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Determination of trace arsenic in high-copper-content sample with atomic fluorescence spectrometry

An atomic fluorescence, trace arsenic technology, applied in the field of analysis and detection, can solve the problems of low measurement results, low data reliability, and difficult to clean, and achieve the effect of simplifying experiments, simple spectral lines, and fast and accurate detection.

Inactive Publication Date: 2016-05-04
JILIN PONY TESTING TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] 2. It is found in the experiment that when the mass fraction of copper ions in the solution is greater than 0.005%, when the arsenic content in the solution is measured by means of an atomic fluorescence spectrometer, the solution reacts with potassium borohydride to generate black particles that are adsorbed on the tube wall, which is difficult to clean
At the same time, the measurement result is seriously low, and the reliability of the data is not high.

Method used

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  • Determination of trace arsenic in high-copper-content sample with atomic fluorescence spectrometry
  • Determination of trace arsenic in high-copper-content sample with atomic fluorescence spectrometry
  • Determination of trace arsenic in high-copper-content sample with atomic fluorescence spectrometry

Examples

Experimental program
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Effect test

Embodiment 1

[0047]Taking the food additive copper sulfate as an example, the samples are processed with reference to the "National Food Safety Standard Food Additive Copper Sulfate", marked as T1 and T2; T7 and T8; while comparing samples only treated with potassium iodide, marked as T3 and T4, and only treated with potassium thiocyanate, marked as T5 and T6. After the treatment, the sample solution was reacted with thiourea-ascorbic acid mixed solution and potassium hydroxide-potassium borohydride solution to observe the reaction phenomenon. The specific experimental process is as follows:

[0048] Weigh 5.0 g of copper sulfate pentahydrate, a total of 8 parts, respectively marked as T-1, T-2, T-3, T-4, T-5, T-6, T-7 and T-8.

[0049] Add about 20mL of water to dissolve each of T-1 and T-2, transfer to a 100mL volumetric flask, dilute to the mark with water, shake well and set aside.

[0050] Add about 10mL of water to dissolve each of T-3 and T-4, add 20mL of potassium iodide solution ...

Embodiment 2

[0058] The trace arsenic in copper sulfate pentahydrate provided by a reagent factory was tested, and at the same time, standard addition recovery experiments and precision experiments were performed.

[0059] Weigh 5.0g of the sample, a total of 20 parts, marked as S-1, S-2, A-1, A-2, A-3, A-4, A-5, A-6, B-1, B-2, B-3, B-4, B-5, B-6, C-1, C-2, C-3, C-4, C-5 and C-6. After adding water to dissolve, add 20mL of potassium iodide solution with a mass fraction of 100%, stir well with a glass rod, add 10mL of potassium thiocyanate solution with a mass fraction of 100%, continue to stir evenly with a glass rod, and then filter to a capacity of 100mL In the bottle, adjust the volume to the mark with water, and shake well (note: here the reaction mass ratio of the initial copper ion to the added iodide ion and thiocyanate ion is 1:4:2).

[0060] Take 10mL of the above solution into a 50mL volumetric flask, add 2.5mL hydrochloric acid, 2.5mL thiourea-ascorbic acid mixed solution (the ...

Embodiment 3

[0067] Determination of trace arsenic in food additive copper sulfate. Weigh 5.0g of food additive copper sulfate into a 150mL beaker, add an appropriate amount of water to dissolve, add 20mL of potassium iodide solution with a mass fraction of 100%, stir well with a glass rod, then add 10mL of a 100% potassium thiocyanate solution Continue to stir evenly with a glass rod, then filter into a 100mL volumetric flask (note: the mass ratio of the initial copper ion to the added iodide ion and thiocyanate ion here is 1:4:2), add 5mL hydrochloric acid, 5mL sulfur Urea-ascorbic acid mixed solution (the mass fraction of thiourea is 10%, the mass fraction of ascorbic acid is 10%), the volume is made up to the mark with water, shake well and then stand still for 30min, to be measured. Do the same blank test and standard recovery test. Prepare arsenic standard solution working curves with concentrations of 1 μg / L, 2 μg / L, 5 μg / L, 8 μg / L and 10 μg / L respectively. The fluorescence intens...

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Abstract

The invention discloses a determination method of trace arsenic in a high-copper-content sample with an atomic fluorescence spectrometry and belongs to the field of analysis detection. The determination method is characterized by comprising the following steps: reducing copper in a digested sample solution into cuprous iodide by potassium iodide and precipitating copper in a form of cuprous iodide; adding thiocyanate and precipitating free cuprous ions in the solution in a form of cuprous thiocyanate with relatively high stability and relatively low solubility; after filtering and making the volume constant, determining the arsenic content in the sample solution; and calculating the content of the arsenic in the sample. With the adoption of the method, copper in the sample solution and thiourea and potassium borohydride, which are needed by an experiment, are effectively prevented from reacting to generate sediment. The method is simple and reliable and has high accuracy and good repeatability.

Description

technical field [0001] The invention belongs to the field of analysis and detection, and relates to a method for measuring trace arsenic by atomic fluorescence spectrometry and a method for eliminating copper interference in a sample. Background technique [0002] Arsenic is a non-metallic element with biological toxicity and accumulation. Long-term intake of food contaminated by arsenic will be very harmful to health. Therefore, arsenic is listed as a key harmful element in food hygiene testing. [0003] At present, the limit requirement for arsenic in GB29210-2012 "National Food Safety Standard Food Additive Copper Sulfate" is ≤0.0003%, the limit requirement for arsenic in HG2932-1999 "Feed Grade Copper Sulfate" is ≤0.0004%, GB13078-2001 " Feed Hygienic Standards requires that the limit of arsenic in copper sulfate is ≤0.0005%. The determination methods for arsenic content stipulated in the standard include arsenic spot method, silver salt method, and hydride atomic fluor...

Claims

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Application Information

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IPC IPC(8): G01N21/64
CPCG01N21/6404
Inventor 宋薇李梅伍伟超韦英
Owner JILIN PONY TESTING TECH CO LTD
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