Determination of paraldehyde in aqueous solutions of acetaldehyde

Chem. , 1960, 32 (13), pp 1899–1899. DOI: 10.1021/ac50153a063. Publication Date: December 1960. ACS Legacy Archive. Cite this:Anal. Chem. 32, 13, 18...
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Determination of N-Ethyl-mToluidine in N-Ethyl-K(2,3dihydroxypropyl)-m-toluidine

Determination of Paraldehyde in Aqueous Solutions of Acetaldehyde

IC. B. WHETSEL, W. E. ROBERSON, and M. W. KRELL Tennessee Eastrnan Co., Divlslon of Eastrnan Kodak Co., Klngsport, Tenn.

HARVEY POBINER, Esso Research and Engineering Co.. Analytical Reseatsh Divislon, linden, N. J.

Component No.1

1

1

1 Formula

Name

1 1 rz I 2: I Accu-

N-Ethyl-m- CSHI~N toluidine1

Rage

I 1

CS- 147 Concn. mglml Length cm

Slit

hn)

1::4gl;I

1

I

1 . 4 9 2 ~ 0.36 1 . 2 ~

fO.l

&lo

50

Calculation:

Inverse m a t r i x Graphical&

Range Formula

Material Purity:

Comments: See ANAL CHEM. 29, 1006 (1957) for other details o f this type o f analysis. a Relative absorbances are given as the slope of the Beer's law concentration curves used expressed in terms of absorbance per loo'% o f constituent. The calibration line passes through -0.035 absorbance ot 0% N-ethyl-m-toluidine.

Determination of Hydroxybenzoic Acids in Potassium Bromide Disks

cs-149

-

Name

Formula

1

o-Hydroxybenzoic acid

&He03

2

I 1 I

in-Hydroxy- C7HsOa benzoic

acid

3 p-Hydroxybenzoic

acid

I 1 I

Range

Accuracy

%

%

AA or Av -. _ _ _

Concn. length

0-100

f 2

14.33 0.436

1 mg./0.4 g

-I

(mm)

0 . 0 8 0 ~ KBr in 12.7m m diam. disk

--

.~

0-100

14.83 0.592 1 mg./0.4 g 0 . 1 1 7 ~KBr in 12.7-

f 2

mm diam. disk C.iH60~ 0-1001 f 2

mm

9.06~ 66.4

99

+ 70

Relative absorbance is given as the slope of the Beer's law concentration curve used expressed in terms of absorbance per 100% o f constituent.

Instrument: Perkin-Elmer Model 21, NaCl prism Sample Phase: Dispersion in potassium bromide disk Cell Windows: None Absorbance Measurement:

Slit No.

Au

Comments: Two 25-1111. CClr extractions will quantitatively (98% mtn.) remove the paraldehyde, in the specifled range, from a 10-1111. sample. The CCln solvent, saturated with water in the extraction, does not etch the NaCl cell windows. The 9.04-p band is due to the cyclic ether structure"of paraldehyde.

Calculation: or v 0.1. Pts.

ml.

Length

Base I i n e l L Point __

1

Reference compounds 99%

X

mm

AX or

Instrument: Perkin Elmer Model 21, NaCl prism Sample Phase: Carbon tetrachloride extract o f aqueous sample

Component/X

1.492~ 1.98

D. E. NICHOLSON Humble Oil 8, Reflning Co., Baytown, lex.

Concn. 9/50

Slit

Calculation: Inverse matrix _ _ Successive approx. _ _ Graphical X Relative Absorbances"-Analytical Matrix:

Successive approx--

1

70

or X 0.1. Pts.

-I

Relative Absorbancesa-Analytical Matrix:

Material Purify:

7'

-l-.----I-----I-I-

Cell Windows: NaCl Absorbance Measurement:

Point-

Componentjh

X

Accuracy

10

Instrument: Cary Model 14, fused silica prism in series with a 600 linelmm. echelette grating Sample Phase: Solution in carbon tetrachloride Cell Windows: Corex Absorbance Measurements:. Base I i n e X

Component

CS- 148

Base line-

Inverse m a t r i x G r a p h i c a l

P o i n t X Successive appro-

Relative Absorbances-Analytical Matrix:

14.33~ 0.550 0.200 0.147

ComponentlX

1 2

3 Material Purify:

14.83~ 0.173 0.710 0.112

11.69~ 0.210 0.182 1.060

98%.

Comments: Infrared Intensities were derived from potassium bromide disks prepared using a 10-minute grinding time. This method allows the ready detection of components, if any, not provided for in the analytical matrix.

11.69 0.191 1 mg.10.4 g 0.038~KBr in 12.7mm diam. disk

The data represent standard publication and submission is

present series of infrared data. Future plans for continuance of

~ E E M E I T B Y . The Coblentz Society is acting only as an aid to the journal. With this issue ANALYTICAL CHEMISTRY is completing the

The chairman of the present review committeeisD. E. Nicholson, Research and Development Division, Humble Oil and Refining Go., P. 0. Box 3950, Baytown, Tex.

o en to anyone in accordance with regulations of ANALYTICAL the series mill be announced by the Coblentz Society.

VOL. 32, NO. 13, DECEMBER 1960

o

1899