Succinic Acid - ACS Reagent Chemicals (ACS Publications)

Feb 28, 2017 - This monograph for Succinic Acid provides, in addition to common physical constants, a general description including typical appearance...
0 downloads 0 Views 98KB Size
Monograph pubs.acs.org/doi/book/10.1021/acsreagents

Succinic Acid (Butanedioic Acid) Part 4, Monographs for Reagent Chemicals: General Descriptions, Specifications, and Tests eISBN: 9780841230460 Tom Tyner Chair, ACS Committee on Analytical Reagents James Francis Secretary, ACS Committee on Analytical Reagents

ABSTRACT This monograph for Succinic Acid provides, in addition to common physical constants, a general description including typical appearance, applications, change in state (approximate), aqueous solubility, and pKa. The monograph also details the following specifications and corresponding tests for verifying that a substance meets ACS Reagent Grade specifications including: Assay, Melting Point, Insoluble Matter, Residue after Ignition, Chloride, Phosphate, Sulfate, Nitrogen Compounds, Heavy Metals, and Iron.

HOOCCH2CH2COOH

Formula Wt 118.09

CAS No. 110-15-6

GENERAL DESCRIPTION Typical appearance . . . . . . . . Applications . . . . . . . . . . . . . Change in state (approximate) . Aqueous solubility . . . . . . . . . pKa . . . . . . . . . . . . . . . . . .

. . . . .

. . . . .

. . . . .

. . . . .

. . . . .

. . . . .

. . . . .

. . . . .

. . . . .

. . . . .

. . . . .

colorless solid internal standard in chromatography melting point, 185–191 °C 6.8 g in 100 mL at 20 °C; 121 g in 100 mL at 100 °C 4.2

SPECIFICATIONS Assay . . . . . . . . . . . . . . . . . . . . . . . . . . . . ≥99.0% HOOCCH2CH2COOH Melting point . . . . . . . . . . . . . . . . . . . . . . . 185.0–191.0 °C Maximum Allowable Insoluble matter . . . . . . . . . . . . . . . . . . . . . 0.01% Residue after ignition. . . . . . . . . . . . . . . . . . 0.02% Chloride (Cl) . . . . . . . . . . . . . . . . . . . . . . . 0.001%

© 2017 American Chemical Society

A

DOI:10.1021/acsreagents.4382 ACS Reagent Chemicals, Part 4

ACS Reagent Chemicals

Monograph

pubs.acs.org/doi/book/10.1021/acsreagents

Phosphate (PO4) . . . . . . . Sulfate (SO4) . . . . . . . . . Nitrogen compounds (as N) Heavy metals (as Pb) . . . . Iron (Fe) . . . . . . . . . . . .

. . . . .

. . . . .

. . . . .

. . . . .

. . . . .

. . . . .

. . . . .

. . . . .

. . . . .

. . . . .

. . . . .

. . . . .

. . . . .

. . . . .

0.001% 0.003% 0.001% 5 ppm 5 ppm

TESTS Assay (By acid–base titrimetry). Weigh accurately about 0.3 g, dissolve in 25 mL of water in a conical flask, add 0.15 mL of phenolphthalein indicator solution, and titrate with 0.1 N sodium hydroxide. One milliliter of 0.1 N sodium hydroxide corresponds to 0.005905 g of HOOCCH2CH2COOH.

Melting Point [Part 2: Measurement of Physical Properties; Melting Point].

Insoluble Matter [Part 2: Gravimetric Methods; Insoluble Matter]. Use 10.0 g dissolved in 150 mL of water.

Residue after Ignition [Part 2: Gravimetric Methods; Residue after Ignition]. Ignite 10.0 g, omitting the use of sulfuric acid.

Chloride [Part 2: Colorimetry and Turbidimetry; Chloride]. Use 1.0 g.

Phosphate [Part 2: Colorimetry and Turbidimetry; Phosphate; Procedure for Phosphate, Method 1 (Direct Molybdenum Blue)]. Dissolve 2.0 g of sample in 40 mL of water. Add 5 mL of 5 N sulfuric acid, and continue as directed, using equal amounts of reagents and volume for the control solution.

Sulfate Dissolve 1.0 g of sample in 20 mL of water, and filter through small, fine-porosity filter paper. Add two 2 mL portions of water through the filter, and collect the sample. For the control, use 0.03 mg of sulfate ion (SO4) in the same volume of water. To the sample and control solutions, add 5 mL of ethyl alcohol, 1 mL of dilute hydrochloric acid (1:19), and 1 mL of 12% barium chloride reagent solution. After 30 min, the turbidity of the sample should not exceed that of the control.

© 2017 American Chemical Society

B

DOI:10.1021/acsreagents.4382 ACS Reagent Chemicals, Part 4

ACS Reagent Chemicals

Monograph

pubs.acs.org/doi/book/10.1021/acsreagents

Nitrogen Compounds [Part 2: Colorimetry and Turbidimetry; Nitrogen Compounds: Test for Ammonia, Amines, and Nitrogen Compounds Reduced by Aluminum]. Use 1.0 g. For the standard, use 0.01 mg of nitrogen ion (N).

Heavy Metals To 30 mL of ammonium hydroxide (1:9), add 25 mL of water. While stirring, add 6.0 g of sample, dissolve, and dilute to 60 mL with water. For the sample, take 50 mL of sample solution. For the control, take 10 mL of sample solution, add 0.02 mg of lead ion (Pb), and dilute to 50 mL. Add 10 mL of freshly prepared hydrogen sulfide water to each, and mix. Any brown color produced in the test solution within 5 min should not be darker than that produced in the control.

Iron [Part 2: Colorimetry and Turbidimetry; Iron; Procedure for Iron, Method 1 (Ammonium Thiocyanate)]. Use 2.0 g.

© 2017 American Chemical Society

C

DOI:10.1021/acsreagents.4382 ACS Reagent Chemicals, Part 4