, and the detection limit of the sulfur element method is calculated.
Further, the linear correlation coefficient of the curve of the sulfur element analysis line obtained in step S4 must be greater than 0.999.
The closer the curve linear correlation coefficient of the analysis spectral line is to 1, the closer the correlation among the explanatory variables is, and the better the linear relation is.
Further, 0.1g of sample, 0.2g of sample and 0.3g of sample are respectively weighed, a method linear experiment is carried out, the signal response value of the instrument is ensured to be in a direct proportional relation with the concentration content of the sample, the test results of the same sample under different sample weighing amounts are close to each other and are smaller than the method allowable error, and the linear experiment meets the requirements; respectively weighing 0.1g, 0.2g and 0.3g of the same sample to be accurate to 0.01g, adding the sample into a 100mL volumetric flask which is filled with 10mL of 2% boric acid solution in advance, carrying out constant volume by using distilled water to obtain a linear analysis sample, and inspecting the analysis sample at a spectral line of 180.731nm by using an inductively coupled plasma atomic emission spectrometer.
The concentration range mentioned in the 5.3 linear range in the national standard GB/T27417-~150%, 0.2g of sample was removed in step S1, and 0.1g, 0.2g, 0.3g of sample was weighed to cover 50% of the concentration of interest~150 percent, and the test result meets the requirement, which indicates that the test result with the content (concentration) in the linear range meets the requirement. The development of the linear assay in determining the linear range of the assay indicates good stability of the target analyte in the sample and in the matrix components.
Further, weighing six equal-quantity 0.2g industrial hydrofluoric acid samples, accurately measuring the samples to 0.01g, adding the samples into a 100mL volumetric flask which is filled with 10mL of 2% boric acid solution in advance, selecting 1000ug/mL of sulfur standard solution, preparing a calibration solution with the concentration of 0.01ug/mL, adding the calibration solution into the six volumetric flasks respectively by taking 0mL, 0.2mL, 0.4mL, 0.6mL, 0.8mL and 1.0mL, respectively analyzing the six volumetric flasks according to the steps S2-S5, subtracting the result of the nonstandard test from the result of the sulfur element test after adding the standard, and obtaining the ratio of the difference value to the theoretical value of the added standard substance, namely the formula:
and calculating the standard adding recovery rate of the five samples according to a formula, wherein the standard adding recovery rate range is required to be 93.5-103.5%.
The standard addition recovery rate range is required to be 93.5-103.5%, which shows that the standard addition recovery rate is better, and the accuracy and precision of the real reaction determination result are better.
The first embodiment is as follows:
experiments of the invention were performed using an inductively coupled plasma atomic emission spectrometer model ARCOS FHS16, according to the steps of the invention:
s1, sample moving: using a liquid transfer gun or a polytetrafluoroethylene dropper to transfer 0.2g of industrial hydrofluoric acid sample to be accurate to 0.01g, adding the industrial hydrofluoric acid sample into a 100mL volumetric flask which is previously filled with 10mL of 2% boric acid solution, using distilled water to fix the volume, and carrying out blank experiments along with batches;
s2, preparing a primary stock solution, namely selecting 1000ug/mL of sulfur standard solution, transferring 1mL of the standard solution into a 1000mL volumetric flask for constant volume to serve as the primary stock solution with the concentration of 1 ug/mL;
s3, respectively transferring 0mL, 1mL, 2mL, 3mL, 4mL and 5mL of the primary stock solution prepared in the step S2 into a 100mL volumetric flask which is previously filled with 10mL of 2% boric acid solution, and fixing the volume by using distilled water;
s4, drawing a standard curve on the six solutions in the step S3 at the spectral line 180.731nm by using an ARCOS FHS16 inductively coupled plasma atomic emission spectrometer to obtain a sulfur element analysis spectral line;
and S5, detecting the sulfur content of the sample according to the sulfur analysis spectral line obtained in the step S4.
In step S4, the ARCOS FHS16 inductively coupled plasma atomic emission spectrometer was set up as follows.
Further, the blank test is repeated for 7 times, the blank test uses 10mL of 2% boric acid solution to be added into a 100mL volumetric flask, the volume is fixed, a blank sample is prepared, the standard deviation is determined according to the test result of the sulfur element in the 7 blank tests, the detection limit of the sulfur element method is calculated, and the 7 blank test result is shown in the following table.
Further, 0.1g, 0.2g and 0.3g of samples were weighed respectively, and a method linear experiment was performed, and experimental data are shown in the following table.
Further, six equal 0.2g industrial hydrofluoric acid samples with known sulfur content are weighed again to be accurate to 0.01g, added into a volumetric flask which is filled with 10mL of 2% boric acid solution in advance, 1000ug/mL of sulfur standard solution is selected, and calibration solution with concentration of 0.01ug/mL is preparedAdding 0mL, 0.2mL, 0.4mL, 0.6mL, 0.8mL and 1.0mL decibels of the calibration solution into six volumetric flasks, respectively analyzing the six volumetric flasks according to the steps S2-S5, subtracting the result of the nonstandard test from the result of the sulfur element test after the standard addition, and determining the ratio of the difference to the theoretical value of the added standard substance as the sample standard addition recovery rate according to the formula:
the normalized recovery of five samples was calculated and the structure is given in the table below.
The calculated structure shows that the recovery rate of the added standard is 93.5 percent~Within the range of 103.5%, the method is proved to have good accuracy and feasible method.
Claims (6)
1. An experimental method for detecting sulfur element in industrial hydrofluoric acid is characterized in that: the method comprises the following steps:
s1, sample moving: using a liquid transfer gun or a polytetrafluoroethylene dropper to transfer 0.2g of industrial hydrofluoric acid sample to be accurate to 0.01g, adding the industrial hydrofluoric acid sample into a 100mL volumetric flask which is previously filled with 10mL of 2% boric acid solution, using distilled water to fix the volume, and carrying out blank experiments along with batches;
s2, preparing a primary stock solution, namely selecting 1000ug/mL of sulfur standard solution, transferring 1mL of the standard solution into a 1000mL volumetric flask for constant volume to serve as the primary stock solution with the concentration of 1 ug/mL;
s3, respectively transferring 0mL, 1mL, 2mL, 3mL, 4mL and 5mL of the primary stock solution prepared in the step S2 into a 100mL volumetric flask which is previously filled with 10mL of 2% boric acid solution, and fixing the volume by using distilled water;
s4, detecting the six solutions in the step S3 by using an inductively coupled plasma atomic emission spectrometer, drawing a standard curve, and selecting a spectral line suitable for sulfur element analysis;
and S5, detecting the sulfur content of the sample according to the sulfur analysis spectral line obtained in the step S4.
2. The experimental method for detecting sulfur element in industrial hydrofluoric acid according to claim 1, wherein: the elemental sulfur analysis line obtained in step S4 was analyzed using 180.731 nm.
3. The experimental method for detecting sulfur element in industrial hydrofluoric acid according to claim 2, wherein: determining the detection limit of the sulfur element detected by the method, and performing sample blank detection; and repeating the blank test for 7 times, wherein in the blank test, 10mL of 2% boric acid solution is added into a 100mL volumetric flask, the volume is constant, a blank sample is prepared, the standard deviation is determined according to the detection result of the sulfur element in the blank test for 7 times, and the detection limit of the sulfur element method is calculated.
4. The experimental method for detecting sulfur element in industrial hydrofluoric acid according to claim 3, wherein: the linear correlation coefficient of the curve of the sulfur element analysis line obtained in step S4 must be greater than 0.999.
5. The experimental method for detecting sulfur element in industrial hydrofluoric acid according to claim 4, wherein: respectively weighing 0.1g, 0.2g and 0.3g of samples, developing a method linear experiment, ensuring that the signal response value of the instrument is in a direct proportional relation with the concentration content of the samples, and the test results of the same sample under different sample weighing amounts are close to each other and smaller than the method allowable error, so that the linear experiment meets the requirements; respectively weighing 0.1g, 0.2g and 0.3g of the same sample to be accurate to 0.01g, adding the sample into a 100mL volumetric flask which is filled with 10mL of 2% boric acid solution in advance, carrying out constant volume by using distilled water to obtain a linear analysis sample, and inspecting the analysis sample at a spectral line of 180.731nm by using an inductively coupled plasma atomic emission spectrometer.
6. The experimental method for detecting sulfur element in industrial hydrofluoric acid according to claim 5, wherein: weighing six equal industrial hydrofluoric acid samples of 0.2g again to the accuracy of 0.01g, adding the samples into a 100mL volumetric flask which is filled with 10mL of 2% boric acid solution in advance, and selecting a sulfur standard solution 1000ug/mL, preparing a calibration solution with a concentration of 0.01ug/mL, adding 0mL, 0.2mL, 0.4mL, 0.6mL, 0.8mL and 1.0mL of the calibration solution into six volumetric flasks, respectively, analyzing the six volumetric flasks according to steps S1-S5, subtracting the result of the un-labeled test from the result of the labeled sulfur element test, and determining the ratio of the difference to the theoretical value of the added standard substance as the sample labeled recovery rate, namely the formula:
and calculating the standard adding recovery rate of the five samples according to a formula, wherein the standard adding recovery rate range is required to be 93.5-103.5%.
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