2-propanol and 2-butanol production, distn. residues

Boiling point

Link to relevant study record(s)

Reference

Endpoint:

boiling point

Type of information:

experimental study

Adequacy of study:

key study

Study period:

15 June 2010 - 25 Sept 2010

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

other: Fully documented study run under GLP and according to international guidelines

Qualifier:

according to guideline

Guideline:

EU Method A.2 (Boiling Temperature)

Deviations:

yes

Remarks:

deviations considered as uncritical; described in field "principles of method if other than guideline"

Qualifier:

according to guideline

Guideline:

other: DIN 53171, “Lösemittel für Beschichtungsstoffe - Bestimmung des Siedeverhaltens (Siedebereich und Siedeverlauf)”, Entwurf, dated Apr. 2008

Deviations:

yes

Remarks:

deviations considered as uncritical; described in field "principles of method if other than guideline"

Principles of method if other than guideline:

- Instead of a measuring cylinder, a beaker was used, which was standing on the scales. This was considered as uncritical, as the amount of the distilled test item could be calculated exactly using the mass of the distilled test item and the known density.
- As heating device, a heating mantle was used instead of a gas burner; because the latter caused superheating (heating rate is too high). This was considered as uncritical, as valid results could only be obtained in this manner.
- The heating rate was less than approximately 5 mL/min. This was considered as uncritical because constant boiling could be observed. A higher heating rate could have caused superheating.
- For the performance no protection cover was used. This considered as uncritical because the whole experiments took place under the fume hood.

GLP compliance:

yes (incl. QA statement)

Type of method:

distillation method

Key result

Boiling pt.:

>= 70 - <= 122 °C

Atm. press.:

101.325 kPa

Decomposition:

no

Remarks on result:

other: average of the 2 experiments, corrected to standard pressure

Boiling pt.:

>= 70 - <= 121 °C

Atm. press.:

98 467 Pa

Decomposition:

no

Remarks on result:

other: Experiment 1

Boiling pt.:

>= 71 - <= 121 °C

Atm. press.:

100 441 Pa

Decomposition:

no

Remarks on result:

other: Experiment 2

Measured data for first experiment:

Time	Temperature in °C	Mass in g
11:12:00	70.0	0.1
11:13:00	74.0	2.6
11:13:30	74.0	4.0
11:14:00	74.0	5.6
11:14:30	75.0	7.0
11:15:00	75.0	8.4
11:15:30	75.0	9.5
11:16:00	75.0	10.6
11:16:30	75.0	11.6
11:17:00	75.0	12.5
11:17:30	75.0	13.3
11:18:00	75.0	14.1
11:18:30	75.5	14.8
11:19:00	76.0	15.5
11:19:30	76.0	16.2
11:20:00	76.0	16.7
11:20:30	76.0	17.4
11:21:00	76.0	18.1
11:21:30	76.0	18.6
11:22:00	76.5	19.3
11:22:30	77.0	19.9
11:23:00	77.0	20.5
11:23:30	77.0	21.0
11:24:00	77.0	21.6
11:24:30	77.0	22.2
11:25:00	77.0	22.7
11:25:30	77.0	23.1
11:26:00	77.5	23.8
11:26:30	77.5	24.3
11:27:00	78.0	24.7
11:27:30	78.0	25.3
11:28:00	78.0	25.7
11:28:30	78.0	26.2
11:29:00	78.0	26.8

11:29:30	78.0	27.2
11:30:00	78.0	27.7
11:30:30	78.5	28.2
11:31:00	78.5	28.6
11:31:30	79.0	29.0
11:32:00	79.0	29.4
11:32:30	79.0	29.8
11:33:00	79.0	30.3
11:33:30	79.0	30.6
11:34:00	79.0	31.0
11:34:30	79.0	31.4
11:35:00	79.0	31.9
11:35:30	79.0	32.1
11:36:00	80.0	32.6
11:36:30	80.0	33.0
11:37:00	80.0	33.4
11:37:30	80.0	33.8
11:38:00	80.0	34.1
11:38:30	80.0	34.5
11:39:00	80.0	34.8
11:39:30	80.0	35.2
11:40:00	80.0	35.5
11:40:30	80.0	36.0
11:41:00	80.0	36.3
11:41:30	80.5	36.6
11:42:00	80.5	36.9
11:42:30	81.0	37.2
11:43:00	81.0	37.5
11:43:30	81.0	37.9
11:44:00	81.0	38.2
11:44:30	81.0	38.5
11:45:00	81.5	38.8
11:45:30	81.5	39.2
11:46:00	82.0	39.5
11:46:30	82.0	39.8
11:47:00	82.0	40.1
11:47:30	82.0	40.4
11:48:00	82.0	40.7
11:48:30	82.0	41.0
11:49:00	82.0	41.4
11:49:30	82.0	41.7
11:50:00	83.0	41.9

11:50:30	83.0	42.2
11:51:00	83.0	42.4
11:51:30	83.0	42.8
11:52:00	83.0	43.1
11:52:30	83.0	43.3
11:53:00	83.0	43.6
11:53:30	83.0	43.8
11:54:00	83.0	44.2
11:54:30	83.0	44.4
11:55:00	83.0	44.6
11:55:30	83.0	44.8
11:56:00	83.0	45.0
11:56:30	83.0	45.2
11:57:00	83.0	45.4
11:57:30	83.0	45.7
11:58:30	83.0	46.0
11:59:30	83.0	46.3
12:00:30	83.0	46.6
12:01:30	83.5	46.8
12:02:30	83.5	47.0
12:03:30	83.5	47.2
12:04:30	83.5	47.3
12:05:30	83.5	47.5
12:06:30	83.5	47.6
12:07:30	83.5	47.7
12:08:30	81.0	47.7
12:09:30	78.0	47.8
12:10:30	85.0	47.8
12:11:30	93.0	48.2
12:12:00	94.0	48.5
12:12:30	96.0	48.9
12:13:00	98.0	49.3
12:13:30	99.0	50.0
12:14:00	100.0	50.3
12:14:30	102.0	50.7
12:15:00	104.0	51.1
12:15:30	105.0	51.8
12:16:00	107.0	52.5
12:16:30	109.0	52.8
12:17:00	112.0	53.5
12:17:30	115.0	54.0
12:18:00	118.0	54.7

12:18:30	118.5	55.5
12:19:00	120.0	56.4
12:19:30	120.0	57.3
12:20:00	120.0	58.3
12:20:30	120.0	59.4
12:21:00	120.5	60.5
12:21:30	121.0	61.6
12:22:00	121.0	62.8

The measured data from the second experiment cannot be given in detail in tabular form since they are too large for this field. However, a graphical presentation of the results is given below. For the graphical presentation, the corrected values (following Sidney Young) were used.

The two determinations showed good correlation of the boiling range.

The different boiling fractions covered for a long period a temperature range between 70 and 83°C. In the first determination, the temperature did not increase at this point anymore; it even decreased as the next fraction had a much higher boiling point. With the adjusted heating rate, it took a longer time to reach the boiling temperature of the next fraction. Over this period of time, no vapour passed the thermometer; therefore, a decreasing temperature was recorded.Then; the heating rate was increased.

In the second determination, this effect was anticipated and the heating rate was increased before decrease of temperature. At approximately 121°C, the last constant distilled fraction was reached. The heating process caused a difference in the distilled volume fractions between the performances. This can be stated as uncritical because the plateau was reached after heating up and both curves correlated again.

Addition of the volumes of the residues (assuming equal density) to the distilled volumes (including tailing) gave total volumes of 94.32 and 96.47 mL, respectively. The differences to 100 mL (5.68 and 3.53 mL) might be explained by remnants in the apparatus and by evaporation from the beaker (test item is highly volatile).

Conclusions:

The boiling range of the test item reaction mass of a representative sample for "2-propanol and 2-butanol production, distn. residues" was determined with 70 - 122 °C (343 – 395 K).

Executive summary:

The boiling range of the test item reaction mass of 2,2'-oxybisbutane (DSBE), DIPE, SBA and 2-methylpropan-2-ol (TBA) as a representative sample for "2-propanol and 2-butanol production, distn. residues" was determined using a distillation method under GLP conditions with 70 - 122 °C (343 – 395 K).

Description of key information

The boiling range of the test item reaction mass of 2,2'-oxybisbutane (DSBE), DIPE, SBA and 2-methylpropan-2-ol (TBA) as a representative sample for "2-propanol and 2-butanol production, distn. residues" was determined using a distillation method under GLP conditions with 70 - 122 °C (343 – 395 K). For risk assessment a median value of 96 °C is used.

Key value for chemical safety assessment

Boiling point at 101 325 Pa:

96 °C

Additional information

The boiling range of the test item reaction mass of 2,2'-oxybisbutane (DSBE), DIPE, SBA and 2-methylpropan-2-ol (TBA) was determined according to the EU A.2 guidance using a distillation method under GLP conditions with 70 - 122 °C (343 – 395 K).