Method for Determination of Silver Boron Tin in Geochemical Exploration Samples

A geochemical and sample technology, applied in the measurement of color/spectral properties, etc., can solve the problems that evaporation and excitation are easily affected by the sample matrix and operating conditions, the accuracy and precision are not good, and the influence of sample analysis can be achieved. Reliable quality, improved analytical precision and accuracy, and simple operation

CN103983583BActive Publication Date: 2016-03-30四川省地质矿产勘查开发局成都综合岩矿测试中心
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Patent Information

Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Publication Date
2016-03-30

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Abstract

The invention relates to a method for measuring silver, boron and tin in a geochemical exploration sample, for solving the problems of poor accuracy and precision while boron, tin and silver in soil are measured simultaneously in the original method; instruments, equipment and reagents are as follows: a grating spectrograph, an automatic photometer, an electrode, a spectrum sensitive plate, an agate mortar, a buffering agent and CdO, wherein the automatic photometer is connected to a computer; the electrode comprises an upper electrode and a lower electrode; the upper electrode is a conical graphite electrode; the lower electrode is 6 mm in outside diameter and is provided with a ring-shaped cup graphite electrode; the ring cup graphite electrode is 2 mm in ring height, 6 mm in ring outside diameter, 4 mm in hole inside diameter, 12.5 mm in hole depth, 13 mm in cup height, 5.2 mm in cup outside diameter, 4.0 mm in neck height and 3.5 mm in neck diameter; the mass percentage of the buffering agent is that mKI:mK2S207:mSiO2:mC:mZnO is 24:20:48:7:1; 0.015% of CdO is additionally added; a specimen is weighed; 0.0500 g of buffering agent is weighed and put into a crucible; after being stirred for one minute, the mixture is put into the electrode and subjected to pressing, spectrograph, development and photographic fixing; the automatic photometer translates a spectrum and analyzes internal standard line pairs as follows: Ag328.07 nm / Cd326.1 nm, B249.7 nm / Si249.4 nm, and Sn317.51 nm / Cd326.1 nm; a standard curve is automatically fit; the content of individual elements in a sample is automatically calculated.
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Description

Technical field:

[0001] The invention relates to the determination of trace elements in geochemical exploration samples by emission spectrometry. Background technique:

[0002] With the development of geochemical surveys such as geological surveys, agricultural geological surveys, and environmental surveys in my country, high requirements have been put forward for the analysis and testing of trace elements in rocks and soils, both in analysis methods and testing techniques in recent years. Developed by leaps and bounds. In the multi-element trace analysis of rock, soil and other samples, Ag, B, Sn are more difficult to analyze, and the detection limit required for analysis is getting lower and lower. The measurement of Ag, B, and Sn by emission spectrometry has a long history; however, due to the many influencing factors of the measurement, its accuracy and reproducibility have been relatively poor. Judging from the existing analytical methods, the emission spectroscopy methods ...

Examples

Embodiment 1

[0021] work process:

[0022] Instruments and reagents.

[0023] WP-1 type 1m grating spectrograph;

[0024] GBZ-Ⅱ Spectral Phase Plate Photometer;

[0025] The composition mass fraction of the buffer is: mKI: mK 2 S 2 O 7 : MSiO 2 :MC:mZnO=24:20:48:7:1, and add 0.015% CdO.

[0026] Electrode: upper electrode: 6mm diameter, 100mm high conical graphite electrode; bottom electrode with ring cup graphite electrode: ring height 2mm, ring outer diameter 6mm, hole inner diameter 4mm, hole depth 12.5mm, cup height 13mm, cup outer diameter 5.2mm, neck height 4.0mm, neck diameter 3.5mm,

[0027] Tianjin Type I Spectral Photosensitive Plate;

[0028] Agate mortar.

[0029] Operating procedures:

[0030] Weigh 0.0700g (accurate to 0.0001g) of the sample with a particle size of less than 74μm and 0.0500g buffer in a 5mL crucible, stir for 1 minute, put it into a special electrode, and compact it.

[0031] Spectrograph: AC arc, pre-ignition for 5 seconds (5A), increase to 15A, hold for 60S, and intercep...

experiment example 1

[0035] Comparison of the differences between the three methods:

[0036]

[0037]

[0038]

[0039] Table 3: Comparison of detection limit, precision and accuracy of three methods

[0040] BACKGROUND 1. Experimental method: Spectrograph: WP-1 type 1m grating spectrograph. 1200 grating lines / mm, reverse line dispersion rate 0.8nm / mm, center wavelength 280nm, three-lens illumination system. The slit width of the spectrograph is 12μm, and the middle aperture is 2μm in height of 1mm. Light source: WJD AC and DC arc generator. GBZ-Ⅱ Spectral Phase Plate Photometer.

[0041] Electrode specifications: spectral pure graphite electrode. The upper electrode is a flat-head cylindrical shape, ф4mm, length 10mm; the lower electrode is a thin-necked cup shape, ф3.8mm, hole depth 4mm, wall thickness 0.6mm, thin neck ф2.6mm, neck length 4mm. The composition of the buffer: mK 2 S 2 0 7 : MNaF: mAl 2 O 3 : M carbon powder=22:20:44:14 (containing 0.007% Ge02 as internal standard).

[0042] Weigh 0....