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Matrix modifier for determining heavy metals absorbed by graphite furnace atoms and preparing method

A graphite furnace atomic and matrix modifier technology, applied in the measurement of color/spectral properties, etc., can solve the problems of unstable volatile analytes, poor reproducibility, increased analysis time, etc., to eliminate interference, reduce or interfere with , the effect of uniform particle distribution

Inactive Publication Date: 2010-06-30
CHENGDU XINDA MEASUREMENT & CONTROL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The earliest proposed compound palladium matrix modifier is palladium chloride, metal palladium and palladium oxides are generally considered to be the active form of palladium matrix modifier, a class of matrix modifiers are palladium compounds such as palladium chloride and palladium nitrate, This type of modifier basically requires high heat to convert it into active palladium. Such a pretreatment method will increase the analysis time by 30-40%, and cannot stabilize volatile analytes; the other type is a palladium complex. and reducing agents, the main disadvantage of this type of improver may be its poor reproducibility

Method used

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  • Matrix modifier for determining heavy metals absorbed by graphite furnace atoms and preparing method
  • Matrix modifier for determining heavy metals absorbed by graphite furnace atoms and preparing method
  • Matrix modifier for determining heavy metals absorbed by graphite furnace atoms and preparing method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] 1. Preparation of colloidal palladium

[0031] Weigh 0.024g-0.036g (0.4mg / mL-0.6mg / mL) palladium chloride in a round bottom flask, convert it to H with concentrated hydrochloric acid 2 PdCl 4 ·nH 2 O, add 0.030g (0.5mg / mL) polyvinylpyrrolidone (PVP) again, then slowly add 60mL of a mixed solution of 1:1 methanol and water, stir and mix constantly during the addition process, and place the solution in a water bath to heat After reflux for 90 minutes, take it out, and the obtained brown colloidal solution is colloidal palladium.

[0032] 2. Quality control of colloidal palladium

[0033] Drop a drop of colloidal palladium solution sample on the copper grid coated with carbon film, and let it dry naturally. Observed on a transmission electron microscope. The size and particle size distribution of metal particles are obtained by statistical measurement of no less than 200 particles on the enlarged electron microscope photos.

[0034] The heavy metal content of the pre...

Embodiment 2

[0051] Determination of arsenic in food

[0052] Arsenic is easy to combine with sulfhydryl groups, thereby causing changes in the biological activity and function of enzymes, coenzymes and proteins containing sulfhydryl groups. The determination of arsenic in food is a routine project. The food samples were digested by acid and then fixed to volume, and then measured by a graphite furnace atomic absorption spectrophotometer. Inject 20 μL of sample, and the volume of colloidal palladium matrix modifier is 5 μL. The program is shown in Table 2. signal see Figure 7 , Figure 8 .

[0053] Colloidal palladium matrix modifier of arsenic in table 2 - graphite furnace atomic absorption determination procedure

[0054]

[0055] see Figure 7 , Figure 8 As shown, they are respectively food sample addition and food sample background signals under the colloidal palladium modifier at an ashing temperature of 1200 ° C. It can be seen from the figure that after adding the matri...

Embodiment 3

[0057] urine thallium determination

[0058] Thallium and its compounds are highly toxic and accumulative. It mainly damages the central nervous system, peripheral nerves, liver and kidney, and can also cause hair loss. Urinary thallium is a good biological monitoring indicator. Graphite furnace atomic absorption spectrometer measurement, urine samples can be directly analyzed. Inject 15 μL of sample and 5 μL of colloidal palladium matrix modifier. See Table 3 for the program. signal see Figure 9 , Figure 10 .

[0059] Table 3 colloidal palladium matrix modifier for thallium - graphite furnace atomic absorption determination procedure

[0060]

[0061] Figure 9 , 10 The colloidal palladium improver with an ashing temperature of 1100°C participates in the thallium standard and poisoned urine sample signals respectively. It can be seen from the figure that after adding the matrix improver of the present invention to the biological material sample solution, the ash...

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Abstract

The invention discloses a matrix modifier for determining heavy metals absorbed by graphite furnace atoms, and a preparing method. The matrix modifier is colloid palladium, and the preparing method of the matrix modifier comprises the following steps of: weighing 0.024g-0.036g of palladium chloride, and placing into a reacting container; converting into H2PdC14.nH2O by using concentrated hydrochloric acid; adding 0.030g of polyvinylpyrrolidone; then, slowly adding 60mL of mixing solution of methanol and water, continuously stirring and uniformly mixing in the adding process, placing the solution into a water bath tank for refluxing by heating for 90 minutes, and then taking out a brown colloid solution which is the target palladium. The novel matrix modifier can achieve high podzolizing temperature, the interference matrix can be effectively removed in the podzolizing stage, and the purpose for reducing or eliminating the interference is achieved. The colloid palladium prepared by the invention has uniform particle distribution, and no obvious aggregation phenomenon.

Description

technical field [0001] The invention relates to a matrix modifier for the determination of heavy metals by graphite furnace atomic absorption and a preparation method. Background technique [0002] Heavy metals generally refer to metals with an atomic weight greater than 55, mostly transition elements. Such as copper, lead, zinc, iron, cobalt, nickel, manganese, cadmium, mercury, tungsten, molybdenum, gold, silver, etc. Although heavy metals such as manganese, copper, and zinc are trace elements needed for life activities, most heavy metals such as mercury, lead, and cadmium are not necessary for life activities, and all heavy metals are harmful to the human body if they exceed a certain concentration. In addition, although arsenic is not a heavy metal, it is usually included in the category of heavy metals for research and discussion because its source and hazards are similar to those of heavy metals. With the progress of toxicology, the neurotoxicity and chronic toxicity...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N21/31
Inventor 谭红龙
Owner CHENGDU XINDA MEASUREMENT & CONTROL TECH
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