Method for analyzing organic acid salts in carbonate rocks

Method for analyzing organic acid salts in carbonate rocks

  • CN 104,730,022 A
  • Filed: 02/06/2015
  • Published: 06/24/2015
  • Est. Priority Date: 02/06/2015
  • Status: Active Application
First Claim
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1. , to the method that acylate in carbonatite is analyzed, it is characterized in that:

  • carry out according to following steps;

    Step 1;

    first carbonate samples be crushed to and be less than 0.147mm, after soxhlet type, is divided into Soluble Organic Matter and rock slag;

    Step 2;

    free organic acid Soluble Organic Matter being obtained after post stratography sample, carries out GC/MS analysis to free organic acid;

    Step 3;

    rock slag is sealed in glass tube, constant temperature 12h after muffle furnace is heated to 280 DEG C, the kerogen network in sample is broken, and the Organic Acid Generated By Kerogen in network structure is vaporized;

    Step 4;

    by the glass tube of sealing at the NaOH of the 10% and CH of 10% 3open in the mixed aqueous solution of OH, by the Organic Acid Generated By Kerogen of rock slag and gasification at 70 DEG C of saponification 3h, form saponification liquor, generate Organic Acid Generated By Kerogen sodium;

    Step 5;

    add watery hydrochloric acid in saponification liquor, generates sodium chloride and Organic Acid Generated By Kerogen, by extracted with diethyl ether, isolates Organic Acid Generated By Kerogen, carry out GC/MS analysis to Organic Acid Generated By Kerogen;

    Step 6;

    the filter residue after first time saponification, first does infrared spectrum qualification, sentences before knowing acidifying whether there is organic acid in sample;

    Step 7;

    if infrared spectrum testing result to confirm before acidifying in sample without organic acid, then with watery hydrochloric acid by sample acidifying before acidifying, filter, filter residue is carried out infrared spectrum qualification again, whether organic acid is there is in sample after qualification acidifying, if there is organic acid, illustrate that organic acid is not here free organic acid and Organic Acid Generated By Kerogen, but the organic acid that acylate in sample and hydrochloric acid generation displacement reaction generate;

    Step 8;

    by the NaOH of the 10% and CH of 10% of sample after acidifying 3oH aqueous solution carries out saponification 3h at 70 DEG C, acylate is transformed acid and becomes sodium salt and enter aqueous phase;

    Step 9;

    add hydrochloric acid in aqueous phase, uses extracted with diethyl ether organic acid, and isolate acylate and transform acid, the acylate namely in sample is separated with organic acid form, transforms acid carry out GC/MS analysis to acylate.

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