A sample pretreatment process for testing metal ion content in carbonyl sulfide

Abstract

The invention discloses a sample pretreatment process for testing the content of metal ions in carbonyl sulfide, comprising the following steps: S1, preparing an HF aqueous solution with a mass concentration of 1-3%; S2, adding Sc to the HF aqueous solution in step S1 2 o 3 , to get a mixed solution; Sc in the mixed solution 2 o 3 The mass concentration is 0.0001 ~ 0.0007%; S3, the carbonyl sulfide gas to be measured is passed into the mixed solution in step S2; at the same time, a filter membrane is set above the mixed solution to filter the gas formed when the carbonyl sulfide to be measured is passed; S4. After the introduction of carbonyl sulfide to be tested is completed, continue to wait for at least 1 minute, then put the filter membrane into the mixed solution, stir and mix well; S5, use the mixed solution obtained in step S4 with the second filter membrane After filtering, the sample after pretreatment can be obtained. The method has high metal ion data precision and high reliability.

Description

A kind of sample pretreatment process for testing metal ion content in carbonyl sulfide technical field The present invention relates to liquefied gas metal content detection technical field, be specially a kind of test carbonyl sulfide containing metal ion content amount of sample preparation. Background technique Inductively coupled plasma mass spectrometry (ICP-MS, inductively coupled plasma mass Spectrometry) as a common metal ion analysis method has a wide range of applications in the field of electronic chemicals. However, the sight The previous sampling systems were all carried out by liquid sampling. The target product was volatilized and dissolved in HF, and then injected by the sampling tube. Direct injection. However, the ICP-MS system with direct gas injection, because there is no gaseous metal ion standard gas, is directly injected by the gas. Gaseous injection is not practical in ICP‑MS systems. For the special gas industry, the vast majority of ma...

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Problems solved by technology

[0004] In the prior art, the use of inductively coupled plasma mass spectrometry to test the content of metal ions in carbonyl sulfide has not yet formed a standard. The main difficulty is that the solubility of carbonyl sulfide is poor, and the metal impurities contained in it will "run away" due to unknown reasons (It may be due to the formation of metal complexes and volatilization, there is no conclusion at present), resulting in the use of existing standard methods to detect it, often there are great deviations: common metals Cu, Fe, Mo, Ni, Cr For example, its RSD (relative standard deviation) is 200%, 100%, 70%, 150%, and 80% respectively. This test result is obviously unacceptable

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