## CiToxLAB Hungary Ltd.

Veszprém

- Szabadságpuszta



# FINAL REPORT

Determination of the Melting 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

- 344AN

Study Director: Zsolt Sárvári, M.Sc.

2 0 February 201 3Study code: 11/ 339

- 344AN Final Report Page 5 of 14

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

hydrate (1:2) [CAS RN 6153

- 56

- 6] (hydrated form of

ethanedioic acid [CA S RN 144

- 62

- 7])

SPONSOR S : 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 5 16 487 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 1 st September 2011)

Address: H

- 8200 Veszprém, Szabadságpuszta

Hungary

Phone: +36 88

- 545

- 300

Fax: +36 88

- 545

- 301

TEST FACILITY

MANAGEMENT: Christopher Banks, DABT

M anaging 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.comStudy code: 11/ 339

- 344AN Final Report Page 6 of 14

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 30 May 2008

laying dow n 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.1, Official Journal of the

European Union L 142 of 31 May 20 08

- Organisation for Economic Co

- operation and Development

(OECD), Guid e lines for Testing of Chemicals, Guideline No.

102, “Melting Point / Melting Range”; adopted July 27,

1995Study code: 11/ 339

- 344AN Final Report Page 7 of 14

CONTENTS

Page

1. SUMMARY 8

2. OBJECTIVE OF STUDY 8

3. MATERIALS 8

3.1. TEST ITEM 8

4. TEST METHODS AND RES ULTS 9

4.1. APPARATUS 9

4.2. CALIBRATION OF THE M ELTING POINT TESTER 9

4.3 PRELIMINARY TEST 9

4.4 MAIN TEST 9

4.5 RESULTS 10

5. ARCHIVES 10

6. DISTRIBUTION OF THE FINAL REPORT 10

7. DEVIATION 10

APPENDI X 1 1

Copy of the GLP Certificate s 12

Certificate of Analysis 14Study code: 11/ 339

- 344AN Final Report Page 8 of 14

1. SUMMARY

This study was perform ed 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 melting point or melting range, the capillary method was

used. A small amount of the test item was h eated in the electronic controlled sample

block and the temperature around the sample was displayed. The sample was observed

visually while raising the temper a ture. The initial and final melting temperatures were

dete r mined.

Using a linear heating rate of 0.5°C/min the melting point of Ethanedioic acid was

found to be 105

. 5 **±** 0. 1 2 °C (95 % confidence interval), i.e. 378

. 7 K.

2

. OBJECTIVE OF STUDY

The objective of the study was to determine the melting point of the test item.

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: C 2 H 2 O 4 ×2H 2 O

Molecular weigh t: 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)

Identification

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

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

Sponsor as well.

Identification of the test item was made by its name, batch, appearance and colour by

Central Dispensary Unit of CiToxLA B Hungary Ltd.Study code: 11/ 339

- 344AN Final Report Page 9 of 14

4. TEST METHODS AND RES ULTS

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 d e vice (Büchi B540 Melting Point

Unit, (No.: 908281)) with a tem perature range up to 400 °C (673 K).

4.2. CALIBRATION OF THE M ELTING POINT TESTER

Melting point standards ( Fluka): Vanillin 82. 4 **±** 0.2 **°** C

Phenacetin 135. 5 **±** 0.2 **°** C

Caffeine 236. 7 **±** 0.2 **°** C

The instrument is checked yearly by means of the above reference substances . New

corrective values are entered if the deviation is higher than **±** 0.3 **°** C.

On the day of the experiment the unit was rechecked using Vanillin, Phenacetin,

Caffeine. The measured values for all three reference substances were determined to be

i n the required ranges.

4.3 PRELIMINARY TEST

A preliminary test with three parallel samples was performed at 10°C/min heating rate.

4.4 MAIN TEST

For the main study three capillaries containing the test item were placed into the

apparatus, the block was hea ted from 9 5 °C to 11 0 °C at 0.5°C/min heating rate. The

transformations of the test item were observed visually through the magnifying glass.

Three parallel experiments were carried out and in each case three parallel samples

were measured. The mean of the m easured temperatures was determined.Study code: 11/ 339

- 344AN Final Report Page 10 of 14

4.5 RESULTS

Using a linear heating rate of 0.5 °C/min, the melting point of Ethanedioic acid was

found to be 105

. 5 **±** 0. 1 2 °C (95% confidence interval), i.e. 378

. 7 K.

The details are summarised in Table 1.

Table 1. Me asured temperatures corresponding to the melting of Ethanedioic acid (three experiments

(I, II, III) with three parallel samples each (1, 2, 3)

Measured Temperatures during the Main Study (°C)

I / 1 I / 2 I / 3 II / 1 II / 2 II / 3 III / 1 III / 2 III / 3 Mean

Melting Point 105.6 105.6 105.4 105. 3 105.4 105.4 105.7 105.7 105.7 105

. 5 ± 0. 1 2

5. ARCHIVES

The study documents:

- study plan , amendment

- all raw data

- sample of the test item

- study report and any amendment(s)

- correspondence

are sto red in the archives of CiTox LAB Hungary Ltd., Hungary 820 0 Veszprém,

Szabadságpuszta according to the Hungarian GLP and to the our SOP

- s.

6. DISTRIBUTION OF THE FINAL REPORT

Sponsor:

- 1 × copy, bound

- 1 × copy, unbound

- 1 × pdf

- file

Archives:

- 1 × origina l, bound

7

. DEVIATION

The melting point of vanillin standard is 82.4 °C instead of 82.3 °C which is in the

Study Plan. A new batch of vanillin arrived for the test. This deviation does not have

any effect on study results.Study code: 11/ 339

- 344AN Final Report Page 11 of 14



## APPENDI XStudy code: 11/ 339

- 344AN Final Report Page 12 of 14



### Copy of the GL P

- 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 vali d for this facility (now known as

CiToxLAB Hungary Ltd. ) until the certificate expires (16 December 2012).Study code: 11/ 339

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- 344AN Final Report Page 14 of 14



### Certificate of Analysis