CN113959966A - Method for measuring chlorine content in antimony-containing arsenic trioxide - Google Patents
Method for measuring chlorine content in antimony-containing arsenic trioxide Download PDFInfo
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- CN113959966A CN113959966A CN202111220637.8A CN202111220637A CN113959966A CN 113959966 A CN113959966 A CN 113959966A CN 202111220637 A CN202111220637 A CN 202111220637A CN 113959966 A CN113959966 A CN 113959966A
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- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 title claims abstract description 47
- 239000000460 chlorine Substances 0.000 title claims abstract description 47
- 229910052801 chlorine Inorganic materials 0.000 title claims abstract description 47
- HJTAZXHBEBIQQX-UHFFFAOYSA-N 1,5-bis(chloromethyl)naphthalene Chemical compound C1=CC=C2C(CCl)=CC=CC2=C1CCl HJTAZXHBEBIQQX-UHFFFAOYSA-N 0.000 title claims abstract description 38
- GOLCXWYRSKYTSP-UHFFFAOYSA-N arsenic trioxide Inorganic materials O1[As]2O[As]1O2 GOLCXWYRSKYTSP-UHFFFAOYSA-N 0.000 title claims abstract description 38
- 229910052787 antimony Inorganic materials 0.000 title claims abstract description 37
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 title claims abstract description 34
- 238000000034 method Methods 0.000 title claims abstract description 27
- 238000002835 absorbance Methods 0.000 claims abstract description 25
- 239000000243 solution Substances 0.000 claims description 71
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 36
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 14
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 12
- 229910017604 nitric acid Inorganic materials 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 10
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 5
- 238000007865 diluting Methods 0.000 claims description 5
- 238000005485 electric heating Methods 0.000 claims description 5
- 239000012086 standard solution Substances 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 238000005303 weighing Methods 0.000 claims description 5
- 239000003153 chemical reaction reagent Substances 0.000 claims description 2
- 238000004458 analytical method Methods 0.000 abstract description 7
- 229910021607 Silver chloride Inorganic materials 0.000 abstract description 3
- 239000002253 acid Substances 0.000 abstract description 3
- 239000003513 alkali Substances 0.000 abstract description 3
- 238000004090 dissolution Methods 0.000 abstract description 3
- 238000001556 precipitation Methods 0.000 abstract description 3
- 238000005272 metallurgy Methods 0.000 abstract description 2
- 238000002203 pretreatment Methods 0.000 abstract 2
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 abstract 2
- 230000001698 pyrogenic effect Effects 0.000 description 3
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- GBZANUMDJPCQHY-UHFFFAOYSA-L mercury(ii) thiocyanate Chemical compound [Hg+2].[S-]C#N.[S-]C#N GBZANUMDJPCQHY-UHFFFAOYSA-L 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000002798 spectrophotometry method Methods 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
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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
- G01N21/17—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
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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
-
- 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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- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention relates to a method for measuring the chlorine content in antimony-containing arsenic trioxide, which belongs to the technical field of metallurgy and comprises the following steps: 1. drawing a standard working curve: drawing a standard working curve by taking the chlorine content as a vertical coordinate and the absorbance as a horizontal coordinate; 2. sample pretreatment: adopting a pretreatment method of alkali dissolution, acid adjustment and silver chloride precipitation; 3. and (3) sample determination: and (4) checking a standard working curve according to the absorbance value, and calculating the chlorine content. According to the method for measuring the chlorine content in the antimony-containing arsenic trioxide, the sample is subjected to the pretreatment method of alkali dissolution, acid adjustment and silver chloride precipitation, the chlorine content in the pretreatment solution can be directly measured by a spectrophotometer, the operation is simple, the safety is high, the consumed time is short, the chlorine content in the pretreatment solution can be measured in a large batch at the same time, the accuracy is high, and the problems that the existing analysis method is not suitable for measuring the chlorine content in a large batch of antimony-containing arsenic trioxide products and the like can be effectively solved.
Description
Technical Field
The invention relates to a method for measuring the content of chlorine in arsenic trioxide, in particular to a method for measuring the content of chlorine in antimony-containing arsenic trioxide, and belongs to the technical field of metallurgy.
Background
No analysis method related to chlorine content exists in national standard GB 26721-; however, the arsenic trioxide product obtained by the pyrogenic process usually contains antimony impurity elements, antimony has adverse effects on an ammonia water dissolution sample, about half of the sample cannot be dissolved, and the subsequent determination of the chlorine content in the arsenic trioxide is affected.
The method adopted by the standard SN/T0837.4-2006 "determination of chloride ion content in arsenic trioxide" of entry and exit inspection and quarantine industry is distillation-mercury thiocyanate spectrophotometry, the method needs distillation, the used mercury thiocyanate is a first-level highly toxic product, about 4 hours is needed for analyzing one sample, the process is complicated, the time consumption is too long, unsafe factors are more, and the method is not suitable for batch detection.
However, the existing arsenic trioxide product has clear requirements on chlorine content in sale, and the chlorine content in the arsenic trioxide needs to be accurately and quantitatively measured, so that a method for measuring the chlorine content in the antimony-containing arsenic trioxide is urgently needed for preparing the antimony-containing arsenic trioxide product by adopting a pyrogenic process.
Disclosure of Invention
The purpose of the invention is: in order to overcome the defects in the prior art, the method for measuring the chlorine content in the antimony-containing arsenic trioxide is provided, and has the advantages of short time consumption, simple operation and high accuracy.
The technical scheme for solving the technical problems is as follows:
a method for measuring the chlorine content in antimony-containing arsenic trioxide comprises the following steps:
step 1, drawing a standard working curve: taking 5 50mL volumetric flasks, respectively transferring 0.00mL, 1.00mL, 2.00mL, 3.00mL and 5.00mL of chloride ion standard solution into the volumetric flasks, sequentially adding 5.00mL of 200g/L sodium hydroxide solution and 6.00mL of 50% nitric acid solution (volume concentration), diluting with water to a scale, and uniformly mixing; keeping out of the sun for 10 minutes, transferring a part of the solution into a 1cm cuvette, and measuring the absorbance of the solution at the wavelength of 420nm of a spectrophotometer; drawing a standard working curve by taking the chlorine content as a vertical coordinate and the absorbance as a horizontal coordinate;
step 2, sample pretreatment: weighing 0.2g (accurate to 0.0001g) of antimony-containing arsenic trioxide sample in a 100mL beaker, accurately adding 5.00mL of super-pure sodium hydroxide solution, slightly heating on a low-temperature electric heating plate until the sample is completely dissolved, accurately adding 6.00mL of super-pure nitric acid solution to adjust the solution to acidity, continuously slightly heating until the solution is clear, taking down and cooling, transferring to a 50mL volumetric flask, adding 1.00mL of silver nitrate solution into the volumetric flask, fixing the volume, uniformly mixing, and placing for 10 minutes in a dark place;
step 3, sample determination: and (3) transferring the solution to be detected, placing the solution in a 1cm cuvette, taking a blank test along with a sample as a reference, measuring the absorbance of the solution at the wavelength of 420nm of a spectrophotometer, and checking a standard working curve according to the absorbance value to calculate the chlorine content.
Further, the concentration of the sodium hydroxide solution with the guaranteed reagent is 200 g/L.
Further, the volume concentration of the superior pure nitric acid solution is 50%.
Further, the concentration of the silver nitrate solution is 17 g/L.
Further, As in the antimony-containing arsenic trioxide sample2O3And the content of Sb is: as2O3≥85%,Sb≤5.0%。
The invention has the beneficial effects that: the method for pretreating the antimony-containing arsenic trioxide sample by adopting alkali dissolution-acid regulation-silver chloride precipitation can be used for directly measuring the chlorine content in the pretreatment solution through a spectrophotometer, is simple to operate, high in safety and short in time consumption, can be used for simultaneously measuring the chlorine content in the pretreatment solution in large batches, is high in accuracy, and can be used for effectively solving the problems that the existing analysis method is not suitable for measuring the chlorine content in antimony-containing arsenic trioxide products in large batches and the like.
Drawings
FIG. 1 is a standard operating curve as described in the present invention;
FIG. 2 is a table of linear relationship data for the standard operating curves described in the present invention.
Detailed Description
The principles and features of the present invention are described below in conjunction with the accompanying fig. 1, which is provided by way of example only to illustrate the present invention and not to limit the scope of the present invention.
Preparing three antimony-containing arsenic trioxide samples according to a pyrogenic process, wherein As in the antimony-containing arsenic trioxide samples2O3And the content of Sb is: as2O3Not less than 85 percent and not more than 5.0 percent of Sb, and the chlorine content is respectively measured aiming at the three samples.
Example 1
A method for measuring the chlorine content in antimony-containing arsenic trioxide comprises the following steps:
step 1, drawing a standard working curve: taking 5 50mL volumetric flasks, respectively transferring 0.00mL, 1.00mL, 2.00mL, 3.00mL and 5.00mL of chloride ion standard solution into the volumetric flasks, sequentially adding 5.00mL of 200g/L sodium hydroxide solution and 6.00mL of 50% nitric acid solution (volume concentration), diluting with water to a scale, and uniformly mixing; keeping out of the sun for 10 minutes, transferring a part of the solution into a 1cm cuvette, and measuring the absorbance of the solution at the wavelength of 420nm of a spectrophotometer; drawing a standard working curve by taking the chlorine content as a vertical coordinate and the absorbance as a horizontal coordinate, as shown in figure 1; meanwhile, feasibility analysis is carried out on the standard working curve, relevant data are calculated, as shown in figure 2, the correlation degree of the absorbance and the chlorine content is high, and the standard working curve can be proved to have accuracy and reliability;
step 2, sample pretreatment: weighing 0.2g (accurate to 0.0001g) of antimony-containing arsenic trioxide sample 1 in a 100mL beaker, accurately adding 5.00mL of 200g/L sodium hydroxide solution, slightly heating on a low-temperature electric heating plate until the sample is completely dissolved, accurately adding 6.00mL of 50% nitric acid solution to adjust the solution to acidity, continuously slightly heating until the solution is clear, taking down and cooling, transferring to a 50mL volumetric flask, adding 1.00mL of 17g/L silver nitrate solution into the volumetric flask, fixing the volume, uniformly mixing, and placing for 10 minutes in a dark place;
step 3, sample determination: transferring 6 groups of solutions to be detected, respectively placing the solutions in a cuvette of 1cm, taking a blank test along with a sample as a reference, measuring the absorbance of the solutions at the position of 420nm wavelength of a spectrophotometer, checking a standard working curve according to the absorbance value, and calculating the chlorine content of the 6 groups of solutions to be detected as follows: 0.0048%, 0.0050%, 0.0047%, 0.0046%, 0.0049%, and 0.0048%, and the measured average value was 0.0048%, the standard deviation was 0.0014%, and the relative standard deviation was 2.95%.
Example 2
A method for measuring the chlorine content in antimony-containing arsenic trioxide comprises the following steps:
step 1, drawing a standard working curve: taking 5 50mL volumetric flasks, respectively transferring 0.00mL, 1.00mL, 2.00mL, 3.00mL and 5.00mL of chloride ion standard solution into the volumetric flasks, sequentially adding 5.00mL of 200g/L sodium hydroxide solution and 6.00mL of 50% nitric acid solution (volume concentration), diluting with water to a scale, and uniformly mixing; keeping out of the sun for 10 minutes, transferring a part of the solution into a 1cm cuvette, and measuring the absorbance of the solution at the wavelength of 420nm of a spectrophotometer; drawing a standard working curve by taking the chlorine content as a vertical coordinate and the absorbance as a horizontal coordinate, as shown in figure 1; meanwhile, feasibility analysis is carried out on the standard working curve, relevant data are calculated, as shown in figure 2, the correlation degree of the absorbance and the chlorine content is high, and the standard working curve can be proved to have accuracy and reliability;
step 2, sample pretreatment: weighing 0.2g (accurate to 0.0001g) of antimony-containing arsenic trioxide sample 2 in a 100mL beaker, accurately adding 5.00mL of 200g/L sodium hydroxide solution, slightly heating on a low-temperature electric heating plate until the sample is completely dissolved, accurately adding 6.00mL of 50% nitric acid solution to adjust the solution to acidity, continuously slightly heating until the solution is clear, taking down and cooling, transferring to a 50mL volumetric flask, adding 1.00mL of 17g/L silver nitrate solution into the volumetric flask, fixing the volume, uniformly mixing, and placing for 10 minutes in a dark place;
step 3, sample determination: transferring 6 groups of solutions to be detected, respectively placing the solutions in a cuvette of 1cm, taking a blank test along with a sample as a reference, measuring the absorbance of the solutions at the position of 420nm wavelength of a spectrophotometer, checking a standard working curve according to the absorbance value, and calculating the chlorine content of the 6 groups of solutions to be detected as follows: 0.0035%, 0.0034%, 0.0033%, 0.0035%, and 0.0036%, and the average value was measured to be 0.0035%, the standard deviation was 0.0010%, and the relative standard deviation was 3.04%.
Example 3
A method for measuring the chlorine content in antimony-containing arsenic trioxide comprises the following steps:
step 1, drawing a standard working curve: taking 5 50mL volumetric flasks, respectively transferring 0.00mL, 1.00mL, 2.00mL, 3.00mL and 5.00mL of chloride ion standard solution into the volumetric flasks, sequentially adding 5.00mL of 200g/L sodium hydroxide solution and 6.00mL of 50% nitric acid solution (volume concentration), diluting with water to a scale, and uniformly mixing; keeping out of the sun for 10 minutes, transferring a part of the solution into a 1cm cuvette, and measuring the absorbance of the solution at the wavelength of 420nm of a spectrophotometer; drawing a standard working curve by taking the chlorine content as a vertical coordinate and the absorbance as a horizontal coordinate, as shown in figure 1; meanwhile, feasibility analysis is carried out on the standard working curve, relevant data are calculated, as shown in figure 2, the correlation degree of the absorbance and the chlorine content is high, and the standard working curve can be proved to have accuracy and reliability;
step 2, sample pretreatment: weighing 0.2g (accurate to 0.0001g) of antimony-containing arsenic trioxide sample 3 in a 100mL beaker, accurately adding 5.00mL of 200g/L sodium hydroxide solution, slightly heating on a low-temperature electric heating plate until the sample is completely dissolved, accurately adding 6.00mL of 50% nitric acid solution to adjust the solution to acidity, continuously slightly heating until the solution is clear, taking down and cooling, transferring to a 50mL volumetric flask, adding 1.00mL of 17g/L silver nitrate solution into the volumetric flask, fixing the volume, uniformly mixing, and placing for 10 minutes in a dark place;
step 3, sample determination: transferring 6 groups of solutions to be detected, respectively placing the solutions in a cuvette of 1cm, taking a blank test along with a sample as a reference, measuring the absorbance of the solutions at the position of 420nm wavelength of a spectrophotometer, checking a standard working curve according to the absorbance value, and calculating the chlorine content of the 6 groups of solutions to be detected as follows: 0.0041%, 0.0038%, 0.0040%, 0.0038%, and 0.0040%, and the average values were measured to be 0.0039%, the standard deviation was 0.0013%, and the relative standard deviation was 3.39%.
The determination of the chlorine content in the three samples gives: the determination method can accurately determine the chlorine content in the antimony-containing arsenic trioxide, is simple to operate, high in safety and short in time consumption, can be used for simultaneously determining the chlorine content in large batches of antimony-containing arsenic trioxide, is high in accuracy, and can effectively solve the problems that the existing analysis method is not suitable for determining the chlorine content in large batches of antimony-containing arsenic trioxide products and the like.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (5)
1. A method for measuring the content of chlorine in antimony-containing arsenic trioxide is characterized by comprising the following steps: the method comprises the following steps:
step 1, drawing a standard working curve: taking 5 50mL volumetric flasks, respectively transferring 0.00mL, 1.00mL, 2.00mL, 3.00mL and 5.00mL of chloride ion standard solution into the volumetric flasks, sequentially adding 5.00mL of 200g/L sodium hydroxide solution and 6.00mL of 50% nitric acid solution (volume concentration), diluting with water to a scale, and uniformly mixing; keeping out of the sun for 10 minutes, transferring a part of the solution into a 1cm cuvette, and measuring the absorbance of the solution at the wavelength of 420nm of a spectrophotometer; drawing a standard working curve by taking the chlorine content as a vertical coordinate and the absorbance as a horizontal coordinate;
step 2, sample pretreatment: weighing 0.2g (accurate to 0.0001g) of antimony-containing arsenic trioxide sample in a 100mL beaker, accurately adding 5.00mL of super-pure sodium hydroxide solution, slightly heating on a low-temperature electric heating plate until the sample is completely dissolved, accurately adding 6.00mL of super-pure nitric acid solution to adjust the solution to acidity, continuously slightly heating until the solution is clear, taking down and cooling, transferring to a 50mL volumetric flask, adding 1.00mL of silver nitrate solution into the volumetric flask, fixing the volume, uniformly mixing, and placing for 10 minutes in a dark place;
step 3, sample determination: and (3) transferring the solution to be detected, placing the solution in a 1cm cuvette, taking a blank test along with a sample as a reference, measuring the absorbance of the solution at the wavelength of 420nm of a spectrophotometer, and checking a standard working curve according to the absorbance value to calculate the chlorine content.
2. The method for determining the chlorine content in antimony-containing arsenic trioxide as claimed in claim 1, wherein: the concentration of the sodium hydroxide solution of the guaranteed reagent is 200 g/L.
3. The method for determining the chlorine content in antimony-containing arsenic trioxide as claimed in claim 1, wherein: the volume concentration of the superior grade pure nitric acid solution is 50%.
4. The method for determining the chlorine content in antimony-containing arsenic trioxide as claimed in claim 1, wherein: the concentration of the silver nitrate solution is 17 g/L.
5. The method for determining the chlorine content in antimony-containing arsenic trioxide as claimed in claim 1, wherein: as in the antimony-containing arsenic trioxide sample2O3And the content of Sb is: as2O3≥85%,Sb≤5.0%。
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