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Method for measuring lead, arsenic, nickel and cobalt in ferric oxide powder

A technology of iron oxide powder and constant volume, which is applied in the field of arsenic, nickel and cobalt determination of lead in iron oxide powder, can solve the problems of unprovided, labor-intensive, cumbersome operation process, etc., and achieve accurate and concise operation. Fast analysis speed and good separation effect

Inactive Publication Date: 2011-02-16
COMPREHENSIVE TECH SERVICE CENT OF CHANGSHU ENTRY EXIT INSPECTION & QUARANTINE BUREAU
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The former method (precipitation method) in the above-mentioned methods is loaded down with trivial details in operation process, and labor intensity is big, and the used organic extraction agent pollutes the environment; And in the latter method (ion exchange method) in the above-mentioned method, though have high concentration factor, labor-intensive The advantages of low strength and safety, but the anion exchange resin has a tendency to adsorb As and Co and cannot be effectively separated from the matrix iron.
[0005] Therefore, the industry expects to have a method that can not only overcome the shortcomings of the aforementioned precipitation method and ion exchange method, but also have good separation effect, high sensitivity, fast analysis speed, accurate measurement, and simple and uncomplicated operation. The determination method of toxic and harmful chemical elements, but no corresponding technical inspiration is given in the domestic and foreign patent documents that have been published at present and in the non-patent documents that are not limited to the above examples. For this reason, the applicant has carried out beneficial Exploration and experimentation, the technical solutions to be introduced below are generated under this background

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  • Method for measuring lead, arsenic, nickel and cobalt in ferric oxide powder
  • Method for measuring lead, arsenic, nickel and cobalt in ferric oxide powder
  • Method for measuring lead, arsenic, nickel and cobalt in ferric oxide powder

Examples

Experimental program
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Effect test

Embodiment 1

[0023] A) Sampling and dissolving, weigh 0.50g of iron oxide powder sample, and place the weighed 0.50g iron oxide powder sample in the first container served by a beaker with a volume of 100mL, and add concentration 25mL of 8mol / L hydrochloric acid, and heated to boiling, then 1mL of hydrogen peroxide was added dropwise to completely dissolve the iron oxide powder, and after cooling, the volume of the dissolved sample was controlled to be 25mL (due to the addition of 25mL of hydrochloric acid and 1mL of hydrogen peroxide when heated loss);

[0024] B) Through the column, the dissolved sample obtained from step A) is introduced into the extraction resin column with a particle size of 60-75 mesh extraction resin under the condition that the flow rate is controlled at 0.5mL / min, and the outflow from the extraction resin column is discarded. 5mL of the effluent of the first part of the first part, and the first part of the effluent was introduced into the container for discarding...

Embodiment 2

[0030] A) Sampling and sample dissolution, weigh 1.00g of iron oxide powder sample, and place the weighed 1.00g iron oxide powder sample in the first container served by a beaker with a volume of 100mL, and add concentration 60mL of 7mol / L hydrochloric acid, and heated to boiling, then dropwise added 3mL of hydrogen peroxide to completely dissolve the iron oxide powder, after cooling, the volume of the dissolved sample was controlled to be 60mL (due to the addition of 60mL of hydrochloric acid and 3mL of hydrogen peroxide when heated loss);

[0031] B) Through the column, the dissolved sample obtained from step A) is introduced into the extraction resin column with a particle size of 60-75 mesh extraction resin under the condition that the flow rate is controlled at 1.0mL / min, and the outflow from the extraction resin column is discarded. 21mL of the effluent of the first part of the first part, and the first part of the effluent was introduced into the container for discardin...

Embodiment 3

[0037] A) Sampling and dissolving, weigh 0.50g of iron oxide powder sample, and place the weighed 0.50g iron oxide powder sample in the first container served by a beaker with a volume of 100mL, and add concentration 40mL of 6mol / L hydrochloric acid, and heated to boiling, then dropwise added 1mL of hydrogen peroxide to completely dissolve the iron oxide powder, after cooling, control the volume of the dissolved sample to 40mL (due to the addition of 40mL of hydrochloric acid and 1mL of hydrogen peroxide when heated loss);

[0038] B) Through the column, the dissolved sample obtained from step A) is introduced into the extraction resin column with a particle size of 60-75 mesh extraction resin under the condition that the flow rate is controlled at 0.7mL / min, and the outflow from the extraction resin column is discarded. 10mL of the first part of the effluent, and the first part of the effluent was introduced into the container for disposal, and the remaining effluent was coll...

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Abstract

The invention relates to a method for measuring lead, arsenic, nickel and cobalt in ferric oxide powder, comprising the following steps of: sampling and dissolving the sample: weighing the ferric oxide powder sample, placing the sample in a first container, adding hydrochloric acid to the first container, heating until boiling, dropping a strong oxidizer until the ferric oxide powder is completely dissolved, cooling to obtain a dissolving sample; column chromatography: introducing the dissolving sample in a gathers drench resin column under the state of controlling the flow speed, removing the front part of effluent liquid flowing from the gathers drench resin column, controlling the amount of the front part of effluent liquid, collecting the remained effluent liquid in a second container, washing the lead, the arsenic, the nickel and the cobalt failing to be adsorbed by the gathers drench resin with hydrochloric acid, collecting in the second container, and evaporating and drying to obtain a constant-volume substance to be measured; volume fixing: fixing the volume of the substance with nitric acid, controlling the proportion of the nitric acid to the ferric oxide powder sample to obtain a constant-volume solution; and measuring: measuring the content of the lead, the arsenic, the nickel and the cobalt in the constant-volume solution with an inductive coupling plasma emission spectrometer. The invention has the advantages of good separation effect, rapid and accurate measurement and analysis, and simple operation.

Description

technical field [0001] The invention belongs to the technical field of iron oxide powder analysis, in particular to a method for determining lead, arsenic, nickel and cobalt in iron oxide powder. Background technique [0002] my country is a traditional big producer of iron oxide, that is, iron oxide powder. High-purity iron oxide is widely used in food, cosmetics, medicine coloring, cooking utensils and toys. Since lead (Pb), arsenic (As), nickel (Ni) and cobalt (Co) present in high-purity iron oxide are highly toxic to the human body, it has been confirmed by the International Health Organization that As, Pb and Ni are carcinogenic, Chronic Co poisoning in the body can cause abnormal heart function. Therefore, the determination of toxic and harmful elements Pb, As, Ni and Co in high-purity iron oxide is a very meaningful research work. [0003] Iron is a multispectral element, and the analysis of trace metals in an iron matrix is ​​generally recognized as a difficult prob...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N1/28G01N21/73
Inventor 许玉宇王国新顾伟王慧周锦帆朱玉燕王卫忠吴骋卢书媛俞璐
Owner COMPREHENSIVE TECH SERVICE CENT OF CHANGSHU ENTRY EXIT INSPECTION & QUARANTINE BUREAU
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