## 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: 11/3 39

- 324AN

Study Director: Zsolt Sárvári, M.Sc.

2 0 February 201 3Study code: 11/3 39

- 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])

SPONSOR S : Univar USA Inc.

Address: 17425 NE Union Hill Road,

Redmond, WA 98 052, 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 Consul ting, 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 1 st Septembe r 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 DIREC TOR: Zsolt Sárvári M.Sc.

Phone: +36 88 545 361

E

- mail: zsolt.sarvari @hu.citoxlab.comStudy code: 11/3 39

- 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 PER SONS: 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

o n 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 Chemical s, Guideline No.

103, “Boiling Point”, adopted July 27, 1995Study code: 11/3 39

- 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 RESU LTS 9

4.1. APPARATUS 9

4.2. PROCEDURE 9

4.3. RE SULTS 10

5. ARCHIVES 10

6. DISTRIBUTION OF THE FINAL REPORT 11

APPENDI X 1 2

Copy of the GLP Certificates 13

Certificate of Analysis 15Study code: 11/3 39

- 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 i n the electronic controlled sample block and the

te m perature 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 tes t item is assessed visually for any possible

changes in its appearance, consi s tency 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: 1 36.1 **±** 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 co ntrolled 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

- 20110 704B

Molecular formula: C 2 H 2 O 4 ×2H 2 O

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

- 25 o C)

3.1.1. Identificati on

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.Study code: 11/3 39

- 324AN Final Report Page 9 of 15

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 boi ling point is 301 **±** 1 **°** C (Vegyészek Zsebkönyve, Műszaki Kiadó 1963)

4. TEST METHOD AND RESU LTS

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 B5 40 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 app roximately 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.Study code: 11/3 39

- 324AN Final Report Page 10 of 15

Main Test

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

heated from 12 0 °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 w as regi s tered.

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 9 7

. 0 kPa atmospheric pressure. Using a linear heatin g rate of

0.5 °C/min, the boiling point of the Test Item was found to be 136

. 1 **±** 0. 1 4 °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 (t hree

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 docum ents:

- 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.Study code: 11/3 39

- 324AN Final Report Page 11 of 15

6. DISTRIBUTION OF THE FINAL REPORT

Sponsor:

- 1 × copy, bound

- 1 × copy, unbound

- 1 × pdf

- file

Archives:

- 1 × original, boundStudy code: 11/3 39

- 324AN Final Report Page 12 of 15



## APPENDI XStudy code: 11/3 39

- 324AN Final Report Page 13 of 15



### Copy of the GLP

- Certificate s

The facility name until 1 st 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).Study code: 11/3 39

- 324AN Final Report Page 14 of 15Study code: 11/3 39

- 324AN Final Report Page 15 of 15



### Certificate of Analysis