CiToxLAB Hungary Ltd.

Veszprém - Szabadságpuszta

FINAL REPORT

Determination of the Boiling Point

of Ethanedioic acid, hydrate (1:2) [CAS RN 6153-56-6] 

(hydrated form of ethanedioic acid [CAS RN 144-62-7])

Study code: 11/339-324AN

Study Director: Zsolt Sárvári, M.Sc.

20 February 2013



Study code: 11/339-324AN Final Report Page 5 of 15

STUDY TITLE: Determination of the Boiling Point of Ethanedioic acid, 

hydrate (1:2) [CAS RN 6153-56-6] (hydrated form of 

ethanedioic acid [CAS RN 144-62-7])

SPONSORS: Univar USA Inc.

Address: 17425 NE Union Hill Road,

Redmond, WA 98052, USA

Phone: +1 425 889 3400

Fax: +1 425 889 3760

WEGO Chemical and Mineral Corp.

Address: 239 Great Neck Road,

Great Neck, NY 11021, USA

Phone: +1 516 487 3510

Fax: +1 516 487 3794

STUDY MONITOR: John V. Massingale

Greenwich Chemical Consulting, Inc.

Address: 3300 PGA Boulevard, Suite 635

Palm Beach Gardens, FL 33410, USA

Phone: +1 561 578 8110

Fax: +1 561 578 8120

E-mail: john@grcci.com

TEST FACILITY: CiToxLAB Hungary Ltd.

(Formerly known as LAB Research Ltd. before 1st September 2011)

Address: H-8200 Veszprém, Szabadságpuszta

Hungary

Phone: +36 88-545-300

Fax: +36 88-545-301

TEST FACILITY

MANAGEMENT: Christopher Banks, DABT

Managing Director

Alyson Leyshon, M.Sc.

Senior Director of Toxicology Operations

STUDY DIRECTOR: Zsolt Sárvári M.Sc.

Phone: +36 88 545 361

E-mail: zsolt.sarvari@hu.citoxlab.com
Study code: 11/339-324AN Final Report Page 6 of 15

ASSISTANT SCIENTIST: Viktória Laky, M.Sc.

LEAD QA: Szabolcs Gáty M.Sc.

Head of Quality Assurance Unit

Vanda Gyimesi, M.Sc.

Deputy Head of QAU

RESPONSIBLE PERSONS: Ildikó Kacz - technical assistant

Andrea Egei - technical assistant

BASIS OF STUDY: - Commission Regulation (EC) No 440/2008 of 2008 laying 

down test methods pursuant to Regulation (EC) No 

1907/2006 of the European Parliament and of the Council 

on the Registration, Evaluation, Authorisation and 

Restriction of Chemicals (REACH), Method A.2, Official 

Journal of the European Union L 142 of 31 May 2008

- Organisation for Economic Co-operation and Development 

(OECD), Guidelines for Testing of Chemicals, Guideline No.

103, “Boiling Point”, adopted July 27, 1995
Study code: 11/339-324AN Final Report Page 7 of 15

CONTENTS

Page

1. SUMMARY 8

2. OBJECTIVE OF STUDY 8

3. MATERIALS 8

3.1. TEST ITEM 8

3.2. CALIBRATION 9

4. TEST METHOD AND RESULTS 9

4.1. APPARATUS 9

4.2. PROCEDURE 9

4.3. RESULTS 10

5. ARCHIVES 10

6. DISTRIBUTION OF THE FINAL REPORT 11

APPENDIX 12

Copy of the GLP Certificates 13

Certificate of Analysis 15
Study code: 11/339-324AN Final Report Page 8 of 15

1. SUMMARY

This study was performed based on the U.S. Toxic Substances Control Act (TSCA) 

Section 4 Test Rule and the regulations set forth at 40 CFR 799.5087.

For the determination of the boiling point, the capillary method is used. A small 

amount of the test item is heated in the electronic controlled sample block and the 

temperature around the sample is displayed. The sample is observed visually while 

raising the temperature. A phase transformation from liquid to vapour usually is 

deduced by the formation of bubbles. The test item is assessed visually for any possible 

changes in its appearance, consistency and colour. The initial temperature of boiling or 

other effects observed is registered with the corresponding heating temperature.

The boiling point of the Test Item is: 136.1 ± 0.14 °C.

2. OBJECTIVE OF STUDY

The purpose of this study was to evaluate the boiling point of Ethanedioic acid, hydrate

(1:2) [CAS RN 6153-56-6] (hydrated form of ethanedioic acid [CAS RN 144-62-7])

by the capillary method using an electronic controlled heating system.

3. MATERIALS

3.1. TEST ITEM

Name: Ethanedioic acid, hydrate (1:2) [CAS RN 6153-56-6] (hydrated 

form of ethanedioic acid [CAS RN 144-62-7])

Chemical name: Oxalic acid, hydrate

CAS number: 6153-56-6

Batch/Lot number: YP2-20110704B

Molecular formula: C2H2O4×2H2O

Molecular weight: 126.1 (dihydrate form)

Appearance: White crystals

Purity: 99.71 %

Manufacture date: 04 July 2011

Expiry date: 03 July 2012

Storage conditions: Controlled room temperature (15-25oC)

3.1.1. Identification

The test item of a suitable chemical purity was supplied by the Sponsor. All safety 

instructions required in the handling and disposal of the test item were supplied by the 

Sponsor as well.
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Identification of the test item was made by its name, batch, appearance and colour by 

Central Dispensary Unit of CiToxLAB Hungary Ltd.

3.2. CALIBRATION

On the day of the experiment the instrument was checked by determining the boiling 

point of the reference substance α-naphthylamine (Batch No.: 1360195).

The boiling point is 301± 1°C (Vegyészek Zsebkönyve, Műszaki Kiadó 1963)

4. TEST METHOD AND RESULTS 

Start of experiment: 04 April 2012

End of experiment: 04 April 2012

4.1. APPARATUS

The test was carried out using a digital melting point device (Büchi B540 Melting Point Unit, 

No.: 908281) with a temperature range up to 400 °C (673 K).

4.2. PROCEDURE

Preparation of the Glass Tube

A small amount of Test Item was placed in a capillary glass tube with a diameter of 

3.2 mm to obtain a filling level of approximately 5 mm. The tube was heated in the 

oven of the device.

Preliminary Test

Preliminary tests with two parallel samples were performed at 10 °C/min, 3 °C/min and 

2 °C/min heating rate until boiling was observed.
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Main Test

Two capillaries containing the test item were placed into the apparatus and the block was 

heated from 120 °C to 145 °C at a 0.5 °C/min heating rate. The sample was observed 

visually through the magnifying glass. The end temperature was registered when a quick 

continuous flow of bubbles was formed at the plunged-in end of the capillary. The 

experiment was repeated three times with two parallel measurements each. The mean of 

the six measurements was reported. The measured values are presented in Table 1.

The atmospheric pressure was registered.

Documentation

The test conditions and temperature measured by a resistance thermometer located in the 

block was documented in the raw data.

4.3. RESULTS

The test was carried out at 97.0 kPa atmospheric pressure. Using a linear heating rate of 

0.5 °C/min, the boiling point of the Test Item was found to be 136.1 ± 0.14 °C (95 % 

confidence interval), i.e. 409.2 K.

The details are summarised in Table 1.

Table 1. Measured temperatures corresponding to the boiling point of the Test Item (three 

experiments (I, II, III) with two parallel samples each (1, 2)

Measured Temperatures during the Main Study (°C)

I / 1 I / 2 II / 1 II / 2 III / 1 III / 2 Mean

Boiling Point 136.0 136.0 136.2 136.3 136.0 136.0 136.1

5. ARCHIVES

The study documents:

- study plan, amendment

- all raw data

- sample of the test item

- study report and any amendment(s)

- correspondence

are stored in the archives of CiToxLAB Hungary Ltd., Hungary 8200 Veszprém, 

Szabadságpuszta according to the Hungarian GLP and to the our SOP-s.
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6. DISTRIBUTION OF THE FINAL REPORT

Sponsor:

- 1 × copy, bound

- 1 × copy, unbound

- 1 × pdf-file

Archives:

- 1 × original, bound
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APPENDI X
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Copy of the GLP-Certificates

The facility name until 1st September 2011 was LAB Research Ltd. From that date, the registered name has been CiToxLAB Hungary Ltd.,

this information has been transmitted to the GLP competent authority. The above GLP certificate is valid for this facility (now known as CiToxLAB 

Hungary Ltd) until the certificate expires (16 December 2012).
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Certificate of Analysis